file_name stringlengths 11 11 | content stringlengths 1.16k 56.6M |
|---|---|
1100593.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-05 03:04:50 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177587 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100593.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100593
loop_
_publ_author_name
'Elschenbroich, Christoph'
'Wolf, Matthias'
'Burghaus, Olaf'
'Harms, Klaus'
'Pebler, J\"urgen'
_publ_section_title
;
The Mono-, Di-, and Tri([5]trovacenyl)boranes: A Study of Intermetallic
Communication Across an sp^2^-Hybridized Boron Atom
;
_journal_coden_ASTM EJICFO
_journal_issue 12
_journal_name_full 'European Journal of Inorganic Chemistry'
_journal_page_first 2173
_journal_page_last 2185
_journal_paper_doi
10.1002/(sici)1099-0682(199912)1999:12<2173::aid-ejic2173>3.0.co;2-0
_journal_volume 1999
_journal_year 1999
_chemical_formula_sum 'C33 H33 B V2'
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 96.139(9)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 10.1842(19)
_cell_length_b 8.9716(13)
_cell_length_c 14.350(2)
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C33 H33 B1 V2'
_cod_database_code 1100593
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
V1 V 0.52894(10) 0.75807(12) 0.84441(6)
V2 V 0.25017(10) 0.82395(12) 0.46515(6)
B1 B 0.2717(7) 0.8887(8) 0.6982(4)
C1 C 0.1699(6) 0.9836(7) 0.7496(4)
C2 C 0.0715(6) 0.9173(8) 0.7983(4)
C3 C -0.0039(6) 1.0037(10) 0.8538(4)
H1 H -0.067(6) 0.944(8) 0.885(4)
C4 C 0.0121(6) 1.1550(9) 0.8617(4)
C5 C 0.1036(7) 1.2220(9) 0.8118(5)
H2 H 0.120(6) 1.331(9) 0.818(4)
C6 C 0.1794(6) 1.1403(9) 0.7557(4)
C7 C 0.0468(7) 0.7514(11) 0.7935(5)
H3 H 0.024(7) 0.715(8) 0.849(5)
H4 H 0.104(7) 0.695(9) 0.774(5)
H5 H -0.040(7) 0.725(8) 0.751(4)
C8 C -0.0702(9) 1.2470(14) 0.9237(5)
H6 H -0.025(7) 1.316(12) 0.967(6)
H7 H -0.094(9) 1.182(11) 0.965(6)
H8 H -0.131(8) 1.310(12) 0.898(5)
C9 C 0.2719(7) 1.2296(10) 0.6983(5)
H9 H 0.221(7) 1.313(11) 0.669(5)
H10 H 0.309(7) 1.178(8) 0.643(5)
H11 H 0.336(7) 1.276(10) 0.729(5)
C10 C 0.4201(6) 0.9051(7) 0.7334(4)
C11 C 0.5354(6) 0.8442(9) 0.6975(4)
H12 H 0.536(5) 0.774(8) 0.643(4)
C12 C 0.6493(7) 0.8933(9) 0.7522(5)
H13 H 0.729(6) 0.870(8) 0.738(4)
C13 C 0.6118(7) 0.9875(9) 0.8228(5)
H14 H 0.673(6) 1.036(8) 0.877(4)
C14 C 0.4717(7) 0.9953(8) 0.8123(5)
H15 H 0.425(6) 1.046(8) 0.845(4)
C15 C 0.3953(8) 0.5692(9) 0.8490(5)
H16 H 0.320(7) 0.540(8) 0.806(5)
C16 C 0.5155(8) 0.5184(9) 0.8210(5)
H17 H 0.512(6) 0.468(8) 0.760(4)
C17 C 0.6454(9) 0.5540(9) 0.8600(5)
H18 H 0.707(6) 0.508(8) 0.823(5)
C18 C 0.6855(8) 0.6468(11) 0.9368(6)
H19 H 0.766(7) 0.648(10) 0.936(5)
C19 C 0.6072(8) 0.7294(10) 0.9909(4)
H20 H 0.653(6) 0.810(9) 1.030(4)
C20 C 0.4698(9) 0.7384(10) 0.9856(4)
H21 H 0.440(6) 0.809(9) 1.020(4)
C21 C 0.3743(7) 0.6678(9) 0.9220(5)
H22 H 0.281(6) 0.696(7) 0.934(4)
C22 C 0.2191(5) 0.7818(8) 0.6175(4)
C23 C 0.0931(6) 0.7956(8) 0.5633(4)
H23 H 0.034(5) 0.882(7) 0.574(4)
C24 C 0.0794(7) 0.6786(9) 0.4962(5)
H24 H 0.016(6) 0.661(8) 0.454(4)
C25 C 0.1953(7) 0.5891(8) 0.5087(5)
H25 H 0.213(6) 0.501(8) 0.471(4)
C26 C 0.2805(7) 0.6525(8) 0.5820(4)
H26 H 0.367(6) 0.621(7) 0.599(4)
C27 C 0.2853(9) 1.0641(9) 0.4492(5)
H27 H 0.269(7) 1.122(9) 0.492(5)
C28 C 0.1766(7) 1.0231(9) 0.3862(5)
H28 H 0.107(7) 1.087(8) 0.390(4)
C29 C 0.1642(7) 0.8960(8) 0.3269(4)
H29 H 0.072(6) 0.903(7) 0.300(4)
C30 C 0.2575(6) 0.7839(8) 0.3158(4)
H30 H 0.232(6) 0.692(7) 0.282(4)
C31 C 0.3855(6) 0.767(1) 0.3620(4)
H31 H 0.429(6) 0.674(8) 0.352(4)
C32 C 0.4515(6) 0.8596(8) 0.4300(5)
H32 H 0.534(6) 0.822(8) 0.463(4)
C33 C 0.4072(7) 0.9886(9) 0.4701(5)
H33 H 0.458(6) 1.021(8) 0.526(4)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
B 0.83
V 1.33
|
1100594.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-05 03:04:50 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177587 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100594.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100594
loop_
_publ_author_name
'Elschenbroich, Christoph'
'Wolf, Matthias'
'Burghaus, Olaf'
'Harms, Klaus'
'Pebler, J\"urgen'
_publ_section_title
;
The Mono-, Di-, and Tri([5]trovacenyl)boranes: A Study of Intermetallic
Communication Across an sp^2^-Hybridized Boron Atom
;
_journal_coden_ASTM EJICFO
_journal_issue 12
_journal_name_full 'European Journal of Inorganic Chemistry'
_journal_page_first 2173
_journal_page_last 2185
_journal_paper_doi
10.1002/(sici)1099-0682(199912)1999:12<2173::aid-ejic2173>3.0.co;2-0
_journal_volume 1999
_journal_year 1999
_chemical_formula_sum 'C36 H33 B V3'
_space_group_IT_number 1
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 1
_symmetry_space_group_name_Hall 'P 1'
_symmetry_space_group_name_H-M 'P 1'
_cell_angle_alpha 98.94(3)
_cell_angle_beta 94.67(3)
_cell_angle_gamma 93.15(2)
_cell_formula_units_Z 2
_cell_length_a 7.796(2)
_cell_length_b 12.429(3)
_cell_length_c 14.599(6)
_cod_original_formula_sum 'C36 H33 B1 V3'
_cod_database_code 1100594
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
V1 V -0.86191(14) 2.03792(10) 0.84195(9)
V2 V -0.71163(13) 1.60411(10) 0.86319(9)
V3 V -0.64586(14) 1.73678(10) 0.50628(9)
B1 B -0.7133(10) 1.8023(7) 0.7228(6)
C1 C -0.7121(8) 1.9297(6) 0.7421(5)
C2 C -0.5914(9) 1.9976(6) 0.8079(6)
H1 H -0.51010 1.97240 0.84930
C3 C -0.6125(10) 2.1084(7) 0.8013(6)
H2 H -0.55110 2.16920 0.83830
C4 C -0.7428(10) 2.1110(7) 0.7288(6)
H3 H -0.78170 2.17410 0.70810
C5 C -0.8041(11) 2.0040(7) 0.6931(6)
H4 H -0.89200 1.98350 0.64450
C6 C -1.1442(11) 2.0362(9) 0.8215(8)
H5 H -1.23130 2.02700 0.77200
C7 C -1.0982(10) 1.9398(8) 0.8543(8)
H6 H -1.15880 1.87480 0.82400
C8 C -0.9725(11) 1.9287(8) 0.9270(7)
H7 H -0.96070 1.85690 0.93810
C9 C -0.8632(11) 2.0084(9) 0.9847(7)
H8 H -0.78770 1.98290 1.02880
C10 C -0.8515(11) 2.1201(9) 0.9856(6)
H9 H -0.77060 2.16120 1.03070
C11 C -0.9494(13) 2.1812(7) 0.9252(8)
H10 H -0.92360 2.25720 0.93580
C12 C -1.0789(12) 2.1415(9) 0.8522(7)
H11 H -1.12670 2.19460 0.82040
C13 C -0.6048(8) 1.7448(6) 0.7944(5)
C14 C -0.5020(8) 1.6515(6) 0.7764(6)
H12 H -0.49000 1.61150 0.71730
C15 C -0.4232(9) 1.6302(6) 0.8609(6)
H13 H -0.34860 1.57450 0.86740
C16 C -0.4732(9) 1.7050(6) 0.9336(6)
H14 H -0.44060 1.70770 0.99740
C17 C -0.5818(8) 1.7760(6) 0.8937(5)
H15 H -0.63180 1.83510 0.92740
C18 C -0.9888(11) 1.6191(9) 0.8590(9)
H16 H -1.06660 1.67190 0.84810
C19 C -0.9563(12) 1.5460(9) 0.7801(8)
H17 H -1.01610 1.55530 0.72370
C20 C -0.8445(12) 1.4599(8) 0.7750(7)
H18 H -0.83770 1.41940 0.71550
C21 C -0.7418(12) 1.4277(7) 0.8490(8)
H19 H -0.67440 1.36870 0.83170
C22 C -0.7254(11) 1.4697(8) 0.9427(7)
H20 H -0.65010 1.43490 0.98040
C23 C -0.8071(13) 1.5581(8) 0.9892(7)
H21 H -0.78090 1.57450 1.05410
C24 C -0.9236(11) 1.6247(8) 0.9498(8)
H22 H -0.96220 1.68130 0.99190
C25 C -0.7975(8) 1.7334(6) 0.6295(5)
C26 C -0.9043(9) 1.7697(7) 0.5568(6)
H23 H -0.94960 1.83860 0.56090
C27 C -0.9309(9) 1.6867(8) 0.4788(6)
H24 H -0.99510 1.69090 0.42230
C28 C -0.8447(10) 1.5967(7) 0.5005(6)
H25 H -0.84040 1.52980 0.46080
C29 C -0.7670(9) 1.6234(6) 0.5905(6)
H26 H -0.70300 1.57600 0.62190
C30 C -0.5078(11) 1.8968(7) 0.5309(7)
H27 H -0.51640 1.96510 0.56760
C31 C -0.6040(11) 1.8806(8) 0.4411(8)
H28 H -0.66620 1.93930 0.42630
C32 C -0.6154(13) 1.7871(11) 0.3731(8)
H29 H -0.68490 1.79110 0.31810
C33 C -0.5383(13) 1.6892(10) 0.3752(7)
H30 H -0.56290 1.63630 0.32160
C34 C -0.4288(14) 1.6583(8) 0.4464(10)
H31 H -0.38970 1.58770 0.43460
C35 C -0.3708(11) 1.7208(9) 0.5336(8)
H32 H -0.29820 1.68590 0.57250
C36 C -0.4058(11) 1.8279(8) 0.5708(7)
H33 H -0.35230 1.85530 0.63060
C37 C -0.4052(9) 1.2167(6) 0.3598(5)
B2 B -0.2873(10) 1.1974(7) 0.2772(6)
V4 V -0.33366(14) 1.27828(10) 0.51653(9)
C38 C -0.4645(9) 1.1378(7) 0.4151(6)
H34 H -0.42730 1.06680 0.41310
V5 V -0.16306(14) 0.9455(1) 0.22924(9)
C39 C -0.5877(10) 1.1844(7) 0.4729(6)
H35 H -0.64640 1.15020 0.51550
V6 V -0.24863(14) 1.38882(10) 0.15266(9)
C40 C -0.6061(9) 1.2923(7) 0.4546(6)
H36 H -0.68110 1.34200 0.48200
C41 C -0.4931(9) 1.3115(7) 0.3888(6)
H37 H -0.47720 1.37800 0.36660
C42 C -0.170(1) 1.4291(7) 0.5565(6)
H38 H -0.14820 1.49510 0.53440
C43 C -0.0651(9) 1.3459(7) 0.5264(6)
H39 H 0.01740 1.36300 0.48640
C44 C -0.0669(10) 1.2390(7) 0.5483(6)
H40 H 0.01520 1.19470 0.52100
C45 C -0.1741(11) 1.1893(9) 0.6051(7)
H41 H -0.15650 1.11620 0.61030
C46 C -0.3058(12) 1.2380(11) 0.6553(7)
H42 H -0.36470 1.19250 0.68990
C47 C -0.3606(12) 1.3432(11) 0.6609(7)
H43 H -0.44770 1.35980 0.70060
C48 C -0.3033(11) 1.4280(9) 0.6151(7)
H44 H -0.36210 1.49220 0.62510
C49 C -0.3207(8) 1.0866(6) 0.2092(5)
C50 C -0.2442(9) 1.0493(6) 0.1242(5)
H45 H -0.16200 1.09040 0.09790
C51 C -0.3098(9) 0.9437(7) 0.0866(6)
H46 H -0.28130 0.90240 0.03100
C52 C -0.4286(9) 0.9095(7) 0.1479(6)
H47 H -0.49090 0.84130 0.14040
C53 C -0.4351(9) 0.9953(6) 0.2207(6)
H48 H -0.50430 0.99410 0.27040
C54 C 0.0513(10) 1.0292(7) 0.3224(7)
H49 H 0.09360 1.10130 0.34620
C55 C 0.1159(10) 0.9832(8) 0.2363(7)
H50 H 0.19120 1.02860 0.20960
C56 C 0.0762(12) 0.8759(9) 0.1885(7)
H51 H 0.13200 0.85790 0.13400
C57 C -0.0333(11) 0.7922(8) 0.2099(7)
H52 H -0.04070 0.72610 0.16810
C58 C -0.1351(11) 0.7941(7) 0.2866(7)
H53 H -0.20240 0.72940 0.28830
C59 C -0.1485(10) 0.8789(7) 0.3595(6)
H54 H -0.22430 0.86360 0.40340
C60 C -0.0658(11) 0.9829(8) 0.3767(6)
H55 H -0.09090 1.02800 0.43120
C61 C -0.1561(8) 1.2903(6) 0.2605(5)
C62 C -0.1456(10) 1.4025(6) 0.3025(6)
H56 H -0.20850 1.43160 0.35170
C63 C -0.0275(10) 1.4626(7) 0.2596(6)
H57 H 0.00020 1.53820 0.27440
C64 C 0.0414(10) 1.3918(7) 0.1917(6)
H58 H 0.12520 1.41130 0.15330
C65 C -0.0348(8) 1.2850(7) 0.1893(6)
H59 H -0.01130 1.22200 0.14890
C66 C -0.5246(9) 1.3370(7) 0.1359(6)
H60 H -0.60390 1.29660 0.16460
C67 C -0.5036(10) 1.4489(7) 0.1687(6)
H61 H -0.56970 1.47440 0.21760
C68 C -0.3959(10) 1.5296(6) 0.1382(6)
H62 H -0.40020 1.60140 0.16920
C69 C -0.2830(11) 1.5152(8) 0.0670(7)
H63 H -0.22070 1.57890 0.05760
C70 C -0.2516(11) 1.4218(9) 0.0099(7)
H64 H -0.17240 1.43040 -0.03420
C71 C -0.3215(10) 1.3149(8) 0.0080(6)
H65 H -0.28340 1.26130 -0.03720
C72 C -0.4402(9) 1.2778(7) 0.0646(7)
H66 H -0.46810 1.20210 0.05350
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
B 0.83
V 1.33
|
1100595.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 05:32:17 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176888 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100595.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100595
loop_
_publ_author_name
'Elschenbroich, Christoph'
'Schiemann, Olav'
'Burghaus, Olaf'
'Harms, Klaus'
'Pebler, J\"urgen'
_publ_section_title
;
[5-5]Bitrovacene,
(\m-\h^5^:\h^5^-Fulvalenediyl)bis[(\h^7^-cycloheptatrienyl)vanadium]:
Synthesis, Structure, and Intermetallic Communication
;
_journal_coden_ASTM ORGND7
_journal_issue 17
_journal_name_full Organometallics
_journal_page_first 3273
_journal_page_last 3277
_journal_paper_doi 10.1021/om9902232
_journal_volume 18
_journal_year 1999
_chemical_formula_sum 'C24 H22 V2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 102.25(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 10.447(2)
_cell_length_b 8.0890(12)
_cell_length_c 10.911(2)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100595
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 -1/2+x,-1/2-y,-1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
V1 V 0.78764(4) 0.19550(6) 0.01215(4)
C1 C 0.9351(2) 0.0149(3) -0.0399(2)
C2 C 0.8183(3) -0.0701(4) -0.0348(3)
C3 C 0.7167(3) -0.0030(4) -0.1284(3)
C4 C 0.7688(3) 0.1233(4) -0.1891(3)
C5 C 0.9025(3) 0.1344(4) -0.1363(3)
C6 C 0.8951(3) 0.4031(4) 0.1094(3)
C7 C 0.8960(3) 0.2754(4) 0.1951(2)
C8 C 0.7920(3) 0.1782(5) 0.2122(3)
C9 C 0.6610(3) 0.1825(5) 0.1468(3)
C10 C 0.6020(3) 0.2857(5) 0.0485(3)
C11 C 0.6602(3) 0.4106(4) -0.0087(3)
C12 C 0.7899(4) 0.4626(4) 0.0186(3)
H1 H 0.809(3) -0.143(4) 0.022(3)
H2 H 0.641(3) -0.029(4) -0.139(3)
H3 H 0.724(3) 0.191(4) -0.252(3)
H4 H 0.958(3) 0.1984(4) -0.157(3)
H5 H 0.975(3) 0.440(4) 0.103(3)
H6 H 0.978(3) 0.240(3) 0.237(3)
H7 H 0.813(3) 0.093(4) 0.251(3)
H8 H 0.617(3) 0.101(4) 0.158(3)
H9 H 0.524(3) 0.260(4) 0.014(3)
H10 H 0.610(3) 0.456(4) -0.077(3)
H11 H 0.810(3) 0.528(4) -0.030(3)
C1B* C 1.0649(2) -0.0149(3) 0.0399(2)
V1B* V 1.21236(4) -0.19550(6) -0.01215(4)
C2B* C 1.1817(3) 0.0701(4) 0.0348(3)
C5B* C 1.0975(3) -0.1344(4) 0.1363(3)
C3B* C 1.2833(3) 0.0030(4) 0.1284(3)
H1B* H 1.191(3) 0.143(4) -0.022(3)
C4B* C 1.2312(3) -0.1233(4) 0.1891(3)
C6B* C 1.1049(3) -0.4031(4) -0.1094(3)
C7B* C 1.1040(3) -0.2754(4) -0.1951(2)
C8B* C 1.2080(3) -0.1782(5) -0.2122(3)
H6B* H 1.022(3) -0.240(3) -0.237(3)
C9B* C 1.3390(3) -0.1825(5) -0.1468(3)
C10B* C 1.3980(3) -0.2857(5) -0.0485(3)
H8B* H 1.383(3) -0.101(4) -0.158(3)
C11B* C 1.3398(3) -0.4106(4) 0.0087(3)
C12B* C 1.2101(4) -0.4626(4) -0.0186(3)
H5B* H 1.025(3) -0.440(4) -0.103(3)
H10B* H 1.390(3) -0.456(4) 0.077(3)
H11B* H 1.190(3) -0.528(4) 0.030(3)
H9B* H 1.476(3) -0.260(4) -0.014(3)
H7B* H 1.187(3) -0.093(4) -0.251(3)
H4B* H 1.042(3) -0.1984(4) 0.157(3)
H3B* H 1.276(3) -0.191(4) 0.252(3)
H2B* H 1.359(3) 0.029(4) 0.139(3)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
V 1.33
|
1100596.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 05:32:17 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176888 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100596.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100596
loop_
_publ_author_name
'Elschenbroich, Christoph'
'Schiemann, Olav'
'Burghaus, Olaf'
'Harms, Klaus'
'Pebler, J\"urgen'
_publ_section_title
;
[5-5]Bitrovacene,
(\m-\h^5^:\h^5^-Fulvalenediyl)bis[(\h^7^-cycloheptatrienyl)vanadium]:
Synthesis, Structure, and Intermetallic Communication
;
_journal_coden_ASTM ORGND7
_journal_issue 17
_journal_name_full Organometallics
_journal_page_first 3273
_journal_page_last 3277
_journal_paper_doi 10.1021/om9902232
_journal_volume 18
_journal_year 1999
_chemical_formula_sum 'C18 H16 V'
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 97.53(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.768(3)
_cell_length_b 7.851(2)
_cell_length_c 16.189(6)
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C18 H16 V1'
_cod_database_code 1100596
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
V1 V 0.07166(13) 0.1996(2) 0.82462(11)
C1 C 0.1630(9) -0.0169(13) 0.7593(6)
C2 C 0.2523(9) 0.1184(14) 0.7826(7)
C3 C 0.2727(10) 0.1335(16) 0.8695(9)
C4 C 0.1975(11) 0.0163(15) 0.9035(8)
C5 C 0.1281(10) -0.0759(15) 0.8381(7)
C6 C 0.1213(10) -0.0844(14) 0.6750(7)
C7 C 0.0111(10) -0.1781(14) 0.6585(8)
C8 C -0.0225(12) -0.2538(13) 0.5810(8)
C9 C 0.0505(15) -0.2426(15) 0.5157(9)
C10 C 0.1565(13) -0.1494(19) 0.5321(9)
C11 C 0.1944(11) -0.0702(16) 0.6106(8)
C12 C 0.0672(8) 0.4653(11) 0.7878(7)
C13 C 0.066(1) 0.4560(13) 0.8752(8)
C14 C -0.0066(10) 0.3497(16) 0.9185(8)
C15 C -0.0941(9) 0.2233(18) 0.8880(7)
C16 C -0.1298(8) 0.1785(16) 0.8030(8)
C17 C -0.0901(9) 0.2410(14) 0.7283(7)
C18 C -0.0017(9) 0.3702(12) 0.7234(7)
V2 V 0.58493(13) -0.3000(2) 0.82782(10)
C19 C 0.4602(9) -0.5159(12) 0.7738(7)
C20 C 0.3869(10) -0.3825(15) 0.8031(9)
C21 C 0.4212(11) -0.3748(18) 0.8925(9)
C22 C 0.5165(11) -0.4867(15) 0.9180(8)
C23 C 0.5433(11) -0.5739(15) 0.8436(8)
C24 C 0.4535(10) -0.5768(14) 0.6846(7)
C25 C 0.5456(13) -0.6826(15) 0.6611(8)
C26 C 0.5397(19) -0.7541(19) 0.5825(10)
C27 C 0.441(3) -0.724(2) 0.5275(13)
C28 C 0.3444(19) -0.618(3) 0.5441(12)
C29 C 0.3495(13) -0.5452(18) 0.6245(9)
C30 C 0.5998(9) -0.1365(14) 0.7188(7)
C31 C 0.5636(9) -0.0386(13) 0.7847(7)
C32 C 0.6119(13) -0.0426(15) 0.8707(10)
C33 C 0.7090(13) -0.1412(17) 0.9125(8)
C34 C 0.7815(10) -0.2644(15) 0.8776(9)
C35 C 0.7740(9) -0.3189(17) 0.7948(9)
C36 C 0.6945(9) -0.2642(13) 0.7238(7)
H1 H 0.29100 0.18640 0.74470
H2 H 0.32870 0.21110 0.90000
H3 H 0.19330 0.00060 0.96120
H4 H 0.06840 -0.16230 0.84470
H5 H -0.04180 -0.19070 0.70070
H6 H -0.09870 -0.31610 0.57200
H7 H 0.02720 -0.29670 0.46350
H8 H 0.20820 -0.13620 0.48930
H9 H 0.27030 -0.00710 0.61900
H10 H 0.12350 0.54680 0.77020
H11 H 0.12110 0.53120 0.90810
H12 H 0.00450 0.36450 0.97730
H13 H -0.13300 0.16200 0.92820
H14 H -0.19120 0.09100 0.79470
H15 H -0.12590 0.19010 0.67750
H16 H 0.01300 0.40310 0.66860
H17 H 0.32730 -0.31280 0.77040
H18 H 0.38300 -0.30190 0.92870
H19 H 0.55660 -0.50360 0.97330
H20 H 0.60680 -0.65730 0.84170
H21 H 0.61610 -0.70760 0.70090
H22 H 0.60600 -0.82370 0.56820
H23 H 0.43630 -0.77660 0.47430
H24 H 0.27590 -0.59510 0.50240
H25 H 0.28290 -0.47520 0.63780
H26 H 0.55610 -0.11480 0.66500
H27 H 0.49800 0.04090 0.76950
H28 H 0.57250 0.03280 0.90500
H29 H 0.72800 -0.12280 0.97080
H30 H 0.84430 -0.31800 0.91550
H31 H 0.83140 -0.40630 0.78510
H32 H 0.70540 -0.31920 0.67290
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
V 1.33
|
1100597.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:33:40 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177949 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100597.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100597
loop_
_publ_author_name
'Anfang, S.'
'Harms, K.'
'Weller, F.'
'Borgmeier, O.'
'Lueken, H.'
'Schilder, H.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe Seltener Erden. Synthese und Kristallstrukturen
von [M~2~(C~5~H~5~)~3~(NPPh~3~)~3~] · 3 C~7~H~8~ mit M = Y, Dy und Er.
Magnetische Eigenschaften von
[Dy~2~(C~5~H~5~)~3~(NPPh~3~)~3~] · 3 C~7~H~8~
;
_journal_coden_ASTM ZAACAB
_journal_issue 1
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 159
_journal_page_last 166
_journal_paper_doi
10.1002/(sici)1521-3749(199801)624:1<159::aid-zaac159>3.0.co;2-z
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C90 H84 N3 P3 Y2'
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 61
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.372(6)
_cell_length_b 19.889(4)
_cell_length_c 28.579(6)
_cod_database_code 1100597
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,y,1/2-z
3 x,1/2-y,1/2+z
4 1/2-x,1/2+y,z
5 -x,-y,-z
6 -1/2-x,-y,-1/2+z
7 -x,-1/2+y,-1/2-z
8 -1/2+x,-1/2-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Y1 Y 0.10576(6) 0.27323(6) 0.36682(5)
P1 P 0.12534(15) 0.43259(19) 0.42851(16)
N1 N 0.1186(3) 0.3701(4) 0.3970(3)
Y2 Y 0.10694(5) 0.30524(5) 0.24764(5)
P2 P -0.00591(13) 0.2993(2) 0.30985(17)
N2 N 0.0513(3) 0.2933(5) 0.3082(4)
P3 P 0.21180(14) 0.23634(19) 0.30639(17)
N3 N 0.1581(3) 0.2617(4) 0.3040(4)
C1 C 0.2141(5) 0.4738(4) 0.3894(3)
C2 C 0.2622(5) 0.4961(4) 0.3904(3)
C3 C 0.2845(3) 0.5108(4) 0.4329(5)
C4 C 0.2587(4) 0.5033(4) 0.4744(3)
C5 C 0.2106(4) 0.4810(4) 0.4735(3)
C6 C 0.1882(3) 0.4663(4) 0.4310(5)
H1 H 0.19860 0.46360 0.36000
H2 H 0.28010 0.50140 0.36150
H3 H 0.31790 0.52630 0.43350
H4 H 0.27420 0.51350 0.50390
H5 H 0.19260 0.47580 0.50230
C7 C 0.1039(3) 0.5731(8) 0.4279(3)
C8 C 0.0813(5) 0.6302(5) 0.4102(5)
C9 C 0.0479(4) 0.6246(6) 0.3738(5)
C10 C 0.0371(3) 0.5618(8) 0.3551(3)
C11 C 0.0596(5) 0.5047(5) 0.3729(5)
C12 C 0.0930(4) 0.5103(5) 0.4093(4)
H6 H 0.12710 0.57700 0.45320
H7 H 0.08890 0.67380 0.42310
H8 H 0.03230 0.66430 0.36140
H9 H 0.01390 0.55790 0.32980
H10 H 0.05210 0.46110 0.35990
C13 C 0.1231(3) 0.3637(7) 0.5110(6)
C14 C 0.1088(5) 0.3473(5) 0.5563(6)
C15 C 0.0758(5) 0.3880(9) 0.5800(3)
C16 C 0.0571(4) 0.4452(8) 0.5585(6)
C17 C 0.0714(5) 0.4616(4) 0.5133(6)
C18 C 0.1043(5) 0.4209(8) 0.4895(3)
H11 H 0.14600 0.33540 0.49450
H12 H 0.12180 0.30760 0.57120
H13 H 0.06590 0.37660 0.61150
H14 H 0.03420 0.47340 0.57500
H15 H 0.05840 0.50130 0.49830
C19 C -0.0495(4) 0.4289(7) 0.3063(3)
C20 C -0.0639(2) 0.4867(4) 0.2827(5)
C21 C -0.0598(3) 0.4902(4) 0.2343(5)
C22 C -0.0412(4) 0.4358(6) 0.2095(3)
C23 C -0.0267(3) 0.3780(4) 0.2330(5)
C24 C -0.0309(3) 0.3745(4) 0.2814(5)
H16 H -0.05240 0.42650 0.33990
H17 H -0.07680 0.52440 0.30000
H18 H -0.06980 0.53030 0.21800
H19 H -0.03830 0.43820 0.17590
H20 H -0.01380 0.34030 0.21580
C25 C -0.0803(4) 0.2369(3) 0.2531(4)
C26 C -0.1042(3) 0.1810(6) 0.2352(3)
C27 C -0.0876(4) 0.1168(4) 0.2460(3)
C28 C -0.0472(4) 0.1086(4) 0.2749(4)
C29 C -0.0233(3) 0.1645(6) 0.2929(3)
C30 C -0.0398(4) 0.2287(4) 0.2820(3)
H21 H -0.09180 0.28150 0.24560
H22 H -0.13220 0.18660 0.21510
H23 H -0.10420 0.07790 0.23360
H24 H -0.03570 0.06400 0.28250
H25 H 0.00480 0.15890 0.31290
C31 C -0.0050(3) 0.3384(4) 0.4030(6)
C32 C -0.0221(5) 0.3412(5) 0.4488(5)
C33 C -0.0657(6) 0.3098(7) 0.4606(3)
C34 C -0.0923(3) 0.2756(5) 0.4267(6)
C35 C -0.0753(5) 0.2728(5) 0.3810(5)
C36 C -0.0316(5) 0.3042(6) 0.3691(3)
H26 H 0.02530 0.36020 0.39470
H27 H -0.00360 0.36500 0.47230
H28 H -0.07750 0.31180 0.49240
H29 H -0.12260 0.25380 0.43500
H30 H -0.09370 0.24900 0.35740
C37 C 0.1815(3) 0.1066(5) 0.2850(3)
C38 C 0.1881(3) 0.0418(4) 0.2679(3)
C39 C 0.2339(4) 0.0214(3) 0.2524(3)
C40 C 0.2731(3) 0.0657(6) 0.2540(3)
C41 C 0.2665(3) 0.1305(5) 0.2711(4)
C42 C 0.2207(4) 0.1510(3) 0.2866(3)
H31 H 0.14970 0.12090 0.29580
H32 H 0.16090 0.01110 0.26680
H33 H 0.23840 -0.02360 0.24050
H34 H 0.30490 0.05160 0.24320
H35 H 0.29370 0.16130 0.27220
C43 C 0.2507(3) 0.2815(4) 0.2231(5)
C44 C 0.2829(5) 0.3181(6) 0.1954(3)
C45 C 0.3195(3) 0.3563(4) 0.2162(5)
C46 C 0.3238(3) 0.3579(4) 0.2647(5)
C47 C 0.2916(5) 0.3213(5) 0.2923(3)
C48 C 0.2550(3) 0.2831(4) 0.2715(4)
H36 H 0.22540 0.25500 0.20860
H37 H 0.27990 0.31700 0.16180
H38 H 0.34180 0.38180 0.19700
H39 H 0.34920 0.38450 0.27910
H40 H 0.29460 0.32240 0.32590
C49 C 0.2625(4) 0.1853(4) 0.3818(4)
C50 C 0.2823(3) 0.1900(5) 0.4264(5)
C51 C 0.2771(3) 0.2489(7) 0.4521(3)
C52 C 0.2521(4) 0.3033(4) 0.4330(4)
C53 C 0.2323(3) 0.2987(4) 0.3883(4)
C54 C 0.2375(3) 0.2397(7) 0.3627(3)
H41 H 0.26610 0.14440 0.36400
H42 H 0.29960 0.15220 0.43970
H43 H 0.29080 0.25220 0.48310
H44 H 0.24850 0.34420 0.45070
H45 H 0.21500 0.33640 0.37510
C55 C 0.0545(6) 0.1786(9) 0.4094(7)
H46 H 0.02090 0.18100 0.40510
C56 C 0.0845(7) 0.1415(8) 0.3811(6)
H47 H 0.07580 0.11650 0.35490
C57 C 0.1325(7) 0.1496(8) 0.4008(7)
H48 H 0.16080 0.12940 0.38950
C58 C 0.1300(7) 0.1919(8) 0.4386(6)
H49 H 0.15660 0.20470 0.45670
C59 C 0.0797(7) 0.2140(8) 0.4466(6)
H50 H 0.06730 0.24280 0.46940
C60 C 0.0725(7) 0.2726(8) 0.1625(6)
H51 H 0.05840 0.30740 0.14550
C61 C 0.0490(5) 0.2282(9) 0.1923(6)
H52 H 0.01550 0.22780 0.19780
C62 C 0.0838(7) 0.1818(7) 0.2141(5)
H53 H 0.07740 0.14950 0.23680
C63 C 0.1297(6) 0.1967(8) 0.1929(6)
H54 H 0.15850 0.17290 0.19750
C64 C 0.1242(6) 0.2535(10) 0.1635(6)
H55 H 0.14920 0.27510 0.14740
C65 C 0.1531(7) 0.4090(9) 0.2084(9)
H56 H 0.17320 0.39870 0.18310
C66 C 0.1031(8) 0.4256(7) 0.2059(7)
H57 H 0.08370 0.42850 0.17930
C67 C 0.0898(6) 0.4367(6) 0.2510(8)
H58 H 0.05840 0.44950 0.25940
C68 C 0.1279(7) 0.4270(7) 0.2844(6)
H59 H 0.12710 0.43060 0.31680
C69 C 0.1671(8) 0.4104(8) 0.2544(8)
H60 H 0.19870 0.40140 0.26470
C70 C 0.0226(12) 0.3892(17) 0.0508(11)
C71 C -0.0348(9) 0.3366(8) 0.0740(9)
C72 C -0.0822(11) 0.3258(9) 0.0898(8)
C73 C -0.1129(5) 0.3801(18) 0.0983(8)
C74 C -0.0962(8) 0.4453(13) 0.0910(8)
C75 C -0.0488(10) 0.4561(6) 0.0751(8)
C76 C -0.0181(6) 0.4017(13) 0.0666(8)
C77 C 0.3930(15) 0.4257(13) 0.5717(18)
C78 C 0.3238(19) 0.3798(15) 0.5472(4)
C79 C 0.2794(12) 0.3561(12) 0.5640(17)
C80 C 0.273(1) 0.3455(10) 0.6116(21)
C81 C 0.3111(21) 0.3586(14) 0.6425(6)
C82 C 0.3555(14) 0.3823(13) 0.6257(15)
C83 C 0.3619(8) 0.3929(11) 0.5781(18)
C84 C 0.1964(11) 0.3738(13) 0.0693(8)
C85 C 0.2552(9) 0.3720(7) 0.0648(7)
C86 C 0.3052(8) 0.3839(9) 0.0675(6)
C87 C 0.3226(5) 0.4393(11) 0.0920(6)
C88 C 0.2900(8) 0.4829(7) 0.1137(6)
C89 C 0.2401(7) 0.4711(8) 0.1110(5)
C90 C 0.2227(5) 0.4157(10) 0.0866(7)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
P 1.05
Y 1.73
|
1100598.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:33:40 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177949 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100598.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100598
loop_
_publ_author_name
'Anfang, S.'
'Harms, K.'
'Weller, F.'
'Borgmeier, O.'
'Lueken, H.'
'Schilder, H.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe Seltener Erden. Synthese und Kristallstrukturen
von [M~2~(C~5~H~5~)~3~(NPPh~3~)~3~] · 3 C~7~H~8~ mit M = Y, Dy und Er.
Magnetische Eigenschaften von
[Dy~2~(C~5~H~5~)~3~(NPPh~3~)~3~] · 3 C~7~H~8~
;
_journal_coden_ASTM ZAACAB
_journal_issue 1
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 159
_journal_page_last 166
_journal_paper_doi
10.1002/(sici)1521-3749(199801)624:1<159::aid-zaac159>3.0.co;2-z
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C90 H84 Dy2 N3 P3'
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 61
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.350(3)
_cell_length_b 19.872(2)
_cell_length_c 28.578(4)
_cod_database_code 1100598
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,y,1/2-z
3 x,1/2-y,1/2+z
4 1/2-x,1/2+y,z
5 -x,-y,-z
6 -1/2-x,-y,-1/2+z
7 -x,-1/2+y,-1/2-z
8 -1/2+x,-1/2-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Dy1 Dy 0.10620(2) 0.27406(2) 0.36694(2)
P1 P 0.12559(10) 0.43359(13) 0.42859(9)
N1 N 0.1182(3) 0.3719(3) 0.3973(3)
C1 C 0.1879(4) 0.4652(5) 0.4330(4)
Dy2 Dy 0.10689(2) 0.30520(2) 0.24733(2)
P2 P -0.00631(9) 0.29958(12) 0.30933(9)
N2 N 0.0507(2) 0.2942(3) 0.3072(3)
C2 C 0.2131(4) 0.4747(5) 0.3919(3)
H1 H 0.1979(4) 0.4654(5) 0.3631(3)
P3 P 0.21201(9) 0.23616(12) 0.30573(10)
N3 N 0.1587(3) 0.2616(3) 0.3030(2)
C3 C 0.2597(5) 0.4974(5) 0.3926(4)
H2 H 0.2763(5) 0.5039(5) 0.3642(4)
C4 C 0.2828(4) 0.5111(5) 0.4335(5)
H3 H 0.3152(4) 0.5270(5) 0.4334(5)
C5 C 0.2582(4) 0.5014(5) 0.4750(4)
H4 H 0.2739(4) 0.5097(5) 0.5037(4)
C6 C 0.2116(4) 0.4800(5) 0.4740(4)
H5 H 0.1946(4) 0.4750(5) 0.5024(4)
C7 C 0.0941(4) 0.5098(5) 0.4094(3)
C8 C 0.1038(4) 0.5714(5) 0.4275(4)
H6 H 0.1262(4) 0.5750(5) 0.4523(4)
C9 C 0.0813(5) 0.6296(6) 0.4105(4)
H7 H 0.0885(5) 0.6719(6) 0.4235(4)
C10 C 0.0487(5) 0.6237(6) 0.3744(4)
H8 H 0.0338(5) 0.6625(6) 0.3621(4)
C11 C 0.0377(4) 0.5625(6) 0.3561(4)
H9 H 0.0146(4) 0.5589(6) 0.3318(4)
C12 C 0.0605(4) 0.5056(5) 0.3734(3)
H10 H 0.0529(4) 0.4633(5) 0.3605(3)
C13 C 0.1060(4) 0.4207(5) 0.4884(3)
C14 C 0.1245(4) 0.3635(6) 0.5115(4)
H11 H 0.1475(4) 0.3358(6) 0.4964(4)
C15 C 0.1092(5) 0.3479(7) 0.5559(5)
H12 H 0.1208(5) 0.3089(7) 0.5709(5)
C16 C 0.0778(6) 0.3888(8) 0.5778(5)
H13 H 0.0687(6) 0.3784(8) 0.6087(5)
C17 C 0.0583(5) 0.4444(8) 0.5578(5)
H14 H 0.0354(5) 0.4710(8) 0.5739(5)
C18 C 0.0731(4) 0.4612(6) 0.5127(4)
H15 H 0.0608(4) 0.5003(6) 0.4984(4)
C19 C -0.0304(3) 0.3744(5) 0.2809(4)
C20 C -0.0503(3) 0.4276(5) 0.3052(4)
H16 H -0.0542(3) 0.4250(5) 0.3378(4)
C21 C -0.0645(4) 0.4850(5) 0.2813(5)
H17 H -0.0778(4) 0.5212(5) 0.2981(5)
C22 C -0.0597(4) 0.4905(6) 0.2341(5)
H18 H -0.0690(4) 0.5305(6) 0.2190(5)
C23 C -0.0412(4) 0.4376(6) 0.2085(4)
H19 H -0.0382(4) 0.4406(6) 0.1758(4)
C24 C -0.0270(4) 0.3800(6) 0.2322(4)
H20 H -0.0146(4) 0.3435(6) 0.2149(4)
C25 C -0.0392(3) 0.2301(5) 0.2842(4)
C26 C -0.0791(4) 0.2355(5) 0.2557(4)
H21 H -0.0910(4) 0.2788(5) 0.2489(4)
C27 C -0.1028(4) 0.1810(6) 0.2364(5)
H22 H -0.1300(4) 0.1874(6) 0.2168(5)
C28 C -0.0862(4) 0.1170(6) 0.2461(5)
H23 H -0.1021(4) 0.0793(6) 0.2332(5)
C29 C -0.0463(4) 0.1087(5) 0.2749(4)
H24 H -0.0352(4) 0.0653(5) 0.2826(4)
C30 C -0.0227(4) 0.1644(5) 0.2923(4)
H25 H 0.0057(4) 0.1582(5) 0.3104(4)
C31 C -0.0317(3) 0.3024(4) 0.3677(4)
C32 C -0.0065(4) 0.3369(5) 0.4028(4)
H26 H 0.0230(4) 0.3587(5) 0.3954(4)
C33 C -0.0242(5) 0.3396(6) 0.4484(4)
H27 H -0.0074(5) 0.3640(6) 0.4716(4)
C34 C -0.0676(6) 0.3053(7) 0.4592(5)
H28 H -0.0793(6) 0.3039(7) 0.4901(5)
C35 C -0.0931(5) 0.2736(7) 0.4234(6)
H29 H -0.1231(5) 0.2527(7) 0.4300(6)
C36 C -0.0755(4) 0.2721(6) 0.3793(4)
H30 H -0.0935(4) 0.2498(6) 0.3559(4)
C37 C 0.2203(3) 0.1511(5) 0.2853(4)
C38 C 0.1821(4) 0.1081(4) 0.2830(4)
H31 H 0.1509(4) 0.1228(4) 0.2923(4)
C39 C 0.1883(4) 0.0422(5) 0.2671(4)
H32 H 0.1617(4) 0.0122(5) 0.2672(4)
C40 C 0.2329(4) 0.0213(5) 0.2514(4)
H33 H 0.2365(4) -0.0223(5) 0.2392(4)
C41 C 0.2721(4) 0.0629(5) 0.2534(4)
H34 H 0.3031(4) 0.0480(5) 0.2438(4)
C42 C 0.2658(4) 0.1268(5) 0.2697(4)
H35 H 0.2929(4) 0.1559(5) 0.2704(4)
C43 C 0.2558(4) 0.2835(5) 0.2713(4)
C44 C 0.2512(4) 0.2831(5) 0.2225(4)
H36 H 0.2258(4) 0.2580(5) 0.2089(4)
C45 C 0.2829(4) 0.3185(6) 0.1931(4)
H37 H 0.2797(4) 0.3166(6) 0.1604(4)
C46 C 0.3180(5) 0.3553(6) 0.2135(5)
H38 H 0.3390(5) 0.3806(6) 0.1943(5)
C47 C 0.3252(4) 0.3578(5) 0.2612(5)
H39 H 0.3505(4) 0.3837(5) 0.2743(5)
C48 C 0.2936(4) 0.3209(5) 0.2894(4)
H40 H 0.2983(4) 0.3216(5) 0.3220(4)
C49 C 0.2380(3) 0.2376(5) 0.3641(4)
C50 C 0.2636(4) 0.1842(5) 0.3832(4)
H41 H 0.2676(4) 0.1441(5) 0.3661(4)
C51 C 0.2835(5) 0.1903(6) 0.4283(5)
H42 H 0.3010(5) 0.1543(6) 0.4416(5)
C52 C 0.2776(5) 0.2486(6) 0.4528(4)
H43 H 0.2907(5) 0.2526(6) 0.4831(4)
C53 C 0.2529(4) 0.3006(6) 0.4337(4)
H44 H 0.2496(4) 0.3408(6) 0.4509(4)
C54 C 0.2322(4) 0.2965(5) 0.3897(4)
H45 H 0.2146(4) 0.3330(5) 0.3773(4)
C55 C 0.0533(4) 0.1790(6) 0.4128(5)
H46 H 0.0190(4) 0.1819(6) 0.4106(5)
C56 C 0.0845(5) 0.1433(5) 0.3823(4)
H47 H 0.0747(5) 0.1193(5) 0.3556(4)
C57 C 0.1310(5) 0.1494(5) 0.3981(5)
H48 H 0.1588(5) 0.1293(5) 0.3847(5)
C58 C 0.1306(5) 0.1916(6) 0.4384(5)
H49 H 0.1579(5) 0.2048(6) 0.4561(5)
C59 C 0.0826(6) 0.2093(6) 0.4467(4)
H50 H 0.0716(6) 0.2372(6) 0.4711(4)
C60 C 0.0734(5) 0.2700(6) 0.1616(4)
H51 H 0.0592(5) 0.3049(6) 0.1442(4)
C61 C 0.0496(4) 0.2266(6) 0.1927(4)
H52 H 0.0159(4) 0.2268(6) 0.1995(4)
C62 C 0.0835(5) 0.1840(5) 0.2115(4)
H53 H 0.0769(5) 0.1506(5) 0.2339(4)
C63 C 0.1293(4) 0.1973(5) 0.1926(4)
H54 H 0.1587(4) 0.1748(5) 0.1993(4)
C64 C 0.1229(4) 0.2508(5) 0.1617(4)
H55 H 0.1478(4) 0.2708(5) 0.1437(4)
C65 C 0.1512(6) 0.4085(6) 0.2044(5)
H56 H 0.1704(6) 0.3975(6) 0.1781(5)
C66 C 0.1019(6) 0.4263(5) 0.2044(4)
H57 H 0.0819(6) 0.4294(5) 0.1777(4)
C67 C 0.0871(4) 0.4387(4) 0.2504(5)
H58 H 0.0557(4) 0.4517(4) 0.2604(5)
C68 C 0.1282(4) 0.4279(4) 0.2790(4)
H59 H 0.1293(4) 0.4320(4) 0.3117(4)
C69 C 0.1665(4) 0.4101(5) 0.2502(5)
H60 H 0.1984(4) 0.4005(5) 0.2604(5)
C70 C -0.0115(4) 0.3925(7) 0.0579(3)
C71 C -0.0344(6) 0.3329(5) 0.0716(4)
H61 H -0.0179(8) 0.2903(6) 0.0677(7)
C72 C -0.0811(6) 0.3348(7) 0.0908(5)
H62 H -0.0969(8) 0.2936(9) 0.1003(7)
C73 C -0.1049(4) 0.3964(10) 0.0964(4)
H63 H -0.1372(4) 0.3978(14) 0.1097(6)
C74 C -0.0821(6) 0.4561(7) 0.0828(5)
H64 H -0.0985(8) 0.4986(9) 0.0866(7)
C75 C -0.0353(6) 0.4541(5) 0.0635(4)
H65 H -0.0195(8) 0.4953(7) 0.0540(6)
C76 C 0.0385(5) 0.4006(13) 0.0500(6)
H66 H 0.0451(6) 0.4465(14) 0.0409(7)
H67 H 0.0562(4) 0.3903(14) 0.0783(7)
H68 H 0.0488(6) 0.3706(15) 0.0255(7)
C77 C 0.3605(4) 0.3953(5) 0.5780(3)
C78 C 0.3211(4) 0.3800(5) 0.5485(3)
H69 H 0.3234(6) 0.3879(8) 0.5153(3)
C79 C 0.2820(4) 0.3554(5) 0.5665(4)
H70 H 0.2581(5) 0.3438(8) 0.5431(5)
C80 C 0.2665(4) 0.3420(5) 0.6105(5)
H71 H 0.2350(4) 0.3255(8) 0.6201(7)
C81 C 0.3078(5) 0.3578(5) 0.6399(3)
H72 H 0.3034(6) 0.3509(8) 0.6730(3)
C82 C 0.3494(4) 0.3799(5) 0.6270(3)
H73 H 0.3744(5) 0.3866(8) 0.6503(4)
C83 C 0.4011(4) 0.4226(7) 0.5661(6)
H74 H 0.4018(6) 0.4289(9) 0.5327(6)
H75 H 0.4043(5) 0.4657(7) 0.5814(7)
H76 H 0.4277(4) 0.3937(9) 0.5753(7)
C84 C 0.2175(4) 0.4040(6) 0.0814(4)
C85 C 0.2505(6) 0.3568(5) 0.0630(4)
H77 H 0.2417(9) 0.3149(6) 0.0482(5)
C86 C 0.2966(5) 0.3795(6) 0.0694(4)
H78 H 0.3184(7) 0.3484(9) 0.0540(5)
C87 C 0.3236(4) 0.4276(8) 0.0885(5)
H79 H 0.3586(4) 0.4310(12) 0.0884(7)
C88 C 0.2880(5) 0.4761(6) 0.1104(4)
H80 H 0.2981(7) 0.5163(7) 0.1266(5)
C89 C 0.2408(4) 0.4587(5) 0.1053(3)
H81 H 0.2184(6) 0.4888(7) 0.1207(5)
C90 C 0.1708(4) 0.3975(11) 0.0726(6)
H82 H 0.1652(6) 0.3559(11) 0.0560(7)
H83 H 0.1529(4) 0.3969(12) 0.1017(7)
H84 H 0.1599(4) 0.4348(12) 0.0537(7)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Dy 1.65
N 0.68
P 1.05
|
1100599.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:33:40 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177949 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/05/1100599.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100599
loop_
_publ_author_name
'Anfang, S.'
'Harms, K.'
'Weller, F.'
'Borgmeier, O.'
'Lueken, H.'
'Schilder, H.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe Seltener Erden. Synthese und Kristallstrukturen
von [M~2~(C~5~H~5~)~3~(NPPh~3~)~3~] · 3 C~7~H~8~ mit M = Y, Dy und Er.
Magnetische Eigenschaften von
[Dy~2~(C~5~H~5~)~3~(NPPh~3~)~3~] · 3 C~7~H~8~
;
_journal_coden_ASTM ZAACAB
_journal_issue 1
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 159
_journal_page_last 166
_journal_paper_doi
10.1002/(sici)1521-3749(199801)624:1<159::aid-zaac159>3.0.co;2-z
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C90 H84 Er2 N3 P3'
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 61
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.333(7)
_cell_length_b 19.811(8)
_cell_length_c 28.511(8)
_cod_database_code 1100599
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,y,1/2-z
3 x,1/2-y,1/2+z
4 1/2-x,1/2+y,z
5 -x,-y,-z
6 -1/2-x,-y,-1/2+z
7 -x,-1/2+y,-1/2-z
8 -1/2+x,-1/2-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Er1 Er 0.10610(2) 0.27347(3) 0.36532(2)
P1 P 0.12550(13) 0.4320(2) 0.42772(13)
N1 N 0.1191(3) 0.3702(4) 0.3972(4)
C1 C 0.1878(4) 0.4652(6) 0.4328(5)
Er2 Er 0.10709(2) 0.30575(2) 0.24728(2)
P2 P -0.00575(11) 0.2998(2) 0.30845(13)
N2 N 0.0515(3) 0.2936(4) 0.3065(3)
C2 C 0.2132(5) 0.4732(6) 0.3908(5)
H1 H 0.1982(5) 0.4611(6) 0.3624(5)
P3 P 0.21186(12) 0.2366(2) 0.30509(13)
N3 N 0.1575(3) 0.2621(5) 0.3027(3)
C3 C 0.2604(5) 0.4990(7) 0.3905(6)
H2 H 0.2769(5) 0.5070(7) 0.3621(6)
C4 C 0.2822(5) 0.5125(7) 0.4327(6)
H3 H 0.3143(5) 0.5297(7) 0.4335(6)
C5 C 0.2578(6) 0.5009(7) 0.4740(6)
H4 H 0.2739(6) 0.5087(7) 0.5026(6)
C6 C 0.2102(5) 0.4782(7) 0.4744(5)
H5 H 0.1935(5) 0.4718(7) 0.5028(5)
C7 C 0.0928(5) 0.5089(6) 0.4091(4)
C8 C 0.1029(5) 0.5708(6) 0.4273(5)
H6 H 0.1256(5) 0.5740(6) 0.4519(5)
C9 C 0.0812(6) 0.6287(7) 0.4112(6)
H7 H 0.0895(6) 0.6712(7) 0.4235(6)
C10 C 0.0464(6) 0.6221(7) 0.3757(6)
H8 H 0.0291(6) 0.6602(7) 0.3650(6)
C11 C 0.0376(5) 0.5613(7) 0.3568(5)
H9 H 0.0158(5) 0.5584(7) 0.3314(5)
C12 C 0.0589(4) 0.5036(6) 0.3730(4)
H10 H 0.0509(4) 0.4614(6) 0.3601(4)
C13 C 0.1065(5) 0.4188(6) 0.4886(4)
C14 C 0.1245(6) 0.3619(8) 0.5116(6)
H11 H 0.1475(6) 0.3341(8) 0.4965(6)
C15 C 0.1091(7) 0.3466(8) 0.5553(5)
H12 H 0.1210(7) 0.3072(8) 0.5697(5)
C16 C 0.0773(8) 0.3859(12) 0.5790(7)
H13 H 0.0675(8) 0.3752(12) 0.6097(7)
C17 C 0.0600(7) 0.4413(10) 0.5569(6)
H14 H 0.0379(7) 0.4696(10) 0.5728(6)
C18 C 0.0738(6) 0.4578(8) 0.5117(5)
H15 H 0.0604(6) 0.4961(8) 0.4970(5)
C19 C -0.0304(4) 0.3744(6) 0.2788(5)
C20 C -0.0502(4) 0.4284(6) 0.3035(5)
H16 H -0.0539(4) 0.4258(6) 0.3362(5)
C21 C -0.0643(5) 0.4858(7) 0.2798(7)
H17 H -0.0775(5) 0.5223(7) 0.2967(7)
C22 C -0.0594(5) 0.4909(9) 0.2321(7)
H18 H -0.0688(5) 0.5306(9) 0.2165(7)
C23 C -0.0403(5) 0.4363(8) 0.2070(6)
H19 H -0.0372(5) 0.4386(8) 0.1742(6)
C24 C -0.0264(5) 0.3806(7) 0.2304(6)
H20 H -0.0134(5) 0.3442(7) 0.2132(6)
C25 C -0.0379(4) 0.2307(6) 0.2830(5)
C26 C -0.0794(5) 0.2367(6) 0.2535(5)
H21 H -0.0914(5) 0.2797(6) 0.2456(5)
C27 C -0.1021(5) 0.1802(7) 0.2365(6)
H22 H -0.1301(5) 0.1858(7) 0.2179(6)
C28 C -0.0861(5) 0.1162(8) 0.2451(6)
H23 H -0.1018(5) 0.0785(8) 0.2318(6)
C29 C -0.0458(6) 0.1088(7) 0.2744(6)
H24 H -0.0341(6) 0.0656(7) 0.2821(6)
C30 C -0.0232(5) 0.1655(7) 0.2919(5)
H25 H 0.0042(5) 0.1593(7) 0.3113(5)
C31 C -0.0306(4) 0.3032(6) 0.3675(5)
C32 C -0.0057(5) 0.3382(6) 0.4024(5)
H26 H 0.0234(5) 0.3612(6) 0.3952(5)
C33 C -0.0236(6) 0.3394(8) 0.4473(5)
H27 H -0.0063(6) 0.3611(8) 0.4714(5)
C34 C -0.0682(7) 0.3074(10) 0.4565(7)
H28 H -0.0812(7) 0.3095(10) 0.4870(7)
C35 C -0.0934(6) 0.2737(9) 0.4230(7)
H29 H -0.1227(6) 0.2512(9) 0.4301(7)
C36 C -0.0750(5) 0.2732(7) 0.3788(6)
H30 H -0.0929(5) 0.2517(7) 0.3549(6)
C37 C 0.2208(4) 0.1514(6) 0.2839(5)
C38 C 0.1822(4) 0.1069(6) 0.2817(5)
H31 H 0.1510(4) 0.1213(6) 0.2915(5)
C39 C 0.1878(5) 0.0426(6) 0.2656(5)
H32 H 0.1609(5) 0.0131(6) 0.2650(5)
C40 C 0.2330(5) 0.0206(6) 0.2501(6)
H33 H 0.2363(5) -0.0235(6) 0.2383(6)
C41 C 0.2737(5) 0.0625(6) 0.2515(6)
H34 H 0.3047(5) 0.0468(6) 0.2424(6)
C42 C 0.2669(5) 0.1282(7) 0.2670(5)
H35 H 0.2934(5) 0.1584(7) 0.2662(5)
C43 C 0.2559(5) 0.2855(7) 0.2695(5)
C44 C 0.2508(6) 0.2832(8) 0.2219(6)
H36 H 0.2257(6) 0.2571(8) 0.2084(6)
C45 C 0.2823(6) 0.3192(8) 0.1933(6)
H37 H 0.2784(6) 0.3187(8) 0.1606(6)
C46 C 0.3202(6) 0.3561(7) 0.2141(7)
H38 H 0.3421(6) 0.3798(7) 0.1948(7)
C47 C 0.3260(6) 0.3588(8) 0.2610(7)
H39 H 0.3507(6) 0.3856(8) 0.2746(7)
C48 C 0.2945(5) 0.3207(6) 0.2888(5)
H40 H 0.2997(5) 0.3190(6) 0.3214(5)
C49 C 0.2384(4) 0.2371(6) 0.3635(5)
C50 C 0.2641(5) 0.1851(7) 0.3827(5)
H41 H 0.2681(5) 0.1450(7) 0.3655(5)
C51 C 0.2838(6) 0.1896(9) 0.4259(7)
H42 H 0.3005(6) 0.1526(9) 0.4389(7)
C52 C 0.2795(6) 0.2499(8) 0.4513(6)
H43 H 0.2951(6) 0.2545(8) 0.4805(6)
C53 C 0.2528(5) 0.3013(8) 0.4336(6)
H44 H 0.2481(5) 0.3407(8) 0.4513(6)
C54 C 0.2325(5) 0.2962(7) 0.3894(5)
H45 H 0.2147(5) 0.3325(7) 0.3769(5)
C55 C 0.0536(6) 0.1796(8) 0.4104(6)
H46 H 0.0194(6) 0.1827(8) 0.4081(6)
C56 C 0.0836(6) 0.1429(7) 0.3804(6)
H47 H 0.0735(6) 0.1178(7) 0.3541(6)
C57 C 0.1315(6) 0.1502(7) 0.3967(6)
H48 H 0.1596(6) 0.1304(7) 0.3836(6)
C58 C 0.1301(6) 0.1933(9) 0.4370(7)
H49 H 0.1568(6) 0.2073(9) 0.4554(7)
C59 C 0.0815(7) 0.2103(7) 0.4433(6)
H50 H 0.0696(7) 0.2389(7) 0.4670(6)
C60 C 0.0746(5) 0.2720(7) 0.1607(5)
H51 H 0.0601(5) 0.3068(7) 0.1431(5)
C61 C 0.0508(5) 0.2273(8) 0.1921(5)
H52 H 0.0171(5) 0.2275(8) 0.1985(5)
C62 C 0.0843(5) 0.1832(6) 0.2121(5)
H53 H 0.0777(5) 0.1495(6) 0.2344(5)
C63 C 0.1304(5) 0.1989(7) 0.1921(5)
H54 H 0.1600(5) 0.1765(7) 0.1983(5)
C64 C 0.1242(5) 0.2539(8) 0.1614(6)
H55 H 0.1492(5) 0.2750(8) 0.1442(6)
C65 C 0.1511(7) 0.4090(7) 0.2057(7)
H56 H 0.1707(7) 0.3995(7) 0.1794(7)
C66 C 0.1025(7) 0.4250(6) 0.2042(5)
H57 H 0.0831(7) 0.4280(6) 0.1771(5)
C67 C 0.0873(4) 0.4360(6) 0.2496(6)
H58 H 0.0553(4) 0.4472(6) 0.2587(6)
C68 C 0.1266(5) 0.4281(6) 0.2796(5)
H59 H 0.1264(5) 0.4344(6) 0.3123(5)
C69 C 0.1673(5) 0.4086(6) 0.2519(7)
H60 H 0.1989(5) 0.3977(6) 0.2626(7)
C70 C -0.0087(6) 0.3956(10) 0.0581(5)
C71 C -0.0321(9) 0.3352(7) 0.0693(6)
H61 H -0.0156(12) 0.2929(9) 0.0646(9)
C72 C -0.0794(9) 0.3362(9) 0.0874(7)
H62 H -0.0955(12) 0.2945(12) 0.0951(10)
C73 C -0.1033(6) 0.3975(13) 0.0942(6)
H63 H -0.1359(6) 0.3981(19) 0.1067(8)
C74 C -0.0799(7) 0.4578(9) 0.0830(6)
H64 H -0.0964(10) 0.5001(11) 0.0877(9)
C75 C -0.0326(7) 0.4569(7) 0.0649(5)
H65 H -0.0165(11) 0.4986(9) 0.0572(8)
C76 C 0.0415(6) 0.4040(18) 0.0519(8)
H66 H 0.0483(8) 0.4504(20) 0.0443(9)
H67 H 0.0583(6) 0.3918(20) 0.0802(9)
H68 H 0.0525(8) 0.3755(22) 0.0267(9)
C77 C 0.3621(5) 0.3962(6) 0.5780(5)
C78 C 0.3237(6) 0.3805(7) 0.5476(4)
H69 H 0.3270(9) 0.3881(10) 0.5144(4)
C79 C 0.2841(5) 0.3557(7) 0.5645(6)
H70 H 0.2610(7) 0.3438(10) 0.5405(7)
C80 C 0.2674(5) 0.3423(7) 0.6081(7)
H71 H 0.2356(6) 0.3257(10) 0.6168(10)
C81 C 0.3077(6) 0.3586(7) 0.6386(4)
H72 H 0.3023(9) 0.3518(10) 0.6715(5)
C82 C 0.3497(6) 0.3809(7) 0.6268(4)
H73 H 0.3739(7) 0.3879(10) 0.6507(6)
C83 C 0.4030(6) 0.4236(10) 0.5672(8)
H74 H 0.4046(8) 0.4298(12) 0.5338(9)
H75 H 0.4056(7) 0.4668(10) 0.5825(10)
H76 H 0.4294(5) 0.3950(12) 0.5772(10)
C84 C 0.2199(6) 0.4050(7) 0.0808(5)
C85 C 0.2543(8) 0.3601(6) 0.0622(5)
H77 H 0.2469(11) 0.3181(8) 0.0469(7)
C86 C 0.2997(7) 0.3852(9) 0.0692(5)
H78 H 0.3225(9) 0.3558(12) 0.0537(8)
C87 C 0.3251(5) 0.4344(11) 0.0891(7)
H79 H 0.3600(5) 0.4397(16) 0.0893(9)
C88 C 0.2879(7) 0.4803(8) 0.1112(5)
H80 H 0.2967(10) 0.5206(9) 0.1280(7)
C89 C 0.2413(6) 0.4603(6) 0.1055(4)
H81 H 0.2179(8) 0.4888(9) 0.1211(6)
C90 C 0.1734(6) 0.3960(13) 0.0716(8)
H82 H 0.1692(9) 0.3545(14) 0.0546(9)
H83 H 0.1554(6) 0.3938(15) 0.1005(9)
H84 H 0.1616(6) 0.4331(15) 0.0531(9)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Er 1.73
N 0.68
P 1.05
|
1100600.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 22:03:05 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177996 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100600.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100600
loop_
_publ_author_name
'Harms, Klaus'
'Merle, Jan'
'Maichle-M\"ossmer, C\"acili\"a'
'Massa, Werner'
'Krieger, Matthias'
_publ_section_title
;
Heterocubane Phosphoraniminato Complexes of Cadmium
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 1099
_journal_page_last 1104
_journal_paper_doi 10.1021/ic9710364
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C25 H62 Cd4 Cl6 N4 P4'
_chemical_formula_weight 1204.97
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 90.57(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 11.007(3)
_cell_length_b 10.988(3)
_cell_length_c 18.528(2)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 21
_cell_measurement_theta_min 15
_cell_volume 2240.8(9)
_diffrn_ambient_temperature 223(2)
_diffrn_radiation_wavelength 0.71073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.02(6)
_refine_ls_extinction_coef 0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_all 1.331
_refine_ls_goodness_of_fit_obs 1.337
_refine_ls_number_parameters 401
_refine_ls_number_reflns 7459
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.331
_refine_ls_restrained_S_obs 1.337
_refine_ls_R_factor_all 0.0582
_refine_ls_R_factor_obs 0.0579
_refine_ls_shift/esd_max -0.028
_refine_ls_shift/esd_mean 0.001
_refine_ls_wR_factor_all 0.1431
_refine_ls_wR_factor_obs 0.1429
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 1100600
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0243(5) 0.0221(6) 0.0224(5) 0.0006(4) -0.0033(4) -0.0002(4)
Cd2 0.0235(5) 0.0235(6) 0.0222(5) 0.0005(4) -0.0023(4) 0.0003(4)
Cd3 0.0260(5) 0.0236(5) 0.0250(5) 0.0031(5) 0.0033(4) -0.0019(5)
Cd4 0.0241(5) 0.0240(5) 0.0266(5) -0.0041(5) 0.0020(4) 0.0007(5)
Cl1 0.047(2) 0.041(2) 0.051(3) -0.013(2) -0.015(2) -0.009(2)
Cl2 0.041(2) 0.065(3) 0.042(2) 0.011(2) -0.005(2) 0.019(2)
Cl3 0.075(3) 0.055(3) 0.045(3) 0.009(2) 0.020(2) -0.025(3)
Cl4 0.041(2) 0.062(3) 0.065(3) -0.029(3) 0.014(2) 0.008(2)
P1 0.030(2) 0.035(2) 0.032(2) 0.006(2) -0.005(2) 0.010(2)
P2 0.031(2) 0.029(2) 0.028(2) -0.005(2) -0.001(2) -0.009(2)
P3 0.032(2) 0.030(2) 0.031(2) -0.006(2) 0.004(2) 0.009(2)
P4 0.031(2) 0.035(2) 0.022(2) 0.006(2) 0.005(2) -0.010(2)
N1 0.038(7) 0.010(6) 0.041(8) 0.009(5) -0.008(6) 0.007(5)
N2 0.021(6) 0.043(8) 0.023(6) -0.006(6) 0.002(5) -0.006(6)
N3 0.013(5) 0.066(11) 0.016(6) -0.004(6) 0.010(4) 0.006(6)
N4 0.029(6) 0.008(6) 0.017(5) 0.002(4) 0.014(5) -0.004(5)
C11 0.035(9) 0.068(14) 0.067(13) 0.015(11) -0.011(9) 0.008(10)
C12 0.032(10) 0.082(16) 0.097(17) 0.039(13) -0.019(10) -0.006(10)
C13 0.038(9) 0.073(13) 0.012(7) 0.002(8) -0.003(6) 0.015(8)
C14 0.110(20) 0.059(14) 0.046(12) 0.005(10) -0.007(12) 0.034(14)
C15 0.060(14) 0.057(13) 0.096(18) -0.014(12) -0.028(13) 0.033(11)
C16 0.081(20) 0.061(19) 0.321(57) -0.003(27) -0.089(28) 0.023(16)
C21 0.053(10) 0.025(8) 0.029(8) 0.002(6) 0.004(7) -0.021(7)
C22 0.119(22) 0.127(26) 0.081(17) 0.045(17) -0.022(16) -0.104(21)
C23 0.071(13) 0.032(10) 0.071(13) -0.003(10) -0.013(11) -0.020(10)
C24 0.107(19) 0.042(12) 0.081(16) -0.023(11) -0.041(14) -0.013(12)
C25 0.040(11) 0.065(13) 0.088(16) -0.033(12) 0.018(10) -0.022(10)
C26 0.033(11) 0.066(17) 0.128(23) -0.006(14) 0.004(12) 0.002(10)
C31 0.033(9) 0.030(9) 0.068(12) -0.005(8) -0.008(8) 0.005(7)
C32 0.032(11) 0.200(32) 0.054(13) -0.057(17) 0.007(9) 0.044(15)
C33 0.093(17) 0.044(11) 0.070(14) -0.031(11) -0.016(12) 0.039(12)
C34 0.089(16) 0.061(13) 0.066(14) 0.009(13) 0.016(12) -0.032(14)
C35 0.026(8) 0.028(9) 0.072(13) -0.011(8) 0.001(8) 0.005(7)
C36 0.123(21) 0.056(13) 0.032(10) -0.005(9) 0.027(12) 0.011(13)
C41 0.071(14) 0.046(11) 0.058(12) -0.001(10) 0.027(11) 0.009(10)
C42 0.124(21) 0.036(12) 0.076(16) 0.007(10) 0.028(15) -0.036(12)
C43 0.044(10) 0.056(12) 0.025(8) 0.005(8) 0.004(7) -0.015(8)
C44 0.039(10) 0.110(18) 0.028(9) 0.019(10) 0.009(8) -0.022(11)
C45 0.044(10) 0.099(16) 0.032(9) 0.037(10) 0.003(8) -0.035(11)
C46 0.051(11) 0.060(12) 0.039(9) -0.004(9) -0.010(8) 0.011(10)
Cl10 0.077(4) 0.081(4) 0.070(4) -0.027(3) 0.011(3) 0.007(3)
Cl20 0.073(3) 0.076(3) 0.051(3) -0.004(3) 0.007(2) -0.014(3)
C100 0.041(10) 0.070(13) 0.054(12) -0.002(10) 0.024(9) 0.005(10)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd1 Cd 0.35033(9) 0.81620(9) 0.30486(5) 0.0230(3) Uani 1 d . .
Cd2 Cd 0.13699(9) 0.78138(9) 0.18593(5) 0.0231(3) Uani 1 d . .
Cd3 Cd 0.16208(9) 0.58566(10) 0.31404(5) 0.0248(2) Uani 1 d . .
Cd4 Cd 0.36842(9) 0.59373(10) 0.19292(5) 0.0249(2) Uani 1 d . .
Cl1 Cl 0.4650(4) 0.9751(4) 0.3626(2) 0.0469(11) Uani 1 d . .
Cl2 Cl -0.0256(4) 0.8775(5) 0.1205(2) 0.0491(11) Uani 1 d . .
Cl3 Cl 0.0506(5) 0.4363(5) 0.3792(3) 0.0582(13) Uani 1 d . .
Cl4 Cl 0.5211(4) 0.4692(5) 0.1381(3) 0.0561(13) Uani 1 d . .
P1 P 0.4546(4) 0.5402(4) 0.3701(2) 0.0321(9) Uani 1 d . .
P2 P 0.0893(4) 0.4832(4) 0.1422(2) 0.0296(8) Uani 1 d . .
P3 P 0.0654(4) 0.8761(4) 0.3583(2) 0.0309(9) Uani 1 d . .
P4 P 0.4244(4) 0.8748(4) 0.1270(2) 0.0293(8) Uani 1 d . .
N1 N 0.3716(11) 0.6116(10) 0.3131(7) 0.030(3) Uani 1 d . .
N2 N 0.1663(10) 0.5763(13) 0.1890(6) 0.029(3) Uani 1 d . .
N3 N 0.1472(10) 0.7919(14) 0.3081(6) 0.032(4) Uani 1 d . .
N4 N 0.3450(10) 0.7986(9) 0.1803(6) 0.018(2) Uani 1 d . .
C11 C 0.6063(15) 0.6055(21) 0.3737(11) 0.057(5) Uani 1 d . .
H11A H 0.6424(15) 0.5987(21) 0.3257(11) 0.068 Uiso 1 calc R .
H11B H 0.5992(15) 0.6924(21) 0.3848(11) 0.068 Uiso 1 calc R .
C12 C 0.6951(17) 0.5463(21) 0.4299(13) 0.071(7) Uani 1 d . .
H12A H 0.7769(32) 0.5757(124) 0.4218(62) 0.106 Uiso 1 calc R .
H12B H 0.6933(117) 0.4585(23) 0.4245(62) 0.106 Uiso 1 calc R .
H12C H 0.6702(95) 0.5680(129) 0.4783(14) 0.106 Uiso 1 calc R .
C13 C 0.3972(16) 0.5431(17) 0.4645(8) 0.041(4) Uani 1 d . .
H13A H 0.3151(16) 0.5085(17) 0.4650(8) 0.049 Uiso 1 calc R .
H13B H 0.4493(16) 0.4912(17) 0.4947(8) 0.049 Uiso 1 calc R .
C14 C 0.3938(24) 0.6594(20) 0.4946(11) 0.072(7) Uani 1 d . .
H14A H 0.3403(118) 0.6593(41) 0.5359(55) 0.107 Uiso 1 calc R .
H14B H 0.3637(146) 0.7168(32) 0.4588(30) 0.107 Uiso 1 calc R .
H14C H 0.4749(33) 0.6830(63) 0.5099(82) 0.107 Uiso 1 calc R .
C15 C 0.4789(20) 0.3800(20) 0.3443(14) 0.071(7) Uani 1 d . .
H15A H 0.5255(20) 0.3780(20) 0.2995(14) 0.086 Uiso 1 calc R .
H15B H 0.5282(20) 0.3405(20) 0.3819(14) 0.086 Uiso 1 calc R .
C16 C 0.3679(26) 0.3097(27) 0.3337(25) 0.155(19) Uani 1 d . .
H16A H 0.3842(84) 0.2244(55) 0.3432(197) 0.232 Uiso 1 calc R .
H16B H 0.3394(183) 0.3192(267) 0.2843(56) 0.232 Uiso 1 calc R .
H16C H 0.3061(110) 0.3388(225) 0.3664(137) 0.232 Uiso 1 calc R .
C21 C 0.0653(15) 0.5342(14) 0.0541(8) 0.036(4) Uani 1 d . .
H21A H 0.0170(15) 0.4737(14) 0.0276(8) 0.043 Uiso 1 calc R .
H21B H 0.0186(15) 0.6101(14) 0.0554(8) 0.043 Uiso 1 calc R .
C22 C 0.1878(25) 0.5570(27) 0.0129(14) 0.109(13) Uani 1 d . .
H22A H 0.1704(32) 0.5960(202) -0.0331(61) 0.164 Uiso 1 calc R .
H22B H 0.2282(109) 0.4799(34) 0.0046(114) 0.164 Uiso 1 calc R .
H22C H 0.2402(95) 0.6093(182) 0.0417(62) 0.164 Uiso 1 calc R .
C23 C 0.1639(20) 0.3346(18) 0.1348(12) 0.058(5) Uani 1 d . .
H23A H 0.2446(20) 0.3466(18) 0.1141(12) 0.070 Uiso 1 calc R .
H23B H 0.1753(20) 0.3013(18) 0.1834(12) 0.070 Uiso 1 calc R .
C24 C 0.0958(24) 0.2410(19) 0.0891(13) 0.077(8) Uani 1 d . .
H24A H 0.1149(130) 0.1598(20) 0.1064(63) 0.116 Uiso 1 calc R .
H24B H 0.1201(124) 0.2485(111) 0.0391(21) 0.116 Uiso 1 calc R .
H24C H 0.0090(25) 0.2550(104) 0.0927(78) 0.116 Uiso 1 calc R .
C25 C -0.0649(17) 0.4481(20) 0.1754(13) 0.064(6) Uani 1 d . .
H25A H -0.1081(17) 0.4000(20) 0.1388(13) 0.077 Uiso 1 calc R .
H25B H -0.0574(17) 0.3979(20) 0.2190(13) 0.077 Uiso 1 calc R .
C26 C -0.1373(17) 0.5556(21) 0.1923(15) 0.076(8) Uani 1 d . .
H26A H -0.2228(20) 0.5372(53) 0.1852(93) 0.113 Uiso 1 calc R .
H26B H -0.1144(111) 0.6220(52) 0.1607(63) 0.113 Uiso 1 calc R .
H26C H -0.1229(121) 0.5791(95) 0.2421(30) 0.113 Uiso 1 calc R .
C31 C -0.0978(15) 0.8518(15) 0.3415(10) 0.044(4) Uani 1 d . .
H31A H -0.1177(15) 0.8787(15) 0.2924(10) 0.052 Uiso 1 calc R .
H31B H -0.1150(15) 0.7645(15) 0.3443(10) 0.052 Uiso 1 calc R .
C32 C -0.1815(18) 0.9201(30) 0.3953(12) 0.095(11) Uani 1 d . .
H32A H -0.2644(37) 0.9192(176) 0.3771(60) 0.143 Uiso 1 calc R .
H32B H -0.1542(120) 1.0036(58) 0.4004(88) 0.143 Uiso 1 calc R .
H32C H -0.1780(152) 0.8800(116) 0.4419(36) 0.143 Uiso 1 calc R .
C33 C 0.1006(23) 1.0377(18) 0.3521(12) 0.069(7) Uani 1 d . .
H33A H 0.0370(23) 1.0840(18) 0.3766(12) 0.083 Uiso 1 calc R .
H33B H 0.1775(23) 1.0533(18) 0.3775(12) 0.083 Uiso 1 calc R .
C34 C 0.1105(22) 1.0827(23) 0.2764(12) 0.072(6) Uani 1 d . .
H34A H 0.1260(152) 1.1696(35) 0.2769(12) 0.108 Uiso 1 calc R .
H34B H 0.0352(59) 1.0666(141) 0.2506(29) 0.108 Uiso 1 calc R .
H34C H 0.1768(100) 1.0412(111) 0.2527(30) 0.108 Uiso 1 calc R .
C35 C 0.0867(15) 0.8583(14) 0.4551(10) 0.042(4) Uani 1 d . .
H35A H 0.1712(15) 0.8787(14) 0.4669(10) 0.050 Uiso 1 calc R .
H35B H 0.0352(15) 0.9183(14) 0.4792(10) 0.050 Uiso 1 calc R .
C36 C 0.0581(25) 0.7276(19) 0.4889(10) 0.070(7) Uani 1 d . .
H36A H 0.0648(148) 0.7319(42) 0.5411(12) 0.105 Uiso 1 calc R .
H36B H 0.1157(96) 0.6685(36) 0.4708(70) 0.105 Uiso 1 calc R .
H36C H -0.0237(59) 0.7031(68) 0.4753(74) 0.105 Uiso 1 calc R .
C41 C 0.4113(20) 1.0340(18) 0.1446(11) 0.058(5) Uani 1 d . .
H41A H 0.3247(20) 1.0537(18) 0.1478(11) 0.070 Uiso 1 calc R .
H41B H 0.4479(20) 1.0502(18) 0.1921(11) 0.070 Uiso 1 calc R .
C42 C 0.4694(25) 1.1227(18) 0.0896(13) 0.079(8) Uani 1 d . .
H42A H 0.4620(147) 1.2055(22) 0.1070(48) 0.118 Uiso 1 calc R .
H42B H 0.4278(107) 1.1152(119) 0.0434(30) 0.118 Uiso 1 calc R .
H42C H 0.5546(46) 1.1026(103) 0.0839(73) 0.118 Uiso 1 calc R .
C43 C 0.3878(15) 0.8500(17) 0.0344(8) 0.042(4) Uani 1 d . .
H43A H 0.4502(15) 0.8897(17) 0.0053(8) 0.050 Uiso 1 calc R .
H43B H 0.3929(15) 0.7624(17) 0.0249(8) 0.050 Uiso 1 calc R .
C44 C 0.2688(16) 0.8925(22) 0.0088(9) 0.059(6) Uani 1 d . .
H44A H 0.2774(27) 0.9309(124) -0.0380(38) 0.088 Uiso 1 calc R .
H44B H 0.2365(62) 0.9509(102) 0.0429(42) 0.088 Uiso 1 calc R .
H44C H 0.2138(42) 0.8239(28) 0.0047(76) 0.088 Uiso 1 calc R .
C45 C 0.5819(16) 0.8350(22) 0.1325(9) 0.058(6) Uani 1 d . .
H45A H 0.5935(16) 0.7586(22) 0.1062(9) 0.070 Uiso 1 calc R .
H45B H 0.6285(16) 0.8980(22) 0.1075(9) 0.070 Uiso 1 calc R .
C46 C 0.6354(17) 0.8197(20) 0.2076(10) 0.050(5) Uani 1 d . .
H46A H 0.7228(22) 0.8105(129) 0.2045(11) 0.076 Uiso 1 calc R .
H46B H 0.6009(96) 0.7480(74) 0.2301(30) 0.076 Uiso 1 calc R .
H46C H 0.6167(110) 0.8909(59) 0.2364(25) 0.076 Uiso 1 calc R .
Cl10 Cl -0.2187(6) 0.1140(6) 0.1910(3) 0.076(2) Uani 1 d . .
Cl20 Cl -0.2124(5) 0.2673(6) 0.3167(3) 0.0668(14) Uani 1 d . .
C100 C -0.3057(17) 0.1934(20) 0.2538(11) 0.055(5) Uani 1 d . .
H10A H -0.3566(17) 0.2534(20) 0.2287(11) 0.066 Uiso 1 calc R .
H10B H -0.3593(17) 0.1365(20) 0.2789(11) 0.066 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cd 1.40
Cl 0.99
N 0.68
P 1.05
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cd1 N1 89.0(5) . . ?
N3 Cd1 N4 90.1(4) . . ?
N1 Cd1 N4 89.2(4) . . ?
N3 Cd1 Cl1 126.3(4) . . ?
N1 Cd1 Cl1 129.7(3) . . ?
N4 Cd1 Cl1 120.9(3) . . ?
N3 Cd1 Cd4 89.7(3) . . ?
N1 Cd1 Cd4 44.1(3) . . ?
N4 Cd1 Cd4 45.1(3) . . ?
Cl1 Cd1 Cd4 143.67(13) . . ?
N3 Cd1 Cd2 44.7(3) . . ?
N1 Cd1 Cd2 90.2(3) . . ?
N4 Cd1 Cd2 45.5(3) . . ?
Cl1 Cd1 Cd2 140.05(12) . . ?
Cd4 Cd1 Cd2 61.21(3) . . ?
N3 Cd1 Cd3 43.9(4) . . ?
N1 Cd1 Cd3 45.1(3) . . ?
N4 Cd1 Cd3 88.7(3) . . ?
Cl1 Cd1 Cd3 150.33(13) . . ?
Cd4 Cd1 Cd3 59.26(3) . . ?
Cd2 Cd1 Cd3 59.19(3) . . ?
N3 Cd2 N2 91.2(5) . . ?
N3 Cd2 N4 90.1(4) . . ?
N2 Cd2 N4 86.6(4) . . ?
N3 Cd2 Cl2 120.8(3) . . ?
N2 Cd2 Cl2 123.6(3) . . ?
N4 Cd2 Cl2 132.8(3) . . ?
N3 Cd2 Cd3 45.1(4) . . ?
N2 Cd2 Cd3 46.2(3) . . ?
N4 Cd2 Cd3 90.6(3) . . ?
Cl2 Cd2 Cd3 136.63(12) . . ?
N3 Cd2 Cd1 44.3(3) . . ?
N2 Cd2 Cd1 89.9(3) . . ?
N4 Cd2 Cd1 45.8(3) . . ?
Cl2 Cd2 Cd1 145.85(13) . . ?
Cd3 Cd2 Cd1 61.20(3) . . ?
N3 Cd2 Cd4 87.8(3) . . ?
N2 Cd2 Cd4 42.8(3) . . ?
N4 Cd2 Cd4 44.0(3) . . ?
Cl2 Cd2 Cd4 150.82(12) . . ?
Cd3 Cd2 Cd4 59.26(3) . . ?
Cd1 Cd2 Cd4 59.19(3) . . ?
N3 Cd3 N2 89.9(4) . . ?
N3 Cd3 N1 87.0(4) . . ?
N2 Cd3 N1 88.2(4) . . ?
N3 Cd3 Cl3 132.3(3) . . ?
N2 Cd3 Cl3 119.4(4) . . ?
N1 Cd3 Cl3 127.1(3) . . ?
N3 Cd3 Cd4 89.4(3) . . ?
N2 Cd3 Cd4 44.1(3) . . ?
N1 Cd3 Cd4 44.2(3) . . ?
Cl3 Cd3 Cd4 138.09(14) . . ?
N3 Cd3 Cd2 44.9(3) . . ?
N2 Cd3 Cd2 45.1(4) . . ?
N1 Cd3 Cd2 89.5(3) . . ?
Cl3 Cd3 Cd2 142.54(15) . . ?
Cd4 Cd3 Cd2 61.39(3) . . ?
N3 Cd3 Cd1 43.4(3) . . ?
N2 Cd3 Cd1 87.9(3) . . ?
N1 Cd3 Cd1 43.7(3) . . ?
Cl3 Cd3 Cd1 152.48(13) . . ?
Cd4 Cd3 Cd1 59.36(3) . . ?
Cd2 Cd3 Cd1 59.61(4) . . ?
N2 Cd4 N1 92.6(4) . . ?
N2 Cd4 N4 88.3(5) . . ?
N1 Cd4 N4 90.9(4) . . ?
N2 Cd4 Cl4 129.7(4) . . ?
N1 Cd4 Cl4 117.8(3) . . ?
N4 Cd4 Cl4 126.8(3) . . ?
N2 Cd4 Cd3 46.3(3) . . ?
N1 Cd4 Cd3 46.4(3) . . ?
N4 Cd4 Cd3 91.1(2) . . ?
Cl4 Cd4 Cd3 141.55(15) . . ?
N2 Cd4 Cd1 91.1(3) . . ?
N1 Cd4 Cd1 44.8(3) . . ?
N4 Cd4 Cd1 46.1(3) . . ?
Cl4 Cd4 Cd1 139.02(12) . . ?
Cd3 Cd4 Cd1 61.38(3) . . ?
N2 Cd4 Cd2 43.9(4) . . ?
N1 Cd4 Cd2 89.4(3) . . ?
N4 Cd4 Cd2 44.6(3) . . ?
Cl4 Cd4 Cd2 152.72(14) . . ?
Cd3 Cd4 Cd2 59.35(3) . . ?
Cd1 Cd4 Cd2 59.60(4) . . ?
N1 P1 C11 110.4(8) . . ?
N1 P1 C15 112.4(9) . . ?
C11 P1 C15 104.5(10) . . ?
N1 P1 C13 114.5(7) . . ?
C11 P1 C13 106.2(9) . . ?
C15 P1 C13 108.1(11) . . ?
N2 P2 C21 112.3(7) . . ?
N2 P2 C23 112.3(8) . . ?
C21 P2 C23 106.3(9) . . ?
N2 P2 C25 116.1(8) . . ?
C21 P2 C25 104.3(10) . . ?
C23 P2 C25 104.6(10) . . ?
N3 P3 C35 116.4(7) . . ?
N3 P3 C33 114.0(10) . . ?
C35 P3 C33 98.1(9) . . ?
N3 P3 C31 112.0(7) . . ?
C35 P3 C31 105.5(8) . . ?
C33 P3 C31 109.8(9) . . ?
N4 P4 C43 113.8(7) . . ?
N4 P4 C41 111.2(8) . . ?
C43 P4 C41 107.9(10) . . ?
N4 P4 C45 112.3(7) . . ?
C43 P4 C45 103.2(8) . . ?
C41 P4 C45 108.0(11) . . ?
P1 N1 Cd4 128.3(7) . . ?
P1 N1 Cd1 126.2(7) . . ?
Cd4 N1 Cd1 91.1(4) . . ?
P1 N1 Cd3 119.8(7) . . ?
Cd4 N1 Cd3 89.5(4) . . ?
Cd1 N1 Cd3 91.1(4) . . ?
P2 N2 Cd4 127.0(7) . . ?
P2 N2 Cd2 123.5(7) . . ?
Cd4 N2 Cd2 93.3(5) . . ?
P2 N2 Cd3 124.0(7) . . ?
Cd4 N2 Cd3 89.6(4) . . ?
Cd2 N2 Cd3 88.7(4) . . ?
P3 N3 Cd1 120.9(7) . . ?
P3 N3 Cd2 126.0(7) . . ?
Cd1 N3 Cd2 91.1(4) . . ?
P3 N3 Cd3 126.1(7) . . ?
Cd1 N3 Cd3 92.8(5) . . ?
Cd2 N3 Cd3 90.0(5) . . ?
P4 N4 Cd4 121.9(6) . . ?
P4 N4 Cd2 129.3(6) . . ?
Cd4 N4 Cd2 91.5(4) . . ?
P4 N4 Cd1 125.1(6) . . ?
Cd4 N4 Cd1 88.8(4) . . ?
Cd2 N4 Cd1 88.7(3) . . ?
C12 C11 P1 115.3(14) . . ?
C12 C11 H11A 108.4(12) . . ?
P1 C11 H11A 108.4(7) . . ?
C12 C11 H11B 108.4(13) . . ?
P1 C11 H11B 108.4(7) . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5(10) . . ?
C11 C12 H12B 109.5(12) . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5(12) . . ?
H12A C12 H12C 109.47(8) . . ?
H12B C12 H12C 109.47(5) . . ?
C14 C13 P1 113.6(14) . . ?
C14 C13 H13A 108.8(14) . . ?
P1 C13 H13A 108.8(6) . . ?
C14 C13 H13B 108.8(11) . . ?
P1 C13 H13B 108.8(5) . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5(13) . . ?
C13 C14 H14B 109.5(10) . . ?
H14A C14 H14B 109.47(5) . . ?
C13 C14 H14C 109.5(13) . . ?
H14A C14 H14C 109.47(6) . . ?
H14B C14 H14C 109.47(8) . . ?
C16 C15 P1 114.6(17) . . ?
C16 C15 H15A 108.6(22) . . ?
P1 C15 H15A 108.6(9) . . ?
C16 C15 H15B 108.6(17) . . ?
P1 C15 H15B 108.6(7) . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5(13) . . ?
C15 C16 H16B 109.5(21) . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5(19) . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C22 C21 P2 112.5(14) . . ?
C22 C21 H21A 109.1(11) . . ?
P2 C21 H21A 109.1(5) . . ?
C22 C21 H21B 109.1(13) . . ?
P2 C21 H21B 109.1(6) . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5(12) . . ?
C21 C22 H22B 109.5(13) . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5(11) . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.47(6) . . ?
C24 C23 P2 115.1(16) . . ?
C24 C23 H23A 108.5(14) . . ?
P2 C23 H23A 108.5(7) . . ?
C24 C23 H23B 108.5(12) . . ?
P2 C23 H23B 108.5(7) . . ?
H23A C23 H23B 107.5 . . ?
C23 C24 H24A 109.5(12) . . ?
C23 C24 H24B 109.5(14) . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5(14) . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 P2 114.0(15) . . ?
C26 C25 H25A 108.7(13) . . ?
P2 C25 H25A 108.8(7) . . ?
C26 C25 H25B 108.8(15) . . ?
P2 C25 H25B 108.8(8) . . ?
H25A C25 H25B 107.6 . . ?
C25 C26 H26A 109.5(11) . . ?
C25 C26 H26B 109.5(14) . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5(15) . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C31 P3 113.9(13) . . ?
C32 C31 H31A 108.8(12) . . ?
P3 C31 H31A 108.8(6) . . ?
C32 C31 H31B 108.8(14) . . ?
P3 C31 H31B 108.8(5) . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5(10) . . ?
C31 C32 H32B 109.5(14) . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5(13) . . ?
H32A C32 H32C 109.47(14) . . ?
H32B C32 H32C 109.47(10) . . ?
C34 C33 P3 113.6(15) . . ?
C34 C33 H33A 108.8(13) . . ?
P3 C33 H33A 108.8(8) . . ?
C34 C33 H33B 108.8(13) . . ?
P3 C33 H33B 108.8(7) . . ?
H33A C33 H33B 107.7 . . ?
C33 C34 H34A 109.5(12) . . ?
C33 C34 H34B 109.5(13) . . ?
H34A C34 H34B 109.47(5) . . ?
C33 C34 H34C 109.5(13) . . ?
H34A C34 H34C 109.47(10) . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 P3 117.4(12) . . ?
C36 C35 H35A 108.0(12) . . ?
P3 C35 H35A 108.0(5) . . ?
C36 C35 H35B 108.0(9) . . ?
P3 C35 H35B 108.0(5) . . ?
H35A C35 H35B 107.2 . . ?
C35 C36 H36A 109.5(10) . . ?
C35 C36 H36B 109.5(10) . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5(12) . . ?
H36A C36 H36C 109.47(8) . . ?
H36B C36 H36C 109.5 . . ?
C42 C41 P4 117.4(14) . . ?
C42 C41 H41A 107.9(13) . . ?
P4 C41 H41A 107.9(7) . . ?
C42 C41 H41B 108.0(13) . . ?
P4 C41 H41B 108.0(8) . . ?
H41A C41 H41B 107.2 . . ?
C41 C42 H42A 109.5(11) . . ?
C41 C42 H42B 109.5(13) . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5(13) . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 P4 117.1(13) . . ?
C44 C43 H43A 108.0(9) . . ?
P4 C43 H43A 108.0(5) . . ?
C44 C43 H43B 108.0(12) . . ?
P4 C43 H43B 108.0(6) . . ?
H43A C43 H43B 107.3 . . ?
C43 C44 H44A 109.5(9) . . ?
C43 C44 H44B 109.5(11) . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5(12) . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 P4 116.5(13) . . ?
C46 C45 H45A 108.2(13) . . ?
P4 C45 H45A 108.2(8) . . ?
C46 C45 H45B 108.2(11) . . ?
P4 C45 H45B 108.2(6) . . ?
H45A C45 H45B 107.3 . . ?
C45 C46 H46A 109.5(10) . . ?
C45 C46 H46B 109.5(11) . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5(13) . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Cl20 C100 Cl10 110.8(10) . . ?
Cl20 C100 H10A 109.5(8) . . ?
Cl10 C100 H10A 109.5(8) . . ?
Cl20 C100 H10B 109.5(7) . . ?
Cl10 C100 H10B 109.5(7) . . ?
H10A C100 H10B 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N3 2.253(11) . ?
Cd1 N1 2.266(11) . ?
Cd1 N4 2.315(10) . ?
Cd1 Cl1 2.400(4) . ?
Cd1 Cd4 3.213(2) . ?
Cd1 Cd2 3.227(2) . ?
Cd1 Cd3 3.278(2) . ?
Cd2 N3 2.269(11) . ?
Cd2 N2 2.277(15) . ?
Cd2 N4 2.301(11) . ?
Cd2 Cl2 2.396(4) . ?
Cd2 Cd3 3.2129(15) . ?
Cd2 Cd4 3.279(2) . ?
Cd3 N3 2.27(2) . ?
Cd3 N2 2.321(11) . ?
Cd3 N1 2.324(13) . ?
Cd3 Cl3 2.384(5) . ?
Cd3 Cd4 3.210(2) . ?
Cd4 N2 2.233(11) . ?
Cd4 N1 2.236(13) . ?
Cd4 N4 2.277(10) . ?
Cd4 Cl4 2.401(4) . ?
P1 N1 1.596(12) . ?
P1 C11 1.82(2) . ?
P1 C15 1.84(2) . ?
P1 C13 1.865(15) . ?
P2 N2 1.582(13) . ?
P2 C21 1.74(2) . ?
P2 C23 1.83(2) . ?
P2 C25 1.85(2) . ?
P3 N3 1.595(12) . ?
P3 C35 1.82(2) . ?
P3 C33 1.82(2) . ?
P3 C31 1.84(2) . ?
P4 N4 1.568(10) . ?
P4 C43 1.78(2) . ?
P4 C41 1.79(2) . ?
P4 C45 1.79(2) . ?
C11 C12 1.56(2) . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C12 H12A 0.9700(13) . ?
C12 H12B 0.97 . ?
C12 H12C 0.97 . ?
C13 C14 1.39(3) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C14 H14A 0.97 . ?
C14 H14B 0.97 . ?
C14 H14C 0.97 . ?
C15 C16 1.46(3) . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C16 H16A 0.97 . ?
C16 H16B 0.97 . ?
C16 H16C 0.97 . ?
C21 C22 1.58(3) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C22 H22C 0.97 . ?
C23 C24 1.52(2) . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
C24 H24C 0.97 . ?
C25 C26 1.46(3) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C26 H26A 0.97 . ?
C26 H26B 0.97 . ?
C26 H26C 0.97 . ?
C31 C32 1.56(2) . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C32 H32A 0.97 . ?
C32 H32B 0.9700(13) . ?
C32 H32C 0.97 . ?
C33 C34 1.49(3) . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C34 H34A 0.97 . ?
C34 H34B 0.97 . ?
C34 H34C 0.9700(12) . ?
C35 C36 1.60(3) . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C36 H36A 0.97 . ?
C36 H36B 0.97 . ?
C36 H36C 0.97 . ?
C41 C42 1.55(3) . ?
C41 H41A 0.98 . ?
C41 H41B 0.98 . ?
C42 H42A 0.97 . ?
C42 H42B 0.97 . ?
C42 H42C 0.9700(15) . ?
C43 C44 1.46(3) . ?
C43 H43A 0.98 . ?
C43 H43B 0.98 . ?
C44 H44A 0.97 . ?
C44 H44B 0.97 . ?
C44 H44C 0.97 . ?
C45 C46 1.52(2) . ?
C45 H45A 0.98 . ?
C45 H45B 0.98 . ?
C46 H46A 0.97 . ?
C46 H46B 0.97 . ?
C46 H46C 0.97 . ?
Cl10 C100 1.75(2) . ?
Cl20 C100 1.75(2) . ?
C100 H10A 0.98 . ?
C100 H10B 0.98 . ?
|
1100601.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 22:03:05 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177996 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100601.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100601
loop_
_publ_author_name
'Harms, Klaus'
'Merle, Jan'
'Maichle-M\"ossmer, C\"acili\"a'
'Massa, Werner'
'Krieger, Matthias'
_publ_section_title
;
Heterocubane Phosphoraniminato Complexes of Cadmium
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 1099
_journal_page_last 1104
_journal_paper_doi 10.1021/ic9710364
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C38 H76 Br4 Cd4 N4 P4'
_chemical_formula_weight 1482.15
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 116.654(12)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 21.601(3)
_cell_length_b 11.942(2)
_cell_length_c 23.550(3)
_cell_measurement_reflns_used 41
_cell_measurement_temperature 213(2)
_cell_measurement_theta_max 14
_cell_measurement_theta_min 10
_cell_volume 5429.4(14)
_diffrn_ambient_temperature 213(2)
_diffrn_radiation_wavelength 0.71073
_refine_ls_extinction_coef 0.00012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_all 1.021
_refine_ls_goodness_of_fit_obs 1.142
_refine_ls_hydrogen_treatment noref
_refine_ls_matrix_type full
_refine_ls_number_parameters 479
_refine_ls_number_reflns 6223
_refine_ls_number_restraints 28
_refine_ls_restrained_S_all 1.022
_refine_ls_restrained_S_obs 1.141
_refine_ls_R_factor_all 0.1536
_refine_ls_R_factor_obs 0.0654
_refine_ls_shift/esd_max 0.001
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.1138
_refine_ls_wR_factor_obs 0.0912
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100601
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0337(8) 0.0311(8) 0.0385(8) 0.0003(7) 0.0163(6) 0.0032(7)
Cd2 0.0400(8) 0.0350(8) 0.0381(8) -0.0011(7) 0.0208(6) -0.0023(7)
Cd3 0.0392(8) 0.0287(9) 0.0430(8) 0.0029(7) 0.0202(7) 0.0013(7)
Cd4 0.0334(7) 0.0365(8) 0.0352(8) 0.0021(7) 0.0143(6) -0.0005(7)
Br1 0.0593(14) 0.0764(18) 0.0852(16) 0.0012(14) 0.0336(13) 0.0312(13)
Br2 0.0884(16) 0.0712(16) 0.0541(13) -0.0100(12) 0.0478(12) -0.0196(14)
Br3 0.0810(16) 0.0360(13) 0.1084(18) 0.0107(13) 0.0582(14) -0.0012(12)
Br4 0.0510(13) 0.0840(18) 0.0477(12) 0.0084(13) -0.0004(10) -0.0194(13)
P1 0.045(3) 0.044(4) 0.042(3) -0.004(3) 0.020(3) -0.008(3)
P2 0.045(3) 0.028(3) 0.036(3) 0.003(2) 0.014(2) -0.004(3)
P3 0.039(3) 0.042(3) 0.057(3) -0.001(3) 0.025(3) 0.006(3)
P4 0.035(3) 0.047(3) 0.038(3) 0.000(3) 0.019(2) 0.002(3)
N1 0.029(8) 0.030(9) 0.035(8) -0.002(7) 0.011(7) -0.009(7)
N2 0.044(9) 0.030(9) 0.035(8) 0.009(7) 0.022(7) -0.001(8)
N3 0.020(7) 0.028(9) 0.051(9) 0.000(7) 0.024(7) 0.011(7)
N4 0.028(7) 0.027(8) 0.037(8) 0.001(7) 0.022(7) 0.005(7)
C11 0.089(17) 0.086(19) 0.049(14) 0.014(14) -0.025(12) -0.047(16)
C12 0.25(4) 0.06(2) 0.11(2) 0.039(18) -0.06(2) -0.04(2)
C13 0.033(10) 0.132(17) 0.053(12) 0.002(12) 0.011(9) -0.045(12)
C14 0.065(15) 0.17(3) 0.050(13) 0.028(15) 0.001(12) -0.064(16)
C15 0.072(19) 0.14(3) 0.14(2) -0.10(2) -0.002(17) -0.018(19)
C16_a 0.10(3) 0.20(5) 0.03(2) -0.06(4) 0.02(3) -0.02(3)
C161_b 0.10(3) 0.20(5) 0.03(2) -0.06(4) 0.02(3) -0.02(3)
C21 0.16(2) 0.023(13) 0.15(2) -0.024(15) 0.10(2) -0.010(15)
C22 0.13(2) 0.048(14) 0.054(13) -0.002(12) 0.041(14) 0.012(14)
C23 0.099(16) 0.037(13) 0.055(13) 0.037(11) -0.016(12) -0.006(12)
C24 0.12(2) 0.048(15) 0.101(17) 0.050(14) 0.002(15) -0.023(14)
C25 0.081(16) 0.079(18) 0.090(17) 0.017(14) 0.048(14) -0.029(14)
C26 0.068(14) 0.054(15) 0.092(16) -0.009(13) 0.061(13) 0.005(12)
C31 0.032(11) 0.080(16) 0.071(14) 0.037(13) 0.018(11) 0.034(11)
C32 0.102(19) 0.15(3) 0.082(17) 0.058(17) 0.044(15) 0.067(19)
C33 0.052(12) 0.049(14) 0.090(15) -0.006(12) 0.039(12) 0.009(11)
C34 0.050(13) 0.082(17) 0.092(16) 0.010(13) 0.036(12) 0.005(12)
C35 0.088(16) 0.036(13) 0.067(14) -0.010(11) 0.031(13) 0.029(12)
C36 0.15(3) 0.09(2) 0.12(2) -0.019(18) 0.04(2) 0.003(19)
C41 0.046(11) 0.079(15) 0.040(11) -0.002(12) 0.027(9) 0.003(12)
C42 0.050(12) 0.072(16) 0.047(12) 0.014(11) 0.023(10) -0.008(12)
C43 0.052(12) 0.058(13) 0.042(11) 0.014(10) 0.033(10) 0.021(11)
C44 0.037(12) 0.083(17) 0.094(16) 0.054(14) 0.006(11) 0.022(12)
C45 0.054(12) 0.043(13) 0.050(12) -0.005(10) 0.027(10) -0.014(10)
C46 0.071(14) 0.080(17) 0.083(15) -0.013(14) 0.051(12) 0.003(13)
C50 0.073(18) 0.08(2) 0.08(2) -0.036(17) 0.012(16) -0.002(18)
C51 0.062(17) 0.070(19) 0.11(2) -0.016(17) 0.014(16) 0.018(16)
C52 0.11(2) 0.08(2) 0.10(2) 0.046(17) 0.048(18) 0.023(18)
C53 0.17(3) 0.09(3) 0.12(3) -0.03(2) 0.07(3) 0.02(3)
C54 0.13(3) 0.17(4) 0.08(2) 0.02(2) 0.02(2) 0.06(3)
C55 0.13(3) 0.063(19) 0.10(2) 0.022(17) 0.049(19) 0.004(19)
C56 0.10(2) 0.09(2) 0.12(2) 0.009(16) 0.032(17) -0.018(16)
C60 0.10(3) 0.26(4) 0.12(3) -0.02(2) 0.01(2) 0.08(2)
C61 0.11(3) 0.22(3) 0.13(3) -0.04(3) -0.002(17) 0.079(18)
C62 0.20(3) 0.16(3) 0.13(3) 0.05(2) 0.04(2) 0.12(2)
C63 0.21(5) 0.27(6) 0.13(3) -0.02(2) 0.03(3) 0.13(3)
C64 0.20(4) 0.16(3) 0.09(2) 0.01(2) -0.051(19) 0.13(2)
C65 0.082(18) 0.23(3) 0.13(3) 0.01(2) -0.058(18) 0.081(18)
C66 0.24(3) 0.42(5) 0.19(3) -0.02(3) 0.11(2) 0.11(3)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd1 Cd 0.69577(6) -0.35876(10) 0.37327(5) 0.0344(4) Uani 1 d . .
Cd2 Cd 0.60730(6) -0.25734(11) 0.44150(5) 0.0365(4) Uani 1 d . .
Cd3 Cd 0.64130(6) -0.10556(10) 0.34659(6) 0.0363(4) Uani 1 d . .
Cd4 Cd 0.53360(6) -0.31367(10) 0.29186(5) 0.0354(4) Uani 1 d . .
Br1 Br 0.79275(10) -0.47801(19) 0.37861(10) 0.0732(7) Uani 1 d . .
Br2 Br 0.58963(11) -0.26004(18) 0.53971(8) 0.0653(6) Uani 1 d . .
Br3 Br 0.67698(11) 0.09022(16) 0.33863(10) 0.0692(7) Uani 1 d . .
Br4 Br 0.42714(10) -0.40020(19) 0.20604(9) 0.0693(7) Uani 1 d . .
P1 P 0.7759(2) -0.1721(4) 0.4923(2) 0.0436(14) Uani 1 d . .
P2 P 0.5849(2) -0.5327(4) 0.3977(2) 0.0381(13) Uani 1 d . .
P3 P 0.4799(2) -0.0797(4) 0.3390(2) 0.0448(14) Uani 1 d . .
P4 P 0.6391(2) -0.2565(4) 0.2222(2) 0.0386(12) Uani 1 d . .
N1 N 0.7043(6) -0.2103(10) 0.4344(5) 0.033(4) Uani 1 d . .
N2 N 0.6000(6) -0.4103(10) 0.3816(5) 0.035(4) Uani 1 d . .
N3 N 0.5435(5) -0.1585(10) 0.3517(5) 0.030(3) Uani 1 d . .
N4 N 0.6289(5) -0.2573(10) 0.2855(5) 0.028(3) Uani 1 d . .
C11 C 0.8121(11) -0.2701(18) 0.5565(8) 0.096(9) Uani 1 d . .
H11A H 0.8609 -0.2495 0.5810 0.115 Uiso 1 calc R .
H11B H 0.7898 -0.2550 0.5839 0.115 Uiso 1 calc R .
C12 C 0.8108(14) -0.379(2) 0.5493(11) 0.191(18) Uani 1 d . .
H12A H 0.7832 -0.4129 0.5678 0.286 Uiso 1 calc R .
H12B H 0.8577 -0.4085 0.5704 0.286 Uiso 1 calc R .
H12C H 0.7906 -0.3974 0.5044 0.286 Uiso 1 calc R .
C13 C 0.8419(8) -0.1499(18) 0.4668(7) 0.076(7) Uani 1 d U .
H13A H 0.8471 -0.2194 0.4472 0.091 Uiso 1 calc R .
H13B H 0.8253 -0.0924 0.4336 0.091 Uiso 1 calc R .
C14 C 0.9130(8) -0.1151(18) 0.5170(8) 0.105(9) Uani 1 d . .
H14A H 0.9440 -0.1063 0.4976 0.157 Uiso 1 calc R .
H14B H 0.9312 -0.1721 0.5498 0.157 Uiso 1 calc R .
H14C H 0.9095 -0.0446 0.5358 0.157 Uiso 1 calc R .
C15 C 0.7710(12) -0.039(2) 0.5253(12) 0.134(12) Uani 1 d . .
H15A_a H 0.8027 -0.0463 0.5706 0.161 Uiso 0.50 calc PR 1
H15B_a H 0.7942 0.0126 0.5085 0.161 Uiso 0.50 calc PR 1
H15C_b H 0.8174 -0.0083 0.5467 0.161 Uiso 0.50 d PR 2
H15D_b H 0.7449 0.0099 0.4895 0.161 Uiso 0.50 d PR 2
C16_a C 0.721(3) 0.020(7) 0.525(2) 0.115(18) Uani 0.41 d P 1
H16A_a H 0.6938 0.0494 0.4823 0.173 Uiso 0.41 calc PR 1
H16B_a H 0.7395 0.0810 0.5546 0.173 Uiso 0.41 calc PR 1
H16C_a H 0.6921 -0.0272 0.5365 0.173 Uiso 0.41 calc PR 1
C161_b C 0.742(2) -0.027(5) 0.5679(14) 0.115(18) Uani 0.59 d P 2
H16D_b H 0.7266 0.0493 0.5669 0.173 Uiso 0.59 calc PR 2
H16E_b H 0.7768 -0.0454 0.6105 0.173 Uiso 0.59 calc PR 2
H16F_b H 0.7031 -0.0777 0.5556 0.173 Uiso 0.59 calc PR 2
C21 C 0.6123(12) -0.6407(15) 0.3598(10) 0.098(8) Uani 1 d . .
H21A H 0.6631 -0.6417 0.3799 0.118 Uiso 1 calc R .
H21B H 0.5969 -0.7133 0.3683 0.118 Uiso 1 calc R .
C22 C 0.5870(10) -0.6298(15) 0.2903(8) 0.078(7) Uani 1 d . .
H22A H 0.6048 -0.6912 0.2750 0.117 Uiso 1 calc R .
H22B H 0.6028 -0.5593 0.2810 0.117 Uiso 1 calc R .
H22C H 0.5368 -0.6317 0.2694 0.117 Uiso 1 calc R .
C23 C 0.6336(10) -0.5652(14) 0.4806(8) 0.083(8) Uani 1 d . .
H23A H 0.6829 -0.5560 0.4923 0.099 Uiso 1 calc R .
H23B H 0.6217 -0.5102 0.5050 0.099 Uiso 1 calc R .
C24 C 0.6227(10) -0.6836(15) 0.5010(9) 0.107(9) Uani 1 d . .
H24A H 0.6503 -0.6919 0.5466 0.161 Uiso 1 calc R .
H24B H 0.6367 -0.7393 0.4791 0.161 Uiso 1 calc R .
H24C H 0.5741 -0.6940 0.4903 0.161 Uiso 1 calc R .
C25 C 0.4951(9) -0.5580(17) 0.3768(9) 0.080(7) Uani 1 d . .
H25A H 0.4698 -0.5645 0.3305 0.096 Uiso 1 calc R .
H25B H 0.4916 -0.6305 0.3947 0.096 Uiso 1 calc R .
C26 C 0.4600(9) -0.4747(14) 0.3973(8) 0.062(6) Uani 1 d . .
H26A H 0.4122 -0.4967 0.3832 0.092 Uiso 1 calc R .
H26B H 0.4616 -0.4025 0.3791 0.092 Uiso 1 calc R .
H26C H 0.4830 -0.4693 0.4433 0.092 Uiso 1 calc R .
C31 C 0.4316(8) -0.0335(16) 0.2590(8) 0.063(6) Uani 1 d . .
H31A H 0.4159 -0.0993 0.2313 0.076 Uiso 1 calc R .
H31B H 0.3903 0.0063 0.2555 0.076 Uiso 1 calc R .
C32 C 0.4713(10) 0.0428(19) 0.2354(9) 0.111(9) Uani 1 d . .
H32A H 0.4419 0.0635 0.1916 0.166 Uiso 1 calc R .
H32B H 0.5120 0.0039 0.2381 0.166 Uiso 1 calc R .
H32C H 0.4855 0.1097 0.2615 0.166 Uiso 1 calc R .
C33 C 0.4178(8) -0.1491(15) 0.3589(8) 0.061(6) Uani 1 d . .
H33A H 0.3978 -0.2118 0.3295 0.073 Uiso 1 calc R .
H33B H 0.4429 -0.1807 0.4017 0.073 Uiso 1 calc R .
C34 C 0.3585(8) -0.0784(16) 0.3576(8) 0.073(7) Uani 1 d . .
H34A H 0.3289 -0.1245 0.3690 0.110 Uiso 1 calc R .
H34B H 0.3317 -0.0484 0.3152 0.110 Uiso 1 calc R .
H34C H 0.3771 -0.0172 0.3876 0.110 Uiso 1 calc R .
C35 C 0.5040(9) 0.0493(14) 0.3836(8) 0.065(6) Uani 1 d . .
H35A H 0.5298 0.0960 0.3673 0.078 Uiso 1 calc R .
H35B H 0.4619 0.0900 0.3768 0.078 Uiso 1 calc R .
C36 C 0.5470(12) 0.0319(18) 0.4529(10) 0.127(10) Uani 1 d . .
H36A H 0.5588 0.1038 0.4742 0.190 Uiso 1 calc R .
H36B H 0.5891 -0.0076 0.4600 0.190 Uiso 1 calc R .
H36C H 0.5212 -0.0121 0.4697 0.190 Uiso 1 calc R .
C41 C 0.7268(8) -0.2472(16) 0.2352(7) 0.053(5) Uani 1 d . .
H41A H 0.7503 -0.3177 0.2539 0.063 Uiso 1 calc R .
H41B H 0.7273 -0.2385 0.1940 0.063 Uiso 1 calc R .
C42 C 0.7678(8) -0.1506(15) 0.2785(7) 0.056(6) Uani 1 d . .
H42A H 0.8149 -0.1518 0.2837 0.084 Uiso 1 calc R .
H42B H 0.7682 -0.1588 0.3197 0.084 Uiso 1 calc R .
H42C H 0.7461 -0.0800 0.2596 0.084 Uiso 1 calc R .
C43 C 0.5953(8) -0.1460(14) 0.1699(7) 0.046(5) Uani 1 d . .
H43A H 0.6117 -0.0750 0.1927 0.055 Uiso 1 calc R .
H43B H 0.6080 -0.1467 0.1348 0.055 Uiso 1 calc R .
C44 C 0.5172(8) -0.1495(16) 0.1424(8) 0.080(7) Uani 1 d . .
H44A H 0.4975 -0.0856 0.1146 0.120 Uiso 1 calc R .
H44B H 0.5038 -0.1471 0.1766 0.120 Uiso 1 calc R .
H44C H 0.5001 -0.2181 0.1183 0.120 Uiso 1 calc R .
C45 C 0.6060(8) -0.3848(13) 0.1784(7) 0.047(5) Uani 1 d . .
H45A H 0.6292 -0.4479 0.2066 0.057 Uiso 1 calc R .
H45B H 0.5565 -0.3901 0.1671 0.057 Uiso 1 calc R .
C46 C 0.6147(9) -0.3980(16) 0.1169(8) 0.072(6) Uani 1 d . .
H46A H 0.5962 -0.4699 0.0975 0.108 Uiso 1 calc R .
H46B H 0.6635 -0.3940 0.1273 0.108 Uiso 1 calc R .
H46C H 0.5899 -0.3385 0.0875 0.108 Uiso 1 calc R .
C50 C 0.9053(13) 0.279(2) 0.5390(12) 0.087(8) Uani 1 d . .
C51 C 0.9407(13) 0.362(2) 0.5252(11) 0.090(8) Uani 1 d . .
H51A H 0.9162 0.4147 0.4935 0.108 Uiso 1 calc R .
C52 C 1.0130(14) 0.367(2) 0.5583(12) 0.098(9) Uani 1 d . .
H52A H 1.0383 0.4224 0.5490 0.117 Uiso 1 calc R .
C53 C 1.0454(19) 0.289(3) 0.6048(16) 0.122(12) Uani 1 d . .
H53A H 1.0940 0.2914 0.6278 0.147 Uiso 1 calc R .
C54 C 1.0124(18) 0.210(3) 0.6188(14) 0.135(14) Uani 1 d . .
H54A H 1.0372 0.1583 0.6512 0.163 Uiso 1 calc R .
C55 C 0.9407(17) 0.203(2) 0.5860(13) 0.099(9) Uani 1 d . .
H55 H 0.9168 0.1466 0.5960 0.118 Uiso 1 calc R .
C56 C 0.8273(11) 0.2772(18) 0.5017(10) 0.109(9) Uani 1 d . .
H56A H 0.8105 0.3530 0.4895 0.163 Uiso 0.50 calc PR .
H56B H 0.8074 0.2459 0.5278 0.163 Uiso 0.50 calc PR .
H56C H 0.8140 0.2317 0.4639 0.163 Uiso 0.50 calc PR .
H56D H 0.8108 0.2007 0.4980 0.163 Uiso 0.50 calc PR .
H56E H 0.8139 0.3079 0.4597 0.163 Uiso 0.50 calc PR .
H56F H 0.8072 0.3220 0.5236 0.163 Uiso 0.50 calc PR .
C60 C 0.2685(12) -0.792(3) 0.2564(8) 0.178(15) Uani 1 d GDU .
C61 C 0.3165(11) -0.7237(15) 0.2497(10) 0.172(13) Uani 1 d GU .
H61A H 0.3381 -0.6644 0.2794 0.206 Uiso 1 d G .
C62 C 0.3331(9) -0.7407(19) 0.2000(13) 0.172(12) Uani 1 d GU .
H62A H 0.3663 -0.6932 0.1954 0.207 Uiso 1 d G .
C63 C 0.3018(12) -0.827(2) 0.1570(8) 0.22(2) Uani 1 d GU .
H63A H 0.3133 -0.8384 0.1226 0.265 Uiso 1 d G .
C64 C 0.2538(11) -0.8954(14) 0.1636(10) 0.195(18) Uani 1 d GU .
H64A H 0.2321 -0.9547 0.1339 0.234 Uiso 1 d G .
C65 C 0.2371(8) -0.878(2) 0.2134(13) 0.187(12) Uani 1 d GU .
H65A H 0.2040 -0.9259 0.2180 0.224 Uiso 1 d G .
C66 C 0.2469(16) -0.756(3) 0.3029(13) 0.284(19) Uani 1 d DU .
H66A H 0.2862 -0.7573 0.3447 0.425 Uiso 0.50 calc PR .
H66B H 0.2111 -0.8057 0.3023 0.425 Uiso 0.50 calc PR .
H66C H 0.2288 -0.6804 0.2930 0.425 Uiso 0.50 calc PR .
H66D H 0.1978 -0.7383 0.2820 0.425 Uiso 0.50 calc PR .
H66E H 0.2729 -0.6899 0.3244 0.425 Uiso 0.50 calc PR .
H66F H 0.2553 -0.8152 0.3337 0.425 Uiso 0.50 calc PR .
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Br 1.21
Cd 1.39
N 0.68
P 1.05
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N2 88.6(4) . . ?
N1 Cd1 N4 89.9(4) . . ?
N2 Cd1 N4 89.5(4) . . ?
N1 Cd1 Br1 126.6(3) . . ?
N2 Cd1 Br1 128.7(3) . . ?
N4 Cd1 Br1 122.0(3) . . ?
N1 Cd1 Cd4 90.2(3) . . ?
N2 Cd1 Cd4 45.2(3) . . ?
N4 Cd1 Cd4 44.3(3) . . ?
Br1 Cd1 Cd4 142.93(7) . . ?
N1 Cd1 Cd3 45.2(3) . . ?
N2 Cd1 Cd3 90.2(3) . . ?
N4 Cd1 Cd3 44.7(3) . . ?
Br1 Cd1 Cd3 140.97(8) . . ?
Cd4 Cd1 Cd3 61.04(4) . . ?
N1 Cd1 Cd2 44.0(3) . . ?
N2 Cd1 Cd2 44.6(3) . . ?
N4 Cd1 Cd2 88.6(3) . . ?
Br1 Cd1 Cd2 149.41(7) . . ?
Cd4 Cd1 Cd2 60.12(4) . . ?
Cd3 Cd1 Cd2 59.80(4) . . ?
N1 Cd2 N3 89.9(4) . . ?
N1 Cd2 N2 87.8(4) . . ?
N3 Cd2 N2 89.8(4) . . ?
N1 Cd2 Br2 127.2(3) . . ?
N3 Cd2 Br2 125.9(3) . . ?
N2 Cd2 Br2 124.5(3) . . ?
N1 Cd2 Cd3 45.1(3) . . ?
N3 Cd2 Cd3 44.8(3) . . ?
N2 Cd2 Cd3 89.7(3) . . ?
Br2 Cd2 Cd3 145.79(7) . . ?
N1 Cd2 Cd4 89.4(3) . . ?
N3 Cd2 Cd4 45.1(3) . . ?
N2 Cd2 Cd4 44.7(3) . . ?
Br2 Cd2 Cd4 143.28(7) . . ?
Cd3 Cd2 Cd4 60.72(4) . . ?
N1 Cd2 Cd1 43.8(3) . . ?
N3 Cd2 Cd1 88.8(3) . . ?
N2 Cd2 Cd1 44.1(3) . . ?
Br2 Cd2 Cd1 145.28(7) . . ?
Cd3 Cd2 Cd1 59.63(4) . . ?
Cd4 Cd2 Cd1 59.35(4) . . ?
N4 Cd3 N3 87.9(4) . . ?
N4 Cd3 N1 89.4(4) . . ?
N3 Cd3 N1 89.5(4) . . ?
N4 Cd3 Br3 131.2(3) . . ?
N3 Cd3 Br3 126.4(3) . . ?
N1 Cd3 Br3 120.3(3) . . ?
N4 Cd3 Cd1 45.1(3) . . ?
N3 Cd3 Cd1 89.8(3) . . ?
N1 Cd3 Cd1 44.3(3) . . ?
Br3 Cd3 Cd1 143.20(7) . . ?
N4 Cd3 Cd2 89.5(3) . . ?
N3 Cd3 Cd2 45.0(3) . . ?
N1 Cd3 Cd2 44.5(3) . . ?
Br3 Cd3 Cd2 139.17(7) . . ?
Cd1 Cd3 Cd2 60.58(4) . . ?
N4 Cd3 Cd4 43.3(3) . . ?
N3 Cd3 Cd4 44.5(3) . . ?
N1 Cd3 Cd4 88.3(3) . . ?
Br3 Cd3 Cd4 151.31(7) . . ?
Cd1 Cd3 Cd4 59.37(4) . . ?
Cd2 Cd3 Cd4 59.82(4) . . ?
N4 Cd4 N2 90.0(4) . . ?
N4 Cd4 N3 87.9(4) . . ?
N2 Cd4 N3 89.6(4) . . ?
N4 Cd4 Br4 127.6(3) . . ?
N2 Cd4 Br4 120.7(3) . . ?
N3 Cd4 Br4 129.2(3) . . ?
N4 Cd4 Cd1 45.2(3) . . ?
N2 Cd4 Cd1 44.8(3) . . ?
N3 Cd4 Cd1 89.6(3) . . ?
Br4 Cd4 Cd1 141.01(7) . . ?
N4 Cd4 Cd2 89.6(3) . . ?
N2 Cd4 Cd2 44.8(3) . . ?
N3 Cd4 Cd2 44.8(3) . . ?
Br4 Cd4 Cd2 142.52(7) . . ?
Cd1 Cd4 Cd2 60.53(4) . . ?
N4 Cd4 Cd3 43.8(3) . . ?
N2 Cd4 Cd3 88.8(3) . . ?
N3 Cd4 Cd3 44.1(3) . . ?
Br4 Cd4 Cd3 150.52(7) . . ?
Cd1 Cd4 Cd3 59.59(4) . . ?
Cd2 Cd4 Cd3 59.46(4) . . ?
N1 P1 C11 114.9(8) . . ?
N1 P1 C15 113.5(9) . . ?
C11 P1 C15 107.7(12) . . ?
N1 P1 C13 111.4(7) . . ?
C11 P1 C13 105.5(10) . . ?
C15 P1 C13 102.9(11) . . ?
N2 P2 C23 112.2(7) . . ?
N2 P2 C25 113.8(8) . . ?
C23 P2 C25 107.1(9) . . ?
N2 P2 C21 113.1(8) . . ?
C23 P2 C21 102.7(10) . . ?
C25 P2 C21 107.2(10) . . ?
N3 P3 C31 115.7(7) . . ?
N3 P3 C35 113.5(7) . . ?
C31 P3 C35 103.3(9) . . ?
N3 P3 C33 111.1(7) . . ?
C31 P3 C33 105.3(8) . . ?
C35 P3 C33 107.1(9) . . ?
N4 P4 C43 113.6(7) . . ?
N4 P4 C41 114.9(7) . . ?
C43 P4 C41 105.6(8) . . ?
N4 P4 C45 109.9(7) . . ?
C43 P4 C45 106.6(7) . . ?
C41 P4 C45 105.6(8) . . ?
P1 N1 Cd1 122.9(7) . . ?
P1 N1 Cd2 125.7(6) . . ?
Cd1 N1 Cd2 92.2(4) . . ?
P1 N1 Cd3 125.0(6) . . ?
Cd1 N1 Cd3 90.5(4) . . ?
Cd2 N1 Cd3 90.4(4) . . ?
P2 N2 Cd1 124.8(7) . . ?
P2 N2 Cd4 125.6(7) . . ?
Cd1 N2 Cd4 90.1(4) . . ?
P2 N2 Cd2 124.0(6) . . ?
Cd1 N2 Cd2 91.4(4) . . ?
Cd4 N2 Cd2 90.5(4) . . ?
P3 N3 Cd3 125.3(7) . . ?
P3 N3 Cd2 126.9(6) . . ?
Cd3 N3 Cd2 90.2(4) . . ?
P3 N3 Cd4 122.4(6) . . ?
Cd3 N3 Cd4 91.4(4) . . ?
Cd2 N3 Cd4 90.1(4) . . ?
P4 N4 Cd4 125.5(6) . . ?
P4 N4 Cd3 124.2(7) . . ?
Cd4 N4 Cd3 92.8(4) . . ?
P4 N4 Cd1 123.6(6) . . ?
Cd4 N4 Cd1 90.5(4) . . ?
Cd3 N4 Cd1 90.2(4) . . ?
C12 C11 P1 124.4(18) . . ?
C14 C13 P1 117.2(12) . . ?
C16_a C15 P1 134(4) . . ?
C161_b C15 P1 122(3) . . ?
C22 C21 P2 116.2(15) . . ?
C24 C23 P2 116.1(13) . . ?
C26 C25 P2 116.8(14) . . ?
C32 C31 P3 114.4(13) . . ?
C34 C33 P3 117.1(13) . . ?
C36 C35 P3 113.2(14) . . ?
C42 C41 P4 114.4(12) . . ?
C44 C43 P4 115.1(12) . . ?
C46 C45 P4 115.9(12) . . ?
C55 C50 C51 120(2) . . ?
C55 C50 C56 122(3) . . ?
C51 C50 C56 118(3) . . ?
C50 C51 C52 120(2) . . ?
C53 C52 C51 117(3) . . ?
C54 C53 C52 123(4) . . ?
C53 C54 C55 120(4) . . ?
C50 C55 C54 119(3) . . ?
C65 C60 C61 120.0 . . ?
C65 C60 C66 124(3) . . ?
C61 C60 C66 115(3) . . ?
C62 C61 C60 120.0 . . ?
C61 C62 C63 120.0 . . ?
C64 C63 C62 120.1 . . ?
C63 C64 C65 120.0 . . ?
C64 C65 C60 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N1 2.238(12) . ?
Cd1 N2 2.250(12) . ?
Cd1 N4 2.268(11) . ?
Cd1 Br1 2.489(2) . ?
Cd1 Cd4 3.1956(17) . ?
Cd1 Cd3 3.2030(18) . ?
Cd1 Cd2 3.2337(17) . ?
Cd2 N1 2.248(11) . ?
Cd2 N3 2.270(11) . ?
Cd2 N2 2.270(12) . ?
Cd2 Br2 2.507(2) . ?
Cd2 Cd3 3.2085(17) . ?
Cd2 Cd4 3.2205(17) . ?
Cd3 N4 2.254(11) . ?
Cd3 N3 2.261(11) . ?
Cd3 N1 2.273(11) . ?
Cd3 Br3 2.495(2) . ?
Cd3 Cd4 3.2496(18) . ?
Cd4 N4 2.233(11) . ?
Cd4 N2 2.266(11) . ?
Cd4 N3 2.280(12) . ?
Cd4 Br4 2.504(2) . ?
P1 N1 1.603(11) . ?
P1 C11 1.790(18) . ?
P1 C15 1.80(2) . ?
P1 C13 1.798(15) . ?
P2 N2 1.580(12) . ?
P2 C23 1.796(16) . ?
P2 C25 1.801(17) . ?
P2 C21 1.812(18) . ?
P3 N3 1.578(11) . ?
P3 C31 1.782(16) . ?
P3 C35 1.805(16) . ?
P3 C33 1.810(16) . ?
P4 N4 1.603(11) . ?
P4 C43 1.762(15) . ?
P4 C41 1.782(15) . ?
P4 C45 1.806(15) . ?
C11 C12 1.31(3) . ?
C13 C14 1.517(18) . ?
C15 C16_a 1.28(7) . ?
C15 C161_b 1.40(4) . ?
C21 C22 1.48(2) . ?
C23 C24 1.55(2) . ?
C25 C26 1.46(2) . ?
C31 C32 1.52(2) . ?
C33 C34 1.522(19) . ?
C35 C36 1.49(2) . ?
C41 C42 1.53(2) . ?
C43 C44 1.514(19) . ?
C45 C46 1.549(19) . ?
C50 C55 1.37(3) . ?
C50 C51 1.38(3) . ?
C50 C56 1.51(3) . ?
C51 C52 1.40(3) . ?
C52 C53 1.37(3) . ?
C53 C54 1.31(3) . ?
C54 C55 1.39(3) . ?
C60 C65 1.3861 . ?
C60 C61 1.3865 . ?
C60 C66 1.436(17) . ?
C61 C62 1.3852 . ?
C62 C63 1.3862 . ?
C63 C64 1.3858 . ?
C64 C65 1.3860 . ?
|
1100602.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 22:03:05 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177996 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100602.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100602
loop_
_publ_author_name
'Harms, Klaus'
'Merle, Jan'
'Maichle-M\"ossmer, C\"acili\"a'
'Massa, Werner'
'Krieger, Matthias'
_publ_section_title
;
Heterocubane Phosphoraniminato Complexes of Cadmium
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 1099
_journal_page_last 1104
_journal_paper_doi 10.1021/ic9710364
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C45 H84 Cd4 I4 N4 P4'
_chemical_formula_weight 1762.24
_space_group_IT_number 160
_symmetry_cell_setting rhombohedral
_symmetry_space_group_name_Hall 'R 3 -2"'
_symmetry_space_group_name_H-M 'R 3 m :H'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 17.842(2)
_cell_length_b 17.842(2)
_cell_length_c 17.290(3)
_cell_measurement_reflns_used 32
_cell_measurement_temperature 223(2)
_cell_measurement_theta_max 12.49
_cell_measurement_theta_min 5.32
_cell_volume 4766.6(11)
_diffrn_ambient_temperature 223(2)
_diffrn_radiation_wavelength 0.71073
_exptl_absorpt_coefficient_mu 3.394
_exptl_absorpt_correction_T_max 0.4291
_exptl_absorpt_correction_T_min 0.2353
_exptl_absorpt_correction_type empirical
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.06(6)
_refine_ls_extinction_coef 0.00152(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.177
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 143
_refine_ls_number_reflns 2066
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.177
_refine_ls_R_factor_all 0.0400
_refine_ls_R_factor_gt 0.0398
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+26.3894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0971
_refine_ls_wR_factor_ref 0.0972
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+26.3894P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+26.3894P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M 'R 3 m'
_cod_database_code 1100602
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -y,-x,z
5 -x+y,y,z
6 x,x-y,z
7 -1/3+x,1/3+y,1/3+z
8 -1/3-y,1/3+x-y,1/3+z
9 -1/3-x+y,1/3-x,1/3+z
10 -1/3-y,1/3-x,1/3+z
11 -1/3-x+y,1/3+y,1/3+z
12 -1/3+x,1/3+x-y,1/3+z
13 1/3+x,-1/3+y,-1/3+z
14 1/3-y,-1/3+x-y,-1/3+z
15 1/3-x+y,-1/3-x,-1/3+z
16 1/3-y,-1/3-x,-1/3+z
17 1/3-x+y,-1/3+y,-1/3+z
18 1/3+x,-1/3+x-y,-1/3+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 1.39329(2) 0.60671(2) 0.18395(3) 0.0309(2) Uani 1 d S . .
Cd2 Cd 1.3333 0.6667 0.02899(6) 0.0331(3) Uani 1 d S . .
I1 I 1.47444(3) 0.52556(3) 0.23698(6) 0.0780(4) Uani 1 d S . .
I2 I 1.3333 0.6667 -0.12704(7) 0.0641(5) Uani 1 d S . .
P1 P 1.22483(9) 0.44966(18) 0.07923(15) 0.0381(6) Uani 1 d S . .
P2 P 1.3333 0.6667 0.3515(2) 0.0321(9) Uani 1 d S . .
N1 N 1.2742(2) 0.5484(5) 0.1075(6) 0.0311(16) Uani 1 d S . .
N2 N 1.3333 0.6667 0.2594(8) 0.034(3) Uani 1 d S . .
C11 C 1.1522(15) 0.4257(14) -0.0005(11) 0.051(4) Uani 0.50 d P . .
H11A H 1.1412 0.3725 -0.0242 0.061 Uiso 0.50 d PR . .
H11B H 1.1795 0.4708 -0.0384 0.061 Uiso 0.50 d PR . .
C12 C 1.0636(16) 0.4184(13) 0.0224(15) 0.061(5) Uani 0.50 d P . .
H12A H 1.0276 0.4059 -0.0225 0.091 Uiso 0.50 d PR . .
H12B H 1.0351 0.3725 0.0594 0.091 Uiso 0.50 d PR . .
H12C H 1.0738 0.4719 0.0450 0.091 Uiso 0.50 d PR . .
C13 C 1.3006(15) 0.4147(13) 0.0423(18) 0.063(6) Uani 0.50 d P . .
H13A H 1.2678 0.3551 0.0269 0.075 Uiso 0.50 d PR . .
H13B H 1.3373 0.4183 0.0844 0.075 Uiso 0.50 d PR . .
C14 C 1.3523(18) 0.4622(19) -0.0216(19) 0.090(9) Uani 0.50 d P . .
H14A H 1.3894 0.4400 -0.0360 0.135 Uiso 0.50 d PR . .
H14B H 1.3164 0.4578 -0.0647 0.135 Uiso 0.50 d PR . .
H14C H 1.3868 0.5218 -0.0066 0.135 Uiso 0.50 d PR . .
C15 C 1.2068(10) 0.3740(10) 0.1584(9) 0.045(5) Uani 0.50 d P . .
H15A H 1.1728 0.3818 0.1972 0.054 Uiso 0.50 d PR . .
H15B H 1.2620 0.3903 0.1811 0.054 Uiso 0.50 d PR . .
C16 C 1.1624(13) 0.2791(11) 0.1386(11) 0.058(6) Uani 0.50 d P . .
H16A H 1.1568 0.2465 0.1846 0.086 Uiso 0.50 d PR . .
H16B H 1.1060 0.2608 0.1176 0.086 Uiso 0.50 d PR . .
H16C H 1.1965 0.2695 0.1012 0.086 Uiso 0.50 d PR . .
C21 C 1.2467(12) 0.6820(15) 0.3935(9) 0.055(5) Uani 0.50 d P . .
H21A H 1.2541 0.6871 0.4486 0.066 Uiso 0.50 d PR . .
H21B H 1.1919 0.6312 0.3832 0.066 Uiso 0.50 d PR . .
C22 C 1.2426(5) 0.7574(5) 0.3663(8) 0.063(4) Uani 1 d S . .
H22A H 1.1960 0.7610 0.3910 0.094 Uiso 0.50 d PR . .
H22B H 1.2963 0.8096 0.3776 0.094 Uiso 0.50 d PR . .
H22C H 1.2333 0.7530 0.3114 0.094 Uiso 0.50 d PR . .
C100 C 1.0369(17) 0.5185(8) 0.5005(16) 0.17(2) Uani 1 d S . .
C200 C 1.0721(18) 0.6014(14) 0.530(2) 0.166(13) Uani 1 d . . .
H20A H 1.0444 0.6346 0.5197 0.199 Uiso 1 d R . .
C300 C 1.1400(17) 0.6364(12) 0.5806(16) 0.150(12) Uani 1 d . . .
H30A H 1.1616 0.6959 0.5942 0.180 Uiso 1 d R . .
C400 C 1.170(3) 0.5849(13) 0.605(2) 0.168(18) Uani 1 d S . .
H40A H 1.2172 0.6086 0.6407 0.202 Uiso 1 d SR . .
C700 C 0.971(4) 0.4857(19) 0.454(2) 0.37(6) Uani 1 d S . .
H70B H 0.9592 0.5305 0.4377 0.548 Uiso 0.50 calc PR . .
H70C H 0.9213 0.4402 0.4803 0.548 Uiso 0.50 calc PR . .
H70D H 0.9847 0.4619 0.4090 0.548 Uiso 0.50 calc PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0339(3) 0.0339(3) 0.0295(3) 0.00030(14) -0.00030(14) 0.0206(3)
Cd2 0.0377(4) 0.0377(4) 0.0239(5) 0.000 0.000 0.0189(2)
I1 0.1104(8) 0.1104(8) 0.0660(6) 0.0062(2) -0.0062(2) 0.0947(8)
I2 0.0826(7) 0.0826(7) 0.0270(6) 0.000 0.000 0.0413(4)
P1 0.0471(12) 0.0281(13) 0.0328(12) -0.0037(10) -0.0019(5) 0.0141(6)
P2 0.0367(14) 0.0367(14) 0.0228(19) 0.000 0.000 0.0184(7)
N1 0.031(3) 0.027(4) 0.034(3) -0.003(4) -0.0013(18) 0.013(2)
N2 0.041(5) 0.041(5) 0.021(6) 0.000 0.000 0.020(3)
C11 0.058(11) 0.060(13) 0.037(7) -0.005(8) -0.003(9) 0.031(10)
C12 0.043(11) 0.047(11) 0.074(12) 0.000(10) 0.005(10) 0.009(10)
C13 0.045(11) 0.044(11) 0.104(19) -0.039(12) -0.004(11) 0.026(8)
C14 0.083(18) 0.085(18) 0.13(2) -0.033(18) 0.011(16) 0.059(15)
C15 0.051(12) 0.037(7) 0.043(7) -0.004(6) 0.004(6) 0.019(6)
C16 0.071(14) 0.041(8) 0.062(9) -0.009(7) -0.006(8) 0.029(8)
C21 0.046(9) 0.072(12) 0.028(7) -0.003(8) 0.001(6) 0.015(8)
C22 0.079(8) 0.079(8) 0.049(7) 0.000(3) 0.000(3) 0.054(9)
C100 0.054(12) 0.28(5) 0.083(15) 0.012(6) 0.023(11) 0.027(6)
C200 0.103(15) 0.072(12) 0.29(4) 0.022(18) -0.01(2) 0.019(12)
C300 0.17(2) 0.075(11) 0.24(3) 0.061(15) 0.12(2) 0.088(14)
C400 0.18(4) 0.14(2) 0.20(4) 0.063(16) 0.13(3) 0.088(18)
C700 0.23(6) 0.61(14) 0.14(4) 0.06(2) 0.13(5) 0.11(3)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cd 1.40
I 1.40
N 0.68
P 1.05
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cd1 N1 89.8(2) . . ?
N2 Cd1 N1 89.8(2) . 2_755 ?
N1 Cd1 N1 88.6(4) . 2_755 ?
N2 Cd1 I1 124.8(3) . . ?
N1 Cd1 I1 126.12(17) . . ?
N1 Cd1 I1 126.12(17) 2_755 . ?
N2 Cd1 Cd1 44.9(2) . 3_775 ?
N1 Cd1 Cd1 44.91(16) . 3_775 ?
N1 Cd1 Cd1 89.45(17) 2_755 3_775 ?
I1 Cd1 Cd1 144.427(14) . 3_775 ?
N2 Cd1 Cd1 44.9(2) . 2_755 ?
N1 Cd1 Cd1 89.46(17) . 2_755 ?
N1 Cd1 Cd1 44.91(16) 2_755 2_755 ?
I1 Cd1 Cd1 144.427(14) . 2_755 ?
Cd1 Cd1 Cd1 60.0 3_775 2_755 ?
N2 Cd1 Cd2 90.5(3) . . ?
N1 Cd1 Cd2 44.3(2) . . ?
N1 Cd1 Cd2 44.3(2) 2_755 . ?
I1 Cd1 Cd2 144.75(3) . . ?
Cd1 Cd1 Cd2 60.490(13) 3_775 . ?
Cd1 Cd1 Cd2 60.490(13) 2_755 . ?
N1 Cd2 N1 88.1(3) 3_775 2_755 ?
N1 Cd2 N1 88.1(3) 3_775 . ?
N1 Cd2 N1 88.1(3) 2_755 . ?
N1 Cd2 I2 126.6(2) 3_775 . ?
N1 Cd2 I2 126.6(2) 2_755 . ?
N1 Cd2 I2 126.6(2) . . ?
N1 Cd2 Cd1 44.05(16) 3_775 3_775 ?
N1 Cd2 Cd1 88.1(2) 2_755 3_775 ?
N1 Cd2 Cd1 44.05(16) . 3_775 ?
I2 Cd2 Cd1 145.335(16) . 3_775 ?
N1 Cd2 Cd1 44.05(16) 3_775 2_755 ?
N1 Cd2 Cd1 44.05(16) 2_755 2_755 ?
N1 Cd2 Cd1 88.1(2) . 2_755 ?
I2 Cd2 Cd1 145.334(16) . 2_755 ?
Cd1 Cd2 Cd1 59.02(3) 3_775 2_755 ?
N1 Cd2 Cd1 88.1(2) 3_775 . ?
N1 Cd2 Cd1 44.05(16) 2_755 . ?
N1 Cd2 Cd1 44.05(16) . . ?
I2 Cd2 Cd1 145.335(16) . . ?
Cd1 Cd2 Cd1 59.02(3) 3_775 . ?
Cd1 Cd2 Cd1 59.02(3) 2_755 . ?
N1 P1 C11 115.6(7) . . ?
N1 P1 C11 115.6(7) . 5_755 ?
C11 P1 C11 74.3(15) . 5_755 ?
N1 P1 C15 112.3(6) . 5_755 ?
C11 P1 C15 109.1(9) . 5_755 ?
C11 P1 C15 124.0(9) 5_755 5_755 ?
N1 P1 C15 112.3(6) . . ?
C11 P1 C15 124.0(9) . . ?
C11 P1 C15 109.1(9) 5_755 . ?
C15 P1 C15 22.2(10) 5_755 . ?
N1 P1 C13 112.4(6) . . ?
C11 P1 C13 102.5(14) . . ?
C11 P1 C13 30.3(10) 5_755 . ?
C15 P1 C13 104.1(11) 5_755 . ?
C15 P1 C13 84.2(11) . . ?
N1 P1 C13 112.4(6) . 5_755 ?
C11 P1 C13 30.3(10) . 5_755 ?
C11 P1 C13 102.5(14) 5_755 5_755 ?
C15 P1 C13 84.2(11) 5_755 5_755 ?
C15 P1 C13 104.1(11) . 5_755 ?
C13 P1 C13 126.6(15) . 5_755 ?
N2 P2 C21 113.1(5) . . ?
N2 P2 C21 113.1(5) . 4_775 ?
C21 P2 C21 40.3(14) . 4_775 ?
N2 P2 C21 113.1(5) . 6 ?
C21 P2 C21 69.0(14) . 6 ?
C21 P2 C21 105.6(6) 4_775 6 ?
N2 P2 C21 113.1(5) . 3_775 ?
C21 P2 C21 105.6(6) . 3_775 ?
C21 P2 C21 69.0(14) 4_775 3_775 ?
C21 P2 C21 131.2(10) 6 3_775 ?
N2 P2 C21 113.1(5) . 2_755 ?
C21 P2 C21 105.6(6) . 2_755 ?
C21 P2 C21 131.2(10) 4_775 2_755 ?
C21 P2 C21 40.3(14) 6 2_755 ?
C21 P2 C21 105.6(6) 3_775 2_755 ?
N2 P2 C21 113.1(5) . 5_755 ?
C21 P2 C21 131.2(10) . 5_755 ?
C21 P2 C21 105.6(6) 4_775 5_755 ?
C21 P2 C21 105.6(6) 6 5_755 ?
C21 P2 C21 40.3(14) 3_775 5_755 ?
C21 P2 C21 69.0(14) 2_755 5_755 ?
P1 N1 Cd1 123.9(3) . . ?
P1 N1 Cd1 123.9(3) . 3_775 ?
Cd1 N1 Cd1 90.2(3) . 3_775 ?
P1 N1 Cd2 125.6(5) . . ?
Cd1 N1 Cd2 91.6(2) . . ?
Cd1 N1 Cd2 91.6(2) 3_775 . ?
P2 N2 Cd1 125.1(3) . 3_775 ?
P2 N2 Cd1 125.1(3) . 2_755 ?
Cd1 N2 Cd1 90.2(4) 3_775 2_755 ?
P2 N2 Cd1 125.1(3) . . ?
Cd1 N2 Cd1 90.2(4) 3_775 . ?
Cd1 N2 Cd1 90.2(4) 2_755 . ?
C13 C11 C14 78(3) 5_755 5_755 ?
C13 C11 C12 37(2) 5_755 . ?
C14 C11 C12 44.3(18) 5_755 . ?
C13 C11 P1 79.0(17) 5_755 . ?
C14 C11 P1 129.9(19) 5_755 . ?
C12 C11 P1 113.8(16) . . ?
C13 C12 C14 84(3) 5_755 5_755 ?
C13 C12 C11 36(2) 5_755 . ?
C14 C12 C11 53.3(19) 5_755 . ?
C11 C13 C12 107(4) 5_755 5_755 ?
C11 C13 C14 61(3) 5_755 . ?
C12 C13 C14 51(2) 5_755 . ?
C11 C13 P1 70.7(17) 5_755 . ?
C12 C13 P1 160(2) 5_755 . ?
C14 C13 P1 116(2) . . ?
C12 C14 C11 82(3) 5_755 5_755 ?
C12 C14 C13 44(2) 5_755 . ?
C11 C14 C13 41.3(15) 5_755 . ?
C15 C15 C16 92.1(9) 5_755 . ?
C15 C15 C16 63.2(9) 5_755 5_755 ?
C16 C15 C16 28.9(14) . 5_755 ?
C15 C15 P1 78.9(5) 5_755 . ?
C16 C15 P1 117.2(11) . . ?
C16 C15 P1 108.4(11) 5_755 . ?
C16 C16 C15 87.9(9) 5_755 . ?
C16 C16 C15 63.2(9) 5_755 5_755 ?
C15 C16 C15 24.7(11) . 5_755 ?
C21 C21 C22 64.2(8) 4_775 . ?
C21 C21 P2 69.9(7) 4_775 . ?
C22 C21 P2 116.1(11) . . ?
C21 C22 C21 51.6(16) 4_775 . ?
C700 C100 C200 122.6(16) . 6 ?
C700 C100 C200 122.6(16) . . ?
C200 C100 C200 114(3) 6 . ?
C300 C200 C100 123(3) . . ?
C400 C300 C200 117(3) . . ?
C300 C400 C300 125(5) . 6 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N2 2.266(8) . ?
Cd1 N1 2.266(6) . ?
Cd1 N1 2.266(6) 2_755 ?
Cd1 I1 2.6703(11) . ?
Cd1 Cd1 3.2093(12) 3_775 ?
Cd1 Cd1 3.2094(12) 2_755 ?
Cd1 Cd2 3.2577(12) . ?
Cd2 N1 2.277(8) 3_775 ?
Cd2 N1 2.277(9) 2_755 ?
Cd2 N1 2.277(8) . ?
Cd2 I2 2.6977(17) . ?
Cd2 Cd1 3.2577(12) 3_775 ?
Cd2 Cd1 3.2577(12) 2_755 ?
P1 N1 1.602(8) . ?
P1 C11 1.791(18) . ?
P1 C11 1.791(18) 5_755 ?
P1 C15 1.835(16) 5_755 ?
P1 C15 1.835(16) . ?
P1 C13 1.86(2) . ?
P1 C13 1.86(2) 5_755 ?
P2 N2 1.593(14) . ?
P2 C21 1.85(2) . ?
P2 C21 1.85(2) 4_775 ?
P2 C21 1.85(2) 6 ?
P2 C21 1.85(2) 3_775 ?
P2 C21 1.85(2) 2_755 ?
P2 C21 1.85(2) 5_755 ?
N1 Cd1 2.266(6) 3_775 ?
N2 Cd1 2.266(8) 3_775 ?
N2 Cd1 2.266(8) 2_755 ?
C11 C13 0.96(3) 5_755 ?
C11 C14 1.27(3) 5_755 ?
C11 C12 1.57(3) . ?
C12 C13 1.00(3) 5_755 ?
C12 C14 1.11(4) 5_755 ?
C13 C11 0.96(3) 5_755 ?
C13 C12 1.00(3) 5_755 ?
C13 C14 1.42(4) . ?
C14 C12 1.11(4) 5_755 ?
C14 C11 1.27(3) 5_755 ?
C15 C15 0.71(3) 5_755 ?
C15 C16 1.51(2) . ?
C15 C16 1.69(2) 5_755 ?
C16 C16 0.81(4) 5_755 ?
C16 C15 1.69(2) 5_755 ?
C21 C21 1.27(4) 4_775 ?
C21 C22 1.46(3) . ?
C22 C21 1.46(3) 4_775 ?
C100 C700 1.29(6) . ?
C100 C200 1.39(3) 6 ?
C100 C200 1.39(3) . ?
C200 C300 1.36(4) . ?
C300 C400 1.34(3) . ?
C400 C300 1.34(3) 6 ?
|
1100603.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 22:03:05 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177996 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100603.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100603
loop_
_publ_author_name
'Harms, Klaus'
'Merle, Jan'
'Maichle-M\"ossmer, C\"acili\"a'
'Massa, Werner'
'Krieger, Matthias'
_publ_section_title
;
Heterocubane Phosphoraniminato Complexes of Cadmium
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 1099
_journal_page_last 1104
_journal_paper_doi 10.1021/ic9710364
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C44 H96 Cd4 N4 P4 Si4'
_chemical_formula_weight 1367.09
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-I 2ya'
_symmetry_space_group_name_H-M 'I 1 2/a 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 107.512(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 19.7939(12)
_cell_length_b 10.5997(15)
_cell_length_c 32.094(2)
_cell_measurement_reflns_used 5000
_cell_measurement_temperature 213(2)
_cell_volume 6421.5(11)
_diffrn_ambient_temperature 213(2)
_diffrn_radiation_wavelength 0.71069
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 0.866
_refine_ls_goodness_of_fit_obs 0.989
_refine_ls_hydrogen_treatment ?
_refine_ls_matrix_type full
_refine_ls_number_parameters 388
_refine_ls_number_reflns 6236
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.866
_refine_ls_restrained_S_obs 0.989
_refine_ls_R_factor_all 0.0711
_refine_ls_R_factor_obs 0.0364
_refine_ls_shift/esd_max 0.299
_refine_ls_shift/esd_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.0856
_refine_ls_wR_factor_obs 0.0761
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M 'I 2/a'
_cod_database_code 1100603
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2+y,1/2+z
3 1/2+x,-y,z
4 x,1/2-y,1/2+z
5 -x,-y,-z
6 -1/2-x,-1/2-y,-1/2-z
7 -1/2-x,y,-z
8 -x,-1/2+y,-1/2-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0700(3) 0.04349(18) 0.03213(17) -0.00148(14) 0.01812(15) 0.00859(17)
Cd2 0.04189(19) 0.04876(18) 0.03047(16) -0.00189(13) 0.00801(13) -0.00041(16)
N1 0.044(2) 0.0411(18) 0.0323(17) 0.0005(15) 0.0119(15) -0.0021(17)
N2 0.068(3) 0.048(2) 0.0327(18) 0.0016(16) 0.0167(17) 0.018(2)
P1 0.0535(8) 0.0468(6) 0.0423(6) 0.0042(5) 0.0219(5) -0.0026(6)
C1_a 0.21(2) 0.065(8) 0.037(7) 0.013(6) 0.038(9) 0.050(11)
C2_a 0.22(2) 0.140(14) 0.044(7) 0.014(8) 0.039(10) -0.011(14)
C3_a 0.065(7) 0.051(5) 0.034(5) 0.016(4) 0.006(5) -0.016(5)
C4_a 0.122(11) 0.054(6) 0.083(8) -0.002(6) 0.032(8) -0.001(7)
C5_a 0.085(10) 0.065(8) 0.141(13) 0.005(8) 0.077(10) -0.001(7)
C1A_b 0.065(8) 0.088(9) 0.049(7) 0.014(6) 0.020(6) 0.003(7)
C2A_b 0.074(8) 0.117(11) 0.049(7) 0.024(8) 0.024(6) -0.021(8)
C3A_b 0.087(10) 0.057(6) 0.090(9) -0.011(6) 0.037(8) -0.018(7)
C4A_b 0.146(14) 0.066(7) 0.096(10) 0.004(7) 0.048(9) -0.030(8)
C5A_b 0.074(9) 0.091(9) 0.058(7) 0.009(6) 0.038(6) -0.014(8)
C6 0.069(5) 0.127(7) 0.266(14) 0.050(7) 0.056(7) 0.021(5)
P2 0.0730(9) 0.0539(7) 0.0411(6) 0.0091(5) 0.0155(6) 0.0234(7)
C7 0.076(4) 0.080(4) 0.064(3) 0.012(3) 0.011(3) 0.007(3)
C8_a 0.062(8) 0.102(9) 0.124(11) 0.050(8) 0.030(8) 0.000(7)
C8A_b 0.061(8) 0.110(9) 0.067(7) 0.001(6) 0.020(6) 0.009(7)
C9 0.081(5) 0.071(4) 0.091(5) 0.022(3) 0.018(4) 0.011(3)
C10_a 0.094(9) 0.057(7) 0.082(8) -0.007(6) 0.029(7) 0.003(6)
C10A_b 0.120(13) 0.090(10) 0.110(12) -0.009(8) 0.028(9) 0.010(9)
C11 0.126(6) 0.100(5) 0.043(3) 0.020(3) 0.021(3) 0.047(4)
C12 0.222(11) 0.164(8) 0.047(4) 0.022(4) 0.007(5) 0.084(8)
C13 0.092(4) 0.065(3) 0.043(3) -0.002(2) 0.022(3) 0.029(3)
C14 0.102(5) 0.075(4) 0.048(3) -0.009(2) 0.024(3) 0.028(3)
Si1 0.1334(18) 0.1072(14) 0.0473(9) -0.0177(9) 0.0329(10) 0.0248(12)
C15_a 0.157(17) 0.142(15) 0.062(9) -0.026(9) 0.005(9) 0.001(12)
C16_a 0.164(17) 0.116(11) 0.099(11) 0.019(9) 0.085(12) 0.038(12)
C17_a 0.170(17) 0.070(8) 0.072(9) -0.016(7) 0.048(11) 0.037(9)
C15A_b 0.21(2) 0.192(19) 0.058(9) 0.008(10) -0.003(11) -0.098(18)
C16A_b 0.114(18) 0.69(8) 0.16(2) -0.27(4) 0.010(15) 0.06(3)
C17A_b 0.30(3) 0.118(14) 0.067(10) -0.030(9) 0.023(14) -0.058(16)
C18 0.060(3) 0.097(4) 0.039(3) -0.008(3) 0.014(2) -0.030(3)
C19 0.085(5) 0.127(5) 0.046(3) -0.010(3) 0.012(3) -0.057(4)
Si2_a 0.082(4) 0.079(3) 0.050(2) -0.017(3) 0.004(2) -0.028(3)
C20_a 0.50(8) 0.19(3) 0.17(3) -0.11(3) -0.13(4) 0.18(5)
C22_a 0.099(15) 0.58(6) 0.064(11) -0.06(2) 0.004(10) -0.11(3)
Si2A_b 0.095(4) 0.066(3) 0.0408(18) -0.020(2) 0.003(2) -0.012(3)
C20A_b 0.064(9) 0.136(13) 0.086(9) -0.052(9) 0.014(8) -0.026(9)
C22A_b 0.134(15) 0.088(12) 0.084(11) -0.034(8) 0.042(12) -0.018(11)
C21 0.290(16) 0.173(9) 0.064(5) -0.013(6) -0.023(7) 0.056(10)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd1 Cd 0.707353(19) 0.36442(3) 0.036483(9) 0.04792(11) Uani 1 d . .
Cd2 Cd 0.673631(16) 0.14195(3) -0.037379(9) 0.04101(10) Uani 1 d . .
N1 N 0.70914(17) 0.1475(3) 0.03583(10) 0.0390(8) Uani 1 d . .
N2 N 0.6750(2) 0.3594(3) -0.03650(10) 0.0493(9) Uani 1 d . .
P1 P 0.68005(7) 0.06361(11) 0.06738(4) 0.0459(3) Uani 1 d . .
C1_a C 0.7179(12) 0.1197(14) 0.1239(4) 0.103(6) Uani 0.50 d P 1
H1A_a H 0.7675 0.1404 0.1271 0.124 Uiso 0.50 calc PR 1
H1B_a H 0.6942 0.1999 0.1256 0.124 Uiso 0.50 calc PR 1
C2_a C 0.7186(11) 0.0510(16) 0.1626(4) 0.135(7) Uani 0.50 d P 1
H2A_a H 0.7427 0.1005 0.1882 0.203 Uiso 0.50 calc PR 1
H2B_a H 0.7434 -0.0283 0.1633 0.203 Uiso 0.50 calc PR 1
H2C_a H 0.6704 0.0345 0.1625 0.203 Uiso 0.50 calc PR 1
C3_a C 0.7078(6) -0.1014(8) 0.0711(3) 0.051(2) Uani 0.50 d P 1
H3A_a H 0.7596 -0.1046 0.0829 0.062 Uiso 0.50 calc PR 1
H3B_a H 0.6884 -0.1443 0.0920 0.062 Uiso 0.50 calc PR 1
C4_a C 0.6854(8) -0.1734(10) 0.0283(4) 0.086(4) Uani 0.50 d P 1
H4A_a H 0.7018 -0.2599 0.0333 0.129 Uiso 0.50 calc PR 1
H4B_a H 0.7058 -0.1339 0.0077 0.129 Uiso 0.50 calc PR 1
H4C_a H 0.6341 -0.1724 0.0166 0.129 Uiso 0.50 calc PR 1
C5_a C 0.5851(8) 0.0530(13) 0.0557(6) 0.088(4) Uani 0.50 d P 1
H5A_a H 0.5674 -0.0085 0.0321 0.105 Uiso 0.50 calc PR 1
H5B_a H 0.5751 0.0192 0.0817 0.105 Uiso 0.50 calc PR 1
C1A_b C 0.7353(6) 0.0352(14) 0.1208(3) 0.067(3) Uani 0.50 d P 2
H1C_b H 0.7087 -0.0183 0.1353 0.080 Uiso 0.50 calc PR 2
H1D_b H 0.7756 -0.0147 0.1184 0.080 Uiso 0.50 calc PR 2
C2A_b C 0.7625(7) 0.1359(13) 0.1487(4) 0.079(4) Uani 0.50 d P 2
H2D_b H 0.7914 0.1038 0.1767 0.118 Uiso 0.50 calc PR 2
H2E_b H 0.7238 0.1854 0.1528 0.118 Uiso 0.50 calc PR 2
H2F_b H 0.7913 0.1885 0.1360 0.118 Uiso 0.50 calc PR 2
C3A_b C 0.6530(8) -0.0893(11) 0.0436(4) 0.076(3) Uani 0.50 d P 2
H3C_b H 0.6203 -0.0764 0.0142 0.091 Uiso 0.50 calc PR 2
H3D_b H 0.6950 -0.1321 0.0403 0.091 Uiso 0.50 calc PR 2
C4A_b C 0.6173(9) -0.1785(11) 0.0681(5) 0.101(5) Uani 0.50 d P 2
H4D_b H 0.6048 -0.2567 0.0519 0.151 Uiso 0.50 calc PR 2
H4E_b H 0.5747 -0.1390 0.0711 0.151 Uiso 0.50 calc PR 2
H4F_b H 0.6496 -0.1961 0.0969 0.151 Uiso 0.50 calc PR 2
C5A_b C 0.5980(7) 0.1336(15) 0.0748(4) 0.070(3) Uani 0.50 d P 2
H5C_b H 0.5800 0.0723 0.0917 0.084 Uiso 0.50 calc PR 2
H5D_b H 0.6130 0.2076 0.0936 0.084 Uiso 0.50 calc PR 2
C6 C 0.5448(5) 0.1686(8) 0.0432(4) 0.153(4) Uani 1 d . .
H6A_a H 0.4991 0.1493 0.0224 0.229 Uiso 0.50 calc PR 1
H6B_a H 0.5705 0.2260 0.0300 0.229 Uiso 0.50 calc PR 1
H6C_a H 0.5377 0.2077 0.0689 0.229 Uiso 0.50 calc PR 1
H6D_b H 0.5248 0.0961 0.0252 0.229 Uiso 0.50 calc PR 2
H6E_b H 0.5599 0.2307 0.0257 0.229 Uiso 0.50 calc PR 2
H6F_b H 0.5092 0.2054 0.0547 0.229 Uiso 0.50 calc PR 2
P2 P 0.61740(8) 0.43564(12) -0.07260(4) 0.0564(3) Uani 1 d . .
C7 C 0.5282(3) 0.4201(6) -0.07022(18) 0.0752(16) Uani 1 d . .
H7A_a H 0.5274 0.4621 -0.0432 0.090 Uiso 0.50 calc PR 1
H7B_a H 0.4988 0.4715 -0.0942 0.090 Uiso 0.50 calc PR 1
H7C_b H 0.4959 0.4631 -0.0954 0.090 Uiso 0.50 calc PR 2
H7D_b H 0.5153 0.3305 -0.0721 0.090 Uiso 0.50 calc PR 2
C8_a C 0.4873(7) 0.2934(12) -0.0718(5) 0.095(4) Uani 0.50 d P 1
H8A_a H 0.4401 0.3108 -0.0701 0.143 Uiso 0.50 calc PR 1
H8B_a H 0.5125 0.2408 -0.0473 0.143 Uiso 0.50 calc PR 1
H8C_a H 0.4839 0.2498 -0.0989 0.143 Uiso 0.50 calc PR 1
C8A_b C 0.5198(6) 0.4710(12) -0.0316(4) 0.079(3) Uani 0.50 d P 2
H8D_b H 0.4710 0.4608 -0.0318 0.119 Uiso 0.50 calc PR 2
H8E_b H 0.5317 0.5599 -0.0298 0.119 Uiso 0.50 calc PR 2
H8F_b H 0.5508 0.4272 -0.0065 0.119 Uiso 0.50 calc PR 2
C9 C 0.6304(4) 0.6032(5) -0.0735(2) 0.0823(18) Uani 1 d . .
H9A_a H 0.6702 0.6193 -0.0850 0.099 Uiso 0.50 calc PR 1
H9B_a H 0.5880 0.6406 -0.0940 0.099 Uiso 0.50 calc PR 1
H9C_b H 0.5910 0.6347 -0.0978 0.099 Uiso 0.50 calc PR 2
H9D_b H 0.6223 0.6353 -0.0468 0.099 Uiso 0.50 calc PR 2
C10_a C 0.6433(7) 0.6639(10) -0.0345(4) 0.077(3) Uani 0.50 d P 1
H10A_a H 0.6494 0.7534 -0.0387 0.115 Uiso 0.50 calc PR 1
H10B_a H 0.6861 0.6302 -0.0141 0.115 Uiso 0.50 calc PR 1
H10C_a H 0.6037 0.6514 -0.0231 0.115 Uiso 0.50 calc PR 1
C10A_b C 0.6941(9) 0.6705(13) -0.0771(5) 0.108(5) Uani 0.50 d P 2
H10D_b H 0.6861 0.7608 -0.0772 0.162 Uiso 0.50 calc PR 2
H10E_b H 0.7034 0.6461 -0.1040 0.162 Uiso 0.50 calc PR 2
H10F_b H 0.7345 0.6487 -0.0524 0.162 Uiso 0.50 calc PR 2
C11 C 0.6134(4) 0.3814(6) -0.12716(17) 0.090(2) Uani 1 d . .
H11A H 0.6605 0.3926 -0.1307 0.109 Uiso 1 calc R .
H11B H 0.6036 0.2906 -0.1286 0.109 Uiso 1 calc R .
C12 C 0.5597(6) 0.4432(9) -0.1661(2) 0.152(4) Uani 1 d . .
H12A H 0.5634 0.4061 -0.1929 0.228 Uiso 1 calc R .
H12B H 0.5691 0.5330 -0.1660 0.228 Uiso 1 calc R .
H12C H 0.5123 0.4298 -0.1641 0.228 Uiso 1 calc R .
C13 C 0.6853(3) 0.4608(5) 0.08929(16) 0.0665(15) Uani 1 d . .
C14 C 0.6874(3) 0.4968(5) 0.12487(17) 0.0749(17) Uani 1 d . .
Si1 Si 0.70033(13) 0.53938(19) 0.18225(5) 0.0947(6) Uani 1 d . .
C15_a C 0.7916(10) 0.5148(17) 0.2157(5) 0.127(6) Uani 0.50 d P 1
H15A_a H 0.8117 0.4443 0.2042 0.190 Uiso 0.50 calc PR 1
H15B_a H 0.7928 0.4967 0.2455 0.190 Uiso 0.50 calc PR 1
H15C_a H 0.8191 0.5903 0.2151 0.190 Uiso 0.50 calc PR 1
C16_a C 0.6438(11) 0.4228(15) 0.2019(5) 0.116(6) Uani 0.50 d P 1
H16A_a H 0.6668 0.3410 0.2064 0.174 Uiso 0.50 calc PR 1
H16B_a H 0.5977 0.4155 0.1802 0.174 Uiso 0.50 calc PR 1
H16C_a H 0.6379 0.4524 0.2292 0.174 Uiso 0.50 calc PR 1
C17_a C 0.6684(11) 0.7022(12) 0.1877(5) 0.101(5) Uani 0.50 d P 1
H17A_a H 0.7074 0.7612 0.1921 0.152 Uiso 0.50 calc PR 1
H17B_a H 0.6501 0.7058 0.2125 0.152 Uiso 0.50 calc PR 1
H17C_a H 0.6312 0.7245 0.1613 0.152 Uiso 0.50 calc PR 1
C15A_b C 0.7280(13) 0.408(2) 0.2171(5) 0.164(10) Uani 0.50 d P 2
H15D_b H 0.7664 0.3650 0.2098 0.245 Uiso 0.50 calc PR 2
H15E_b H 0.6886 0.3500 0.2132 0.245 Uiso 0.50 calc PR 2
H15F_b H 0.7443 0.4359 0.2472 0.245 Uiso 0.50 calc PR 2
C16A_b C 0.6197(12) 0.617(4) 0.1894(8) 0.33(3) Uani 0.50 d P 2
H16D_b H 0.5817 0.5553 0.1845 0.492 Uiso 0.50 calc PR 2
H16E_b H 0.6051 0.6853 0.1687 0.492 Uiso 0.50 calc PR 2
H16F_b H 0.6304 0.6496 0.2189 0.492 Uiso 0.50 calc PR 2
C17A_b C 0.7753(14) 0.6547(17) 0.1946(5) 0.170(10) Uani 0.50 d P 2
H17D_b H 0.8187 0.6110 0.1953 0.254 Uiso 0.50 calc PR 2
H17E_b H 0.7806 0.6938 0.2227 0.254 Uiso 0.50 calc PR 2
H17F_b H 0.7654 0.7191 0.1721 0.254 Uiso 0.50 calc PR 2
C18 C 0.5986(3) 0.0403(5) -0.08797(15) 0.0656(15) Uani 1 d . .
C19 C 0.5631(3) -0.0001(6) -0.12243(18) 0.088(2) Uani 1 d . .
Si2_a Si 0.5090(3) -0.0173(5) -0.17930(18) 0.0737(14) Uani 0.50 d P 1
C20_a C 0.544(3) -0.157(3) -0.1944(11) 0.34(4) Uani 0.50 d P 1
H20A_a H 0.5049 -0.2108 -0.2105 0.508 Uiso 0.50 calc PR 1
H20B_a H 0.5717 -0.2003 -0.1684 0.508 Uiso 0.50 calc PR 1
H20C_a H 0.5731 -0.1362 -0.2127 0.508 Uiso 0.50 calc PR 1
C22_a C 0.4150(11) -0.027(4) -0.1902(6) 0.253(19) Uani 0.50 d P 1
H22A_a H 0.3949 0.0570 -0.1937 0.379 Uiso 0.50 calc PR 1
H22B_a H 0.4044 -0.0690 -0.1660 0.379 Uiso 0.50 calc PR 1
H22C_a H 0.3947 -0.0752 -0.2168 0.379 Uiso 0.50 calc PR 1
Si2A_b Si 0.5306(3) -0.0735(5) -0.17866(17) 0.0712(15) Uani 0.50 d P 2
C20A_b C 0.4594(8) -0.1902(17) -0.1822(5) 0.097(5) Uani 0.50 d P 2
H20D_b H 0.4775 -0.2746 -0.1836 0.146 Uiso 0.50 calc PR 2
H20E_b H 0.4202 -0.1742 -0.2083 0.146 Uiso 0.50 calc PR 2
H20F_b H 0.4431 -0.1828 -0.1567 0.146 Uiso 0.50 calc PR 2
C22A_b C 0.5998(10) -0.1569(18) -0.1961(6) 0.100(6) Uani 0.50 d P 2
H22D_b H 0.6107 -0.2367 -0.1808 0.150 Uiso 0.50 calc PR 2
H22E_b H 0.6422 -0.1054 -0.1894 0.150 Uiso 0.50 calc PR 2
H22F_b H 0.5828 -0.1723 -0.2274 0.150 Uiso 0.50 calc PR 2
C21 C 0.5132(7) 0.0865(10) -0.2139(3) 0.193(6) Uani 1 d . .
H21A_a H 0.5208 0.1686 -0.1999 0.289 Uiso 0.50 calc PR 1
H21B_a H 0.4691 0.0873 -0.2376 0.289 Uiso 0.50 calc PR 1
H21C_a H 0.5521 0.0671 -0.2253 0.289 Uiso 0.50 calc PR 1
H21D_b H 0.5141 0.1577 -0.1948 0.289 Uiso 0.50 calc PR 2
H21E_b H 0.4672 0.0821 -0.2359 0.289 Uiso 0.50 calc PR 2
H21F_b H 0.5498 0.0968 -0.2280 0.289 Uiso 0.50 calc PR 2
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cd 1.42
N 0.68
P 1.05
Si 1.20
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Cd1 N2 141.38(16) . . ?
C13 Cd1 N1 119.57(16) . . ?
N2 Cd1 N1 88.10(12) . . ?
C13 Cd1 N2 117.03(19) . 2_655 ?
N2 Cd1 N2 88.32(13) . 2_655 ?
N1 Cd1 N2 87.64(12) . 2_655 ?
C13 Cd1 Cd2 151.18(17) . . ?
N2 Cd1 Cd2 44.83(9) . . ?
N1 Cd1 Cd2 43.29(7) . . ?
N2 Cd1 Cd2 88.25(8) 2_655 . ?
C13 Cd1 Cd1 147.26(16) . 2_655 ?
N2 Cd1 Cd1 45.33(10) . 2_655 ?
N1 Cd1 Cd1 88.90(8) . 2_655 ?
N2 Cd1 Cd1 43.05(8) 2_655 2_655 ?
Cd2 Cd1 Cd1 61.160(10) . 2_655 ?
C13 Cd1 Cd2 130.26(14) . 2_655 ?
N2 Cd1 Cd2 88.33(9) . 2_655 ?
N1 Cd1 Cd2 43.84(8) . 2_655 ?
N2 Cd1 Cd2 43.81(8) 2_655 2_655 ?
Cd2 Cd1 Cd2 58.953(13) . 2_655 ?
Cd1 Cd1 Cd2 59.328(10) 2_655 2_655 ?
C18 Cd2 N1 137.56(16) . . ?
C18 Cd2 N2 121.15(18) . . ?
N1 Cd2 N2 87.83(11) . . ?
C18 Cd2 N1 119.62(16) . 2_655 ?
N1 Cd2 N1 88.89(11) . 2_655 ?
N2 Cd2 N1 88.06(12) . 2_655 ?
C18 Cd2 Cd2 147.45(17) . 2_655 ?
N1 Cd2 Cd2 45.29(8) . 2_655 ?
N2 Cd2 Cd2 89.19(9) . 2_655 ?
N1 Cd2 Cd2 43.68(7) 2_655 2_655 ?
C18 Cd2 Cd1 149.35(16) . . ?
N1 Cd2 Cd1 44.72(8) . . ?
N2 Cd2 Cd1 43.14(8) . . ?
N1 Cd2 Cd1 88.94(8) 2_655 . ?
Cd2 Cd2 Cd1 61.450(9) 2_655 . ?
C18 Cd2 Cd1 133.89(13) . 2_655 ?
N1 Cd2 Cd1 88.54(8) . 2_655 ?
N2 Cd2 Cd1 44.39(10) . 2_655 ?
N1 Cd2 Cd1 43.68(8) 2_655 2_655 ?
Cd2 Cd2 Cd1 59.597(10) 2_655 2_655 ?
Cd1 Cd2 Cd1 59.510(13) . 2_655 ?
P1 N1 Cd2 126.66(18) . . ?
P1 N1 Cd1 123.15(17) . . ?
Cd2 N1 Cd1 91.99(11) . . ?
P1 N1 Cd2 122.01(18) . 2_655 ?
Cd2 N1 Cd2 91.04(11) . 2_655 ?
Cd1 N1 Cd2 92.48(11) . 2_655 ?
P2 N2 Cd1 132.17(19) . . ?
P2 N2 Cd2 119.9(2) . . ?
Cd1 N2 Cd2 92.03(12) . . ?
P2 N2 Cd1 119.27(19) . 2_655 ?
Cd1 N2 Cd1 91.62(13) . 2_655 ?
Cd2 N2 Cd1 91.79(12) . 2_655 ?
N1 P1 C1A_b 118.8(4) . . ?
N1 P1 C3A_b 110.7(4) . . ?
C1A_b P1 C3A_b 106.1(7) . . ?
N1 P1 C5_a 117.3(5) . . ?
N1 P1 C3_a 114.9(3) . . ?
C5_a P1 C3_a 103.1(5) . . ?
N1 P1 C1_a 109.4(6) . . ?
C5_a P1 C1_a 108.3(9) . . ?
C3_a P1 C1_a 102.6(5) . . ?
N1 P1 C5A_b 111.0(4) . . ?
C1A_b P1 C5A_b 104.6(6) . . ?
C3A_b P1 C5A_b 104.7(6) . . ?
C2_a C1_a P1 125.8(13) . . ?
C4_a C3_a P1 115.0(7) . . ?
C6 C5_a P1 117.1(9) . . ?
C2A_b C1A_b P1 120.1(11) . . ?
C4A_b C3A_b P1 117.4(9) . . ?
C6 C5A_b P1 123.7(10) . . ?
N2 P2 C9 116.3(3) . . ?
N2 P2 C7 115.0(2) . . ?
C9 P2 C7 103.8(3) . . ?
N2 P2 C11 110.9(2) . . ?
C9 P2 C11 105.2(3) . . ?
C7 P2 C11 104.6(3) . . ?
C8A_b C7 P2 112.4(6) . . ?
C8_a C7 P2 125.8(6) . . ?
C10_a C9 P2 116.1(6) . . ?
C10A_b C9 P2 127.3(7) . . ?
C12 C11 P2 118.1(5) . . ?
C14 C13 Cd1 163.2(5) . . ?
C13 C14 Si1 172.8(5) . . ?
C15A_b Si1 C14 111.3(7) . . ?
C15_a Si1 C14 111.7(5) . . ?
C15_a Si1 C17_a 112.4(8) . . ?
C14 Si1 C17_a 111.8(5) . . ?
C15A_b Si1 C16A_b 112.5(16) . . ?
C14 Si1 C16A_b 111.4(7) . . ?
C15A_b Si1 C17A_b 107.9(9) . . ?
C14 Si1 C17A_b 103.6(6) . . ?
C16A_b Si1 C17A_b 109.9(14) . . ?
C15_a Si1 C16_a 106.9(8) . . ?
C14 Si1 C16_a 104.8(6) . . ?
C17_a Si1 C16_a 108.8(7) . . ?
C19 C18 Cd2 164.8(5) . . ?
C18 C19 Si2_a 164.6(6) . . ?
C18 C19 Si2A_b 164.8(6) . . ?
C21 Si2_a C20_a 106.5(17) . . ?
C21 Si2_a C22_a 100.1(11) . . ?
C20_a Si2_a C22_a 111.4(19) . . ?
C21 Si2_a C19 119.5(5) . . ?
C20_a Si2_a C19 101.6(10) . . ?
C22_a Si2_a C19 117.6(7) . . ?
C20A_b Si2A_b C22A_b 106.3(8) . . ?
C20A_b Si2A_b C19 111.6(6) . . ?
C22A_b Si2A_b C19 114.5(8) . . ?
C20A_b Si2A_b C21 122.0(8) . . ?
C22A_b Si2A_b C21 104.4(8) . . ?
C19 Si2A_b C21 98.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 C13 2.134(5) . ?
Cd1 N2 2.235(3) . ?
Cd1 N1 2.300(3) . ?
Cd1 N2 2.329(4) 2_655 ?
Cd1 Cd2 3.2670(5) . ?
Cd1 Cd1 3.2731(6) 2_655 ?
Cd1 Cd2 3.3273(5) 2_655 ?
Cd2 C18 2.133(5) . ?
Cd2 N1 2.241(3) . ?
Cd2 N2 2.305(3) . ?
Cd2 N1 2.307(3) 2_655 ?
Cd2 Cd2 3.2452(7) 2_655 ?
Cd2 Cd1 3.3272(5) 2_655 ?
N1 P1 1.580(3) . ?
N1 Cd2 2.307(3) 2_655 ?
N2 P2 1.582(4) . ?
N2 Cd1 2.329(4) 2_655 ?
P1 C1A_b 1.759(11) . ?
P1 C3A_b 1.803(11) . ?
P1 C5_a 1.807(14) . ?
P1 C3_a 1.826(9) . ?
P1 C1_a 1.841(14) . ?
P1 C5A_b 1.865(14) . ?
C1_a C2_a 1.436(17) . ?
C3_a C4_a 1.516(15) . ?
C5_a C6 1.451(14) . ?
C1A_b C2A_b 1.393(18) . ?
C3A_b C4A_b 1.532(16) . ?
C5A_b C6 1.278(14) . ?
P2 C9 1.796(6) . ?
P2 C7 1.797(6) . ?
P2 C11 1.822(6) . ?
C7 C8A_b 1.408(12) . ?
C7 C8_a 1.561(13) . ?
C9 C10_a 1.361(12) . ?
C9 C10A_b 1.483(17) . ?
C11 C12 1.524(8) . ?
C13 C14 1.193(7) . ?
C14 Si1 1.837(5) . ?
Si1 C15A_b 1.77(2) . ?
Si1 C15_a 1.822(17) . ?
Si1 C17_a 1.864(12) . ?
Si1 C16A_b 1.87(2) . ?
Si1 C17A_b 1.87(2) . ?
Si1 C16_a 1.899(16) . ?
C18 C19 1.198(7) . ?
C19 Si2_a 1.826(8) . ?
C19 Si2A_b 1.891(7) . ?
Si2_a C21 1.583(12) . ?
Si2_a C20_a 1.76(3) . ?
Si2_a C22_a 1.79(2) . ?
Si2A_b C20A_b 1.852(15) . ?
Si2A_b C22A_b 1.855(18) . ?
Si2A_b C21 2.009(11) . ?
|
1100604.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 22:03:05 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177996 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100604.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100604
loop_
_publ_author_name
'Harms, Klaus'
'Merle, Jan'
'Maichle-M\"ossmer, C\"acili\"a'
'Massa, Werner'
'Krieger, Matthias'
_publ_section_title
;
Heterocubane Phosphoraniminato Complexes of Cadmium
;
_journal_coden_ASTM INOCAJ
_journal_issue 5
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 1099
_journal_page_last 1104
_journal_paper_doi 10.1021/ic9710364
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C23 H57 Cd4 I4 N4 O P3 Si'
_chemical_formula_weight 1483.93
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 111.44(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 20.111(9)
_cell_length_b 11.9913(8)
_cell_length_c 20.655(10)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 203(2)
_cell_measurement_theta_max 12.0
_cell_measurement_theta_min 9.3
_cell_volume 4638.5(30)
_diffrn_ambient_temperature 203(2)
_diffrn_radiation_wavelength 0.70930
_exptl_absorpt_coefficient_mu 4.621
_exptl_absorpt_correction_T_max 0.9998
_exptl_absorpt_correction_T_min 0.7667
_exptl_absorpt_correction_type psi-scan
_refine_diff_density_max 1.015
_refine_diff_density_min -1.050
_refine_diff_density_rms 0.130
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.038
_refine_ls_goodness_of_fit_obs 1.066
_refine_ls_hydrogen_treatment calculated
_refine_ls_matrix_type full
_refine_ls_number_parameters 371
_refine_ls_number_reflns 10074
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.038
_refine_ls_restrained_S_obs 1.066
_refine_ls_R_factor_all 0.0617
_refine_ls_R_factor_obs 0.0385
_refine_ls_shift/esd_max 0.313
_refine_ls_shift/esd_mean 0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0386P)^2^+12.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.0903
_refine_ls_wR_factor_obs 0.0813
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0386P)^2^+12.4494P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0386P)^2^+12.4494P]
where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C23 H57 Cd4 I4 N4 O1 P3 Si1'
_cod_database_code 1100604
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,-1/2-y,-1/2+z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0342(2) 0.0326(2) 0.0340(2) 0.0044(2) 0.0162(2) 0.0028(2)
Cd2 0.0316(2) 0.0303(2) 0.0285(2) -0.0024(2) 0.0102(2) 0.0005(2)
Cd3 0.0294(2) 0.0297(2) 0.0370(2) -0.0048(2) 0.0113(2) -0.0008(2)
Cd4 0.0381(2) 0.0390(3) 0.0372(2) 0.0062(2) 0.0113(2) 0.0129(2)
I1 0.0495(3) 0.0624(3) 0.0630(3) 0.0071(2) 0.0361(2) -0.0021(2)
I2 0.0670(3) 0.0651(3) 0.0308(2) -0.0084(2) 0.0125(2) 0.0004(2)
I3 0.0437(2) 0.0364(2) 0.0791(4) -0.0154(2) 0.0127(2) -0.0070(2)
I4 0.0601(3) 0.0724(4) 0.0687(3) 0.0272(3) 0.0190(3) 0.0353(3)
Si1 0.0483(10) 0.0619(13) 0.0283(8) -0.0046(9) 0.0091(8) 0.0071(9)
P2 0.0280(7) 0.0284(8) 0.0336(8) 0.0043(6) 0.0106(6) 0.0039(6)
P3 0.0281(7) 0.0457(9) 0.0367(8) -0.0032(7) 0.0128(6) 0.0052(6)
P4 0.0783(14) 0.0245(9) 0.0812(15) 0.0010(9) 0.0412(12) -0.0059(9)
O1 0.038(2) 0.042(2) 0.032(2) -0.001(2) 0.008(2) 0.005(2)
N2 0.027(2) 0.023(2) 0.028(2) 0.001(2) 0.010(2) 0.001(2)
N3 0.028(2) 0.038(3) 0.033(3) -0.004(2) 0.013(2) 0.003(2)
N4 0.040(3) 0.031(3) 0.039(3) 0.003(2) 0.018(2) 0.003(2)
C111 0.089(6) 0.106(8) 0.041(4) 0.020(5) 0.022(4) 0.023(6)
C121 0.137(9) 0.073(6) 0.052(5) -0.010(5) 0.037(6) 0.019(6)
C131 0.068(6) 0.138(10) 0.058(6) -0.028(6) -0.002(5) -0.004(6)
C211 0.039(3) 0.031(3) 0.049(4) -0.001(3) 0.013(3) 0.007(3)
C212 0.082(6) 0.056(5) 0.057(5) -0.010(4) 0.031(4) 0.015(4)
C221 0.051(4) 0.044(4) 0.039(3) 0.014(3) 0.021(3) 0.015(3)
C222 0.057(4) 0.074(6) 0.068(5) 0.020(4) 0.031(4) 0.008(4)
C231 0.035(3) 0.039(4) 0.050(4) 0.000(3) 0.008(3) -0.002(3)
C232 0.034(3) 0.066(5) 0.064(5) 0.010(4) 0.007(3) 0.005(3)
C311 0.044(4) 0.056(4) 0.047(4) 0.009(3) 0.025(3) 0.005(3)
C312 0.050(4) 0.073(5) 0.069(5) 0.011(4) 0.033(4) 0.003(4)
C321 0.033(3) 0.065(5) 0.051(4) -0.002(4) 0.012(3) 0.004(3)
C322 0.053(5) 0.089(7) 0.066(5) -0.019(5) 0.004(4) -0.005(4)
C331 0.047(4) 0.065(5) 0.053(4) -0.022(4) 0.020(3) 0.007(3)
C332 0.082(6) 0.050(5) 0.106(7) -0.028(5) 0.056(5) -0.008(4)
C411 0.094(7) 0.041(5) 0.139(10) -0.017(6) 0.049(7) -0.001(5)
C412 0.100(8) 0.106(9) 0.123(10) -0.025(8) 0.050(8) 0.000(7)
C421 0.235(19) 0.090(10) 0.154(14) 0.030(10) 0.088(14) -0.030(11)
C422 0.089(8) 0.232(19) 0.088(9) 0.042(11) -0.007(7) 0.019(10)
C431 0.074(9) 0.081(10) 0.413(34) -0.109(15) 0.092(15) -0.054(8)
C43B 0.078(9) 0.056(7) 0.104(11) 0.018(7) -0.024(8) -0.010(6)
C43A 0.087(42) 0.166(69) 0.005(16) -0.046(26) 0.049(22) -0.088(45)
N1 0.085(6) 0.068(5) 0.093(6) 0.009(4) 0.044(5) -0.005(4)
C2 0.103(7) 0.049(5) 0.056(5) 0.004(4) 0.043(5) 0.009(5)
C3 0.120(10) 0.157(12) 0.070(7) 0.011(7) 0.035(7) 0.065(9)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cd1 Cd 0.66268(2) 0.23565(4) 0.01246(2) 0.03254(10) Uani 1 d . .
Cd2 Cd 0.70945(2) 0.21531(3) -0.12009(2) 0.03037(10) Uani 1 d . .
Cd3 Cd 0.78747(2) 0.39910(4) -0.00368(2) 0.03227(10) Uani 1 d . .
Cd4 Cd 0.81910(2) 0.12953(4) 0.02872(2) 0.03875(11) Uani 1 d . .
I1 I 0.56436(2) 0.22447(4) 0.07081(3) 0.05395(13) Uani 1 d . .
I2 I 0.66195(3) 0.19215(5) -0.25803(2) 0.05580(13) Uani 1 d . .
I3 I 0.83765(2) 0.60592(4) 0.02983(3) 0.05583(14) Uani 1 d . .
I4 I 0.91658(3) -0.01228(5) 0.10891(3) 0.0683(2) Uani 1 d . .
Si1 Si 0.80826(10) 0.2981(2) 0.16291(9) 0.0475(5) Uani 1 d . .
P2 P 0.61324(7) 0.44425(12) -0.10662(8) 0.0302(3) Uani 1 d . .
P3 P 0.88876(8) 0.25896(15) -0.07783(8) 0.0365(4) Uani 1 d . .
P4 P 0.66761(12) -0.02367(15) -0.04985(12) 0.0579(5) Uani 1 d . .
O1 O 0.7799(2) 0.2752(4) 0.0795(2) 0.0385(9) Uani 1 d . .
N2 N 0.6728(2) 0.3555(4) -0.0659(2) 0.0264(9) Uani 1 d . .
N3 N 0.8245(2) 0.2534(4) -0.0503(2) 0.0323(11) Uani 1 d . .
N4 N 0.7041(3) 0.0962(4) -0.0360(3) 0.0356(11) Uani 1 d . .
C111 C 0.7846(5) 0.1772(9) 0.2072(4) 0.079(3) Uani 1 d . .
H11A H 0.8000(5) 0.1921(9) 0.2566(4) 0.119 Uiso 1 calc R .
H11B H 0.8083(5) 0.1107(9) 0.1997(4) 0.119 Uiso 1 calc R .
H11C H 0.7333(5) 0.1659(9) 0.1882(4) 0.119 Uiso 1 calc R .
C121 C 0.7638(6) 0.4231(8) 0.1819(5) 0.087(3) Uani 1 d . .
H12A H 0.7807(6) 0.4351(8) 0.2318(5) 0.130 Uiso 1 calc R .
H12B H 0.7125(6) 0.4116(8) 0.1642(5) 0.130 Uiso 1 calc R .
H12C H 0.7750(6) 0.4879(8) 0.1597(5) 0.130 Uiso 1 calc R .
C131 C 0.9068(5) 0.3167(10) 0.1985(5) 0.095(3) Uani 1 d . .
H13A H 0.9241(5) 0.3151(10) 0.2489(5) 0.142 Uiso 1 calc R .
H13B H 0.9189(5) 0.3877(10) 0.1832(5) 0.142 Uiso 1 calc R .
H13C H 0.9289(5) 0.2568(10) 0.1819(5) 0.142 Uiso 1 calc R .
C211 C 0.6154(3) 0.5698(5) -0.0577(3) 0.0407(14) Uani 1 d . .
H21A H 0.6605(3) 0.6088(5) -0.0502(3) 0.049 Uiso 1 calc R .
H21B H 0.5765(3) 0.6186(5) -0.0857(3) 0.049 Uiso 1 calc R .
C212 C 0.6087(5) 0.5517(7) 0.0114(4) 0.064(2) Uani 1 d . .
H21C H 0.6103(5) 0.6231(7) 0.0341(4) 0.096 Uiso 1 calc R .
H21D H 0.6477(5) 0.5053(7) 0.0402(4) 0.096 Uiso 1 calc R .
H21E H 0.5636(5) 0.5151(7) 0.0046(4) 0.096 Uiso 1 calc R .
C221 C 0.6203(3) 0.4901(6) -0.1867(3) 0.044(2) Uani 1 d . .
H22A H 0.6066(3) 0.4284(6) -0.2202(3) 0.052 Uiso 1 calc R .
H22B H 0.5864(3) 0.5511(6) -0.2058(3) 0.052 Uiso 1 calc R .
C222 C 0.6948(4) 0.5297(7) -0.1787(4) 0.064(2) Uani 1 d . .
H22C H 0.6949(4) 0.5531(7) -0.2236(4) 0.096 Uiso 1 calc R .
H22D H 0.7285(4) 0.4692(7) -0.1609(4) 0.096 Uiso 1 calc R .
H22E H 0.7084(4) 0.5920(7) -0.1466(4) 0.096 Uiso 1 calc R .
C231 C 0.5242(3) 0.3864(5) -0.1302(4) 0.0433(15) Uani 1 d . .
H23A H 0.5204(3) 0.3217(5) -0.1603(4) 0.052 Uiso 1 calc R .
H23B H 0.5184(3) 0.3595(5) -0.0878(4) 0.052 Uiso 1 calc R .
C232 C 0.4626(3) 0.4658(7) -0.1673(4) 0.058(2) Uani 1 d . .
H23C H 0.4175(3) 0.4270(7) -0.1776(4) 0.087 Uiso 1 calc R .
H23D H 0.4665(3) 0.4914(7) -0.2103(4) 0.087 Uiso 1 calc R .
H23E H 0.4646(3) 0.5293(7) -0.1375(4) 0.087 Uiso 1 calc R .
C311 C 0.8864(4) 0.3865(6) -0.1259(4) 0.047(2) Uani 1 d . .
H31A H 0.8407(4) 0.3891(6) -0.1651(4) 0.056 Uiso 1 calc R .
H31B H 0.8874(4) 0.4497(6) -0.0955(4) 0.056 Uiso 1 calc R .
C312 C 0.9455(4) 0.4033(7) -0.1539(4) 0.061(2) Uani 1 d . .
H31C H 0.9386(4) 0.4738(7) -0.1785(4) 0.091 Uiso 1 calc R .
H31D H 0.9444(4) 0.3430(7) -0.1856(4) 0.091 Uiso 1 calc R .
H31E H 0.9913(4) 0.4038(7) -0.1157(4) 0.091 Uiso 1 calc R .
C321 C 0.9765(3) 0.2470(7) -0.0099(4) 0.050(2) Uani 1 d . .
H32A H 0.9806(3) 0.1734(7) 0.0118(4) 0.061 Uiso 1 calc R .
H32B H 1.0127(3) 0.2515(7) -0.0312(4) 0.061 Uiso 1 calc R .
C322 C 0.9921(4) 0.3335(8) 0.0450(4) 0.074(3) Uani 1 d . .
H32C H 1.0397(4) 0.3219(8) 0.0793(4) 0.111 Uiso 1 calc R .
H32D H 0.9573(4) 0.3286(8) 0.0673(4) 0.111 Uiso 1 calc R .
H32E H 0.9895(4) 0.4068(8) 0.0243(4) 0.111 Uiso 1 calc R .
C331 C 0.8859(4) 0.1466(6) -0.1386(4) 0.054(2) Uani 1 d . .
H33A H 0.8432(4) 0.1560(6) -0.1807(4) 0.065 Uiso 1 calc R .
H33B H 0.9277(4) 0.1531(6) -0.1521(4) 0.065 Uiso 1 calc R .
C332 C 0.8848(5) 0.0317(7) -0.1099(5) 0.073(3) Uani 1 d . .
H33C H 0.8833(5) -0.0235(7) -0.1447(5) 0.110 Uiso 1 calc R .
H33D H 0.8429(5) 0.0237(7) -0.0975(5) 0.110 Uiso 1 calc R .
H33E H 0.9275(5) 0.0209(7) -0.0689(5) 0.110 Uiso 1 calc R .
C411 C 0.7154(6) -0.1282(7) -0.0747(6) 0.089(3) Uani 1 d . .
H41A H 0.7659(6) -0.1227(7) -0.0446(6) 0.107 Uiso 1 calc R .
H41B H 0.6980(6) -0.2012(7) -0.0664(6) 0.107 Uiso 1 calc R .
C412 C 0.7100(6) -0.1232(10) -0.1480(7) 0.107(4) Uani 1 d . .
H41C H 0.7377(6) -0.1833(10) -0.1570(7) 0.160 Uiso 1 calc R .
H41D H 0.7283(6) -0.0522(10) -0.1566(7) 0.160 Uiso 1 calc R .
H41E H 0.6603(6) -0.1309(10) -0.1784(7) 0.160 Uiso 1 calc R .
C421 C 0.6463(10) -0.0825(12) 0.0214(8) 0.155(6) Uani 1 d . .
H42A H 0.6158(10) -0.0298(12) 0.0339(8) 0.186 Uiso 1 calc R .
H42B H 0.6188(10) -0.1511(12) 0.0051(8) 0.186 Uiso 1 calc R .
C422 C 0.7033(7) -0.1059(15) 0.0786(7) 0.147(6) Uani 1 d . .
H42C H 0.6875(7) -0.1368(15) 0.1139(7) 0.221 Uiso 1 calc R .
H42D H 0.7303(7) -0.0381(15) 0.0961(7) 0.221 Uiso 1 calc R .
H42E H 0.7334(7) -0.1596(15) 0.0672(7) 0.221 Uiso 1 calc R .
C431 C 0.5778(8) -0.0217(14) -0.1103(13) 0.188(12) Uani 1 d . .
H43A H 0.5818(8) -0.0237(14) -0.1562(13) 0.226 Uiso 1 calc R 1
H43B H 0.5579(8) -0.0942(14) -0.1048(13) 0.226 Uiso 1 calc R 1
C43B C 0.5236(7) 0.0541(10) -0.1172(8) 0.096(7) Uani 0.82(3) d P 1
H43C H 0.4808(7) 0.0318(10) -0.1555(8) 0.143 Uiso 0.82(3) calc PR 1
H43D H 0.5383(7) 0.1277(10) -0.1263(8) 0.143 Uiso 0.82(3) calc PR 1
H43E H 0.5138(7) 0.0559(10) -0.0746(8) 0.143 Uiso 0.82(3) calc PR 1
C43A C 0.5693(34) -0.0091(70) -0.1296(20) 0.077(30) Uani 0.18(3) d P 2
H43F H 0.5414(34) 0.0478(70) -0.1178(20) 0.116 Uiso 0.18(3) calc PR 2
H43G H 0.5443(34) -0.0799(70) -0.1362(20) 0.116 Uiso 0.18(3) calc PR 2
H43H H 0.5761(34) 0.0116(70) -0.1721(20) 0.116 Uiso 0.18(3) calc PR 2
N1 N 0.4847(5) 0.2617(7) 0.2209(5) 0.078(2) Uani 1 d . .
C2 C 0.5435(6) 0.2520(7) 0.2453(5) 0.066(2) Uani 1 d . .
C3 C 0.6214(6) 0.2430(11) 0.2769(5) 0.116(5) Uani 1 d . .
H3A H 0.6366(6) 0.1733(11) 0.2629(5) 0.173 Uiso 1 calc R .
H3B H 0.6361(6) 0.2449(11) 0.3272(5) 0.173 Uiso 1 calc R .
H3C H 0.6432(6) 0.3048(11) 0.2617(5) 0.173 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cd 1.40
I 1.40
N 0.68
O 0.68
P 1.05
Si 1.20
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cd1 N4 90.5(2) . . ?
N2 Cd1 O1 87.7(2) . . ?
N4 Cd1 O1 87.5(2) . . ?
N2 Cd1 I1 129.75(11) . . ?
N4 Cd1 I1 128.15(13) . . ?
O1 Cd1 I1 120.15(11) . . ?
N2 Cd1 Cd2 45.34(11) . . ?
N4 Cd1 Cd2 45.25(12) . . ?
O1 Cd1 Cd2 88.54(11) . . ?
I1 Cd1 Cd2 151.30(2) . . ?
N2 Cd1 Cd3 42.96(11) . . ?
N4 Cd1 Cd3 88.67(13) . . ?
O1 Cd1 Cd3 44.76(11) . . ?
I1 Cd1 Cd3 142.45(2) . . ?
Cd2 Cd1 Cd3 59.18(2) . . ?
N2 Cd1 Cd4 89.24(11) . . ?
N4 Cd1 Cd4 42.73(13) . . ?
O1 Cd1 Cd4 44.73(11) . . ?
I1 Cd1 Cd4 140.51(3) . . ?
Cd2 Cd1 Cd4 59.46(2) . . ?
Cd3 Cd1 Cd4 60.42(3) . . ?
N3 Cd2 N4 87.8(2) . . ?
N3 Cd2 N2 88.7(2) . . ?
N4 Cd2 N2 88.5(2) . . ?
N3 Cd2 I2 125.48(12) . . ?
N4 Cd2 I2 130.59(13) . . ?
N2 Cd2 I2 123.05(11) . . ?
N3 Cd2 Cd1 89.49(12) . . ?
N4 Cd2 Cd1 44.66(12) . . ?
N2 Cd2 Cd1 43.92(11) . . ?
I2 Cd2 Cd1 144.69(3) . . ?
N3 Cd2 Cd3 44.41(12) . . ?
N4 Cd2 Cd3 90.26(13) . . ?
N2 Cd2 Cd3 44.48(11) . . ?
I2 Cd2 Cd3 139.12(2) . . ?
Cd1 Cd2 Cd3 61.65(3) . . ?
N3 Cd2 Cd4 43.90(12) . . ?
N4 Cd2 Cd4 43.98(13) . . ?
N2 Cd2 Cd4 89.94(11) . . ?
I2 Cd2 Cd4 146.86(3) . . ?
Cd1 Cd2 Cd4 61.54(3) . . ?
Cd3 Cd2 Cd4 61.95(2) . . ?
N3 Cd3 N2 90.4(2) . . ?
N3 Cd3 O1 86.6(2) . . ?
N2 Cd3 O1 86.80(15) . . ?
N3 Cd3 I3 132.77(12) . . ?
N2 Cd3 I3 124.97(11) . . ?
O1 Cd3 I3 121.57(10) . . ?
N3 Cd3 Cd2 45.19(12) . . ?
N2 Cd3 Cd2 45.34(11) . . ?
O1 Cd3 Cd2 88.26(11) . . ?
I3 Cd3 Cd2 149.81(2) . . ?
N3 Cd3 Cd1 88.03(12) . . ?
N2 Cd3 Cd1 42.43(11) . . ?
O1 Cd3 Cd1 44.38(10) . . ?
I3 Cd3 Cd1 139.02(2) . . ?
Cd2 Cd3 Cd1 59.17(2) . . ?
N3 Cd3 Cd4 42.26(13) . . ?
N2 Cd3 Cd4 88.35(11) . . ?
O1 Cd3 Cd4 44.39(10) . . ?
I3 Cd3 Cd4 145.72(2) . . ?
Cd2 Cd3 Cd4 59.25(2) . . ?
Cd1 Cd3 Cd4 59.82(2) . . ?
N3 Cd4 N4 89.8(2) . . ?
N3 Cd4 O1 86.9(2) . . ?
N4 Cd4 O1 87.5(2) . . ?
N3 Cd4 I4 131.01(12) . . ?
N4 Cd4 I4 128.37(13) . . ?
O1 Cd4 I4 119.61(10) . . ?
N3 Cd4 Cd2 44.92(12) . . ?
N4 Cd4 Cd2 44.97(13) . . ?
O1 Cd4 Cd2 87.89(10) . . ?
I4 Cd4 Cd2 152.46(2) . . ?
N3 Cd4 Cd1 88.14(11) . . ?
N4 Cd4 Cd1 43.13(13) . . ?
O1 Cd4 Cd1 44.34(10) . . ?
I4 Cd4 Cd1 140.16(3) . . ?
Cd2 Cd4 Cd1 59.01(3) . . ?
N3 Cd4 Cd3 42.48(12) . . ?
N4 Cd4 Cd3 88.40(13) . . ?
O1 Cd4 Cd3 44.37(11) . . ?
I4 Cd4 Cd3 142.31(2) . . ?
Cd2 Cd4 Cd3 58.805(13) . . ?
Cd1 Cd4 Cd3 59.755(14) . . ?
O1 Si1 C131 110.4(4) . . ?
O1 Si1 C121 110.4(3) . . ?
C131 Si1 C121 110.3(5) . . ?
O1 Si1 C111 109.6(3) . . ?
C131 Si1 C111 108.9(5) . . ?
C121 Si1 C111 107.1(4) . . ?
N2 P2 C221 113.2(3) . . ?
N2 P2 C211 113.7(3) . . ?
C221 P2 C211 105.4(3) . . ?
N2 P2 C231 111.4(3) . . ?
C221 P2 C231 105.8(3) . . ?
C211 P2 C231 106.8(3) . . ?
N3 P3 C321 114.0(3) . . ?
N3 P3 C311 111.6(3) . . ?
C321 P3 C311 108.3(3) . . ?
N3 P3 C331 112.9(3) . . ?
C321 P3 C331 104.5(3) . . ?
C311 P3 C331 104.9(4) . . ?
N4 P4 C411 115.4(4) . . ?
N4 P4 C431 113.3(6) . . ?
C411 P4 C431 109.1(7) . . ?
N4 P4 C421 115.7(6) . . ?
C411 P4 C421 105.9(7) . . ?
C431 P4 C421 95.5(9) . . ?
N4 P4 C43A 108.1(22) . . ?
C411 P4 C43A 107.0(19) . . ?
C431 P4 C43A 8.4(15) . . ?
C421 P4 C43A 103.8(11) . . ?
Si1 O1 Cd1 123.8(2) . . ?
Si1 O1 Cd3 125.8(2) . . ?
Cd1 O1 Cd3 90.87(14) . . ?
Si1 O1 Cd4 124.0(2) . . ?
Cd1 O1 Cd4 90.93(15) . . ?
Cd3 O1 Cd4 91.24(15) . . ?
P2 N2 Cd1 124.3(2) . . ?
P2 N2 Cd3 124.2(2) . . ?
Cd1 N2 Cd3 94.6(2) . . ?
P2 N2 Cd2 123.2(2) . . ?
Cd1 N2 Cd2 90.7(2) . . ?
Cd3 N2 Cd2 90.2(2) . . ?
P3 N3 Cd4 123.3(3) . . ?
P3 N3 Cd3 124.1(3) . . ?
Cd4 N3 Cd3 95.3(2) . . ?
P3 N3 Cd2 123.4(3) . . ?
Cd4 N3 Cd2 91.2(2) . . ?
Cd3 N3 Cd2 90.4(2) . . ?
P4 N4 Cd4 125.1(3) . . ?
P4 N4 Cd1 121.8(3) . . ?
Cd4 N4 Cd1 94.1(2) . . ?
P4 N4 Cd2 125.1(3) . . ?
Cd4 N4 Cd2 91.1(2) . . ?
Cd1 N4 Cd2 90.1(2) . . ?
C212 C211 P2 114.9(5) . . ?
C222 C221 P2 113.6(5) . . ?
C232 C231 P2 115.9(5) . . ?
C312 C311 P3 117.0(5) . . ?
C322 C321 P3 114.1(5) . . ?
C332 C331 P3 113.8(6) . . ?
C412 C411 P4 115.1(8) . . ?
C422 C421 P4 114.7(14) . . ?
C43B C431 P4 129.7(12) . . ?
N1 C2 C3 178.1(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N2 2.230(4) . ?
Cd1 N4 2.259(5) . ?
Cd1 O1 2.304(4) . ?
Cd1 I1 2.6692(11) . ?
Cd1 Cd2 3.2142(14) . ?
Cd1 Cd3 3.2941(11) . ?
Cd1 Cd4 3.2963(14) . ?
Cd2 N3 2.281(5) . ?
Cd2 N4 2.283(5) . ?
Cd2 N2 2.287(4) . ?
Cd2 I2 2.6688(14) . ?
Cd2 Cd3 3.2144(9) . ?
Cd2 Cd4 3.2293(14) . ?
Cd3 N3 2.249(5) . ?
Cd3 N2 2.252(4) . ?
Cd3 O1 2.320(4) . ?
Cd3 I3 2.6702(6) . ?
Cd3 Cd4 3.3163(7) . ?
Cd4 N3 2.240(5) . ?
Cd4 N4 2.243(5) . ?
Cd4 O1 2.320(4) . ?
Cd4 I4 2.6676(9) . ?
Si1 O1 1.628(4) . ?
Si1 C131 1.858(9) . ?
Si1 C121 1.860(9) . ?
Si1 C111 1.866(10) . ?
P2 N2 1.595(4) . ?
P2 C221 1.798(6) . ?
P2 C211 1.804(6) . ?
P2 C231 1.811(6) . ?
P3 N3 1.592(5) . ?
P3 C321 1.815(6) . ?
P3 C311 1.815(7) . ?
P3 C331 1.828(7) . ?
P4 N4 1.591(5) . ?
P4 C411 1.767(9) . ?
P4 C431 1.78(2) . ?
P4 C421 1.818(14) . ?
P4 C43A 2.07(7) . ?
C211 C212 1.500(10) . ?
C221 C222 1.521(9) . ?
C231 C232 1.530(9) . ?
C311 C312 1.513(9) . ?
C321 C322 1.483(11) . ?
C331 C332 1.504(11) . ?
C411 C412 1.48(2) . ?
C421 C422 1.34(2) . ?
C431 C43B 1.39(2) . ?
N1 C2 1.110(11) . ?
C2 C3 1.465(15) . ?
|
1100605.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 02:29:13 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177972 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100605.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100605
loop_
_publ_author_name
'Boche, Gernot'
'Bosold, Ferdinand'
'Marsch, Michael'
'Harms, Klaus'
_publ_section_title
;
The Crystal Structures of a Lower Order and a "Higher Order" Cyanocuprate:
[tBuCu(CN)Li(OEt~2~)~2~]~\\infty ~ and [tBuCutBu{Li(thf)(pmdeta)}~2~CN]
;
_journal_coden_ASTM ACIEF5
_journal_issue 12
_journal_name_full 'Angewandte Chemie, International Edition'
_journal_page_first 1684
_journal_page_last 1686
_journal_paper_doi
10.1002/(sici)1521-3773(19980703)37:12<1684::aid-anie1684>3.0.co;2-2
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C44 H98 Cu2 Li4 N4 O8'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 91.095(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.0874(10)
_cell_length_b 14.9790(11)
_cell_length_c 19.4176(16)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100605
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Cu1 Cu 0.23794(7) -0.29789(6) -0.07214(5)
Cu2 Cu 0.24920(7) -0.20374(6) 0.04716(4)
N1 N 0.0590(5) -0.4103(4) -0.0070(3)
N2 N 0.0570(5) -0.0893(4) -0.0021(3)
C1 C 0.1284(6) -0.3668(4) -0.0300(4)
C2 C 0.3455(7) -0.2371(5) -0.1309(4)
C3 C 0.3595(8) -0.1380(6) -0.1103(5)
H1 H 0.40970 -0.10870 -0.14220
H2 H 0.28730 -0.10830 -0.11230
H3 H 0.39040 -0.13430 -0.06340
C4 C 0.3034(8) -0.2421(7) -0.2052(5)
H4 H 0.35030 -0.20510 -0.23430
H5 H 0.30590 -0.30420 -0.22110
H6 H 0.22710 -0.22030 -0.20800
C5 C 0.4591(8) -0.2792(6) -0.1275(5)
H7 H 0.50880 -0.24670 -0.15790
H8 H 0.48810 -0.27650 -0.08010
H9 H 0.45400 -0.34170 -0.14230
C6 C 0.1310(6) -0.1346(5) 0.0145(4)
C7 C 0.3706(7) -0.2603(5) 0.0983(4)
C8 C 0.4818(7) -0.2179(6) 0.0823(5)
H10 H 0.53890 -0.24180 0.11370
H11 H 0.50130 -0.23160 0.03460
H12 H 0.47690 -0.15300 0.08810
C9 C 0.3792(8) -0.3611(5) 0.0840(5)
H13 H 0.44770 -0.38440 0.10500
H14 H 0.31560 -0.39180 0.10370
H15 H 0.37970 -0.37130 0.03410
C10 C 0.3513(8) -0.2496(7) 0.1749(5)
H16 H 0.41550 -0.27260 0.20090
H17 H 0.34100 -0.18630 0.18570
H18 H 0.28510 -0.28310 0.18760
Li1 Li 0.057(1) -0.5380(8) -0.0575(6)
Li2 Li 0.0790(11) 0.0370(9) 0.0472(7)
O1 O 0.2072(5) -0.5886(4) -0.0616(3)
C11 C 0.2872(8) -0.5896(6) -0.0084(5)
H19 H 0.34100 -0.63820 -0.01640
H20 H 0.32780 -0.53220 -0.00750
C12 C 0.2309(9) -0.6041(7) 0.0597(5)
H21 H 0.28690 -0.60630 0.09690
H22 H 0.17960 -0.55480 0.06810
H23 H 0.18990 -0.66050 0.05830
C13 C 0.2591(7) -0.5940(6) -0.1290(5)
H24 H 0.30520 -0.64860 -0.13030
H25 H 0.20030 -0.60010 -0.16490
C14 C 0.3298(8) -0.5157(7) -0.1464(5)
H26 H 0.35300 -0.52040 -0.19440
H27 H 0.28750 -0.46050 -0.14040
H28 H 0.39530 -0.51470 -0.11590
O2 O -0.0050(4) -0.5292(3) -0.1515(3)
C15 C -0.0553(8) -0.5995(5) -0.1913(4)
H29 H -0.13550 -0.58790 -0.19730
H30 H -0.02210 -0.60170 -0.23750
C16 C -0.0376(7) -0.6875(5) -0.1550(4)
H31 H -0.06330 -0.73620 -0.18490
H32 H 0.04130 -0.69530 -0.14420
H33 H -0.07940 -0.68810 -0.11220
C17 C -0.0155(8) -0.4433(5) -0.1860(4)
H34 H -0.09130 -0.43780 -0.20580
H35 H -0.00520 -0.39510 -0.15150
C18 C 0.0654(8) -0.4311(6) -0.2416(5)
H36 H 0.05720 -0.37120 -0.26120
H37 H 0.14060 -0.43840 -0.22260
H38 H 0.05190 -0.47580 -0.27760
O3 O 0.0587(5) 0.0323(3) 0.1476(3)
C19 C -0.0037(8) 0.1020(5) 0.1790(5)
H39 H 0.00820 0.10030 0.22960
H40 H -0.08350 0.09300 0.16910
C20 C 0.0315(10) 0.1907(5) 0.1520(5)
H41 H -0.00680 0.23820 0.17680
H42 H 0.01260 0.19460 0.10270
H43 H 0.11160 0.19760 0.15860
C21 C 0.0544(7) -0.0506(5) 0.1863(4)
H44 H 0.07210 -0.10100 0.15550
H45 H -0.02180 -0.05960 0.20280
C22 C 0.1333(9) -0.0514(7) 0.2469(5)
H46 H 0.12370 -0.10670 0.27300
H47 H 0.11830 -0.00010 0.27660
H48 H 0.20940 -0.04790 0.23060
O4 O 0.2132(5) 0.0997(4) 0.0205(3)
C23 C 0.2041(10) 0.1589(7) -0.0397(6)
H49 H 0.25980 0.20710 -0.03520
H50 H 0.12990 0.18690 -0.04090
C24 C 0.2211(10) 0.1104(7) -0.1050(5)
H51 H 0.21130 0.15160 -0.14380
H52 H 0.16710 0.06180 -0.10920
H53 H 0.29610 0.08560 -0.10520
C25 C 0.3230(8) 0.0785(8) 0.0364(6)
H54 H 0.36820 0.13360 0.03650
H55 H 0.35200 0.03800 0.00080
C26 C 0.3321(9) 0.0347(8) 0.1053(6)
H56 H 0.41040 0.02750 0.11820
H57 H 0.29650 -0.02410 0.10320
H58 H 0.29550 0.07170 0.13960
Li1B* Li -0.057(1) -0.4620(8) 0.0575(6)
Li2B Li -0.0790(11) -0.0370(9) -0.0472(7)
N1B* N -0.0590(5) -0.5897(4) 0.0070(3)
C1B* C -0.1284(6) -0.6332(4) 0.0300(4)
Cu2B Cu -0.24920(7) 0.20374(6) -0.04716(4)
N2B N -0.0570(5) 0.0893(4) 0.0021(3)
C6B C -0.1310(6) 0.1346(5) -0.0145(4)
O1B* O -0.2072(5) -0.4114(4) 0.0616(3)
C11B* C -0.2872(8) -0.4104(6) 0.0084(5)
H19B* H -0.34100 -0.36180 0.01640
H20B* H -0.32780 -0.46780 0.00750
C12B* C -0.2309(9) -0.3959(7) -0.0597(5)
H21B* H -0.28690 -0.39370 -0.09690
H22B* H -0.17960 -0.44520 -0.06810
H23B* H -0.18990 -0.33950 -0.05830
C13B* C -0.2591(7) -0.4060(6) 0.1290(5)
H24B* H -0.30520 -0.35140 0.13030
H25B* H -0.20030 -0.39990 0.16490
C14B* C -0.3298(8) -0.4843(7) 0.1464(5)
H26B* H -0.35300 -0.47960 0.19440
H27B* H -0.28750 -0.53950 0.14040
H28B* H -0.39530 -0.48530 0.11590
O2B* O 0.0050(4) -0.4708(3) 0.1515(3)
C15B* C 0.0553(8) -0.4005(5) 0.1913(4)
H29B* H 0.13550 -0.41210 0.19730
H30B* H 0.02210 -0.39830 0.23750
C16B* C 0.0376(7) -0.3125(5) 0.1550(4)
H31B* H 0.06330 -0.26380 0.18490
H32B* H -0.04130 -0.30470 0.14420
H33B* H 0.07940 -0.31190 0.11220
C17B* C 0.0155(8) -0.5567(5) 0.1860(4)
H34B* H 0.09130 -0.56220 0.20580
H35B* H 0.00520 -0.60490 0.15150
C18B* C -0.0654(8) -0.5689(6) 0.2416(5)
H36B* H -0.05720 -0.62880 0.26120
H37B* H -0.14060 -0.56160 0.22260
H38B* H -0.05190 -0.52420 0.27760
O3B O -0.0587(5) -0.0323(3) -0.1476(3)
C19B C 0.0037(8) -0.1020(5) -0.1790(5)
H39B H -0.00820 -0.10030 -0.22960
H40B H 0.08350 -0.09300 -0.16910
C20B C -0.0315(10) -0.1907(5) -0.1520(5)
H41B H 0.00680 -0.23820 -0.17680
H42B H -0.01260 -0.19460 -0.10270
H43B H -0.11160 -0.19760 -0.15860
C21B C -0.0544(7) 0.0506(5) -0.1863(4)
H44B H -0.07210 0.10100 -0.15550
H45B H 0.02180 0.05960 -0.20280
C22B C -0.1333(9) 0.0514(7) -0.2469(5)
H46B H -0.12370 0.10670 -0.27300
H47B H -0.11830 0.00010 -0.27660
H48B H -0.20940 0.04790 -0.23060
O4B O -0.2132(5) -0.0997(4) -0.0205(3)
C23B C -0.2041(10) -0.1589(7) 0.0397(6)
H49B H -0.25980 -0.20710 0.03520
H50B H -0.12990 -0.18690 0.04090
C24B C -0.2211(10) -0.1104(7) 0.1050(5)
H51B H -0.21130 -0.15160 0.14380
H52B H -0.16710 -0.06180 0.10920
H53B H -0.29610 -0.08560 0.10520
C25B C -0.3230(8) -0.0785(8) -0.0364(6)
H54B H -0.36820 -0.13360 -0.03650
H55B H -0.35200 -0.03800 -0.00080
C26B C -0.3321(9) -0.0347(8) -0.1053(6)
H56B H -0.41040 -0.02750 -0.11820
H57B H -0.29650 0.02410 -0.10320
H58B H -0.29550 -0.07170 -0.13960
Cu1B* Cu -0.23794(7) -0.70211(6) 0.07214(5)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cu 1.52
Li 1.07
N 0.68
O 0.68
|
1100606.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 02:29:13 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177972 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100606.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100606
loop_
_publ_author_name
'Boche, Gernot'
'Bosold, Ferdinand'
'Marsch, Michael'
'Harms, Klaus'
_publ_section_title
;
The Crystal Structures of a Lower Order and a "Higher Order" Cyanocuprate:
[tBuCu(CN)Li(OEt~2~)~2~]~\\infty ~ and [tBuCutBu{Li(thf)(pmdeta)}~2~CN]
;
_journal_coden_ASTM ACIEF5
_journal_issue 12
_journal_name_full 'Angewandte Chemie, International Edition'
_journal_page_first 1684
_journal_page_last 1686
_journal_paper_doi
10.1002/(sici)1521-3773(19980703)37:12<1684::aid-anie1684>3.0.co;2-2
_journal_volume 37
_journal_year 1998
_chemical_formula_sum 'C35 H80 Cu Li2 N7 O2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 100.950(11)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 9.1693(8)
_cell_length_b 14.9849(9)
_cell_length_c 16.6183(16)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C35 H80 Cu1 Li2 N7 O2'
_cod_database_code 1100606
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Cu1 Cu 1.00000 0.50000 0.50000
C1 C 0.8168(4) 0.4340(3) 0.5026(3)
C2 C 0.6854(10) 0.4719(9) 0.4388(7)
H1 H 0.59510 0.43780 0.44130
H2 H 0.70850 0.46700 0.38370
H3 H 0.66990 0.53470 0.45120
C3 C 0.8368(12) 0.3379(6) 0.4796(9)
H4 H 0.74520 0.30470 0.48090
H5 H 0.91890 0.31140 0.51880
H6 H 0.85930 0.33520 0.42440
C4 C 0.7699(12) 0.4383(8) 0.5830(6)
H7 H 0.67800 0.40410 0.58050
H8 H 0.75260 0.50070 0.59640
H9 H 0.84800 0.41310 0.62540
C5? C 0.717(2) 0.4887(13) 0.547(2)
H10? H 0.62540 0.45550 0.54820
H11? H 0.69240 0.54540 0.51810
H12? H 0.76860 0.50060 0.60310
C6? C 0.746(3) 0.406(2) 0.4191(13)
H13? H 0.65420 0.37300 0.42150
H14? H 0.81380 0.36750 0.39600
H15? H 0.72170 0.45880 0.38430
C7? C 0.8433(16) 0.3481(13) 0.5541(16)
H16? H 0.74830 0.31790 0.55350
H17? H 0.88880 0.36330 0.61070
H18? H 0.90980 0.30840 0.53100
Li1 Li 0.6251(8) 0.9031(4) 0.6307(4)
N1 N 0.5261(5) 0.9795(3) 0.5286(3)
C8 C 0.5261(5) 0.9795(3) 0.5286(3)
N2 N 0.4200(5) 0.9011(3) 0.6886(3)
N3 N 0.6762(5) 0.7829(3) 0.7231(2)
N4 N 0.7310(4) 0.8047(2) 0.55873(19)
C9 C 0.4576(10) 0.8383(5) 0.7617(5)
H19 H 0.51510 0.87210 0.80830
H20 H 0.36360 0.81940 0.77760
C10 C 0.5365(9) 0.7633(5) 0.7500(4)
H21 H 0.47440 0.72490 0.70850
H22 H 0.55860 0.72930 0.80200
C11 C 0.7134(7) 0.7077(3) 0.6722(3)
H23 H 0.76630 0.66080 0.70840
H24 H 0.62050 0.68140 0.64110
C12 C 0.8062(6) 0.7368(3) 0.6150(3)
H25 H 0.83050 0.68490 0.58310
H26 H 0.90040 0.76150 0.64600
C13 C 0.3954(8) 0.9884(3) 0.7204(4)
H27 H 0.30720 0.98670 0.74570
H28 H 0.38030 1.03180 0.67550
H29 H 0.48210 1.00570 0.76150
C14 C 0.2896(7) 0.8783(5) 0.6270(5)
H30 H 0.20150 0.87740 0.65240
H31 H 0.30360 0.81930 0.60420
H32 H 0.27620 0.92280 0.58300
C15 C 0.8008(7) 0.8026(4) 0.7923(3)
H33 H 0.81830 0.75080 0.82890
H34 H 0.77530 0.85440 0.82290
H35 H 0.89090 0.81550 0.77080
C16 C 0.6104(6) 0.7666(3) 0.4979(3)
H36 H 0.65120 0.72270 0.46440
H37 H 0.56080 0.81430 0.46250
H38 H 0.53850 0.73740 0.52590
C17 C 0.8375(6) 0.8464(4) 0.5150(3)
H39 H 0.88100 0.80070 0.48450
H40 H 0.91640 0.87530 0.55440
H41 H 0.78650 0.89120 0.47670
O1 O 0.7683(5) 0.9966(2) 0.6871(3)
C18 C 0.7252(10) 1.0918(5) 0.6789(7)
H42 H 0.64900 1.10100 0.62880
H43 H 0.68350 1.11110 0.72680
C19 C 0.8435(9) 1.1377(5) 0.6746(11)
H44 H 0.88370 1.16780 0.72720
H45 H 0.82430 1.18250 0.63010
C20 C 0.9396(18) 1.0688(10) 0.6572(15)
H46 H 1.04520 1.08720 0.66870
H47 H 0.91190 1.04690 0.60010
C21 C 0.9032(11) 0.9989(6) 0.7214(9)
H48 H 0.95490 0.94110 0.71950
H49 H 0.91940 1.02230 0.77810
C1B* C 1.1832(4) 0.5660(3) 0.4974(3)
C2B* C 1.3146(10) 0.5281(9) 0.5612(7)
H1B* H 1.40490 0.56220 0.55870
H2B* H 1.29150 0.53300 0.61630
H3B* H 1.33010 0.46530 0.54880
C3B* C 1.1632(12) 0.6621(6) 0.5204(9)
H4B* H 1.25480 0.69530 0.51910
H5B* H 1.08110 0.68860 0.48120
H6B* H 1.14070 0.66480 0.57560
C4B* C 1.2301(12) 0.5617(8) 0.4170(6)
H7B* H 1.32200 0.59590 0.41950
H8B* H 1.24740 0.49930 0.40360
H9B* H 1.15200 0.58690 0.37460
N1B* N 0.4739(5) 1.0205(3) 0.4714(3)
Li1B* Li 0.3749(8) 1.0969(4) 0.3693(4)
N2B* N 0.5800(5) 1.0989(3) 0.3114(3)
C9B* C 0.5424(10) 1.1617(5) 0.2383(5)
H19B* H 0.48490 1.12790 0.19170
H20B* H 0.63640 1.18060 0.22240
C10B* C 0.4635(9) 1.2367(5) 0.2500(4)
N3B* N 0.3238(5) 1.2171(3) 0.2769(2)
N4B* N 0.2690(4) 1.1953(2) 0.44127(19)
C12B* C 0.1938(6) 1.2632(3) 0.3850(3)
C11B* C 0.2866(7) 1.2923(3) 0.3278(3)
C15B* C 0.1992(7) 1.1974(4) 0.2077(3)
H33B* H 0.18170 1.24920 0.17110
H34B* H 0.22470 1.14560 0.17710
H35B* H 0.10910 1.18450 0.22920
H23B* H 0.23370 1.33920 0.29160
H24B* H 0.37950 1.31860 0.35890
H25B* H 0.16950 1.31510 0.41690
H26B* H 0.09960 1.23850 0.35400
C16B* C 0.3896(6) 1.2334(3) 0.5021(3)
H36B* H 0.34880 1.27730 0.53560
H37B* H 0.43920 1.18570 0.53750
H38B* H 0.46150 1.26260 0.47410
C17B* C 0.1625(6) 1.1536(4) 0.4850(3)
H39B* H 0.11900 1.19930 0.51550
H40B* H 0.08360 1.12470 0.44560
H41B* H 0.21350 1.10880 0.52330
O1B* O 0.2317(5) 1.0034(2) 0.3129(3)
C18B* C 0.2748(10) 0.9082(5) 0.3211(7)
H42B* H 0.35100 0.89900 0.37120
H43B* H 0.31650 0.88890 0.27320
C19B* C 0.1565(9) 0.8623(5) 0.3254(11)
H44B* H 0.11630 0.83220 0.27280
H45B* H 0.17570 0.81750 0.36990
C20B* C 0.0604(18) 0.9312(10) 0.3428(15)
H46B* H -0.04520 0.91280 0.33130
H47B* H 0.08810 0.95310 0.39990
C21B* C 0.0968(11) 1.0011(6) 0.2786(9)
H48B* H 0.04510 1.05890 0.28050
H49B* H 0.08060 0.97770 0.22190
H21B* H 0.52560 1.27510 0.29150
H22B* H 0.44140 1.27070 0.19800
C13B* C 0.6046(8) 1.0116(3) 0.2796(4)
H27B* H 0.69280 1.01330 0.25430
H28B* H 0.61970 0.96820 0.32450
H29B* H 0.51790 0.99430 0.23850
C14B* C 0.7104(7) 1.1217(5) 0.3730(5)
H30B* H 0.79850 1.12260 0.34760
H31B* H 0.69640 1.18070 0.39580
H32B* H 0.72380 1.07720 0.41700
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cu 1.52
Li 1.28
N 0.68
O 0.68
|
1100607.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 02:17:08 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177971 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100607.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100607
loop_
_publ_author_name
'M\"ohlen, Michael'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Krautscheid, Harald'
'Fenske, Dieter'
'Diedenhofen, Michael'
'Frenking, Gernot'
'Dehnicke, Kurt'
_publ_section_title
;
Tri(phosphorano)borazinium-Ionen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1105
_journal_page_last 1110
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1105::aid-zaac1105>3.0.co;2-t
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C18 H48 B3 I3 N3 P3'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 97.67(1)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 22.786(2)
_cell_length_b 19.874(2)
_cell_length_c 14.373(1)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100607
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
I1 I 0.36830(3) 0.26565(4) 0.19114(6)
I2 I 0.18454(3) 0.11893(4) 0.29225(6)
I3 I -0.37612(3) 0.01735(3) 0.14367(7)
I4 I -0.12725(4) 0.24400(4) 0.46813(6)
I5 I 0.07643(4) 0.44974(4) 0.32075(7)
I6 I 0.38336(4) -0.14942(4) 0.37566(8)
B1 B 0.4319(5) 0.1977(5) 0.4478(8)
H1 H 0.4826(42) 0.1721(47) 0.4622(70)
N1 N 0.3764(4) 0.1649(4) 0.4514(6)
P1 P 0.37857(12) 0.08116(12) 0.4695(2)
C1 C 0.4285(5) 0.0612(6) 0.5743(9)
H2 H 0.4688(5) 0.0769(6) 0.5665(9)
H3 H 0.4158(5) 0.0858(6) 0.6281(9)
C2 C 0.4309(6) -0.0137(6) 0.5966(10)
H4 H 0.4585(6) -0.0216(6) 0.6539(10)
H5 H 0.4443(6) -0.0384(6) 0.5443(10)
H6 H 0.3913(6) -0.0294(6) 0.606(1)
C3 C 0.3083(5) 0.0465(6) 0.4798(10)
H7 H 0.2795(5) 0.0647(6) 0.4284(10)
H8 H 0.3104(5) -0.0028(6) 0.4703(10)
C4 C 0.2850(6) 0.0590(7) 0.5712(11)
H9 H 0.2461(6) 0.0378(7) 0.5696(11)
H10 H 0.2813(6) 0.1075(7) 0.5808(11)
H11 H 0.3124(6) 0.0398(7) 0.6228(11)
C5 C 0.4067(6) 0.0450(6) 0.3715(9)
H12 H 0.4465(6) 0.0638(6) 0.3673(9)
H13 H 0.4110(6) -0.0041(6) 0.3814(9)
C6 C 0.3662(6) 0.0580(7) 0.277(1)
H14 H 0.3837(6) 0.0371(7) 0.2255(10)
H15 H 0.3624(6) 0.1066(7) 0.266(1)
H16 H 0.3269(6) 0.0386(7) 0.280(1)
B2 B 0.3773(5) 0.3025(6) 0.3939(9)
H17 H 0.3689(44) 0.3615(54) 0.3929(75)
N2 N 0.4333(3) 0.2674(4) 0.4218(6)
P2 P 0.49885(11) 0.30652(12) 0.4243(2)
C7 C 0.5203(5) 0.3347(5) 0.5412(8)
H18 H 0.5276(5) 0.2949(5) 0.5827(8)
H19 H 0.5581(5) 0.3596(5) 0.5437(8)
C8 C 0.4754(5) 0.3794(6) 0.5789(9)
H20 H 0.4903(5) 0.3928(6) 0.6433(9)
H21 H 0.4381(5) 0.3548(6) 0.5784(9)
H22 H 0.4686(5) 0.4196(6) 0.5394(9)
C9 C 0.5538(4) 0.2499(5) 0.3915(8)
H23 H 0.5905(4) 0.2758(5) 0.3869(8)
H24 H 0.5631(4) 0.2163(5) 0.4421(8)
C10 C 0.5363(5) 0.2125(6) 0.2986(9)
H25 H 0.5688(5) 0.1829(6) 0.2863(9)
H26 H 0.5283(5) 0.2452(6) 0.2474(9)
H27 H 0.5007(5) 0.1856(6) 0.3027(9)
C11 C 0.4918(5) 0.3751(5) 0.3435(8)
H28 H 0.4842(5) 0.3571(5) 0.2788(8)
H29 H 0.4572(5) 0.4027(5) 0.3543(8)
C12 C 0.5467(6) 0.4199(6) 0.3521(10)
H30 H 0.5403(6) 0.4565(6) 0.3063(10)
H31 H 0.5810(6) 0.3931(6) 0.3401(10)
H32 H 0.5539(6) 0.4387(6) 0.4156(10)
B3 B 0.3223(5) 0.2030(6) 0.4514(9)
H33 H 0.2774(39) 0.1790(44) 0.4737(65)
N3 N 0.3233(3) 0.2732(4) 0.4225(6)
P3 P 0.26731(13) 0.32679(14) 0.4286(2)
C13 C 0.2945(6) 0.3886(6) 0.5177(10)
H34 H 0.3080(6) 0.3647(6) 0.5771(10)
H35 H 0.3294(6) 0.4116(6) 0.4978(10)
C14 C 0.2498(9) 0.4413(7) 0.5365(13)
H36 H 0.2679(9) 0.4723(7) 0.5850(13)
H37 H 0.2155(9) 0.4193(7) 0.5581(13)
H38 H 0.2369(9) 0.4664(7) 0.4787(13)
C15 C 0.2473(5) 0.3703(6) 0.3206(10)
H39 H 0.2230(5) 0.4101(6) 0.3316(10)
H40 H 0.2835(5) 0.3863(6) 0.2965(10)
C16 C 0.2129(6) 0.3259(8) 0.2485(12)
H41 H 0.2026(6) 0.3512(8) 0.1901(12)
H42 H 0.1767(6) 0.3106(8) 0.2717(12)
H43 H 0.2371(6) 0.2868(8) 0.2366(12)
C17 C 0.2002(7) 0.2867(8) 0.4452(14)
H44 H 0.1950(7) 0.2473(8) 0.4062(14)
H45 H 0.1674(7) 0.3163(8) 0.4270(14)
C18 C 0.2013(8) 0.2655(9) 0.5481(15)
H46 H 0.1647(8) 0.2435(9) 0.5554(15)
H47 H 0.2337(8) 0.2353(9) 0.5662(15)
H48 H 0.2058(8) 0.3049(9) 0.5871(15)
C19? C 0.2128(13) 0.2724(15) 0.4897(27)
H49? H 0.2317(13) 0.2610(15) 0.5514(27)
H50? H 0.2026(13) 0.2315(15) 0.4556(27)
C20? C 0.1565(15) 0.3161(17) 0.5004(26)
H51? H 0.1292(15) 0.2909(17) 0.5323(26)
H52? H 0.1673(15) 0.3568(17) 0.5345(26)
H53? H 0.1381(15) 0.3271(17) 0.4383(26)
B4 B 0.1840(7) 0.7750(6) 0.2936(17)
H54 H 0.2233(52) 0.7855(56) 0.2686(82)
N4 N 0.1755(3) 0.7036(4) 0.2987(6)
P4 P 0.23212(12) 0.64934(13) 0.3173(2)
C21 C 0.2529(5) 0.6384(6) 0.4411(9)
H55 H 0.2166(5) 0.6341(6) 0.4716(9)
H56 H 0.2755(5) 0.5959(6) 0.4520(9)
C22 C 0.2894(7) 0.6943(8) 0.4861(13)
H57 H 0.2992(7) 0.6853(8) 0.5534(13)
H58 H 0.2670(7) 0.7365(8) 0.4771(13)
H59 H 0.3259(7) 0.6982(8) 0.4575(13)
C23 C 0.2948(5) 0.6799(6) 0.2701(10)
H60 H 0.3026(5) 0.7267(6) 0.2922(10)
H61 H 0.3296(5) 0.6524(6) 0.2951(10)
C24 C 0.2891(7) 0.6793(10) 0.1627(13)
H62 H 0.3256(7) 0.697(1) 0.1426(13)
H63 H 0.2556(7) 0.7075(10) 0.1369(13)
H64 H 0.2826(7) 0.6331(10) 0.1398(13)
C25 C 0.2096(5) 0.5680(5) 0.272(1)
H65 H 0.2453(5) 0.5393(5) 0.2748(10)
H66 H 0.1835(5) 0.5477(5) 0.3142(10)
C26 C 0.1772(6) 0.5652(7) 0.1718(9)
H67 H 0.1672(6) 0.5184(7) 0.1551(9)
H68 H 0.2028(6) 0.5835(7) 0.1284(9)
H69 H 0.1408(6) 0.5919(7) 0.1679(9)
B5 B 0.0772(5) 0.7929(6) 0.2514(10)
H70 H 0.0349(52) 0.8275(60) 0.2061(87)
N5 N 0.1349(3) 0.8196(4) 0.2710(6)
P5 P 0.14614(15) 0.90302(14) 0.2657(3)
C27 C 0.2201(6) 0.9225(7) 0.2688(15)
H71 H 0.2250(6) 0.9719(7) 0.2734(15)
H72 H 0.2426(6) 0.9023(7) 0.3256(15)
C28 C 0.2473(8) 0.8959(10) 0.1773(14)
H73 H 0.2893(8) 0.9083(10) 0.1824(14)
H74 H 0.2258(8) 0.9166(10) 0.1208(14)
H75 H 0.2434(8) 0.8469(10) 0.1731(14)
C29 C 0.1183(35) 0.9184(46) 0.1404(18)
H76 H 0.0773(35) 0.9125(46) 0.1473(18)
H77 H 0.1291(35) 0.8813(46) 0.1035(18)
C30 C 0.1105(18) 0.9742(21) 0.0917(29)
H78 H 0.0854(18) 0.9695(21) 0.0328(29)
H79 H 0.0979(18) 1.0123(21) 0.1250(29)
H80 H 0.1507(18) 0.9805(21) 0.0804(29)
C31 C 0.0892(7) 0.9506(9) 0.3187(14)
H81 H 0.0513(7) 0.9287(9) 0.3103(14)
H82 H 0.0855(7) 0.9963(9) 0.2972(14)
C32 C 0.1279(13) 0.9432(15) 0.4225(22)
H83 H 0.1052(13) 0.9655(15) 0.4650(22)
H84 H 0.1323(13) 0.8966(15) 0.4392(22)
H85 H 0.1663(13) 0.9638(15) 0.4262(22)
C33? C 0.0906(13) 0.9608(15) 0.2033(25)
H86? H 0.1056(13) 1.0059(15) 0.2076(25)
H87? H 0.0514(13) 0.9592(15) 0.2208(25)
C34? C 0.1000(11) 0.9296(14) 0.1032(20)
H88? H 0.0758(11) 0.9538(14) 0.0545(20)
H89? H 0.1404(11) 0.9303(14) 0.0912(20)
H90? H 0.0865(11) 0.8839(14) 0.1043(20)
C35? C 0.1514(18) 0.9312(20) 0.3892(9)
H91? H 0.1720(18) 0.9734(20) 0.3967(9)
H92? H 0.1733(18) 0.899(2) 0.4297(9)
C36? C 0.0825(10) 0.9410(11) 0.4200(17)
H93? H 0.0862(10) 0.9556(11) 0.4841(17)
H94? H 0.0606(10) 0.9739(11) 0.3805(17)
H95? H 0.0619(10) 0.8988(11) 0.4138(17)
C37 C -0.0132(11) 0.6263(11) 0.3331(24)
H96 H 0.0082(11) 0.5886(11) 0.3128(24)
H97 H -0.0547(11) 0.6162(11) 0.3222(24)
H98? H 0.0243(11) 0.6047(11) 0.3514(24)
H99? H -0.0352(11) 0.5971(11) 0.2880(24)
C38 C 0.0001(9) 0.6348(10) 0.4178(15)
H100 H -0.0076(9) 0.5959(10) 0.4538(15)
H101 H 0.0417(9) 0.6447(10) 0.4277(15)
H102 H -0.0216(9) 0.6725(10) 0.4372(15)
C39? C -0.0521(12) 0.6231(14) 0.4249(20)
H103? H -0.0552(12) 0.5776(14) 0.4461(20)
H104? H -0.0303(12) 0.6495(14) 0.4738(20)
H105? H -0.0910(12) 0.6418(14) 0.4091(20)
B6 B 0.1167(6) 0.6797(6) 0.3023(10)
H106 H 0.1098(6) 0.6250(6) 0.3226(10)
N6 N 0.0664(3) 0.7232(4) 0.2757(6)
P6 P -0.00240(14) 0.6918(2) 0.2648(4)
C40 C -0.0543(4) 0.7570(6) 0.2763(9)
H107 H -0.0537(4) 0.7884(6) 0.2229(9)
H108 H -0.0943(4) 0.7367(6) 0.2703(9)
C41 C -0.0451(6) 0.7979(7) 0.3671(10)
H109 H -0.0761(6) 0.8322(7) 0.3655(10)
H110 H -0.0062(6) 0.8199(7) 0.3732(10)
H111 H -0.0469(6) 0.7679(7) 0.4207(10)
C42 C -0.0256(12) 0.6785(14) 0.1378(5)
H112 H -0.0142(12) 0.7172(14) 0.1045(5)
H113 H -0.0679(12) 0.6750(14) 0.1266(5)
C43 C 0.0054(10) 0.6100(11) 0.0970(17)
H114 H -0.008(1) 0.6058(11) 0.0310(17)
H115 H 0.0478(10) 0.6136(11) 0.1069(17)
H116 H -0.0065(10) 0.5710(11) 0.1292(17)
C44? C -0.0147(12) 0.6266(13) 0.1948(20)
H117? H -0.0506(12) 0.6038(13) 0.2037(20)
H118? H 0.0176(12) 0.5953(13) 0.2007(20)
C45? C -0.0208(12) 0.6610(14) 0.1049(22)
H119? H -0.0289(12) 0.6300(14) 0.0536(22)
H120? H -0.0526(12) 0.6929(14) 0.1029(22)
H121? H 0.0155(12) 0.6844(14) 0.0998(22)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
B 0.83
I 1.40
N 0.68
P 1.05
|
1100608.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 02:17:08 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177971 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100608.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100608
loop_
_publ_author_name
'M\"ohlen, Michael'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Krautscheid, Harald'
'Fenske, Dieter'
'Diedenhofen, Michael'
'Frenking, Gernot'
'Dehnicke, Kurt'
_publ_section_title
;
Tri(phosphorano)borazinium-Ionen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1105
_journal_page_last 1110
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1105::aid-zaac1105>3.0.co;2-t
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C18 H49 B3 I2 N3 P3'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 90.671(16)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.690(2)
_cell_length_b 7.9335(7)
_cell_length_c 22.382(3)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100608
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
P1 P 0.92368(14) -0.7455(4) 0.11155(14)
N1 N 0.8402(4) -0.8401(12) 0.1143(4)
B1 B 0.7997(7) -0.8721(18) 0.1676(6)
H1 H 0.821(5) -0.825(14) 0.215(5)
I1 I 0.46281(4) -0.68448(14) 0.12930(4)
I2 I 1.10222(4) -1.30941(15) 0.13049(4)
P2 P 0.67399(15) -0.9890(4) 0.22268(14)
N2 N 0.7231(4) -0.9353(12) 0.1624(4)
B2 B 0.6811(7) -0.9237(18) 0.1059(6)
H2 H 0.630(5) -0.926(13) 0.106(5)
P3 P 0.68132(15) -0.8340(5) -0.01147(13)
N3 N 0.7210(4) -0.8890(12) 0.0523(4)
B3 B 0.8108(7) -0.906(2) 0.0531(7)
H3 H 0.821(6) -0.760(13) 0.009(5)
H4 H 0.821(6) -1.056(15) 0.043(6)
C1 C 0.9677(6) -0.7196(17) 0.1837(5)
H5 H 1.01110 -0.64170 0.17980
H6 H 0.93100 -0.66630 0.21090
C2 C 0.9959(7) -0.8836(18) 0.2123(6)
H7 H 1.01460 -0.86070 0.25280
H8 H 1.03680 -0.93060 0.18830
H9 H 0.95410 -0.96470 0.21400
C3 C 0.9124(6) -0.5415(17) 0.0784(6)
H10 H 0.96260 -0.48720 0.07550
H11 H 0.89200 -0.55510 0.03730
C4 C 0.8603(9) -0.4270(19) 0.1131(9)
H12 H 0.88270 -0.40360 0.15250
H13 H 0.81130 -0.48230 0.11800
H14 H 0.85330 -0.32090 0.09130
C5 C 0.9854(5) -0.8673(17) 0.0662(5)
H15 H 0.98830 -0.98300 0.08270
H16 H 0.96320 -0.87520 0.02550
C6 C 1.0645(5) -0.7975(19) 0.0618(6)
H17 H 1.09110 -0.81270 0.10010
H18 H 1.06210 -0.67720 0.05210
H19 H 1.09180 -0.85740 0.03040
C7 C 0.6259(6) -0.810(2) 0.2529(5)
H20 H 0.58510 -0.77650 0.22460
H21 H 0.60170 -0.84390 0.29070
C8 C 0.6720(9) -0.666(2) 0.2645(8)
H22 H 0.64220 -0.58020 0.28500
H23 H 0.69030 -0.62050 0.22660
H24 H 0.71510 -0.69910 0.28970
C9 C 0.7345(6) -1.0661(19) 0.2792(6)
H25 H 0.76500 -0.97030 0.29440
H26 H 0.70270 -1.10530 0.31250
C10 C 0.7903(7) -1.2120(19) 0.2633(7)
H27 H 0.82600 -1.17250 0.23320
H28 H 0.76160 -1.30800 0.24730
H29 H 0.81810 -1.24690 0.29930
C11 C 0.6034(7) -1.142(2) 0.2029(6)
H30 H 0.58330 -1.19010 0.24030
H31 H 0.56120 -1.08200 0.18260
C12 C 0.627(1) -1.284(2) 0.1637(10)
H32 H 0.64250 -1.24020 0.12480
H33 H 0.58440 -1.36210 0.15800
H34 H 0.66940 -1.34440 0.18250
C13 C 0.7246(7) -0.948(2) -0.0713(6)
H35 H 0.69580 -0.92460 -0.10860
H36 H 0.77640 -0.90370 -0.07660
C14 C 0.7297(7) -1.145(2) -0.0628(7)
H37 H 0.75870 -1.17100 -0.02630
H38 H 0.75480 -1.19560 -0.09730
H39 H 0.67860 -1.19220 -0.05950
C15 C 0.5835(5) -0.8800(15) -0.0141(5)
H40 H 0.57670 -1.00360 -0.01130
H41 H 0.55930 -0.82880 0.02120
C16 C 0.5429(6) -0.816(2) -0.0710(5)
H42 H 0.55010 -0.69380 -0.07450
H43 H 0.48880 -0.84100 -0.06850
H44 H 0.56400 -0.87200 -0.10600
C17 C 0.6946(7) -0.615(2) -0.0225(7)
H45 H 0.74950 -0.59100 -0.02400
H46 H 0.67210 -0.58250 -0.06150
C18 C 0.6603(10) -0.508(2) 0.0255(9)
H47 H 0.66770 -0.56340 0.06430
H48 H 0.60600 -0.49500 0.01740
H49 H 0.68460 -0.39750 0.02610
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.24
B 0.90
I 1.40
N 0.68
P 1.05
|
1100609.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 02:17:08 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177971 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100609.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100609
loop_
_publ_author_name
'M\"ohlen, Michael'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Krautscheid, Harald'
'Fenske, Dieter'
'Diedenhofen, Michael'
'Frenking, Gernot'
'Dehnicke, Kurt'
_publ_section_title
;
Tri(phosphorano)borazinium-Ionen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1105
_journal_page_last 1110
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1105::aid-zaac1105>3.0.co;2-t
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C22 H54 B3 I3 N5 P3'
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 19
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.546(4)
_cell_length_b 14.113(5)
_cell_length_c 20.899(9)
_cod_database_code 1100609
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 1/2+x,1/2-y,-z
4 -x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
B1 B 0.5117(10) 0.4250(8) 0.7176(5)
H1 H 0.5031(10) 0.4105(8) 0.7701(5)
B2 B 0.6226(10) 0.4979(9) 0.6282(5)
H2 H 0.6976(10) 0.5353(9) 0.6136(5)
B3 B 0.4413(10) 0.4298(10) 0.6038(5)
H3 H 0.3664(10) 0.4482(10) 0.5775(5)
N1 N 0.6163(6) 0.4456(6) 0.6891(3)
N2 N 0.5300(6) 0.4996(5) 0.5881(3)
N3 N 0.4213(6) 0.4241(6) 0.6757(4)
N4 N 0.4839(7) 0.3282(6) 0.5830(3)
P1 P 0.7273(2) 0.4413(2) 0.73339(11)
P2 P 0.5236(2) 0.5614(2) 0.52118(11)
P3 P 0.2988(2) 0.4096(2) 0.70161(14)
C1 C 0.8251(8) 0.3692(7) 0.6938(5)
H4 H 0.8365(8) 0.3944(7) 0.6501(5)
H5 H 0.8935(8) 0.3747(7) 0.7172(5)
C2 C 0.7953(9) 0.2641(8) 0.6889(5)
H6 H 0.8449(33) 0.2320(13) 0.6599(26)
H7 H 0.7225(21) 0.2582(8) 0.6723(30)
H8 H 0.7993(53) 0.2349(14) 0.7314(7)
C3 C 0.7826(9) 0.5591(7) 0.7415(4)
H9 H 0.8124(9) 0.5789(7) 0.6997(4)
H10 H 0.7244(9) 0.6036(7) 0.7524(4)
C4 C 0.8702(9) 0.5671(9) 0.7925(5)
H11 H 0.8375(9) 0.5752(60) 0.8347(7)
H12 H 0.9157(40) 0.6218(34) 0.7831(23)
H13 H 0.9135(41) 0.5093(24) 0.7924(27)
C5 C 0.7024(8) 0.3897(8) 0.8099(4)
H14 H 0.6559(8) 0.3337(8) 0.8036(4)
H15 H 0.7711(8) 0.3665(8) 0.8272(4)
C6 C 0.6504(11) 0.4539(9) 0.8607(5)
H16 H 0.7060(11) 0.4821(45) 0.8876(25)
H17 H 0.6023(49) 0.4161(14) 0.8874(25)
H18 H 0.6100(54) 0.5042(34) 0.8395(5)
C7 C 0.6380(9) 0.6362(9) 0.5127(5)
H19 H 0.7022(9) 0.5955(9) 0.5129(5)
H20 H 0.6342(9) 0.6669(9) 0.4701(5)
C8 C 0.6540(11) 0.7156(10) 0.5641(6)
H21 H 0.7290(17) 0.7347(45) 0.5650(29)
H22 H 0.6333(66) 0.6914(21) 0.6063(9)
H23 H 0.6096(53) 0.7704(25) 0.5532(24)
C9 C 0.4052(9) 0.6284(8) 0.5184(4)
H24 H 0.4086(9) 0.6694(8) 0.4800(4)
H25 H 0.3452(9) 0.5838(8) 0.5119(4)
C10 C 0.3778(11) 0.6904(9) 0.5747(5)
H26 H 0.3016(17) 0.7057(51) 0.5737(23)
H27 H 0.4194(51) 0.7491(28) 0.5725(23)
H28 H 0.3945(65) 0.6568(25) 0.6145(5)
C11 C 0.5293(9) 0.4883(8) 0.4516(5)
H29 H 0.5443(9) 0.5297(8) 0.4144(5)
H30 H 0.5910(9) 0.4451(8) 0.4564(5)
C12 C 0.4311(11) 0.4275(10) 0.4352(6)
H31 H 0.4398(32) 0.400(5) 0.3925(18)
H32 H 0.3670(14) 0.4672(16) 0.4360(39)
H33 H 0.4238(40) 0.3765(37) 0.4667(25)
C13 C 0.2925(10) 0.3806(10) 0.7845(5)
H34 H 0.2209(10) 0.354(1) 0.7932(5)
H35 H 0.3449(10) 0.3296(10) 0.7927(5)
C14 C 0.3126(11) 0.4594(11) 0.8326(6)
H36 H 0.3806(40) 0.4903(47) 0.8228(29)
H37 H 0.3154(79) 0.4326(15) 0.8758(7)
H38 H 0.2549(43) 0.5060(38) 0.8301(33)
C15 C 0.2298(8) 0.5189(8) 0.6885(5)
H39 H 0.2732(8) 0.5708(8) 0.7068(5)
H40 H 0.2251(8) 0.5298(8) 0.6418(5)
C16 C 0.1165(10) 0.5258(9) 0.7167(7)
H41 H 0.0872(30) 0.5889(23) 0.7081(39)
H42 H 0.1195(14) 0.5152(67) 0.7630(9)
H43 H 0.0709(22) 0.4776(43) 0.6969(33)
C17 C 0.2387(9) 0.3135(10) 0.6580(8)
H44 H 0.2806(9) 0.3065(10) 0.6182(8)
H45 H 0.2520(9) 0.2556(10) 0.6835(8)
C18 C 0.1298(14) 0.3099(14) 0.6396(9)
H46 H 0.0846(15) 0.320(11) 0.6772(16)
H47 H 0.1142(33) 0.2478(38) 0.6208(67)
H48 H 0.1156(32) 0.3596(69) 0.6080(56)
C19 C 0.5184(10) 0.2559(8) 0.5740(4)
C20 C 0.5652(9) 0.1638(8) 0.5596(5)
H49 H 0.5139(21) 0.1256(19) 0.5354(28)
H50 H 0.5831(50) 0.1313(22) 0.5996(5)
H51 H 0.6299(30) 0.1726(9) 0.5340(27)
I1 I 0.00868(6) 0.28759(5) 0.83804(3)
I2 I 0.49624(7) 0.67389(4) 0.75467(3)
I3 I 0.71908(6) 0.65023(6) 0.00688(3)
N5 N 0.3602(12) 0.4568(11) 0.0184(6)
C21 C 0.4417(11) 0.4389(11) 0.0318(6)
C22 C 0.5496(12) 0.4233(14) 0.0460(7)
H52 H 0.5816(25) 0.3838(64) 0.0126(29)
H53 H 0.5556(13) 0.391(7) 0.0874(26)
H54 H 0.5871(22) 0.4842(15) 0.0481(50)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
B 0.83
I 1.40
N 0.68
P 1.05
|
1100610.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:42:33 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177950 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100610.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100610
loop_
_publ_author_name
'Anfang, S.'
'Seybert, G.'
'Harms, K.'
'Geiseler, G.'
'Massa, W.'
'Dehnicke, K.'
_publ_section_title
;
Reaktionen von LiNPPh~3~ mit den Cyclooctatetraenid-Komplexen
[Ln(C~8~H~8~)Cl(THF)~2~]~2~ von Cer und Samarium. Die Kristallstrukturen
von [LiNPPh~3~]~6~, [Ln(C~8~H~8~)Li~3~Cl~2~(NPPh~3~)~2~(THF)~3~]
(Ln = Ce, Sm) und [Li(THF)~4~][Sm(C~8~H~8~)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1187
_journal_page_last 1192
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1187::aid-zaac1187>3.0.co;2-1
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C128 H130 Li6 N6 O5 P6'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 93.18(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.194(1)
_cell_length_b 29.539(3)
_cell_length_c 27.230(2)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100610
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Li1 Li 0.1993(5) 0.2868(2) 0.1663(3)
Li2 Li 0.3321(5) 0.2822(2) 0.2281(3)
Li3 Li 0.2375(5) 0.3550(2) 0.2927(3)
Li4 Li 0.1956(5) 0.2755(2) 0.2802(3)
Li5 Li 0.1127(5) 0.3642(2) 0.2287(3)
Li6 Li 0.2524(5) 0.3664(2) 0.1790(3)
P1 P 0.22142(8) 0.18892(4) 0.21970(5)
P2 P 0.39198(8) 0.31324(4) 0.11811(5)
P3 P 0.40613(7) 0.30399(4) 0.33739(4)
P4 P 0.03902(8) 0.35459(4) 0.12457(5)
P5 P 0.03056(7) 0.31812(4) 0.32655(5)
P6 P 0.25328(8) 0.45187(4) 0.24808(5)
N1 N 0.2155(2) 0.24126(9) 0.21969(14)
N2 N 0.3318(2) 0.31227(11) 0.16306(13)
N3 N 0.3258(2) 0.3033(1) 0.29737(12)
N4 N 0.1235(2) 0.34319(10) 0.16001(13)
N5 N 0.1056(2) 0.32833(10) 0.28969(12)
N6 N 0.2321(2) 0.40094(10) 0.24030(13)
C1 C 0.3401(3) 0.16514(13) 0.22559(17)
C2 C 0.3697(3) 0.12738(14) 0.19968(18)
H1 H 0.32670 0.11260 0.17700
C3 C 0.4615(3) 0.11121(16) 0.2067(2)
H2 H 0.48040 0.08540 0.18890
C4 C 0.5251(4) 0.13223(18) 0.2393(2)
H3 H 0.58770 0.12090 0.24380
C5 C 0.4980(3) 0.16985(17) 0.2653(2)
H4 H 0.54130 0.18460 0.28780
C6 C 0.4061(3) 0.18569(15) 0.25779(17)
H5 H 0.38780 0.21170 0.27550
C7 C 0.1621(3) 0.16078(13) 0.26897(18)
C8 C 0.2052(4) 0.12961(15) 0.30148(19)
H6 H 0.26920 0.12120 0.29820
C9 C 0.1543(4) 0.11089(16) 0.3386(2)
H7 H 0.18430 0.08960 0.36050
C10 C 0.0614(4) 0.12245(18) 0.3445(2)
H8 H 0.02760 0.10990 0.37040
C11 C 0.0185(4) 0.15305(17) 0.3114(2)
H9 H -0.04600 0.16080 0.31400
C12 C 0.0689(3) 0.17203(14) 0.2752(2)
H10 H 0.03890 0.19360 0.25360
C13 C 0.1717(3) 0.16057(15) 0.1653(2)
C14 C 0.1098(3) 0.12345(16) 0.1663(2)
H11 H 0.09320 0.11130 0.19690
C15 C 0.0725(4) 0.1042(2) 0.1221(3)
H12 H 0.03120 0.07900 0.12340
C16 C 0.0940(5) 0.1206(2) 0.0785(3)
H13 H 0.06680 0.10770 0.04900
C17 C 0.1563(5) 0.1566(2) 0.0764(2)
H14 H 0.17390 0.16760 0.04550
C18 C 0.1933(4) 0.17664(17) 0.1199(2)
H15 H 0.23430 0.20190 0.11800
C19 C 0.5063(3) 0.28532(15) 0.12320(17)
C20 C 0.5878(3) 0.30303(15) 0.10376(16)
H16 H 0.58560 0.33180 0.08810
C21 C 0.6722(3) 0.27870(19) 0.10730(19)
H17 H 0.72700 0.29090 0.09370
C22 C 0.6766(4) 0.23707(19) 0.13040(19)
H18 H 0.73390 0.22030 0.13220
C23 C 0.5983(4) 0.22020(16) 0.15053(19)
H19 H 0.60170 0.19180 0.16700
C24 C 0.5139(3) 0.24368(16) 0.14741(18)
H20 H 0.46030 0.23130 0.16190
C25 C 0.3407(3) 0.28639(15) 0.06170(17)
C26 C 0.2424(3) 0.28507(14) 0.05461(19)
H21 H 0.20440 0.29770 0.07880
C27 C 0.1998(4) 0.26547(17) 0.0126(2)
H22 H 0.13290 0.26480 0.00830
C28 C 0.2533(4) 0.24711(19) -0.0226(2)
H23 H 0.22390 0.23400 -0.05140
C29 C 0.3505(4) 0.2479(2) -0.0159(2)
H24 H 0.38810 0.23480 -0.04000
C30 C 0.3936(4) 0.26766(17) 0.0260(2)
H25 H 0.46050 0.26820 0.03000
C31 C 0.4218(3) 0.36978(15) 0.09723(19)
C32 C 0.4125(3) 0.38548(19) 0.0497(2)
H26 H 0.39210 0.36520 0.02410
C33 C 0.4323(4) 0.4307(2) 0.0378(3)
H27 H 0.42660 0.44060 0.00460
C34 C 0.4595(4) 0.4601(2) 0.0742(3)
H28 H 0.47140 0.49080 0.06630
C35 C 0.4698(4) 0.44608(19) 0.1220(3)
H29 H 0.49100 0.46660 0.14710
C36 C 0.4489(4) 0.40120(17) 0.1336(2)
H30 H 0.45320 0.39190 0.16700
C37 C 0.3940(3) 0.34371(13) 0.38810(17)
C38 C 0.4192(3) 0.33458(15) 0.4372(2)
H31 H 0.44570 0.30600 0.44600
C39 C 0.4062(4) 0.36682(18) 0.4737(2)
H32 H 0.42360 0.35990 0.50700
C40 C 0.3681(4) 0.40870(18) 0.4616(2)
H33 H 0.35910 0.43060 0.48640
C41 C 0.3437(4) 0.41808(17) 0.4135(2)
H34 H 0.31740 0.44680 0.40500
C42 C 0.3565(3) 0.38661(15) 0.37716(19)
H35 H 0.33950 0.39420 0.34390
C43 C 0.5221(3) 0.31860(13) 0.31680(17)
C44 C 0.5419(3) 0.31103(14) 0.26866(18)
H36 H 0.49420 0.29840 0.24700
C45 C 0.6293(3) 0.32118(15) 0.25043(19)
H37 H 0.64060 0.31540 0.21690
C46 C 0.6992(3) 0.33962(14) 0.2814(2)
H38 H 0.75910 0.34640 0.26940
C47 C 0.6819(3) 0.34805(14) 0.3292(2)
H39 H 0.72990 0.36120 0.35030
C48 C 0.5944(3) 0.33760(13) 0.34765(18)
H40 H 0.58380 0.34340 0.38120
C49 C 0.4271(3) 0.25026(13) 0.37069(16)
C50 C 0.5163(3) 0.23422(15) 0.38605(18)
H41 H 0.57090 0.25150 0.37990
C51 C 0.5256(4) 0.19241(17) 0.41075(19)
H42 H 0.58620 0.18170 0.42170
C52 C 0.4468(5) 0.16734(16) 0.4188(2)
H43 H 0.45330 0.13890 0.43510
C53 C 0.3581(4) 0.18273(17) 0.4038(2)
H44 H 0.30390 0.16520 0.41000
C54 C 0.3485(3) 0.22416(15) 0.37939(17)
H45 H 0.28750 0.23460 0.36860
C55 C -0.0569(3) 0.38587(14) 0.15078(16)
C56 C -0.1472(3) 0.36958(15) 0.15565(18)
H46 H -0.16210 0.33980 0.14450
C57 C -0.2166(4) 0.39516(19) 0.1762(2)
H47 H -0.27780 0.38280 0.17920
C58 C -0.1969(4) 0.43851(18) 0.1924(2)
H48 H -0.24440 0.45650 0.20590
C59 C -0.1069(4) 0.45535(16) 0.18848(19)
H49 H -0.09260 0.48510 0.20000
C60 C -0.0375(3) 0.43003(15) 0.16830(18)
H50 H 0.02390 0.44240 0.16610
C61 C 0.0603(3) 0.39039(13) 0.07114(16)
C62 C -0.0129(3) 0.41380(14) 0.04578(18)
H51 H -0.07540 0.41170 0.05640
C63 C 0.0052(4) 0.44010(14) 0.00521(19)
H52 H -0.04500 0.45590 -0.01170
C64 C 0.0947(4) 0.44346(15) -0.01070(19)
H53 H 0.10640 0.46130 -0.03880
C65 C 0.1681(4) 0.42080(16) 0.0143(2)
H54 H 0.23040 0.42310 0.00340
C66 C 0.1508(3) 0.39478(14) 0.05522(19)
H55 H 0.20170 0.37980 0.07250
C67 C -0.0195(3) 0.30463(14) 0.09575(17)
C68 C -0.0668(3) 0.30360(15) 0.05044(19)
H56 H -0.07110 0.33050 0.03140
C69 C -0.1086(3) 0.26412(18) 0.0316(2)
H57 H -0.13970 0.26380 -0.00020
C70 C -0.1039(3) 0.22582(18) 0.0600(2)
H58 H -0.13560 0.19930 0.04830
C71 C -0.0550(3) 0.22460(15) 0.1048(2)
H59 H -0.04950 0.19720 0.12300
C72 C -0.0133(3) 0.26460(14) 0.12326(18)
H60 H 0.01950 0.26450 0.15470
C73 C -0.0380(3) 0.36624(14) 0.34712(18)
C74 C -0.0624(3) 0.37331(15) 0.39523(19)
H61 H -0.04230 0.35230 0.42000
C75 C -0.1165(3) 0.41113(18) 0.4079(2)
H62 H -0.13370 0.41520 0.44080
C76 C -0.1443(3) 0.44200(17) 0.3726(2)
H63 H -0.17860 0.46820 0.38130
C77 C -0.1226(3) 0.43523(15) 0.3248(2)
H64 H -0.14420 0.45620 0.30020
C78 C -0.0692(3) 0.39777(14) 0.31165(19)
H65 H -0.05400 0.39380 0.27840
C79 C -0.0671(3) 0.28127(13) 0.30575(18)
C80 C -0.0739(3) 0.27023(14) 0.25622(19)
H66 H -0.02710 0.28080 0.23540
C81 C -0.1476(3) 0.24405(15) 0.2364(2)
H67 H -0.15140 0.23700 0.20230
C82 C -0.2155(3) 0.22831(16) 0.2666(2)
H68 H -0.26610 0.21020 0.25330
C83 C -0.2099(3) 0.23881(16) 0.3155(2)
H69 H -0.25600 0.22750 0.33630
C84 C -0.1373(3) 0.26592(14) 0.33500(19)
H70 H -0.13570 0.27410 0.36880
C85 C 0.0756(3) 0.29191(15) 0.38345(17)
C86 C 0.0593(3) 0.24741(17) 0.3959(2)
H71 H 0.01970 0.22940 0.37450
C87 C 0.0987(4) 0.2285(2) 0.4382(2)
H72 H 0.08540 0.19780 0.44560
C88 C 0.1560(4) 0.2527(3) 0.4695(2)
H73 H 0.18220 0.23940 0.49890
C89 C 0.1760(3) 0.2973(2) 0.4580(2)
H74 H 0.21620 0.31490 0.47950
C90 C 0.1370(3) 0.31610(18) 0.4150(2)
H75 H 0.15260 0.34640 0.40680
C91 C 0.2177(3) 0.47505(13) 0.30608(17)
C92 C 0.1466(3) 0.45287(15) 0.32964(19)
H76 H 0.11970 0.42630 0.31500
C93 C 0.1132(3) 0.46796(16) 0.3738(2)
H77 H 0.06420 0.45200 0.38870
C94 C 0.1519(3) 0.50631(16) 0.39569(19)
H78 H 0.12940 0.51710 0.42580
C95 C 0.2240(3) 0.52911(14) 0.37348(19)
H79 H 0.25170 0.55520 0.38870
C96 C 0.2552(3) 0.51396(15) 0.32948(19)
H80 H 0.30360 0.53030 0.31450
C97 C 0.3761(3) 0.46825(13) 0.24768(17)
C98 C 0.4457(3) 0.43617(15) 0.25860(18)
H81 H 0.42770 0.40580 0.26480
C99 C 0.5407(3) 0.44727(17) 0.26063(19)
H82 H 0.58670 0.42460 0.26830
C100 C 0.5689(4) 0.49140(18) 0.2515(2)
H83 H 0.63390 0.49920 0.25340
C101 C 0.5014(3) 0.52358(16) 0.2398(2)
H84 H 0.52000 0.55370 0.23300
C102 C 0.4077(3) 0.51264(14) 0.23778(18)
H85 H 0.36250 0.53550 0.22950
C103 C 0.1977(3) 0.48967(13) 0.20206(18)
C104 C 0.1333(3) 0.52367(14) 0.2133(2)
H86 H 0.12160 0.52970 0.24660
C105 C 0.0867(4) 0.54850(16) 0.1763(2)
H87 H 0.04370 0.57160 0.18460
C106 C 0.1017(4) 0.54025(17) 0.1287(2)
H88 H 0.06890 0.55740 0.10370
C107 C 0.1648(4) 0.50690(17) 0.1160(2)
H89 H 0.17600 0.50120 0.08250
C108 C 0.2112(3) 0.48210(15) 0.1533(2)
H90 H 0.25390 0.45900 0.14470
O1 O 0.4319(5) 0.0821(3) 1.0265(2)
C109 C 0.4344(13) 0.1242(6) 1.0538(5)
H91 H 0.42640 0.11880 1.08920
H92 H 0.38470 0.14530 1.04090
C110 C 0.5313(12) 0.1423(4) 1.0453(5)
H93 H 0.56360 0.15140 1.07690
H94 H 0.52670 0.16910 1.02350
C111 C 0.5864(10) 0.1047(5) 1.0214(5)
H95 H 0.59420 0.11120 0.98620
H96 H 0.64940 0.10070 1.03830
C112 C 0.5288(9) 0.0657(4) 1.0271(4)
H97 H 0.54610 0.05030 1.05860
H98 H 0.53670 0.04410 0.99990
O2 O 0.2396(8) 0.4346(3) -0.1482(4)
C113 C 0.3301(8) 0.4456(4) -0.1192(5)
H99 H 0.38190 0.44900 -0.14190
H100 H 0.32320 0.47460 -0.10160
C114 C 0.3508(5) 0.4134(3) -0.0877(3)
H101 H 0.33800 0.42400 -0.05420
H102 H 0.41890 0.40630 -0.08810
C115 C 0.3004(8) 0.3752(3) -0.0977(3)
H103 H 0.26970 0.36490 -0.06790
H104 H 0.34250 0.35090 -0.10840
C116 C 0.2287(7) 0.3858(3) -0.1371(4)
H105 H 0.16460 0.37960 -0.12610
H106 H 0.23880 0.36730 -0.16670
O3 O 0.169(1) -0.0128(2) 0.9416(4)
C117 C 0.0964(6) 0.0484(4) 0.9013(5)
H107 H 0.14210 0.05060 0.87520
H108 H 0.03720 0.06440 0.89100
C118 C 0.1353(6) 0.0633(3) 0.9483(4)
H109 H 0.08480 0.07760 0.96650
H110 H 0.18400 0.08650 0.94320
C119 C 0.1769(8) 0.0272(4) 0.9778(4)
H111 H 0.14110 0.02140 1.00730
H112 H 0.24350 0.03380 0.98800
C120 C 0.0803(9) 0.0023(3) 0.9162(5)
H113 H 0.06450 -0.01700 0.88720
H114 H 0.02780 0.00080 0.93860
O4 O 1.2856(8) -0.0782(5) 0.8518(6)
C121 C 1.2093(9) -0.1123(5) 0.8591(6)
H115 H 1.23570 -0.14180 0.87030
H116 H 1.16390 -0.10150 0.88280
C122 C 1.1674(8) -0.1149(4) 0.8105(7)
H117 H 1.10370 -0.10120 0.80970
H118 H 1.16060 -0.14710 0.80070
C123 C 1.2253(12) -0.0913(7) 0.7759(5)
H119 H 1.26870 -0.11260 0.76050
H120 H 1.18520 -0.07640 0.74980
C124 C 1.2690(9) -0.0635(5) 0.8006(9)
H121 H 1.23350 -0.03470 0.79990
H122 H 1.33040 -0.05790 0.78620
O5 O 0.2259(6) 0.1129(3) 0.5341(5)
C125 C 0.2036(13) 0.1078(6) 0.4828(7)
H123 H 0.15330 0.12960 0.47250
H124 H 0.26010 0.11510 0.46450
C126 C 0.2033(8) 0.0395(2) 0.5133(4)
H125 H 0.15410 0.01640 0.51790
H126 H 0.26400 0.02410 0.50840
C127 C 0.2114(6) 0.0687(4) 0.5535(3)
H127 H 0.26540 0.05980 0.57600
H128 H 0.15320 0.06790 0.57190
C128 C 0.1769(10) 0.0690(5) 0.4717(4)
H129 H 0.20730 0.05850 0.44190
H130 H 0.10760 0.06850 0.46500
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 0.98
N 0.68
O 0.68
P 1.05
|
1100611.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:42:33 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177950 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100611.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100611
loop_
_publ_author_name
'Anfang, S.'
'Seybert, G.'
'Harms, K.'
'Geiseler, G.'
'Massa, W.'
'Dehnicke, K.'
_publ_section_title
;
Reaktionen von LiNPPh~3~ mit den Cyclooctatetraenid-Komplexen
[Ln(C~8~H~8~)Cl(THF)~2~]~2~ von Cer und Samarium. Die Kristallstrukturen
von [LiNPPh~3~]~6~, [Ln(C~8~H~8~)Li~3~Cl~2~(NPPh~3~)~2~(THF)~3~]
(Ln = Ce, Sm) und [Li(THF)~4~][Sm(C~8~H~8~)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1187
_journal_page_last 1192
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1187::aid-zaac1187>3.0.co;2-1
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C68 H86 Ce Cl2 Li3 N2 O6 P2'
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-I 2ya'
_symmetry_space_group_name_H-M 'I 1 2/a 1'
_cell_angle_alpha 90
_cell_angle_beta 98.887(8)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 22.2109(17)
_cell_length_b 21.430(2)
_cell_length_c 31.644(3)
_cod_original_sg_symbol_H-M 'I 2/a'
_cod_original_formula_sum 'C68 H86 Ce1 Cl2 Li3 N2 O6 P2'
_cod_database_code 1100611
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2+y,1/2+z
3 1/2+x,-y,z
4 x,1/2-y,1/2+z
5 -x,-y,-z
6 -1/2-x,-1/2-y,-1/2-z
7 -1/2-x,y,-z
8 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Ce1 Ce 0.11785(1) 0.43789(1) -0.32496(1)
Cl1 Cl 0.25057(6) 0.44164(7) -0.31362(5)
P1 P 0.12073(6) 0.43472(7) -0.20660(5)
N1 N 0.1422(2) 0.4617(2) -0.24740(16)
O1 O 0.10591(18) 0.62109(19) -0.22601(15)
Li1 Li 0.1419(4) 0.5556(4) -0.2591(3)
C1 C 0.1100(3) 0.3912(3) -0.4080(2)
H1 H 0.14110 0.41090 -0.42340
P2 P 0.09926(7) 0.60485(7) -0.35396(5)
N2 N 0.1327(2) 0.5524(2) -0.32541(15)
O2 O 0.2793(2) 0.5898(2) -0.35188(18)
Li2 Li 0.2256(4) 0.5534(5) -0.3164(4)
C2 C 0.1359(3) 0.3420(3) -0.3809(3)
H2 H 0.18020 0.33690 -0.38280
Cl2 Cl 0.25176(6) 0.57936(6) -0.24330(5)
O3 O 0.30225(19) 0.4348(2) -0.20105(16)
C3 C 0.1210(3) 0.3118(3) -0.3446(3)
H3 H 0.15760 0.29120 -0.32800
Li3 Li 0.2371(4) 0.4688(5) -0.2428(4)
C4 C 0.0738(3) 0.3168(3) -0.3198(2)
H4 H 0.08660 0.29910 -0.29060
C5 C 0.0225(3) 0.3559(3) -0.3206(2)
H5 H 0.00900 0.35760 -0.29190
C6 C -0.0032(3) 0.4042(3) -0.3468(2)
H6 H -0.03000 0.43090 -0.33160
C7 C 0.0119(3) 0.4354(3) -0.3838(2)
H7 H -0.00740 0.47770 -0.38720
C8 C 0.0583(3) 0.4296(3) -0.4093(2)
H8 H 0.06310 0.46910 -0.42530
C9 C 0.0431(3) 0.6302(3) -0.2225(3)
H9 H 0.03300 0.60850 -0.19690
H10 H 0.01680 0.61330 -0.24810
C10 C 0.0332(4) 0.6974(4) -0.2190(4)
H11 H 0.00550 0.70640 -0.19800
H12 H 0.01550 0.71540 -0.24700
C11 C 0.0957(4) 0.7230(4) -0.2041(4)
H13 H 0.10750 0.75280 -0.22530
H14 H 0.09710 0.74480 -0.17640
C12 C 0.1371(3) 0.6686(4) -0.1995(3)
H15 H 0.17630 0.67900 -0.20900
H16 H 0.14530 0.65460 -0.16930
C13 C 0.3115(4) 0.5575(4) -0.3807(3)
H17 H 0.28550 0.52520 -0.39670
H18 H 0.34850 0.53730 -0.36510
C14 C 0.3282(5) 0.6072(5) -0.4104(3)
H19 H 0.29550 0.61270 -0.43520
H20 H 0.36660 0.59670 -0.42100
C15 C 0.3354(5) 0.6640(5) -0.3832(3)
H21 H 0.37900 0.67420 -0.37470
H22 H 0.31490 0.70010 -0.39890
C16 C 0.3069(4) 0.6499(4) -0.3450(3)
H23 H 0.33800 0.64950 -0.31900
H24 H 0.27580 0.68170 -0.34140
C17 C 0.3397(5) 0.4651(5) -0.1679(3)
H25 H 0.31990 0.46590 -0.14200
H26 H 0.34690 0.50870 -0.17620
C18 C 0.3998(4) 0.4298(6) -0.1589(5)
H27 H 0.40710 0.41390 -0.12920
H28 H 0.43440 0.45690 -0.16360
C19 C 0.3917(7) 0.3761(8) -0.1911(8)
H29 H 0.41450 0.38400 -0.21510
H30 H 0.40550 0.33610 -0.17730
C20? C 0.3765(13) 0.3650(16) -0.1654(15)
H31? H 0.35820 0.34990 -0.14070
H32? H 0.40860 0.33560 -0.17120
C21 C 0.3274(4) 0.3753(4) -0.2057(4)
H33 H 0.30780 0.34440 -0.18890
H34 H 0.31950 0.36260 -0.23610
C22 C 0.1299(3) 0.4861(3) -0.1600(2)
C23 C 0.0841(4) 0.4961(4) -0.1350(3)
H35 H 0.04550 0.47650 -0.14210
C24 C 0.0959(5) 0.5354(6) -0.0995(3)
H36 H 0.06690 0.54200 -0.08080
C25 C 0.1493(3) 0.5625(3) -0.0934(3)
H37 H 0.15480 0.59300 -0.07130
C26 C 0.1953(5) 0.5542(5) -0.1129(3)
H38 H 0.23400 0.57240 -0.10330
C27 C 0.1845(4) 0.5174(4) -0.1481(3)
H39 H 0.21570 0.51280 -0.16530
C28 C 0.1601(3) 0.3631(3) -0.1865(2)
C29 C 0.1754(4) 0.3502(4) -0.1426(3)
H40 H 0.16560 0.37890 -0.12180
C30 C 0.2056(4) 0.2935(4) -0.1299(3)
H41 H 0.21670 0.28460 -0.10030
C31 C 0.2191(3) 0.2513(4) -0.1595(4)
H42 H 0.23900 0.21330 -0.15050
C32 C 0.2040(3) 0.2641(3) -0.2015(3)
H43 H 0.21310 0.23460 -0.22200
C33 C 0.1750(3) 0.3200(3) -0.2153(3)
H44 H 0.16540 0.32830 -0.24510
C34 C 0.0402(3) 0.4139(3) -0.2130(2)
C35 C -0.0027(3) 0.4536(3) -0.2342(2)
H45 H 0.01050 0.49150 -0.24540
C36 C -0.0645(3) 0.4406(3) -0.2400(2)
H46 H -0.09280 0.46890 -0.25530
C37 C -0.0847(3) 0.3866(3) -0.2234(3)
H47 H -0.12710 0.37760 -0.22680
C38 C -0.0428(3) 0.3455(4) -0.2018(3)
H48 H -0.05630 0.30750 -0.19090
C39 C 0.0197(3) 0.3596(3) -0.1958(3)
H49 H 0.04800 0.33200 -0.17990
C40 C 0.0890(3) 0.5903(3) -0.4108(2)
C41 C 0.0346(3) 0.5980(3) -0.4382(2)
H50 H -0.00030 0.61250 -0.42720
C42 C 0.0299(4) 0.5847(4) -0.4821(3)
H51 H -0.00800 0.58970 -0.50030
C43 C 0.0789(5) 0.5649(4) -0.4982(2)
H52 H 0.07530 0.55680 -0.52800
C44 C 0.1353(4) 0.5560(5) -0.4723(3)
H53 H 0.16970 0.54130 -0.48380
C45 C 0.1391(3) 0.5695(4) -0.4287(2)
H54 H 0.17710 0.56440 -0.41060
C46 C 0.0219(3) 0.6223(3) -0.3436(2)
C47 C -0.0116(3) 0.5749(3) -0.3290(2)
H55 H 0.00650 0.53490 -0.32390
C48 C -0.0713(3) 0.5840(3) -0.3217(2)
H56 H -0.09380 0.55020 -0.31270
C49 C -0.0969(3) 0.6416(3) -0.3275(3)
H57 H -0.13710 0.64860 -0.32170
C50 C -0.0645(3) 0.6896(3) -0.3419(3)
H58 H -0.08280 0.72960 -0.34640
C51 C -0.0054(3) 0.6804(3) -0.3498(3)
H59 H 0.01650 0.71420 -0.35960
C52 C 0.1365(3) 0.6814(3) -0.3498(2)
C53 C 0.1616(3) 0.7036(3) -0.3099(2)
H60 H 0.15990 0.67820 -0.28550
C54 C 0.1891(3) 0.7615(3) -0.3043(2)
H61 H 0.20630 0.77530 -0.27650
C55 C 0.1915(3) 0.7985(3) -0.3391(3)
H62 H 0.21150 0.83780 -0.33580
C56 C 0.1649(5) 0.7788(4) -0.3789(3)
H63 H 0.16490 0.80540 -0.40290
C57 C 0.1379(4) 0.7205(3) -0.3843(3)
H64 H 0.12030 0.70720 -0.41210
O4 O 0.36310 0.08200 0.04640
C58 C 0.35910 0.15360 0.03460
H65 H 0.35460 0.16150 0.00340
H66 H 0.39320 0.17840 0.05000
C59 C 0.29520 0.16240 0.05410
H67 H 0.30150 0.18770 0.08060
H68 H 0.26350 0.18240 0.03300
C60 C 0.27890 0.09790 0.06280
H69 H 0.28600 0.09170 0.09410
H70 H 0.23460 0.09270 0.05300
C61 C 0.31060 0.04890 0.04350
H71 H 0.31510 0.01010 0.06070
H72 H 0.29230 0.03960 0.01360
C62 C 0.46240 0.72020 0.09190
O5 O 0.46750 0.77380 0.05950
C63 C 0.51070 0.75740 0.03070
C64 C 0.53920 0.69440 0.06490
C65 C 0.49310 0.67500 0.07950
C66? C 0.20280 0.71770 0.00900
O6? O 0.25000 0.67980 0.02000
C67? C 0.22570 0.76970 0.01090
O7 O 0.12730 0.92720 -0.42150
C68 C 0.12150 0.93580 -0.46610
C69 C 0.06180 0.93860 -0.46860
C70 C 0.01480 0.89230 -0.44090
C71 C 0.06650 0.92220 -0.40690
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.70
H 0.23
Ce 1.83
Cl 1.04
Li 1.03
N 0.68
O 0.68
P 1.05
|
1100612.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:42:33 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177950 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100612.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100612
loop_
_publ_author_name
'Anfang, S.'
'Seybert, G.'
'Harms, K.'
'Geiseler, G.'
'Massa, W.'
'Dehnicke, K.'
_publ_section_title
;
Reaktionen von LiNPPh~3~ mit den Cyclooctatetraenid-Komplexen
[Ln(C~8~H~8~)Cl(THF)~2~]~2~ von Cer und Samarium. Die Kristallstrukturen
von [LiNPPh~3~]~6~, [Ln(C~8~H~8~)Li~3~Cl~2~(NPPh~3~)~2~(THF)~3~]
(Ln = Ce, Sm) und [Li(THF)~4~][Sm(C~8~H~8~)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1187
_journal_page_last 1192
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1187::aid-zaac1187>3.0.co;2-1
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C68 H86 Cl2 Li3 N2 O6 P2 Sm'
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-I 2ya'
_symmetry_space_group_name_H-M 'I 1 2/a 1'
_cell_angle_alpha 90
_cell_angle_beta 98.881(11)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 22.099(2)
_cell_length_b 21.4538(14)
_cell_length_c 31.526(3)
_cod_original_sg_symbol_H-M 'I 2/a'
_cod_original_formula_sum 'C68 H86 Cl2 Li3 N2 O6 P2 Sm1'
_cod_database_code 1100612
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2+y,1/2+z
3 1/2+x,-y,z
4 x,1/2-y,1/2+z
5 -x,-y,-z
6 -1/2-x,-1/2-y,-1/2-z
7 -1/2-x,y,-z
8 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Sm1 Sm 0.38409(1) 0.44241(2) 0.32312(1)
P1 P 0.38183(6) 0.43955(10) 0.20584(4)
N1 N 0.36038(18) 0.4649(2) 0.24660(13)
C1 C 0.3888(3) 0.3964(3) 0.4037(2)
H1 H 0.36580 0.40540 0.42610
Cl1 Cl 0.25331(5) 0.44515(9) 0.31363(4)
O1 O 0.39708(17) 0.6247(2) 0.22609(12)
Li1 Li 0.3610(3) 0.5597(5) 0.2583(3)
P2 P 0.40394(7) 0.60616(7) 0.35458(5)
N2 N 0.37097(16) 0.5543(3) 0.32529(13)
C2 C 0.3625(3) 0.3485(3) 0.3767(2)
H2 H 0.32640 0.33210 0.38550
O2 O 0.22294(19) 0.5913(2) 0.35194(14)
Li2 Li 0.2760(4) 0.5567(6) 0.3167(3)
Cl2 Cl 0.25063(6) 0.58207(7) 0.24311(5)
C3 C 0.3771(3) 0.3186(3) 0.3394(2)
H3 H 0.34770 0.28820 0.32840
O3 O 0.19863(16) 0.4355(2) 0.20318(13)
Li3 Li 0.2645(4) 0.4707(5) 0.2417(3)
C4 C 0.4246(3) 0.3235(3) 0.3150(2)
H4 H 0.42140 0.29380 0.29240
C5 C 0.4767(3) 0.3628(3) 0.3165(2)
H5 H 0.49920 0.35510 0.29370
C6 C 0.5028(3) 0.4111(3) 0.3445(2)
H6 H 0.53920 0.42720 0.33620
C7 C 0.4887(3) 0.4404(4) 0.38070(19)
H7 H 0.51750 0.47170 0.39120
C8 C 0.4412(3) 0.4347(3) 0.40575(18)
H8 H 0.44550 0.46290 0.42920
C9 C 0.4609(3) 0.6337(4) 0.2223(2)
H9 H 0.47010 0.61500 0.19530
H10 H 0.48760 0.61410 0.24670
C10 C 0.4708(3) 0.7018(4) 0.2222(3)
H11 H 0.50000 0.71320 0.20260
H12 H 0.48690 0.71700 0.25150
C11 C 0.4094(4) 0.7281(4) 0.2070(3)
H13 H 0.40950 0.75130 0.17990
H14 H 0.39720 0.75690 0.22870
C12 C 0.3659(3) 0.6741(4) 0.1999(2)
H15 H 0.32640 0.68440 0.20930
H16 H 0.35830 0.66190 0.16930
C13 C 0.1906(3) 0.5572(4) 0.3803(2)
H17 H 0.21780 0.52610 0.39690
H18 H 0.15500 0.53510 0.36400
C14 C 0.1702(4) 0.6041(4) 0.4092(3)
H19 H 0.20080 0.60940 0.43540
H20 H 0.13050 0.59210 0.41770
C15 C 0.1639(4) 0.6633(4) 0.3826(3)
H21 H 0.12510 0.66340 0.36220
H22 H 0.16520 0.70060 0.40120
C16 C 0.216(2) 0.6614(18) 0.3603(16)
H23 H 0.25300 0.67840 0.37840
H24 H 0.20810 0.68520 0.33310
C17? C 0.1894(8) 0.6483(7) 0.3421(5)
H25? H 0.15600 0.64250 0.31770
H26? H 0.21670 0.68200 0.33500
C18 C 0.1673(3) 0.4609(4) 0.1648(2)
H27 H 0.19120 0.45510 0.14100
H28 H 0.15970 0.50600 0.16820
C19 C 0.1063(4) 0.4244(5) 0.1562(3)
H29 H 0.10570 0.39500 0.13190
H30 H 0.07080 0.45290 0.15010
C20 C 0.107(2) 0.387(3) 0.2023(19)
H31 H 0.08720 0.41200 0.22290
H32 H 0.08640 0.34590 0.19800
C21? C 0.1213(7) 0.3649(7) 0.1771(8)
H33? H 0.13890 0.33580 0.15790
H34? H 0.08470 0.34550 0.18610
C22 C 0.1670(4) 0.3816(4) 0.2147(3)
H35 H 0.18210 0.34440 0.20100
H36 H 0.17550 0.37570 0.24620
C23 C 0.3734(3) 0.4931(3) 0.15985(17)
C24 C 0.4192(4) 0.5028(4) 0.1350(2)
H37 H 0.45780 0.48260 0.14190
C25 C 0.4078(4) 0.5426(5) 0.0999(3)
H38 H 0.43890 0.54890 0.08270
C26 C 0.3541(4) 0.5723(5) 0.0896(2)
H39 H 0.34730 0.59900 0.06530
C27 C 0.3097(4) 0.5636(5) 0.1144(2)
H40 H 0.27170 0.58460 0.10730
C28 C 0.3189(3) 0.5254(4) 0.1490(2)
H41 H 0.28740 0.52060 0.16610
C29 C 0.3413(3) 0.3714(3) 0.1828(2)
C30 C 0.3274(3) 0.3583(4) 0.1391(2)
H42 H 0.34000 0.38630 0.11880
C31 C 0.2950(4) 0.3041(5) 0.1249(3)
H43 H 0.28450 0.29620 0.09500
C32 C 0.2784(3) 0.2626(5) 0.1541(4)
H44 H 0.25790 0.22520 0.14420
C33 C 0.2909(3) 0.2740(4) 0.1963(3)
H45 H 0.27850 0.24520 0.21620
C34 C 0.3217(3) 0.3279(3) 0.2109(2)
H46 H 0.32980 0.33560 0.24090
C35 C 0.4618(3) 0.4170(3) 0.2109(2)
C36 C 0.5064(3) 0.4573(3) 0.23234(18)
H47 H 0.49380 0.49510 0.24400
C37 C 0.5688(2) 0.4432(4) 0.23692(18)
H48 H 0.59810 0.47160 0.25110
C38 C 0.5878(3) 0.3878(3) 0.2209(2)
H49 H 0.63010 0.37770 0.22450
C39 C 0.5448(3) 0.3472(3) 0.1994(2)
H50 H 0.55760 0.30940 0.18790
C40 C 0.4813(3) 0.3624(3) 0.1945(2)
H51 H 0.45200 0.33440 0.17970
C41 C 0.4140(3) 0.5907(3) 0.41153(17)
C42 C 0.4687(3) 0.5974(3) 0.43923(19)
H52 H 0.50400 0.61170 0.42840
C43 C 0.4727(4) 0.5835(3) 0.4827(2)
H53 H 0.51090 0.58740 0.50110
C44 C 0.4220(4) 0.5640(4) 0.4993(2)
H54 H 0.42470 0.55480 0.52900
C45 C 0.3670(3) 0.5580(5) 0.4722(2)
H55 H 0.33140 0.54460 0.48310
C46 C 0.3640(3) 0.5716(3) 0.42945(18)
H56 H 0.32570 0.56760 0.41130
C47 C 0.4816(2) 0.6250(3) 0.34456(17)
C48 C 0.5152(3) 0.5784(3) 0.32849(17)
H57 H 0.49720 0.53850 0.32230
C49 C 0.5750(3) 0.5893(3) 0.3213(2)
H58 H 0.59750 0.55660 0.31080
C50 C 0.6017(3) 0.6465(4) 0.3293(2)
H59 H 0.64240 0.65350 0.32410
C51 C 0.5695(3) 0.6938(3) 0.3449(2)
H60 H 0.58770 0.73370 0.35030
C52 C 0.5093(3) 0.6829(3) 0.35299(19)
H61 H 0.48750 0.71550 0.36430
C53 C 0.3657(2) 0.6823(3) 0.35044(17)
C54 C 0.3396(2) 0.7036(3) 0.31064(18)
H62 H 0.34090 0.67840 0.28600
C55 C 0.3116(3) 0.7612(3) 0.30591(19)
H63 H 0.29410 0.77480 0.27800
C56 C 0.3082(3) 0.7986(3) 0.3396(2)
H64 H 0.28870 0.83810 0.33600
C57 C 0.3338(4) 0.7779(4) 0.3791(2)
H65 H 0.33160 0.80330 0.40350
C58 C 0.3630(4) 0.7206(3) 0.3847(2)
H66 H 0.38120 0.70780 0.41260
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 1.03
Li 1.04
N 0.68
O 0.68
P 1.05
Sm 1.79
|
1100613.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:42:33 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177950 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100613.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100613
loop_
_publ_author_name
'Anfang, S.'
'Seybert, G.'
'Harms, K.'
'Geiseler, G.'
'Massa, W.'
'Dehnicke, K.'
_publ_section_title
;
Reaktionen von LiNPPh~3~ mit den Cyclooctatetraenid-Komplexen
[Ln(C~8~H~8~)Cl(THF)~2~]~2~ von Cer und Samarium. Die Kristallstrukturen
von [LiNPPh~3~]~6~, [Ln(C~8~H~8~)Li~3~Cl~2~(NPPh~3~)~2~(THF)~3~]
(Ln = Ce, Sm) und [Li(THF)~4~][Sm(C~8~H~8~)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1187
_journal_page_last 1192
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1187::aid-zaac1187>3.0.co;2-1
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C40 H64 Li O6 Sm'
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 106.869(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 17.7767(12)
_cell_length_b 13.1856(11)
_cell_length_c 18.0575(13)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_original_formula_sum 'C40 H64 Li1 O6 Sm1'
_cod_database_code 1100613
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2+y,z
3 x,-y,1/2+z
4 1/2+x,1/2-y,1/2+z
5 -x,-y,-z
6 -1/2-x,-1/2-y,-z
7 -x,y,-1/2-z
8 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Sm1 Sm -0.25000 0.75000 0.00000
C1 C -0.2655(5) 0.9492(4) -0.0314(5)
H1 H -0.30030 0.99900 -0.02220
O1 O 0.0561(2) 0.9821(3) 0.1967(2)
Li1 Li 0.00000 1.0649(8) 0.25000
C2 C -0.2951(4) 0.9022(5) -0.1027(4)
H2 H -0.34480 0.92870 -0.13120
O2 O 0.0728(3) 1.1528(3) 0.3231(2)
C3 C -0.2695(4) 0.8252(5) -0.1426(3)
H3 H -0.30650 0.81110 -0.19120
C4 C -0.2034(4) 0.7643(4) -0.1288(3)
H4 H -0.20590 0.71800 -0.16970
C5 C -0.1349(4) 0.7558(4) -0.0690(4)
H5 H -0.10060 0.70570 -0.07880
C6 C -0.1035(4) 0.8034(6) 0.0030(4)
H6 H -0.05340 0.77750 0.03070
C7 C -0.1295(5) 0.8808(7) 0.0434(3)
H7 H -0.09230 0.89600 0.09160
C8 C -0.1975(7) 0.9409(5) 0.0291(4)
H8 H -0.19640 0.98590 0.07050
C9 C 0.0711(4) 0.9999(4) 0.1235(3)
H9 H 0.09740 1.06620 0.12380
H10 H 0.02130 0.99970 0.08080
C10 C 0.1228(5) 0.9163(5) 0.1136(4)
H11 H 0.09150 0.86040 0.08300
H12 H 0.16090 0.94060 0.08700
C11 C 0.1612(7) 0.8844(10) 0.1879(5)
H13 H 0.20830 0.92650 0.21120
H14 H 0.17740 0.81250 0.18830
C12 C 0.0998(7) 0.8980(9) 0.2308(4)
H15 H 0.06600 0.83720 0.22490
H16 H 0.12530 0.91010 0.28660
C13 C 0.1337(8) 1.1992(12) 0.3078(6)
H17 H 0.11550 1.23610 0.25810
H18 H 0.17320 1.14830 0.30350
C14 C 0.1682(10) 1.2687(11) 0.3691(9)
H19 H 0.22500 1.25400 0.39070
H20 H 0.16240 1.33900 0.34890
C15 C 0.1329(8) 1.2594(10) 0.4235(7)
H21 H 0.10910 1.32490 0.43120
H22 H 0.17150 1.23970 0.47290
C16 C 0.0735(5) 1.1838(7) 0.4004(4)
H23 H 0.02170 1.21180 0.40010
H24 H 0.08570 1.12540 0.43640
O3 O 0.1427(10) 0.5679(19) 0.1299(14)
C17 C 0.0768(12) 0.5989(19) 0.0958(15)
H25 H 0.06130 0.57060 0.04270
H26 H 0.07920 0.67360 0.09110
C18 C 0.0218(10) 0.576(2) 0.1288(18)
H27 H 0.01910 0.63110 0.16550
H28 H -0.02970 0.57350 0.08860
C19 C 0.0324(11) 0.5014(15) 0.1611(11)
H29 H 0.00600 0.44530 0.12700
H30 H 0.01260 0.50380 0.20690
C20 C 0.1032(14) 0.4905(13) 0.1804(7)
H31 H 0.11620 0.41940 0.17140
H32 H 0.12500 0.50520 0.23630
C1E* C -0.2345(5) 0.5508(4) 0.0314(5)
H1E* H -0.19970 0.50100 0.02220
C2E* C -0.2049(4) 0.5978(5) 0.1027(4)
C3E* C -0.2305(4) 0.6748(5) 0.1426(3)
H2E* H -0.15520 0.57130 0.13120
H3E* H -0.19350 0.68890 0.19120
C4E* C -0.2966(4) 0.7357(4) 0.1288(3)
C5E* C -0.3651(4) 0.7442(4) 0.0690(4)
H4E* H -0.29410 0.78200 0.16970
H5E* H -0.39940 0.79430 0.07880
C6E* C -0.3965(4) 0.6966(6) -0.0030(4)
C7E* C -0.3705(5) 0.6192(7) -0.0434(3)
H6E* H -0.44660 0.72250 -0.03070
H7E* H -0.40770 0.60400 -0.09160
C8E* C -0.3025(7) 0.5591(5) -0.0291(4)
H8E* H -0.30360 0.51410 -0.07050
O1F* O -0.0561(2) 0.9821(3) 0.3033(2)
C9F* C -0.0711(4) 0.9999(4) 0.3765(3)
H9F* H -0.09740 1.06620 0.37620
H10F* H -0.02130 0.99970 0.41920
C10F* C -0.1228(5) 0.9163(5) 0.3864(4)
H11F* H -0.09150 0.86040 0.41700
H12F* H -0.16090 0.94060 0.41300
C11F* C -0.1612(7) 0.8844(10) 0.3121(5)
H13F* H -0.20830 0.92650 0.28880
H14F* H -0.17740 0.81250 0.31170
C12F* C -0.0998(7) 0.8980(9) 0.2692(4)
H15F* H -0.06600 0.83720 0.27510
H16F* H -0.12530 0.91010 0.21340
O2F* O -0.0728(3) 1.1528(3) 0.1769(2)
C13F* C -0.1337(8) 1.1992(12) 0.1922(6)
H17F* H -0.11550 1.23610 0.24190
H18F* H -0.17320 1.14830 0.19650
C14F* C -0.1682(10) 1.2687(11) 0.1309(9)
H19F* H -0.22500 1.25400 0.10930
H20F* H -0.16240 1.33900 0.15110
C15F* C -0.1329(8) 1.2594(10) 0.0765(7)
H21F* H -0.10910 1.32490 0.06880
H22F* H -0.17150 1.23970 0.02710
C16F* C -0.0735(5) 1.1838(7) 0.0996(4)
H23F* H -0.02170 1.21180 0.09990
H24F* H -0.08570 1.12540 0.06360
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 0.98
O 0.68
Sm 1.80
|
1100614.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100614.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100614
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C32 H52 Br4 N2 O5 Sm2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 95.46(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.022(3)
_cell_length_b 17.683(4)
_cell_length_c 16.181(3)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100614
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Sm1 Sm 0.19766(2) 0.10099(1) 0.85762(1)
Sm2 Sm 0.30836(2) -0.02670(1) 0.69536(2)
Br1 Br 0.18209(5) -0.02746(3) 0.95789(4)
Br2 Br 0.20882(4) 0.23230(3) 0.75906(4)
Br3 Br 0.30374(5) 0.07370(4) 0.55762(4)
Br4 Br 0.30901(6) -0.16055(3) 0.78951(4)
O1 O 0.1244(3) 0.1634(2) 0.9771(3)
O2 O 0.3235(3) 0.1661(2) 0.9517(2)
O3 O 0.0212(3) 0.1128(2) 0.8236(2)
O4 O 0.2760(4) -0.1184(2) 0.5819(3)
O5 O 0.4796(3) -0.0442(2) 0.6760(2)
N1 N 0.1651(4) 0.0390(3) 0.7191(3)
H1 H 0.1628(4) 0.0790(3) 0.6816(3)
N2 N 0.3499(3) 0.0385(2) 0.8246(3)
H2 H 0.3610(3) 0.0005(2) 0.8641(3)
C1 C 0.0819(4) -0.0047(3) 0.6932(3)
C2 C 0.0238(6) 0.0197(4) 0.6228(4)
H3 H 0.0414(6) 0.0631(4) 0.5931(4)
C3 C -0.0614(6) -0.0204(5) 0.5960(4)
H4 H -0.1024(6) -0.0037(5) 0.5495(4)
C4 C -0.0823(6) -0.0834(5) 0.6390(5)
H5 H -0.1384(6) -0.1114(5) 0.6219(5)
C5 C -0.0265(6) -0.1059(4) 0.7035(5)
H6 H -0.0436(6) -0.1499(4) 0.7324(5)
C6 C 0.0551(5) -0.0687(4) 0.7308(4)
H7 H 0.0943(5) -0.0880(4) 0.7772(4)
C7 C 0.4371(4) 0.0785(3) 0.8263(3)
C8 C 0.5143(4) 0.0619(4) 0.8839(4)
H8 H 0.5099(4) 0.0219(4) 0.9226(4)
C9 C 0.5993(5) 0.1049(4) 0.8844(5)
H9 H 0.6516(5) 0.0946(4) 0.9246(5)
C10 C 0.6069(5) 0.1610(4) 0.8278(5)
H10 H 0.6639(5) 0.1901(4) 0.8291(5)
C11 C 0.5321(5) 0.1754(4) 0.7688(4)
H11 H 0.5386(5) 0.2129(4) 0.7276(4)
C12 C 0.4478(4) 0.1357(3) 0.7691(4)
H12 H 0.3958(4) 0.1476(3) 0.7293(4)
C13 C 0.0876(6) 0.1371(4) 1.0524(4)
H13 H 0.1403(6) 0.1295(4) 1.0968(4)
H14 H 0.0528(6) 0.0887(4) 1.0426(4)
C14 C 0.0221(7) 0.1972(4) 1.0754(5)
H15 H 0.0276(7) 0.2042(4) 1.1364(5)
H16 H -0.0450(7) 0.1842(4) 1.0564(5)
C15 C 0.0523(7) 0.2679(4) 1.0330(5)
H17 H -0.0002(7) 0.2871(4) 0.9934(5)
H18 H 0.0712(7) 0.3079(4) 1.0741(5)
H19? H -0.0021(7) 0.3032(4) 1.0221(5)
H20? H 0.1049(7) 0.2939(4) 1.0670(5)
C16 C 0.1346(9) 0.2440(6) 0.9893(8)
H21 H 0.1342(9) 0.2703(6) 0.9353(8)
H22 H 0.1955(9) 0.2557(6) 1.0230(8)
C17? C 0.0835(13) 0.2405(9) 0.9581(10)
H23? H 0.1328(13) 0.2743(9) 0.9385(10)
H24? H 0.0290(13) 0.2374(9) 0.9146(10)
C18 C 0.3573(6) 0.1343(4) 1.0308(4)
H25 H 0.3873(6) 0.0844(4) 1.0238(4)
H26 H 0.3039(6) 0.1283(4) 1.0662(4)
H27? H 0.4098(6) 0.0978(4) 1.0253(4)
H28? H 0.3048(6) 0.1086(4) 1.0566(4)
C19 C 0.4282(16) 0.1889(12) 1.0679(13)
H29 H 0.4052(16) 0.2103(12) 1.1189(13)
H30 H 0.4894(16) 0.1624(12) 1.0837(13)
C20? C 0.3945(10) 0.2061(7) 1.0836(8)
H31? H 0.3414(10) 0.2364(7) 1.1026(8)
H32? H 0.4403(10) 0.1923(7) 1.1316(8)
C21 C 0.4434(6) 0.2456(5) 1.0148(6)
H33 H 0.5090(6) 0.2420(5) 0.9971(6)
H34 H 0.4366(6) 0.2951(5) 1.0421(6)
H35? H 0.4567(6) 0.2993(5) 1.0285(6)
H36? H 0.5042(6) 0.2201(5) 1.0048(6)
C22 C 0.3714(7) 0.2383(4) 0.9418(5)
H37 H 0.3248(7) 0.2804(4) 0.9404(5)
H38 H 0.4030(7) 0.2389(4) 0.8897(5)
C23 C -0.0304(5) 0.1647(4) 0.7660(5)
H39 H -0.0217(5) 0.1511(4) 0.7079(5)
H40 H -0.0084(5) 0.2173(4) 0.7763(5)
H41? H 0.0009(5) 0.1678(4) 0.7138(5)
H42? H -0.0318(5) 0.2159(4) 0.7905(5)
C24 C -0.1314(13) 0.1558(10) 0.7830(11)
H43 H -0.1531(13) 0.2026(10) 0.8090(11)
H44 H -0.1715(13) 0.1484(10) 0.7299(11)
C25? C -0.1327(10) 0.1332(8) 0.749(1)
H45? H -0.1806(10) 0.1715(8) 0.7622(10)
H46? H -0.1459(10) 0.1182(8) 0.6901(10)
C26 C -0.1428(14) 0.1005(12) 0.8302(13)
H47 H -0.1850(14) 0.0626(12) 0.8003(13)
H48 H -0.1742(14) 0.1180(12) 0.8790(13)
C27? C -0.1357(9) 0.0663(7) 0.8045(7)
H49? H -0.1912(9) 0.0700(7) 0.8377(7)
H50? H -0.1424(9) 0.0194(7) 0.7710(7)
C28 C -0.0470(5) 0.0643(5) 0.8591(5)
H51 H -0.0361(5) 0.0636(5) 0.9205(5)
H52 H -0.0434(5) 0.0119(5) 0.8380(5)
H53? H -0.0585(5) 0.0823(5) 0.9152(5)
H54? H -0.0221(5) 0.0119(5) 0.8639(5)
C29 C 0.1918(7) -0.1626(7) 0.5620(6)
H55 H 0.1326(7) -0.1335(7) 0.5686(6)
H56 H 0.1922(7) -0.2095(7) 0.5954(6)
H57? H 0.1377(7) -0.1299(7) 0.5406(6)
H58? H 0.1739(7) -0.1896(7) 0.6119(6)
C30 C 0.2052(14) -0.1792(12) 0.4671(12)
H59 H 0.1797(14) -0.2300(12) 0.4518(12)
H60 H 0.1687(14) -0.1415(12) 0.4315(12)
C31? C 0.2160(12) -0.2185(9) 0.4961(10)
H61? H 0.2120(12) -0.2709(9) 0.5172(10)
H62? H 0.1702(12) -0.2132(9) 0.446(1)
C32 C 0.2998(13) -0.1757(10) 0.4539(11)
H63 H 0.3090(13) -0.1443(10) 0.4046(11)
H64 H 0.3257(13) -0.2269(10) 0.4454(11)
C33? C 0.3009(16) -0.2042(12) 0.4786(13)
H65? H 0.2991(16) -0.1905(12) 0.4191(13)
H66? H 0.3405(16) -0.2504(12) 0.4875(13)
C34 C 0.3475(8) -0.1408(7) 0.5302(7)
H67 H 0.3916(8) -0.1776(7) 0.5598(7)
H68 H 0.3852(8) -0.0962(7) 0.5156(7)
H69? H 0.4058(8) -0.1586(7) 0.5638(7)
H70? H 0.3648(8) -0.0984(7) 0.4946(7)
C35 C 0.5389(6) -0.0957(5) 0.7268(7)
H71 H 0.5282(6) -0.1481(5) 0.7066(7)
H72 H 0.5228(6) -0.0931(5) 0.7850(7)
C36 C 0.6388(6) -0.0740(5) 0.7220(8)
H73 H 0.6736(6) -0.1147(5) 0.6957(8)
H74 H 0.6707(6) -0.0647(5) 0.7784(8)
C37 C 0.6384(6) -0.0040(5) 0.6715(5)
H75 H 0.6874(6) -0.0068(5) 0.6314(5)
H76 H 0.6516(6) 0.0409(5) 0.7074(5)
C38 C 0.5411(5) 0.0002(5) 0.6277(4)
H77 H 0.5189(5) 0.0533(5) 0.6238(4)
H78 H 0.5408(5) -0.0206(5) 0.5709(4)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Br 1.21
N 0.68
O 0.68
Sm 1.74
|
1100615.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100615.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100615
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C40 H96 Li4 N6 O6 Si4 Sm2'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 69.71(1)
_cell_angle_beta 81.81(1)
_cell_angle_gamma 67.38(1)
_cell_formula_units_Z 1
_cell_length_a 11.195(1)
_cell_length_b 12.156(1)
_cell_length_c 12.551(1)
_cod_database_code 1100615
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Sm1 Sm 0.45250(2) 0.46038(2) 0.16267(1)
Si1 Si 0.25150(9) 0.5889(1) -0.10526(9)
Li1 Li 0.4521(7) 0.3256(6) -0.0052(5)
O1 O 0.3743(2) 0.5061(2) -0.0175(2)
N1 N 0.4057(4) 0.6783(4) 0.1302(3)
C1 C 0.3963(4) 0.7738(4) 0.1801(4)
Si2 Si 0.36008(10) 0.23608(10) 0.24203(9)
Li2 Li 0.6474(7) 0.1910(6) 0.1936(7)
O2 O 0.4769(2) 0.2539(2) 0.1503(2)
N2 N 0.6775(3) 0.3361(3) 0.2225(3)
C2 C 0.4504(6) 0.8708(5) 0.0991(5)
H1 H 0.54270 0.83060 0.08880
H2 H 0.43500 0.93750 0.13070
H3 H 0.40790 0.90590 0.02620
N3 N 0.3231(3) 0.3619(3) 0.2877(3)
C3 C 0.4755(6) 0.7097(6) 0.2876(5)
H4 H 0.44420 0.64600 0.33950
H5 H 0.46730 0.77150 0.32320
H6 H 0.56560 0.67060 0.26890
O3 O 0.7621(3) 0.0256(3) 0.1915(4)
C4 C 0.2572(6) 0.8431(6) 0.2107(7)
H7 H 0.21990 0.78260 0.25940
H8 H 0.20680 0.89150 0.14190
H9 H 0.25630 0.89920 0.25020
C5 C 0.1826(5) 0.4790(5) -0.1262(4)
H10 H 0.11600 0.52570 -0.18360
H11 H 0.14530 0.44070 -0.05520
H12 H 0.25090 0.41390 -0.15060
C6 C 0.1197(4) 0.6916(5) -0.0343(4)
H13 H 0.04300 0.73450 -0.08110
H14 H 0.14820 0.75330 -0.02420
H15 H 0.09950 0.64030 0.03920
C7 C 0.7315(4) 0.2779(4) 0.3393(3)
C8 C 0.6970(6) 0.3755(5) 0.3986(4)
H16 H 0.60370 0.41270 0.40490
H17 H 0.73430 0.33590 0.47390
H18 H 0.73100 0.44050 0.35490
C9 C 0.6735(5) 0.1795(5) 0.4091(4)
H19 H 0.57980 0.21750 0.40650
H20 H 0.70240 0.11060 0.37800
H21 H 0.70140 0.14780 0.48730
C10 C 0.8789(4) 0.2110(5) 0.3393(4)
H22 H 0.91940 0.27220 0.30020
H23 H 0.90910 0.16970 0.41700
H24 H 0.90160 0.14890 0.30070
C11 C 0.4164(5) 0.0763(4) 0.3515(4)
H25 H 0.34610 0.06650 0.40430
H26 H 0.48850 0.06720 0.39260
H27 H 0.44370 0.01240 0.31440
C12 C 0.2268(4) 0.2335(5) 0.1685(4)
H28 H 0.17090 0.19860 0.22480
H29 H 0.26400 0.18200 0.11930
H30 H 0.17680 0.31850 0.12350
C13 C 0.2272(4) 0.3988(4) 0.3737(3)
C14 C 0.1183(14) 0.354(2) 0.3903(15)
H31 H 0.14940 0.26390 0.42540
H32 H 0.08060 0.37660 0.31730
H33 H 0.05330 0.39380 0.43900
C15? C 0.0956(10) 0.460(2) 0.3214(15)
H34? H 0.07440 0.39900 0.30230
H35? H 0.09530 0.52930 0.25300
H36? H 0.03190 0.49190 0.37500
C16? C 0.254(2) 0.486(3) 0.413(2)
H37? H 0.34360 0.44970 0.43730
H38? H 0.19720 0.50100 0.47620
H39? H 0.24050 0.56430 0.35160
C17 C 0.1744(19) 0.5397(10) 0.3449(15)
H40 H 0.12770 0.57770 0.27400
H41 H 0.24530 0.56930 0.33710
H42 H 0.11620 0.56300 0.40510
C18 C 0.2952(12) 0.3514(19) 0.4853(10)
H43 H 0.30940 0.26280 0.52110
H44 H 0.24200 0.39810 0.53480
H45 H 0.37770 0.36300 0.47180
C19? C 0.223(2) 0.2869(14) 0.4730(15)
H46? H 0.31090 0.22710 0.49150
H47? H 0.17290 0.24730 0.45360
H48? H 0.18420 0.31410 0.53800
C20 C 0.7098(6) -0.0687(6) 0.2106(7)
H49 H 0.63160 -0.03550 0.16550
H50 H 0.68740 -0.09940 0.29110
C21 C 0.8121(8) -0.1717(7) 0.1754(10)
H51 H 0.81170 -0.25410 0.22490
H52 H 0.79980 -0.16300 0.09670
C22 C 0.9279(8) -0.1574(9) 0.1863(13)
H53 H 0.98810 -0.17580 0.12460
H54 H 0.96890 -0.21530 0.25880
C23 C 0.8965(7) -0.0313(7) 0.1815(12)
H55 H 0.93940 -0.02940 0.24340
H56 H 0.92700 0.01500 0.10930
H57 H 0.349(5) 0.713(5) 0.085(4)
Sm1A* Sm 0.54750(2) 0.53962(2) -0.16267(1)
O1A* O 0.6257(2) 0.4939(2) 0.0175(2)
Li1A* Li 0.5479(7) 0.6744(6) 0.0052(5)
Si1A* Si 0.74850(9) 0.4111(1) 0.10526(9)
N2A* N 0.3225(3) 0.6639(3) -0.2225(3)
N1A* N 0.5943(4) 0.3217(4) -0.1302(3)
C1A* C 0.6037(4) 0.2262(4) -0.1801(4)
C2A* C 0.5496(6) 0.1292(5) -0.0991(5)
H1A* H 0.45730 0.16940 -0.08880
H2A* H 0.56500 0.06250 -0.13070
H3A* H 0.59210 0.09410 -0.02620
C3A* C 0.5245(6) 0.2903(6) -0.2876(5)
H4A* H 0.55580 0.35400 -0.33950
H5A* H 0.53270 0.22850 -0.32320
H6A* H 0.43440 0.32940 -0.26890
C4A* C 0.7428(6) 0.1569(6) -0.2107(7)
H7A* H 0.78010 0.21740 -0.25940
H8A* H 0.79320 0.10850 -0.14190
H9A* H 0.74370 0.10080 -0.25020
H57A* H 0.651(5) 0.287(5) -0.085(4)
O2A* O 0.5231(2) 0.7461(2) -0.1503(2)
Si2A* Si 0.63992(10) 0.76392(10) -0.24203(9)
N3A* N 0.6769(3) 0.6381(3) -0.2877(3)
C13A* C 0.7728(4) 0.6012(4) -0.3737(3)
C14A* C 0.8817(14) 0.646(2) -0.3903(15)
H31A* H 0.85060 0.73610 -0.42540
H32A* H 0.91940 0.62340 -0.31730
H33A* H 0.94670 0.60620 -0.43900
C17A* C 0.8256(19) 0.4603(10) -0.3449(15)
H40A* H 0.87230 0.42230 -0.27400
H41A* H 0.75470 0.43070 -0.33710
H42A* H 0.88380 0.43700 -0.40510
C18A* C 0.7048(12) 0.6486(19) -0.4853(10)
H43A* H 0.69060 0.73720 -0.52110
H44A* H 0.75800 0.60190 -0.53480
H45A* H 0.62230 0.63700 -0.47180
C11A* C 0.5836(5) 0.9237(4) -0.3515(4)
H25A* H 0.65390 0.93350 -0.40430
H26A* H 0.51150 0.93280 -0.39260
H27A* H 0.55630 0.98760 -0.31440
C12A* C 0.7732(4) 0.7665(5) -0.1685(4)
H28A* H 0.82910 0.80140 -0.22480
H29A* H 0.73600 0.81800 -0.11930
H30A* H 0.82320 0.68150 -0.12350
Li2A* Li 0.3526(7) 0.8090(6) -0.1936(7)
C7A* C 0.2685(4) 0.7221(4) -0.3393(3)
C8A* C 0.3030(6) 0.6245(5) -0.3986(4)
H16A* H 0.39630 0.58730 -0.40490
H17A* H 0.26570 0.66410 -0.47390
H18A* H 0.26900 0.55950 -0.35490
C9A* C 0.3265(5) 0.8205(5) -0.4091(4)
H19A* H 0.42020 0.78250 -0.40650
H20A* H 0.29760 0.88940 -0.37800
H21A* H 0.29860 0.85220 -0.48730
C10A* C 0.1211(4) 0.7890(5) -0.3393(4)
H22A* H 0.08060 0.72780 -0.30020
H23A* H 0.09090 0.83030 -0.41700
H24A* H 0.09840 0.85110 -0.30070
O3A* O 0.2379(3) 0.9744(3) -0.1915(4)
C20A* C 0.2902(6) 1.0687(6) -0.2106(7)
H49A* H 0.36840 1.03550 -0.16550
H50A* H 0.31260 1.09940 -0.29110
C21A* C 0.1879(8) 1.1717(7) -0.1754(10)
H51A* H 0.18830 1.25410 -0.22490
H52A* H 0.20020 1.16300 -0.09670
C22A* C 0.0721(8) 1.1574(9) -0.1863(13)
H53A* H 0.01190 1.17580 -0.12460
H54A* H 0.03110 1.21530 -0.25880
C23A* C 0.1035(7) 1.0313(7) -0.1815(12)
H55A* H 0.06060 1.02940 -0.24340
H56A* H 0.07300 0.98500 -0.10930
C5A* C 0.8174(5) 0.5210(5) 0.1262(4)
H10A* H 0.88400 0.47430 0.18360
H11A* H 0.85470 0.55930 0.05520
H12A* H 0.74910 0.58610 0.15060
C6A* C 0.8803(4) 0.3084(5) 0.0343(4)
H13A* H 0.95700 0.26550 0.08110
H14A* H 0.85180 0.24670 0.02420
H15A* H 0.90050 0.35970 -0.03920
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 0.98
N 0.70
O 0.68
Si 1.10
Sm 1.57
|
1100616.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100616.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100616
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C40 H96 Gd2 Li4 N6 O6 Si4'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 69.663(11)
_cell_angle_beta 81.851(12)
_cell_angle_gamma 67.865(16)
_cell_formula_units_Z 1
_cell_length_a 11.2049(18)
_cell_length_b 12.1604(15)
_cell_length_c 12.5925(18)
_cod_database_code 1100616
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Gd1 Gd 0.45424(2) 0.45887(2) 0.16109(1)
Si1 Si 0.25232(10) 0.5875(1) -0.10378(9)
Li1 Li 0.4515(7) 0.3254(6) -0.0060(5)
O1 O 0.3742(2) 0.5064(2) -0.0163(2)
N1 N 0.4074(4) 0.6737(4) 0.1322(3)
C1 C 0.3974(5) 0.7711(4) 0.1813(4)
Si2 Si 0.36041(11) 0.2363(1) 0.24155(9)
Li2 Li 0.6479(7) 0.1915(7) 0.1931(7)
O2 O 0.4774(3) 0.2543(2) 0.1489(2)
N2 N 0.6770(3) 0.3376(3) 0.2211(3)
C2 C 0.4527(7) 0.8679(5) 0.0995(5)
H1 H 0.54500 0.82830 0.09140
H2 H 0.43540 0.93620 0.12920
H3 H 0.41260 0.90040 0.02620
N3 N 0.3233(3) 0.3620(3) 0.2861(3)
C3 C 0.4756(7) 0.7079(6) 0.2891(5)
H4 H 0.44180 0.64650 0.34210
H5 H 0.47010 0.77030 0.32270
H6 H 0.56490 0.66640 0.27130
O3 O 0.7603(4) 0.0257(3) 0.1923(4)
C4 C 0.2588(6) 0.8391(7) 0.2113(7)
H7 H 0.22250 0.77860 0.26200
H8 H 0.20840 0.88450 0.14270
H9 H 0.25730 0.89760 0.24820
C5 C 0.1840(5) 0.4767(5) -0.1240(4)
H10 H 0.11780 0.52260 -0.18130
H11 H 0.14680 0.43830 -0.05310
H12 H 0.25210 0.41210 -0.14810
C6 C 0.1210(4) 0.6899(5) -0.0335(4)
H13 H 0.04540 0.73320 -0.08100
H14 H 0.15020 0.75080 -0.02260
H15 H 0.09950 0.63870 0.03930
C7 C 0.7301(4) 0.2805(4) 0.3374(3)
C8 C 0.6969(7) 0.3777(5) 0.3977(4)
H16 H 0.60410 0.41270 0.40650
H17 H 0.73650 0.33810 0.47170
H18 H 0.72890 0.44410 0.35320
C9 C 0.6718(5) 0.1823(5) 0.4079(4)
H19 H 0.57850 0.22000 0.40620
H20 H 0.69920 0.11380 0.37690
H21 H 0.70040 0.15060 0.48550
C10 C 0.8783(5) 0.2135(6) 0.3362(4)
H22 H 0.91920 0.27530 0.30070
H23 H 0.90840 0.16810 0.41330
H24 H 0.90010 0.15530 0.29390
C11 C 0.4172(5) 0.0763(5) 0.3509(4)
H25 H 0.34790 0.06630 0.40470
H26 H 0.49020 0.06730 0.39050
H27 H 0.44260 0.01270 0.31400
C12 C 0.2277(5) 0.2313(5) 0.1686(4)
H28 H 0.17900 0.18600 0.22410
H29 H 0.26490 0.18930 0.11250
H30 H 0.17090 0.31610 0.13160
C13 C 0.2280(4) 0.3975(4) 0.3731(4)
C14 C 0.1138(13) 0.364(2) 0.3835(14)
H31 H 0.13720 0.27370 0.41830
H32 H 0.07910 0.38890 0.30890
H33 H 0.04940 0.40590 0.43010
C15? C 0.1029(13) 0.482(2) 0.3129(11)
H34? H 0.06770 0.43340 0.28820
H35? H 0.11820 0.54710 0.24760
H36? H 0.04210 0.52020 0.36420
C16? C 0.2690(18) 0.461(3) 0.4309(19)
H37? H 0.35890 0.41490 0.45110
H38? H 0.21710 0.46400 0.49910
H39? H 0.25840 0.54500 0.38160
C17 C 0.1863(15) 0.5395(9) 0.3473(11)
H40 H 0.13880 0.58260 0.27700
H41 H 0.26190 0.56230 0.34000
H42 H 0.13170 0.56340 0.40850
C18 C 0.2931(13) 0.3422(14) 0.4867(8)
H43 H 0.30440 0.25390 0.51780
H44 H 0.24000 0.38560 0.53800
H45 H 0.37650 0.35160 0.47710
C19? C 0.204(2) 0.2838(13) 0.4583(16)
H46? H 0.28600 0.21740 0.48350
H47? H 0.15490 0.25530 0.42310
H48? H 0.15620 0.30620 0.52270
C20 C 0.7106(7) -0.0696(6) 0.2107(7)
H49 H 0.63260 -0.03740 0.16610
H50 H 0.68840 -0.10090 0.29100
C21 C 0.8111(8) -0.1714(8) 0.1756(10)
H51 H 0.81310 -0.25390 0.22680
H52 H 0.79730 -0.16470 0.09810
C22 C 0.9243(9) -0.1514(9) 0.1828(14)
H53 H 0.97000 -0.21170 0.25210
H54 H 0.98080 -0.16450 0.11790
C23 C 0.8963(8) -0.0317(8) 0.1837(13)
H55 H 0.92870 0.01660 0.11400
H56 H 0.93790 -0.03390 0.24820
H57 H 0.325(7) 0.729(7) 0.079(6)
Gd1A* Gd 0.54576(2) 0.54113(2) -0.16109(1)
O1A* O 0.6258(2) 0.4936(2) 0.0163(2)
Li1A* Li 0.5485(7) 0.6746(6) 0.0060(5)
Si1A* Si 0.74768(10) 0.4125(1) 0.10378(9)
N2A* N 0.3230(3) 0.6624(3) -0.2211(3)
N1A* N 0.5926(4) 0.3263(4) -0.1322(3)
C1A* C 0.6026(5) 0.2289(4) -0.1813(4)
C2A* C 0.5473(7) 0.1321(5) -0.0995(5)
H1A* H 0.45500 0.17170 -0.09140
H2A* H 0.56460 0.06380 -0.12920
H3A* H 0.58740 0.09960 -0.02620
C3A* C 0.5244(7) 0.2921(6) -0.2891(5)
H4A* H 0.55820 0.35350 -0.34210
H5A* H 0.52990 0.22970 -0.32270
H6A* H 0.43510 0.33360 -0.27130
C4A* C 0.7412(6) 0.1609(7) -0.2113(7)
H7A* H 0.77750 0.22140 -0.26200
H8A* H 0.79160 0.11550 -0.14270
H9A* H 0.74270 0.10240 -0.24820
H57A* H 0.675(7) 0.271(7) -0.079(6)
O2A* O 0.5226(3) 0.7457(2) -0.1489(2)
Si2A* Si 0.63959(11) 0.7637(1) -0.24155(9)
N3A* N 0.6767(3) 0.6380(3) -0.2861(3)
C13A* C 0.7720(4) 0.6025(4) -0.3731(4)
C14A* C 0.8862(13) 0.636(2) -0.3835(14)
H31A* H 0.86280 0.72630 -0.41830
H32A* H 0.92090 0.61110 -0.30890
H33A* H 0.95060 0.59410 -0.43010
C17A* C 0.8137(15) 0.4605(9) -0.3473(11)
H40A* H 0.86120 0.41740 -0.27700
H41A* H 0.73810 0.43770 -0.34000
H42A* H 0.86830 0.43660 -0.40850
C18A* C 0.7069(13) 0.6578(14) -0.4867(8)
H43A* H 0.69560 0.74610 -0.51780
H44A* H 0.76000 0.61440 -0.53800
H45A* H 0.62350 0.64840 -0.47710
C11A* C 0.5828(5) 0.9237(5) -0.3509(4)
H25A* H 0.65210 0.93370 -0.40470
H26A* H 0.50980 0.93270 -0.39050
H27A* H 0.55740 0.98730 -0.31400
C12A* C 0.7723(5) 0.7687(5) -0.1686(4)
H28A* H 0.82100 0.81400 -0.22410
H29A* H 0.73510 0.81070 -0.11250
H30A* H 0.82910 0.68390 -0.13160
Li2A* Li 0.3521(7) 0.8085(7) -0.1931(7)
C7A* C 0.2699(4) 0.7195(4) -0.3374(3)
C8A* C 0.3031(7) 0.6223(5) -0.3977(4)
H16A* H 0.39590 0.58730 -0.40650
H17A* H 0.26350 0.66190 -0.47170
H18A* H 0.27110 0.55590 -0.35320
C9A* C 0.3282(5) 0.8177(5) -0.4079(4)
H19A* H 0.42150 0.78000 -0.40620
H20A* H 0.30080 0.88620 -0.37690
H21A* H 0.29960 0.84940 -0.48550
C10A* C 0.1217(5) 0.7865(6) -0.3362(4)
H22A* H 0.08080 0.72470 -0.30070
H23A* H 0.09160 0.83190 -0.41330
H24A* H 0.09990 0.84470 -0.29390
O3A* O 0.2397(4) 0.9743(3) -0.1923(4)
C20A* C 0.2894(7) 1.0696(6) -0.2107(7)
H49A* H 0.36740 1.03740 -0.16610
H50A* H 0.31160 1.10090 -0.29100
C21A* C 0.1889(8) 1.1714(8) -0.1756(10)
H51A* H 0.18690 1.25390 -0.22680
H52A* H 0.20270 1.16470 -0.09810
C22A* C 0.0757(9) 1.1514(9) -0.1828(14)
H53A* H 0.03000 1.21170 -0.25210
H54A* H 0.01920 1.16450 -0.11790
C23A* C 0.1037(8) 1.0317(8) -0.1837(13)
H55A* H 0.07130 0.98340 -0.11400
H56A* H 0.06210 1.03390 -0.24820
C5A* C 0.8160(5) 0.5233(5) 0.1240(4)
H10A* H 0.88220 0.47740 0.18130
H11A* H 0.85320 0.56170 0.05310
H12A* H 0.74790 0.58790 0.14810
C6A* C 0.8790(4) 0.3101(5) 0.0335(4)
H13A* H 0.95460 0.26680 0.08100
H14A* H 0.84980 0.24920 0.02260
H15A* H 0.90050 0.36130 -0.03930
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Gd 1.51
Li 0.98
N 0.70
O 0.68
Si 1.15
|
1100617.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100617.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100617
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C32 H52 Br4 Gd2 N2 O5'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 94.74(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.042(3)
_cell_length_b 17.720(4)
_cell_length_c 16.159(3)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100617
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Gd1 Gd 0.19640(3) 0.09997(3) 0.85512(3)
Gd2 Gd 0.30919(4) -0.02680(3) 0.69520(3)
Br1 Br 0.20880(9) 0.22841(6) 0.75581(7)
Br2 Br 0.18119(10) -0.02584(6) 0.95686(7)
Br3 Br 0.30696(10) 0.07431(8) 0.56052(7)
Br4 Br 0.30606(13) -0.15940(7) 0.78841(9)
O1 O 0.1216(7) 0.1641(4) 0.9723(5)
O2 O 0.0216(6) 0.1120(5) 0.8212(5)
O3 O 0.3194(6) 0.1642(4) 0.9496(4)
O4 O 0.4782(6) -0.0451(4) 0.6771(5)
O5 O 0.2743(8) -0.1161(5) 0.5820(5)
N1 N 0.1606(8) 0.0341(6) 0.7183(7)
H1 H 0.1580(8) 0.0737(6) 0.6804(7)
N2 N 0.3502(7) 0.0411(5) 0.8216(5)
H2 H 0.3603(7) 0.0033(5) 0.8612(5)
C1 C 0.0798(8) -0.0073(6) 0.6936(6)
C2 C 0.0471(11) -0.0712(8) 0.7304(8)
H3 H 0.0837(11) -0.0910(8) 0.7775(8)
C3 C -0.0321(15) -0.1063(9) 0.7038(12)
H4 H -0.0510(15) -0.1502(9) 0.7320(12)
C4 C -0.0855(12) -0.0813(12) 0.6384(12)
H5 H -0.1427(12) -0.1077(12) 0.6214(12)
C5 C -0.0626(13) -0.0207(10) 0.5951(8)
H6 H -0.1017(13) -0.004(1) 0.5478(8)
C6 C 0.0235(13) 0.0179(7) 0.6233(9)
H7 H 0.0427(13) 0.0611(7) 0.5941(9)
C7 C 0.4371(8) 0.0794(6) 0.8256(6)
C8 C 0.4496(9) 0.1369(6) 0.7691(8)
H8 H 0.3987(9) 0.1493(6) 0.7290(8)
C9 C 0.5358(10) 0.1771(8) 0.770(1)
H9 H 0.5435(10) 0.2156(8) 0.7301(10)
C10 C 0.6093(11) 0.1603(9) 0.8291(10)
H10 H 0.6671(11) 0.1883(9) 0.8315(10)
C11 C 0.5982(10) 0.1027(10) 0.8843(9)
H11 H 0.6488(10) 0.091(1) 0.9250(9)
C12 C 0.5114(9) 0.0602(8) 0.8812(8)
H12 H 0.5056(9) 0.0188(8) 0.9178(8)
C13 C 0.0878(11) 0.1369(8) 1.0495(7)
H13 H 0.1417(11) 0.1291(8) 1.0921(7)
H14 H 0.0524(11) 0.0889(8) 1.0407(7)
C14 C 0.0228(15) 0.1989(7) 1.0749(8)
H15 H -0.0449(15) 0.1867(7) 1.0581(8)
H16 H 0.0302(15) 0.2066(7) 1.1358(8)
C15 C 0.0537(14) 0.2673(9) 1.0304(10)
H17 H 0.0007(14) 0.2870(9) 0.9922(10)
H18 H 0.0749(14) 0.3074(9) 1.0703(10)
H19? H 0.0011(14) 0.3045(9) 1.0227(10)
H20? H 0.1093(14) 0.2915(9) 1.0613(10)
C16 C 0.1314(19) 0.2423(12) 0.9849(15)
H21 H 0.1299(19) 0.2688(12) 0.9309(15)
H22 H 0.1932(19) 0.2535(12) 1.0167(15)
C17? C 0.0794(17) 0.2380(11) 0.9497(13)
H23? H 0.0223(17) 0.2325(11) 0.9099(13)
H24? H 0.1262(17) 0.2713(11) 0.9252(13)
C18 C -0.0466(15) 0.0734(12) 0.8635(12)
H25 H -0.0375(15) 0.0837(12) 0.9239(12)
H26 H -0.0419(15) 0.0183(12) 0.8545(12)
C19? C -0.0430(25) 0.0458(20) 0.8534(21)
H27? H -0.0197(25) -0.0047(20) 0.8383(21)
H28? H -0.0479(25) 0.0485(20) 0.9140(21)
C20 C -0.1397(31) 0.1023(24) 0.8284(26)
H29 H -0.1771(31) 0.0607(24) 0.8009(26)
H30 H -0.1760(31) 0.1223(24) 0.8736(26)
C21? C -0.1325(18) 0.0655(14) 0.8063(15)
H31? H -0.1549(18) 0.0204(14) 0.7742(15)
H32? H -0.1802(18) 0.0760(14) 0.8467(15)
C22 C -0.1280(27) 0.1542(21) 0.7762(24)
H33 H -0.1530(27) 0.2023(21) 0.7967(24)
H34 H -0.1645(27) 0.1419(21) 0.7228(24)
C23? C -0.1333(23) 0.1294(18) 0.7487(20)
H35? H -0.1818(23) 0.1672(18) 0.7616(20)
H36? H -0.1468(23) 0.1124(18) 0.6906(20)
C24 C -0.030(1) 0.1628(8) 0.7631(10)
H37 H -0.0092(10) 0.2155(8) 0.7736(10)
H38 H -0.0185(10) 0.1494(8) 0.7053(10)
H39? H 0.0009(10) 0.1649(8) 0.7102(10)
H40? H -0.0318(10) 0.2143(8) 0.7865(10)
C25 C 0.3659(14) 0.2394(9) 0.9381(10)
H41 H 0.3945(14) 0.2416(9) 0.8841(10)
H42 H 0.3191(14) 0.2809(9) 0.9406(10)
C26 C 0.4417(13) 0.2443(9) 1.0090(12)
H43 H 0.5006(13) 0.2177(9) 0.9958(12)
H44 H 0.4575(13) 0.2975(9) 1.0228(12)
H45? H 0.5061(13) 0.2403(9) 0.9886(12)
H46? H 0.4372(13) 0.2929(9) 1.0388(12)
C27 C 0.3970(21) 0.2067(15) 1.0777(16)
H47 H 0.3458(21) 0.2377(15) 1.0990(16)
H48 H 0.4446(21) 0.1930(15) 1.1240(16)
C28? C 0.4237(33) 0.1810(22) 1.0635(25)
H49? H 0.4840(33) 0.1528(22) 1.0768(25)
H50? H 0.4021(33) 0.2005(22) 1.1162(25)
C29 C 0.3544(11) 0.1319(9) 1.0268(7)
H51 H 0.4052(11) 0.0943(9) 1.0195(7)
H52 H 0.3026(11) 0.1078(9) 1.0553(7)
H53? H 0.3017(11) 0.1256(9) 1.0633(7)
H54? H 0.3829(11) 0.0818(9) 1.0178(7)
C30 C 0.5394(10) -0.0006(10) 0.6291(9)
H55 H 0.5173(10) 0.0525(10) 0.6260(9)
H56 H 0.5392(10) -0.0208(10) 0.5720(9)
C31 C 0.6365(12) -0.0052(11) 0.6721(10)
H57 H 0.6855(12) -0.0072(11) 0.6315(10)
H58 H 0.6495(12) 0.0389(11) 0.7089(10)
C32 C 0.6367(14) -0.0759(10) 0.7211(15)
H59 H 0.6690(14) -0.0678(10) 0.7771(15)
H60 H 0.6709(14) -0.1162(10) 0.6932(15)
C33 C 0.5355(14) -0.0975(10) 0.7271(13)
H61 H 0.5242(14) -0.1496(10) 0.7064(13)
H62 H 0.5194(14) -0.0952(10) 0.7855(13)
C34 C 0.1912(16) -0.1614(13) 0.5639(12)
H63 H 0.1316(16) -0.1323(13) 0.5676(12)
H64 H 0.1908(16) -0.2063(13) 0.6003(12)
H65? H 0.1365(16) -0.1295(13) 0.5432(12)
H66? H 0.1742(16) -0.1880(13) 0.6145(12)
C35 C 0.2078(30) -0.1835(24) 0.4701(24)
H67 H 0.1904(30) -0.2370(24) 0.4598(24)
H68 H 0.1668(30) -0.1518(24) 0.4312(24)
C36? C 0.2142(24) -0.2174(19) 0.4986(20)
H69? H 0.2121(24) -0.2692(19) 0.5214(20)
H70? H 0.1659(24) -0.2138(19) 0.4505(20)
C37 C 0.3022(25) -0.1723(20) 0.4574(20)
H71 H 0.3338(25) -0.2208(20) 0.4467(20)
H72 H 0.3083(25) -0.1384(20) 0.4094(20)
C38? C 0.3021(32) -0.2034(24) 0.4738(26)
H73? H 0.2977(32) -0.1880(24) 0.4147(26)
H74? H 0.3430(32) -0.2488(24) 0.4807(26)
C39 C 0.3423(18) -0.1399(12) 0.5289(12)
H75 H 0.3812(18) -0.0960(12) 0.5143(12)
H76 H 0.3857(18) -0.1769(12) 0.5585(12)
H77? H 0.4005(18) -0.1575(12) 0.5621(12)
H78? H 0.3603(18) -0.0971(12) 0.4941(12)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Br 1.21
Gd 1.73
N 0.68
O 0.68
|
1100618.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100618.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100618
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C98 H148 Gd4 N9 Na5 O15 Si6'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 83.31(3)
_cell_angle_beta 78.97(3)
_cell_angle_gamma 74.48(3)
_cell_formula_units_Z 2
_cell_length_a 15.856(3)
_cell_length_b 17.151(3)
_cell_length_c 22.324(5)
_cod_database_code 1100618
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Gd1 Gd 0.00968(1) 0.27862(1) 0.26912(1)
Gd2 Gd 0.21550(1) 0.21037(1) 0.33785(1)
Gd3 Gd 0.15418(1) 0.06954(1) 0.24995(1)
Gd4 Gd 0.23335(1) 0.24425(1) 0.17142(1)
Na1 Na 0.09106(13) 0.44215(11) 0.17351(9)
Na2 Na 0.3577(2) 0.2781(2) 0.5024(2)
Na3? Na 0.3491(8) 0.2398(7) 0.5413(6)
Na4 Na -0.05249(14) 0.12776(12) 0.19482(10)
Na5 Na 0.00684(13) 0.26606(13) 0.43474(9)
Na6 Na 0.39042(15) 0.32152(14) -0.03074(10)
O1 O 0.0935(3) 0.5710(3) 0.1376(2)
C1 C 0.0481(5) 0.6175(5) 0.0912(4)
H1 H -0.0070(5) 0.6549(5) 0.1090(4)
H2 H 0.0338(5) 0.5822(5) 0.0652(4)
C2 C 0.1120(5) 0.6628(5) 0.0556(4)
H3 H 0.1496(5) 0.6318(5) 0.0218(4)
H4 H 0.0802(5) 0.7154(5) 0.0388(4)
C3 C 0.1663(5) 0.6737(5) 0.0999(3)
H5 H 0.2297(5) 0.6583(5) 0.0830(3)
H6 H 0.1500(5) 0.7301(5) 0.1110(3)
C4 C 0.1446(5) 0.6190(5) 0.1532(4)
H7 H 0.1993(5) 0.5841(5) 0.1654(4)
H8 H 0.1111(5) 0.6508(5) 0.1877(4)
O2 O 0.3883(4) 0.3939(4) 0.4598(3)
C5 C 0.3485(6) 0.4440(6) 0.4094(4)
H9 H 0.3357(6) 0.4094(6) 0.3821(4)
H10 H 0.2926(6) 0.4817(6) 0.4257(4)
C6 C 0.4100(7) 0.4887(6) 0.3760(5)
H11 H 0.3966(7) 0.5431(6) 0.3905(5)
H12 H 0.4081(7) 0.4935(6) 0.3321(5)
C7 C 0.4977(7) 0.4394(7) 0.3890(5)
H13 H 0.5227(7) 0.3959(7) 0.3610(5)
H14 H 0.5397(7) 0.4731(7) 0.3858(5)
C8 C 0.4763(7) 0.4070(6) 0.4515(5)
H15 H 0.5196(7) 0.3558(6) 0.4591(5)
H16 H 0.4780(7) 0.4454(6) 0.4803(5)
O3 O 0.4153(4) 0.2934(4) 0.5873(3)
C9 C 0.3823(11) 0.3668(10) 0.6235(8)
H17 H 0.3926(11) 0.4146(10) 0.5974(8)
H18 H 0.3183(11) 0.3758(10) 0.6378(8)
C10 C 0.4249(8) 0.3568(7) 0.6719(6)
H19 H 0.3857(8) 0.3825(7) 0.7076(6)
H20 H 0.4777(8) 0.3781(7) 0.6621(6)
C11 C 0.4483(10) 0.2684(8) 0.6817(7)
H21 H 0.3983(10) 0.2501(8) 0.7066(7)
H22 H 0.4993(10) 0.2503(8) 0.7032(7)
C12 C 0.4709(9) 0.2338(8) 0.6198(6)
H23 H 0.5336(9) 0.2282(8) 0.6021(6)
H24 H 0.4570(9) 0.1811(8) 0.6219(6)
O4 O -0.1456(3) 0.1024(3) 0.1365(2)
C13 C -0.2271(6) 0.0874(6) 0.1642(4)
H25 H -0.2613(6) 0.1309(6) 0.1905(4)
H26 H -0.2179(6) 0.0359(6) 0.1892(4)
C14 C -0.2755(6) 0.0839(6) 0.1126(4)
H27 H -0.3045(6) 0.0391(6) 0.1208(4)
H28 H -0.3204(6) 0.1348(6) 0.1070(4)
C15 C -0.2090(7) 0.0715(7) 0.0611(5)
H29 H -0.2320(7) 0.1016(7) 0.0251(5)
H30 H -0.1895(7) 0.0138(7) 0.0536(5)
C16 C -0.1346(5) 0.0997(5) 0.0719(4)
H31 H -0.0781(5) 0.0622(5) 0.0565(4)
H32 H -0.1357(5) 0.1536(5) 0.0514(4)
O5 O -0.0526(3) 0.2692(3) 0.5346(2)
C17 C -0.0847(8) 0.3352(7) 0.5722(5)
H33 H -0.1483(8) 0.3590(7) 0.5724(5)
H34 H -0.0526(8) 0.3773(7) 0.5583(5)
C18 C -0.0671(9) 0.2971(7) 0.6353(6)
H35 H -0.0169(9) 0.3128(7) 0.6457(6)
H36 H -0.1194(9) 0.3167(7) 0.6662(6)
C19 C -0.0486(8) 0.2143(7) 0.6352(5)
H37 H -0.0889(8) 0.1925(7) 0.6676(5)
H38 H 0.0127(8) 0.1893(7) 0.6412(5)
C20 C -0.0624(7) 0.1986(6) 0.5715(4)
H39 H -0.0179(7) 0.1507(6) 0.5556(4)
H40 H -0.1217(7) 0.1904(6) 0.5733(4)
O6 O 0.3339(3) 0.2553(3) -0.0918(2)
C21 C 0.2513(5) 0.2346(5) -0.0706(4)
H41 H 0.2017(5) 0.2810(5) -0.0777(4)
H42 H 0.2449(5) 0.2185(5) -0.0267(4)
C22 C 0.2525(6) 0.1650(5) -0.1063(4)
H43 H 0.2223(6) 0.1266(5) -0.0811(4)
H44 H 0.2245(6) 0.1842(5) -0.1427(4)
C23 C 0.3473(6) 0.1285(6) -0.1231(4)
H45 H 0.3594(6) 0.0999(6) -0.1605(4)
H46 H 0.3697(6) 0.0902(6) -0.0902(4)
C24 C 0.3882(5) 0.1972(4) -0.1329(4)
H47 H 0.4489(5) 0.1800(4) -0.1241(4)
H48 H 0.3899(5) 0.2201(4) -0.1753(4)
O7 O 0.4757(3) 0.3687(3) -0.1124(2)
C25 C 0.4575(6) 0.3808(5) -0.1737(4)
H49 H 0.3956(6) 0.3813(5) -0.1739(4)
H50 H 0.4963(6) 0.3373(5) -0.1984(4)
C26 C 0.4744(7) 0.4588(6) -0.1980(5)
H51 H 0.4183(7) 0.5004(6) -0.1982(5)
H52 H 0.5071(7) 0.4551(6) -0.2399(5)
C27 C 0.5289(6) 0.4799(6) -0.1564(4)
H53 H 0.5856(6) 0.4876(6) -0.1794(4)
H54 H 0.4966(6) 0.5294(6) -0.1359(4)
C28 C 0.5431(5) 0.4078(5) -0.1112(4)
H55 H 0.6018(5) 0.3711(5) -0.1228(4)
H56 H 0.5390(5) 0.4249(5) -0.0702(4)
O8 O 0.1483(2) 0.2034(2) 0.25727(13)
N1 N 0.1626(3) 0.1914(3) 0.4463(2)
C29 C 0.1723(3) 0.2367(5) 0.4912(2)
C30 C 0.1714(4) 0.3204(5) 0.4779(3)
H57 H 0.1674(4) 0.3434(5) 0.4379(3)
C31 C 0.1763(5) 0.3685(6) 0.5219(4)
H58 H 0.1743(5) 0.4236(6) 0.5116(4)
C32 C 0.1838(7) 0.3371(8) 0.5799(5)
H59 H 0.1868(7) 0.3706(8) 0.6095(5)
C33 C 0.1870(6) 0.2574(7) 0.5954(4)
H60 H 0.1910(6) 0.2366(7) 0.6359(4)
C34 C 0.1842(5) 0.2039(6) 0.5501(3)
H61 H 0.1904(5) 0.1482(6) 0.5603(3)
N2 N 0.0935(3) 0.0266(3) 0.1719(2)
C35 C 0.0508(3) -0.0320(3) 0.1678(3)
C36 C 0.0031(4) -0.0629(4) 0.2200(3)
H62 H 0.0007(4) -0.0436(4) 0.2582(3)
C37 C -0.0410(5) -0.1218(4) 0.2164(4)
H63 H -0.0713(5) -0.1430(4) 0.2523(4)
C38 C -0.0410(6) -0.1491(5) 0.1617(5)
H64 H -0.0724(6) -0.1878(5) 0.1597(5)
C39 C 0.0045(6) -0.1203(5) 0.1099(5)
H65 H 0.0041(6) -0.1389(5) 0.0720(5)
C40 C 0.0517(5) -0.0635(4) 0.1125(3)
H66 H 0.0850(5) -0.0459(4) 0.0765(3)
N3 N 0.2523(3) 0.3811(2) 0.1388(2)
C41 C 0.2626(3) 0.4157(3) 0.0799(2)
C42 C 0.2152(3) 0.4003(3) 0.0365(2)
H67 H 0.1794(3) 0.3636(3) 0.0478(2)
C43 C 0.2201(4) 0.4375(3) -0.0215(3)
H68 H 0.1855(4) 0.4277(3) -0.0482(3)
C44 C 0.2748(5) 0.4889(4) -0.0413(3)
H69 H 0.2777(5) 0.5145(4) -0.0810(3)
C45 C 0.3247(5) 0.5017(4) -0.0017(3)
H70 H 0.3634(5) 0.5356(4) -0.0150(3)
C46 C 0.3201(4) 0.4665(3) 0.0573(3)
H71 H 0.3559(4) 0.4766(3) 0.0830(3)
Si1 Si 0.05648(9) 0.41581(8) 0.33211(6)
N4 N -0.0075(3) 0.4235(2) 0.2768(2)
O9 O 0.0881(2) 0.3176(2) 0.34560(14)
C47 C -0.0687(3) 0.4939(3) 0.2595(2)
C48 C -0.1388(4) 0.4879(4) 0.2320(3)
H72 H -0.1455(4) 0.4363(4) 0.2269(3)
C49 C -0.1980(5) 0.5558(5) 0.2123(4)
H73 H -0.2441(5) 0.5496(5) 0.1938(4)
C50 C -0.1915(6) 0.6336(5) 0.2189(4)
H74 H -0.2321(6) 0.6797(5) 0.2050(4)
C51 C -0.1251(5) 0.6406(4) 0.2461(3)
H75 H -0.1204(5) 0.6927(4) 0.2515(3)
C52 C -0.0629(4) 0.5730(3) 0.2663(3)
H76 H -0.0170(4) 0.5803(3) 0.2845(3)
C53 C -0.0054(4) 0.4658(3) 0.4035(2)
H77 H -0.0220(24) 0.5241(4) 0.3948(5)
H78 H 0.0322(10) 0.4527(20) 0.4347(7)
H79 H -0.0584(15) 0.4465(19) 0.4180(11)
C54 C 0.1575(4) 0.4560(3) 0.3058(3)
H80 H 0.1394(4) 0.5138(6) 0.2950(18)
H81 H 0.1931(14) 0.4285(18) 0.2704(11)
H82 H 0.1923(14) 0.4465(22) 0.3385(7)
Si2 Si 0.39407(8) 0.24860(8) 0.27255(6)
N5 N 0.3615(3) 0.2198(2) 0.3474(2)
O10 O 0.3032(2) 0.2536(2) 0.24632(15)
C55 C 0.4185(3) 0.1915(3) 0.3894(2)
C56 C 0.5000(4) 0.2123(4) 0.3848(3)
H83 H 0.5166(4) 0.2476(4) 0.3519(3)
C57 C 0.5562(4) 0.1824(4) 0.4274(3)
H84 H 0.6102(4) 0.1972(4) 0.4226(3)
C58 C 0.5339(5) 0.1319(5) 0.4757(3)
H85 H 0.5716(5) 0.1126(5) 0.5049(3)
C59 C 0.4547(4) 0.1089(4) 0.4819(3)
H86 H 0.4395(4) 0.0730(4) 0.5148(3)
C60 C 0.3980(4) 0.1389(3) 0.4395(2)
H87 H 0.3443(4) 0.1234(3) 0.4447(2)
C61 C 0.4897(4) 0.1723(3) 0.2334(3)
H88 H 0.4754(11) 0.1202(7) 0.2374(16)
H89 H 0.5417(8) 0.1674(18) 0.2519(12)
H90 H 0.5020(18) 0.1897(13) 0.1904(5)
C62 C 0.4179(3) 0.3506(3) 0.2559(3)
H91 H 0.4703(15) 0.3505(7) 0.2724(15)
H92 H 0.3676(11) 0.3914(4) 0.2746(15)
H93 H 0.4282(25) 0.363(1) 0.2120(3)
Si3 Si 0.00755(8) 0.30654(8) 0.12560(6)
N6 N -0.0699(2) 0.2832(2) 0.1853(2)
O11 O 0.0884(2) 0.3089(2) 0.16042(14)
C63 C -0.1595(3) 0.2939(3) 0.1825(2)
C64 C -0.2224(3) 0.2964(4) 0.2361(3)
H94 H -0.2034(3) 0.2914(4) 0.2741(3)
C65 C -0.3108(4) 0.3060(5) 0.2350(3)
H95 H -0.3508(4) 0.3073(5) 0.2721(3)
C66 C -0.3421(4) 0.3138(4) 0.1805(3)
H96 H -0.4026(4) 0.3196(4) 0.1799(3)
C67 C -0.2822(4) 0.3127(4) 0.1271(3)
H97 H -0.3023(4) 0.3189(4) 0.0894(3)
C68 C -0.1933(3) 0.3028(3) 0.1277(2)
H98 H -0.1541(3) 0.3019(3) 0.0903(2)
C69 C 0.0498(3) 0.2285(3) 0.0678(2)
H99 H 0.0936(18) 0.2453(11) 0.0359(9)
H100 H 0.0008(5) 0.2229(17) 0.0498(13)
H101 H 0.0768(22) 0.1769(6) 0.0875(4)
C70 C -0.0314(3) 0.4078(3) 0.0843(2)
H102 H -0.0823(15) 0.4078(8) 0.0662(14)
H103 H 0.0160(9) 0.4181(10) 0.0524(11)
H104 H -0.0481(23) 0.4498(4) 0.1130(4)
Si4 Si -0.06546(9) 0.13737(8) 0.34813(6)
N7 N -0.0868(3) 0.2387(2) 0.3598(2)
O12 O 0.0060(2) 0.1305(2) 0.28461(15)
C71 C -0.1587(3) 0.2818(3) 0.3994(2)
C72 C -0.1838(4) 0.3667(4) 0.3927(3)
H105 H -0.1532(4) 0.3940(4) 0.3604(3)
C73 C -0.2527(5) 0.4110(5) 0.4326(3)
H106 H -0.2673(5) 0.4679(5) 0.4273(3)
C74 C -0.3000(4) 0.3738(5) 0.4796(3)
H107 H -0.3466(4) 0.4047(5) 0.5065(3)
C75 C -0.2780(4) 0.2898(5) 0.4868(3)
H108 H -0.3106(4) 0.2634(5) 0.5185(3)
C76 C -0.2087(3) 0.2446(4) 0.4479(2)
H109 H -0.1945(3) 0.1878(4) 0.4537(2)
C77 C -0.0135(4) 0.0673(4) 0.4094(3)
H110 H -0.0554(12) 0.0717(21) 0.4474(6)
H111 H 0.0394(18) 0.0820(18) 0.4149(15)
H112 H 0.0025(28) 0.0119(5) 0.3975(10)
C78 C -0.1649(4) 0.1048(4) 0.3375(3)
H113 H -0.1981(18) 0.1446(15) 0.3105(18)
H114 H -0.2025(17) 0.1001(28) 0.3768(4)
H115 H -0.1458(4) 0.0526(14) 0.3197(21)
Si5 Si 0.32916(9) 0.08306(8) 0.11080(6)
N8 N 0.3511(3) 0.1763(2) 0.0954(2)
O13 O 0.2445(2) 0.1045(2) 0.16540(15)
C79 C 0.4278(3) 0.1943(3) 0.0625(2)
C80 C 0.4822(4) 0.1498(4) 0.0135(3)
H116 H 0.4664(4) 0.1053(4) 0.0020(3)
C81 C 0.5583(4) 0.1706(4) -0.0179(3)
H117 H 0.5936(4) 0.1390(4) -0.0496(3)
C82 C 0.5838(4) 0.2361(4) -0.0039(3)
H118 H 0.6353(4) 0.2499(4) -0.0258(3)
C83 C 0.5318(4) 0.2807(4) 0.0431(3)
H119 H 0.5487(4) 0.3251(4) 0.0536(3)
C84 C 0.4549(3) 0.2621(3) 0.0753(2)
H120 H 0.4201(3) 0.2951(3) 0.1064(2)
C85 C 0.2945(4) 0.0414(4) 0.0485(3)
H121 H 0.3437(10) 0.0299(24) 0.0148(8)
H122 H 0.2448(18) 0.0808(11) 0.0342(13)
H123 H 0.2770(27) -0.0082(14) 0.0640(6)
C86 C 0.4227(4) 0.0051(4) 0.1372(3)
H124 H 0.4395(21) 0.0238(13) 0.1715(14)
H125 H 0.4729(11) -0.0045(21) 0.1041(7)
H126 H 0.4047(11) -0.0449(9) 0.1499(20)
Si6 Si 0.26721(10) -0.01613(8) 0.35031(7)
N9 N 0.2297(3) -0.0550(2) 0.2963(2)
O14 O 0.2212(2) 0.0798(2) 0.3366(2)
C87 C 0.2532(4) -0.1361(3) 0.2830(3)
C88 C 0.2890(5) -0.1997(4) 0.3241(4)
H127 H 0.3001(5) -0.1877(4) 0.3614(4)
C89 C 0.3080(6) -0.2805(4) 0.3099(5)
H128 H 0.3296(6) -0.3221(4) 0.3386(5)
C90 C 0.2960(6) -0.2998(5) 0.2562(5)
H129 H 0.3109(6) -0.3542(5) 0.2464(5)
C91 C 0.2619(6) -0.2388(5) 0.2160(5)
H130 H 0.2518(6) -0.2520(5) 0.1787(5)
C92 C 0.2414(4) -0.1579(4) 0.2284(3)
H131 H 0.2191(4) -0.1174(4) 0.1991(3)
C93 C 0.2314(5) -0.0471(4) 0.4330(3)
H132 H 0.2593(25) -0.1040(8) 0.4413(6)
H133 H 0.1674(6) -0.0386(26) 0.4414(6)
H134 H 0.2490(27) -0.0147(20) 0.4589(3)
C94 C 0.3902(4) -0.0343(4) 0.3363(3)
H135 H 0.4172(4) -0.0922(4) 0.3360(23)
H136 H 0.4084(5) -0.0122(27) 0.3684(13)
H137 H 0.4092(5) -0.0080(26) 0.2970(11)
C95 C 0.6303(7) 0.9599(7) 0.2759(5)
C96 C 0.6286(9) 1.0094(9) 0.3290(7)
C97 C 0.6791(11) 0.9614(10) 0.3679(7)
C98 C 0.7563(7) 0.9202(6) 0.3213(5)
C99 C 0.7139(8) 0.9010(7) 0.2747(6)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.80
H 0.23
Gd 1.52
N 0.68
Na 2.05
O 0.62
Si 0.90
|
1100619.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100619.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100619
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C98 H148 N9 Na5 O15 Si6 Yb4'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 83.31(3)
_cell_angle_beta 78.97(3)
_cell_angle_gamma 74.48(3)
_cell_formula_units_Z 2
_cell_length_a 15.856(3)
_cell_length_b 17.151(3)
_cell_length_c 22.324(5)
_cod_database_code 1100619
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Yb1 Yb 0.01303(2) 0.27385(2) 0.26874(2)
Yb2 Yb 0.21395(2) 0.20907(2) 0.33441(2)
Yb3 Yb 0.15665(2) 0.07271(2) 0.24828(2)
Yb4 Yb 0.23204(2) 0.24137(2) 0.17098(2)
Na1 Na 0.0920(2) 0.4360(2) 0.1724(2)
Na2 Na 0.3556(4) 0.2751(4) 0.5027(3)
Na3 Na -0.0487(2) 0.1250(2) 0.1956(2)
Na4 Na 0.0094(2) 0.2625(3) 0.4349(2)
Na5 Na 0.3896(3) 0.3203(3) -0.0308(2)
O1 O 0.0939(5) 0.5653(5) 0.1396(4)
C1 C 0.0473(10) 0.6103(10) 0.0922(7)
H1 H -0.0127(10) 0.6398(10) 0.1097(7)
H2 H 0.0428(10) 0.5738(10) 0.0630(7)
C2 C 0.0999(11) 0.6675(11) 0.0618(9)
H3 H 0.0606(11) 0.7209(11) 0.0534(9)
H4 H 0.1350(11) 0.6476(11) 0.0230(9)
C3 C 0.1594(11) 0.6736(11) 0.1043(8)
H5 H 0.2219(11) 0.6563(11) 0.0855(8)
H6 H 0.1469(11) 0.7292(11) 0.1163(8)
C4 C 0.1382(10) 0.6182(10) 0.1573(7)
H7 H 0.1929(10) 0.5868(10) 0.1716(7)
H8 H 0.1001(10) 0.6495(10) 0.1909(7)
O2 O 0.3845(8) 0.3960(7) 0.4557(6)
C5 C 0.3405(13) 0.4463(13) 0.4108(9)
H9 H 0.2862(13) 0.4833(13) 0.4302(9)
H10 H 0.3241(13) 0.4134(13) 0.3840(9)
C6 C 0.4034(12) 0.4941(13) 0.3739(10)
H11 H 0.4008(12) 0.4978(13) 0.3301(10)
H12 H 0.3901(12) 0.5490(13) 0.3877(10)
C7 C 0.4923(15) 0.4442(15) 0.3872(11)
H13 H 0.5182(15) 0.4015(15) 0.3587(11)
H14 H 0.5338(15) 0.4780(15) 0.3854(11)
C8 C 0.4694(13) 0.4111(14) 0.448(1)
H15 H 0.5135(13) 0.3604(14) 0.4557(10)
H16 H 0.4693(13) 0.4493(14) 0.4774(10)
O3 O 0.4145(7) 0.2920(8) 0.5840(5)
C9 C 0.3788(18) 0.3642(18) 0.6227(14)
H17 H 0.3828(18) 0.4140(18) 0.5972(14)
H18 H 0.3161(18) 0.3683(18) 0.6398(14)
C10 C 0.4278(15) 0.3556(15) 0.6707(11)
H19 H 0.4799(15) 0.3778(15) 0.6582(11)
H20 H 0.3912(15) 0.3812(15) 0.7072(11)
C11 C 0.4518(21) 0.2717(20) 0.6802(15)
H21 H 0.4023(21) 0.252(2) 0.7043(15)
H22 H 0.5027(21) 0.2543(20) 0.7018(15)
C12 C 0.4765(16) 0.2391(16) 0.6154(12)
H23 H 0.5371(16) 0.2410(16) 0.5965(12)
H24 H 0.4710(16) 0.1833(16) 0.6170(12)
O4 O -0.1451(6) 0.0990(6) 0.1394(4)
C13 C -0.2259(10) 0.0844(11) 0.1689(8)
H25 H -0.2589(10) 0.1280(11) 0.1955(8)
H26 H -0.2163(10) 0.0328(11) 0.1937(8)
C14 C -0.2759(12) 0.0817(13) 0.1177(9)
H27 H -0.3074(12) 0.0386(13) 0.1273(9)
H28 H -0.3192(12) 0.1335(13) 0.1118(9)
C15 C -0.2081(13) 0.0654(14) 0.0626(10)
H29 H -0.2314(13) 0.0947(14) 0.0264(10)
H30 H -0.1898(13) 0.0072(14) 0.0564(10)
C16 C -0.1304(10) 0.0947(10) 0.0734(7)
H31 H -0.0738(10) 0.0564(10) 0.0593(7)
H32 H -0.1305(10) 0.1481(10) 0.0522(7)
O5 O -0.0527(5) 0.2710(6) 0.5364(4)
C17 C -0.0860(14) 0.3405(13) 0.570(1)
H33 H -0.1488(14) 0.3647(13) 0.5678(10)
H34 H -0.0523(14) 0.3812(13) 0.5552(10)
C18 C -0.0727(18) 0.3056(18) 0.6373(13)
H35 H -0.0215(18) 0.3196(18) 0.6477(13)
H36 H -0.1255(18) 0.3292(18) 0.6665(13)
C19 C -0.0594(15) 0.2248(15) 0.6403(11)
H37 H -0.1054(15) 0.2078(15) 0.6709(11)
H38 H -0.0014(15) 0.1981(15) 0.6518(11)
C20 C -0.0635(13) 0.2018(13) 0.5763(10)
H39 H -0.0159(13) 0.1538(13) 0.5644(10)
H40 H -0.1208(13) 0.1906(13) 0.5757(10)
O6 O 0.3375(6) 0.2538(6) -0.0948(4)
C21 C 0.2538(10) 0.2325(10) -0.0746(8)
H41 H 0.2038(10) 0.2795(10) -0.0794(8)
H42 H 0.2482(10) 0.2117(10) -0.0316(8)
C22 C 0.2569(12) 0.1691(13) -0.1148(10)
H43 H 0.2275(12) 0.1282(13) -0.0926(10)
H44 H 0.2282(12) 0.1925(13) -0.1502(10)
C23 C 0.3520(13) 0.1335(13) -0.1338(10)
H45 H 0.3625(13) 0.1104(13) -0.1735(10)
H46 H 0.3742(13) 0.0902(13) -0.1037(10)
C24 C 0.3979(10) 0.1985(10) -0.1383(8)
H47 H 0.4566(10) 0.178(1) -0.1262(8)
H48 H 0.4043(10) 0.2246(10) -0.1798(8)
O7 O 0.4732(5) 0.3741(5) -0.1100(4)
C25 C 0.456(1) 0.3866(10) -0.1725(7)
H49 H 0.3951(10) 0.3847(10) -0.1735(7)
H50 H 0.4971(10) 0.3445(10) -0.1975(7)
C26 C 0.4695(13) 0.4681(12) -0.1959(10)
H51 H 0.4123(13) 0.5083(12) -0.1951(10)
H52 H 0.5017(13) 0.4666(12) -0.238(1)
C27 C 0.5228(13) 0.4889(13) -0.1540(9)
H53 H 0.4915(13) 0.5402(13) -0.1356(9)
H54 H 0.5809(13) 0.4939(13) -0.1763(9)
C28 C 0.5335(9) 0.4190(9) -0.1049(7)
H55 H 0.5944(9) 0.3848(9) -0.1112(7)
H56 H 0.5205(9) 0.4398(9) -0.0642(7)
O8 O 0.1482(3) 0.2023(3) 0.2563(3)
N1 N 0.1668(5) 0.1886(5) 0.4415(4)
C29 C 0.1740(6) 0.2340(8) 0.4878(5)
C30 C 0.1729(7) 0.3165(8) 0.4773(6)
H57 H 0.1712(7) 0.3409(8) 0.4375(6)
C31 C 0.1741(8) 0.3638(10) 0.5238(8)
H58 H 0.1699(8) 0.4195(10) 0.5151(8)
C32 C 0.1812(11) 0.3302(16) 0.5814(8)
H59 H 0.1827(11) 0.3630(16) 0.6119(8)
C33 C 0.1861(12) 0.2524(14) 0.5953(7)
H60 H 0.1901(12) 0.2304(14) 0.6355(7)
C34 C 0.1852(9) 0.200(1) 0.5477(6)
H61 H 0.1921(9) 0.144(1) 0.5570(6)
N2 N 0.0997(5) 0.0273(5) 0.1733(4)
C35 C 0.0556(7) -0.0309(6) 0.1705(5)
C36 C 0.0083(8) -0.0593(7) 0.2231(7)
H62 H 0.0086(8) -0.0395(7) 0.2606(7)
C37 C -0.0398(10) -0.116(1) 0.2228(10)
H63 H -0.0713(10) -0.1345(10) 0.2592(10)
C38 C -0.0400(12) -0.1448(10) 0.1668(12)
H64 H -0.0716(12) -0.1838(10) 0.1660(12)
C39 C 0.0054(14) -0.1172(11) 0.1121(11)
H65 H 0.0026(14) -0.1359(11) 0.0747(11)
C40 C 0.0552(9) -0.0612(7) 0.1135(7)
H66 H 0.0881(9) -0.0437(7) 0.0772(7)
N3 N 0.2528(5) 0.3716(4) 0.1385(3)
C41 C 0.2601(5) 0.4079(5) 0.0800(4)
C42 C 0.2153(5) 0.3929(6) 0.0354(4)
H67 H 0.1824(5) 0.3536(6) 0.0449(4)
C43 C 0.2181(7) 0.4344(8) -0.0223(5)
H68 H 0.1856(7) 0.4234(8) -0.0500(5)
C44 C 0.2667(9) 0.4903(8) -0.0398(6)
H69 H 0.2671(9) 0.5184(8) -0.0786(6)
C45 C 0.3148(8) 0.5041(8) 0.0006(6)
H70 H 0.3500(8) 0.5414(8) -0.0114(6)
C46 C 0.3135(7) 0.4641(7) 0.0601(6)
H71 H 0.3480(7) 0.4748(7) 0.0865(6)
Si1 Si 0.0561(2) 0.40970(15) 0.33113(12)
N4 N -0.0086(4) 0.4157(4) 0.2757(3)
O9 O 0.0902(4) 0.3125(3) 0.3439(3)
C47 C -0.0709(6) 0.4826(6) 0.2592(4)
C48 C -0.1424(6) 0.4762(7) 0.2346(5)
H72 H -0.1507(6) 0.4247(7) 0.2313(5)
C49 C -0.2024(8) 0.5456(9) 0.2145(6)
H73 H -0.2489(8) 0.5393(9) 0.1965(6)
C50 C -0.1962(9) 0.6208(9) 0.2200(6)
H74 H -0.2388(9) 0.6661(9) 0.2072(6)
C51 C -0.1267(8) 0.6309(7) 0.2446(6)
H75 H -0.1202(8) 0.6831(7) 0.2476(6)
C52 C -0.0657(7) 0.5618(6) 0.2652(5)
H76 H -0.0199(7) 0.5688(6) 0.2835(5)
C53 C -0.0075(7) 0.4602(7) 0.4036(5)
H77 H -0.0306(44) 0.5177(10) 0.3939(8)
H78 H 0.0321(15) 0.4529(42) 0.4331(15)
H79 H -0.0562(32) 0.4359(32) 0.4207(20)
C54 C 0.1553(6) 0.4544(6) 0.3037(5)
H80 H 0.1347(6) 0.5121(10) 0.2935(31)
H81 H 0.1909(26) 0.4281(30) 0.2677(19)
H82 H 0.1909(26) 0.4458(38) 0.3358(12)
Si2 Si 0.3893(2) 0.2471(2) 0.27203(13)
N5 N 0.3527(5) 0.2193(5) 0.3476(4)
O10 O 0.2998(4) 0.2514(4) 0.2450(3)
C55 C 0.4108(7) 0.1900(7) 0.3888(5)
C56 C 0.4904(7) 0.2146(8) 0.3861(6)
H83 H 0.5056(7) 0.2527(8) 0.3548(6)
C57 C 0.5461(10) 0.1833(12) 0.4290(9)
H84 H 0.5986(10) 0.2002(12) 0.4255(9)
C58 C 0.5268(11) 0.1280(11) 0.4767(8)
H85 H 0.5655(11) 0.1063(11) 0.5049(8)
C59 C 0.4500(9) 0.1071(9) 0.4806(7)
H86 H 0.4343(9) 0.0712(9) 0.5134(7)
C60 C 0.3928(8) 0.1358(8) 0.4385(6)
H87 H 0.3404(8) 0.1183(8) 0.4436(6)
C61 C 0.4867(6) 0.1719(7) 0.2343(6)
H88 H 0.4722(20) 0.1201(14) 0.2359(35)
H89 H 0.5366(18) 0.1656(40) 0.2552(25)
H90 H 0.5022(35) 0.1907(25) 0.1919(13)
C62 C 0.4141(6) 0.3481(7) 0.2547(6)
H91 H 0.4633(34) 0.3494(17) 0.2743(29)
H92 H 0.3622(18) 0.3899(8) 0.2700(31)
H93 H 0.4298(48) 0.3579(20) 0.2108(6)
Si3 Si 0.01021(14) 0.3008(2) 0.12626(11)
N6 N -0.0666(4) 0.2778(5) 0.1872(3)
O11 O 0.0919(3) 0.3020(4) 0.1597(3)
C63 C -0.1568(5) 0.2897(6) 0.1856(5)
C64 C -0.2199(6) 0.2904(7) 0.2412(5)
H94 H -0.2009(6) 0.2838(7) 0.2793(5)
C65 C -0.3084(7) 0.3006(8) 0.2384(6)
H95 H -0.3489(7) 0.3008(8) 0.2752(6)
C66 C -0.3395(6) 0.3106(7) 0.1838(6)
H96 H -0.4003(6) 0.3186(7) 0.1832(6)
C67 C -0.2798(6) 0.3087(7) 0.1302(6)
H97 H -0.3004(6) 0.3147(7) 0.0927(6)
C68 C -0.1905(6) 0.2981(6) 0.1299(5)
H98 H -0.1513(6) 0.2965(6) 0.0925(5)
C69 C 0.0517(6) 0.2226(7) 0.0666(5)
H99 H 0.0849(40) 0.2448(16) 0.0306(13)
H100 H 0.0015(7) 0.2089(33) 0.0554(25)
H101 H 0.0899(38) 0.1742(17) 0.0833(12)
C70 C -0.0283(6) 0.4021(6) 0.0848(5)
H102 H -0.0735(32) 0.3998(13) 0.0617(25)
H103 H 0.0215(10) 0.4157(19) 0.0571(22)
H104 H -0.053(4) 0.4431(9) 0.1142(5)
Si4 Si -0.0604(2) 0.1363(2) 0.34917(14)
N7 N -0.0838(5) 0.2383(5) 0.3594(3)
O12 O 0.0119(4) 0.1295(3) 0.2843(3)
C71 C -0.1573(6) 0.2813(6) 0.3982(4)
C72 C -0.1864(7) 0.3657(7) 0.3906(5)
H105 H -0.1569(7) 0.3940(7) 0.3584(5)
C73 C -0.2574(8) 0.4078(9) 0.4295(7)
H106 H -0.2757(8) 0.4644(9) 0.4227(7)
C74 C -0.3029(8) 0.3704(10) 0.4782(6)
H107 H -0.3509(8) 0.4014(10) 0.5042(6)
C75 C -0.2778(7) 0.2882(9) 0.4883(6)
H108 H -0.3087(7) 0.2618(9) 0.5211(6)
C76 C -0.2055(7) 0.2435(7) 0.4496(5)
H109 H -0.1878(7) 0.1869(7) 0.4572(5)
C77 C -0.0096(8) 0.0693(8) 0.4125(6)
H110 H -0.0509(25) 0.0777(39) 0.4506(9)
H111 H 0.0449(32) 0.0826(37) 0.4162(27)
H112 H 0.0035(53) 0.0130(8) 0.4032(19)
C78 C -0.1595(7) 0.1008(8) 0.3403(6)
H113 H -0.1892(34) 0.1354(33) 0.3091(29)
H114 H -0.2002(29) 0.1033(51) 0.3789(12)
H115 H -0.1401(9) 0.0453(20) 0.3284(40)
Si5 Si 0.3293(2) 0.0874(2) 0.10815(14)
N8 N 0.3473(5) 0.1817(5) 0.0944(4)
O13 O 0.2451(4) 0.1068(4) 0.1649(3)
C79 C 0.4263(6) 0.1985(6) 0.0633(5)
C80 C 0.4831(8) 0.1555(7) 0.0127(6)
H116 H 0.4669(8) 0.1116(7) 0.0005(6)
C81 C 0.5593(8) 0.1743(8) -0.0191(6)
H117 H 0.5938(8) 0.1427(8) -0.0510(6)
C82 C 0.5855(8) 0.2393(9) -0.0042(6)
H118 H 0.6365(8) 0.2536(9) -0.0262(6)
C83 C 0.5329(7) 0.2833(8) 0.0450(5)
H119 H 0.5498(7) 0.3272(8) 0.0565(5)
C84 C 0.4556(6) 0.2631(7) 0.0775(5)
H120 H 0.4223(6) 0.2942(7) 0.1100(5)
C85 C 0.2959(7) 0.0446(7) 0.0449(5)
H121 H 0.3471(14) 0.0283(47) 0.0133(18)
H122 H 0.2501(39) 0.0855(17) 0.0276(25)
H123 H 0.2732(50) -0.0022(30) 0.0613(9)
C86 C 0.4248(8) 0.0110(8) 0.1341(6)
H124 H 0.4481(40) 0.0341(21) 0.1630(34)
H125 H 0.4708(27) -0.0049(43) 0.0991(9)
H126 H 0.4054(16) -0.0363(25) 0.1536(39)
Si6 Si 0.2686(2) -0.0135(2) 0.34465(15)
N9 N 0.2310(5) -0.0504(5) 0.2894(4)
O14 O 0.2222(4) 0.0818(4) 0.3332(3)
C87 C 0.2564(6) -0.1311(6) 0.2728(6)
C88 C 0.2878(9) -0.1950(7) 0.3149(8)
H127 H 0.2943(9) -0.1830(7) 0.3536(8)
C89 C 0.3088(13) -0.2728(10) 0.3008(10)
H128 H 0.3281(13) -0.3148(10) 0.3299(10)
C90 C 0.3019(11) -0.2911(9) 0.2429(11)
H129 H 0.3186(11) -0.3453(9) 0.2323(11)
C91 C 0.2708(11) -0.2304(10) 0.2021(9)
H130 H 0.2635(11) -0.2422(10) 0.1637(9)
C92 C 0.2498(8) -0.1498(8) 0.2176(8)
H131 H 0.2305(8) -0.1077(8) 0.1885(8)
C93 C 0.2334(9) -0.0477(7) 0.4273(6)
H132 H 0.2686(42) -0.1021(22) 0.4361(13)
H133 H 0.1711(18) -0.0476(53) 0.4341(12)
H134 H 0.2424(56) -0.0109(32) 0.4539(6)
C94 C 0.3907(8) -0.0318(8) 0.3302(7)
H135 H 0.4175(8) -0.0897(8) 0.3333(47)
H136 H 0.4089(9) -0.0059(53) 0.3602(29)
H137 H 0.4099(10) -0.0095(55) 0.2895(19)
C95 C 0.6297(20) 0.9616(20) 0.2781(15)
C96 C 0.6237(25) 1.0102(24) 0.3379(20)
C97 C 0.6785(27) 0.9670(26) 0.376(2)
C98 C 0.7583(18) 0.9258(18) 0.3236(14)
C99 C 0.7191(22) 0.8952(21) 0.2747(16)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.75
H 0.23
N 0.68
Na 2.03
O 0.68
Si 1.00
Yb 1.54
|
1100620.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100620.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100620
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C72 H116 N6 Na4 O12 Si6 Yb2'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 76.09(1)
_cell_angle_beta 77.34(1)
_cell_angle_gamma 75.25(1)
_cell_formula_units_Z 2
_cell_length_a 11.401(2)
_cell_length_b 16.468(2)
_cell_length_c 24.831(3)
_cod_database_code 1100620
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C1 C -0.0289(6) 0.8157(5) -0.1418(3)
H1 H -0.0758(19) 0.7943(27) -0.1054(3)
H2 H -0.0106(6) 0.7733(21) -0.1659(15)
H3 H -0.0773(19) 0.8695(7) -0.1599(17)
C2 C 0.1978(7) 0.8775(5) -0.2032(3)
H4 H 0.1407(14) 0.9254(19) -0.2221(8)
H5 H 0.2244(37) 0.8320(9) -0.2253(7)
H6 H 0.2696(24) 0.8972(27) -0.1999(3)
C3 C 0.2389(6) 0.6672(4) -0.1312(3)
C4 C 0.1647(7) 0.6077(4) -0.1185(3)
H7 H 0.0931(7) 0.6138(4) -0.0905(3)
C5 C 0.1943(8) 0.5389(5) -0.1465(3)
H8 H 0.1428(8) 0.4986(5) -0.1370(3)
C6 C 0.2960(8) 0.5287(5) -0.1872(3)
H9 H 0.3156(8) 0.4813(5) -0.2055(3)
C7 C 0.3697(8) 0.5873(5) -0.2014(3)
H10 H 0.4400(8) 0.5810(5) -0.2300(3)
C8 C 0.3417(7) 0.6566(5) -0.1738(3)
H11 H 0.3932(7) 0.6969(5) -0.1841(3)
C9 C 0.3622(7) 0.6174(4) -0.0249(3)
H12 H 0.4103(33) 0.6123(6) 0.0044(13)
H13 H 0.4168(32) 0.5969(9) -0.0575(5)
H14 H 0.2994(7) 0.5829(6) -0.0103(18)
C10 C 0.4069(6) 0.7971(5) -0.0730(3)
H15 H 0.3682(8) 0.8567(7) -0.0869(17)
H16 H 0.4661(24) 0.7743(18) -0.1037(13)
H17 H 0.4498(28) 0.7945(24) -0.0423(6)
C11 C 0.3686(6) 1.0366(5) -0.0481(3)
H18 H 0.3515(10) 1.0634(25) -0.0861(4)
H19 H 0.4287(16) 1.0626(25) -0.0393(12)
H20 H 0.4019(23) 0.9751(5) -0.0461(14)
C12 C 0.2648(6) 1.0146(4) 0.0760(3)
H21 H 0.3203(30) 0.9581(12) 0.0778(6)
H22 H 0.3062(34) 1.0549(14) 0.0836(7)
H23 H 0.1904(7) 1.0103(25) 0.1042(3)
C13 C 0.1661(6) 1.2308(4) -0.0066(3)
C14 C 0.2833(6) 1.2368(4) -0.0008(3)
H24 H 0.3443(6) 1.1859(4) 0.0060(3)
C15 C 0.3122(7) 1.3153(5) -0.0048(3)
H25 H 0.3927(7) 1.3163(5) -0.0006(3)
C16 C 0.2287(7) 1.3913(5) -0.0146(3)
H26 H 0.2503(7) 1.4448(5) -0.0185(3)
C17 C 0.1092(7) 1.3863(5) -0.0185(3)
H27 H 0.0482(7) 1.4375(5) -0.0245(3)
C18 C 0.0789(7) 1.3082(4) -0.0139(3)
H28 H -0.0030(7) 1.3071(4) -0.0156(3)
C19 C -0.0288(6) 1.2018(4) -0.1414(3)
C20 C -0.0973(7) 1.2283(5) -0.1863(3)
H29 H -0.1464(7) 1.1921(5) -0.1903(3)
C21 C -0.0952(8) 1.3048(5) -0.2243(3)
H30 H -0.1412(8) 1.3198(5) -0.2541(3)
C22 C -0.0258(8) 1.3599(5) -0.2189(3)
H31 H -0.0261(8) 1.4134(5) -0.2441(3)
C23 C 0.0440(8) 1.3353(5) -0.1760(3)
H32 H 0.0939(8) 1.3717(5) -0.1730(3)
C24 C 0.0424(6) 1.2593(4) -0.1379(3)
H33 H 0.0899(6) 1.2450(4) -0.1086(3)
C25 C 0.3522(7) 1.1400(5) -0.2040(3)
H34 H 0.3196(7) 1.1788(5) -0.1767(3)
H35 H 0.4349(7) 1.1069(5) -0.1970(3)
C26 C 0.3590(9) 1.1905(6) -0.2635(4)
H36 H 0.4359(9) 1.1670(6) -0.2874(4)
H37 H 0.3566(9) 1.2513(6) -0.2644(4)
C27 C 0.2543(11) 1.1827(7) -0.2828(4)
H38 H 0.1865(11) 1.2332(7) -0.2783(4)
H39 H 0.2752(11) 1.1788(7) -0.3231(4)
C28 C 0.2173(8) 1.1052(5) -0.2490(3)
H40 H 0.2469(8) 1.0580(5) -0.2702(3)
H41 H 0.1265(8) 1.1150(5) -0.2393(3)
C29 C -0.1441(10) 1.5309(6) -0.1209(5)
H42 H -0.1155(10) 1.5217(6) -0.0846(5)
H43 H -0.0719(10) 1.5161(6) -0.1500(5)
C30 C -0.2091(10) 1.6225(6) -0.1373(4)
H44 H -0.2564(10) 1.6461(6) -0.1039(4)
H45 H -0.1506(10) 1.6590(6) -0.1585(4)
H46? H 0.1583(10) 0.3471(6) 0.1696(4)
H47? H 0.225(1) 0.3477(6) 0.1054(4)
C31 C -0.2990(17) 1.6137(12) -0.1766(8)
H48 H -0.2611(17) 1.6249(12) -0.2168(8)
H49 H -0.3789(17) 1.6548(12) -0.1713(8)
C32? C 0.3124(24) 0.3791(16) 0.1506(11)
H50? H 0.3805(24) 0.3360(16) 0.1348(11)
H51? H 0.3070(24) 0.3670(16) 0.1920(11)
C33 C -0.3156(15) 1.5286(11) -0.1594(7)
H52 H -0.4024(15) 1.5282(11) -0.1421(7)
H53 H -0.2952(15) 1.5005(11) -0.1923(7)
C34? C 0.3327(26) 0.4681(18) 0.1257(12)
H54? H 0.3683(26) 0.4878(18) 0.1519(12)
H55? H 0.3920(26) 0.4675(18) 0.0900(12)
C35 C -0.4825(8) 1.3618(5) -0.1358(4)
H56 H -0.5452(8) 1.4012(5) -0.1143(4)
H57 H -0.4437(8) 1.3961(5) -0.1703(4)
C36 C -0.5415(8) 1.2994(5) -0.1508(4)
H58 H -0.6187(8) 1.2922(5) -0.1245(4)
H59 H -0.5589(8) 1.3182(5) -0.1898(4)
C37 C -0.4423(7) 1.2171(5) -0.1448(4)
H60 H -0.3794(7) 1.2156(5) -0.1793(4)
H61 H -0.4783(7) 1.1658(5) -0.1362(4)
C38 C -0.3888(7) 1.2235(5) -0.0956(3)
H62 H -0.3036(7) 1.1892(5) -0.0967(3)
H63 H -0.4392(7) 1.2027(5) -0.0595(3)
C39 C 1.2361(7) -0.1118(5) 0.2927(3)
H64 H 1.1904(21) -0.0556(15) 0.2763(10)
H65 H 1.2501(40) -0.1513(17) 0.2669(8)
H66 H 1.3155(19) -0.1061(30) 0.2988(4)
C40 C 1.0006(7) -0.1692(5) 0.3456(3)
H67 H 0.9508(21) -0.1931(28) 0.3805(4)
H68 H 1.0210(7) -0.2084(24) 0.3193(15)
H69 H 0.9541(21) -0.1137(7) 0.3287(18)
C41 C 1.2500(7) -0.3249(4) 0.3652(3)
C42 C 1.1675(8) -0.3787(5) 0.3800(3)
H70 H 1.0972(8) -0.3672(5) 0.4079(3)
C43 C 1.1846(9) -0.4489(5) 0.3552(3)
H71 H 1.1258(9) -0.4841(5) 0.3659(3)
C44 C 1.2874(9) -0.4674(5) 0.3149(4)
H72 H 1.3006(9) -0.5159(5) 0.2982(4)
C45 C 1.3690(8) -0.4151(6) 0.2996(3)
H73 H 1.4389(8) -0.4269(6) 0.2714(3)
C46 C 1.3520(7) -0.3445(5) 0.3244(3)
H74 H 1.4109(7) -0.3093(5) 0.3133(3)
C47 C 1.4290(7) -0.1956(5) 0.4224(3)
H75 H 1.3918(10) -0.1364(9) 0.4067(18)
H76 H 1.4913(24) -0.2202(19) 0.3933(15)
H77 H 1.4677(30) -0.1964(25) 0.4541(5)
C48 C 1.3845(7) -0.3756(5) 0.4677(3)
H78 H 1.4273(36) -0.3822(7) 0.4992(13)
H79 H 1.4441(31) -0.3934(10) 0.4355(7)
H80 H 1.3230(9) -0.4113(6) 0.4791(19)
C49 C 1.3580(6) 0.0559(5) 0.4565(3)
H81 H 1.3982(23) -0.0037(5) 0.4544(15)
H82 H 1.4138(19) 0.0832(27) 0.4674(11)
H83 H 1.3376(8) 0.0868(26) 0.4196(5)
C50 C 1.2616(7) 0.0077(5) 0.5809(3)
H84 H 1.1894(9) 0.0114(26) 0.6107(3)
H85 H 1.3197(33) 0.0378(19) 0.5873(9)
H86 H 1.3016(37) -0.0525(9) 0.5810(7)
C51 C 1.1363(6) 0.2358(4) 0.5067(3)
C52 C 1.2393(6) 0.2447(5) 0.5274(3)
H87 H 1.2932(6) 0.1948(5) 0.5433(3)
C53 C 1.2618(7) 0.3237(5) 0.5248(3)
H88 H 1.3315(7) 0.3276(5) 0.5384(3)
C54 C 1.1843(7) 0.3975(5) 0.5028(3)
H89 H 1.2028(7) 0.4518(5) 0.4994(3)
C55 C 1.0802(7) 0.3921(5) 0.4857(3)
H90 H 1.0250(7) 0.4429(5) 0.4719(3)
C56 C 1.0553(7) 0.3130(4) 0.4886(3)
H91 H 0.9811(7) 0.3107(4) 0.4781(3)
C57 C 0.9745(6) 0.2055(4) 0.3593(3)
C58 C 0.9156(7) 0.2274(5) 0.3117(3)
H92 H 0.8670(7) 0.1912(5) 0.3070(3)
C59 C 0.9279(8) 0.3013(5) 0.2714(3)
H93 H 0.8857(8) 0.3157(5) 0.2403(3)
C60 C 0.9993(9) 0.3531(5) 0.2760(4)
H94 H 1.0070(9) 0.4033(5) 0.2483(4)
C61 C 1.0619(8) 0.3316(5) 0.3220(3)
H95 H 1.1117(8) 0.3678(5) 0.3254(3)
C62 C 1.0518(7) 0.2586(4) 0.3622(3)
H96 H 1.0972(7) 0.2439(4) 0.3923(3)
C63 C 0.4852(15) 0.2722(12) 0.4182(7)
H97 H 0.4847(15) 0.2159(12) 0.4438(7)
H98 H 0.4789(15) 0.3155(12) 0.4409(7)
C64? C 1.5318(16) -0.3192(13) 0.5968(8)
H99? H 1.5346(16) -0.3815(13) 0.6082(8)
H100? H 1.5433(16) -0.3037(13) 0.5552(8)
C65 C 0.3750(8) 0.2983(6) 0.3834(3)
H101 H 0.3391(8) 0.3605(6) 0.3787(3)
H102 H 0.3095(8) 0.2664(6) 0.4021(3)
H103? H 1.6556(8) -0.2499(6) 0.5900(3)
H104? H 1.6948(8) -0.3480(6) 0.6214(3)
C66 C 0.4352(8) 0.2738(6) 0.3280(4)
H105 H 0.3966(8) 0.2315(6) 0.3200(4)
H106 H 0.4292(8) 0.3247(6) 0.2971(4)
C67 C 0.5676(8) 0.2354(7) 0.3346(4)
H107 H 0.6229(8) 0.2507(7) 0.2988(4)
H108 H 0.5808(8) 0.1722(7) 0.3451(4)
C68 C 0.7954(12) 0.4774(7) 0.3982(5)
H109 H 0.7517(12) 0.4958(7) 0.4338(5)
H110 H 0.8791(12) 0.4448(7) 0.4038(5)
C69 C 0.8030(13) 0.5505(8) 0.3542(5)
H111 H 0.8047(13) 0.6008(8) 0.3690(5)
H112 H 0.8769(13) 0.5391(8) 0.3253(5)
H113? H 1.2308(13) -0.6034(8) 0.6304(5)
H114? H 1.1099(13) -0.5498(8) 0.6632(5)
C70 C 0.6894(22) 0.5633(15) 0.3316(10)
H115 H 0.6205(22) 0.6008(15) 0.3518(10)
H116 H 0.7007(22) 0.5896(15) 0.291(1)
C71? C 1.2675(20) -0.5483(13) 0.6883(9)
H117? H 1.3264(20) -0.6034(13) 0.6971(9)
H118? H 1.2123(20) -0.5356(13) 0.7234(9)
C72 C 0.6652(10) 0.4757(6) 0.3407(4)
H119 H 0.6941(10) 0.4525(6) 0.3057(4)
H120 H 0.5761(10) 0.4769(6) 0.3526(4)
H121? H 1.3359(10) -0.4410(6) 0.6866(4)
H122? H 1.4207(10) -0.4991(6) 0.6430(4)
C73 C 1.2404(8) 0.1348(6) 0.2579(3)
H123 H 1.1660(8) 0.1152(6) 0.2566(3)
H124 H 1.2173(8) 0.1968(6) 0.2583(3)
C74 C 1.3377(9) 0.1176(7) 0.2079(3)
H125 H 1.3356(9) 0.1691(7) 0.1776(3)
H126 H 1.3265(9) 0.0699(7) 0.1931(3)
C75 C 1.4513(9) 0.0951(9) 0.2294(4)
H127 H 1.5132(9) 0.0543(9) 0.2087(4)
H128 H 1.4843(9) 0.1468(9) 0.2253(4)
C76 C 1.4235(7) 0.0550(6) 0.2901(3)
H129 H 1.4727(7) 0.0713(6) 0.3125(3)
H130 H 1.4420(7) -0.0081(6) 0.2951(3)
N1 N 0.2104(5) 0.7381(3) -0.1026(2)
N2 N 0.1327(5) 1.1553(3) -0.0056(2)
N3 N -0.0342(5) 1.1280(3) -0.1020(2)
N4 N 1.2308(5) -0.2535(4) 0.3915(2)
N5 N 1.1141(5) 0.1570(3) 0.5064(2)
N6 N 0.9603(5) 0.1348(3) 0.4019(2)
O1 O 0.1016(4) 0.8996(3) -0.0892(2)
O2 O -0.1914(4) 1.2349(3) -0.0067(2)
O3 O 0.1269(4) 1.0004(2) -0.0057(2)
O4 O -0.2302(5) 1.4795(3) -0.1161(2)
O5 O -0.3904(5) 1.3115(3) -0.1019(2)
O6 O 0.2712(4) 1.0833(3) -0.1983(2)
O7 O 1.1215(4) -0.0917(3) 0.4060(2)
O8 O 0.7868(4) 0.2264(3) 0.4996(2)
O9 O 1.1239(4) 0.0048(3) 0.4959(2)
O10 O 0.5928(5) 0.2685(4) 0.3775(2)
O11 O 0.7316(5) 0.4254(3) 0.3836(2)
O12 O 1.2931(4) 0.0876(3) 0.3073(2)
Na1 Na -0.2039(2) 1.3311(2) -0.09004(11)
Na2 Na 0.1583(2) 1.0258(2) -0.11243(10)
Na3 Na 0.7604(2) 0.2803(2) 0.41002(11)
Na4 Na 1.1630(2) 0.0385(2) 0.39027(11)
Si1 Si 0.1181(2) 0.83472(12) -0.13092(8)
Si2 Si 0.2861(2) 0.73183(12) -0.04669(8)
Si3 Si 0.2218(2) 1.05334(12) 0.00435(8)
Si4 Si 1.1450(2) -0.15468(13) 0.36177(8)
Si5 Si 1.3062(2) -0.26048(12) 0.44742(8)
Si6 Si 1.2121(2) 0.05868(12) 0.51061(8)
Yb1 Yb 0.05050(3) 0.88413(2) 0.00334(1)
Yb2 Yb 1.06069(3) -0.11400(2) 0.49845(1)
O2A* O 0.1914(4) 0.7651(3) 0.0067(2)
Na1A* Na 0.2039(2) 0.6689(2) 0.09004(11)
C19A* C 0.0288(6) 0.7982(4) 0.1414(3)
C20A* C 0.0973(7) 0.7717(5) 0.1863(3)
H29A* H 0.1464(7) 0.8079(5) 0.1903(3)
C21A* C 0.0952(8) 0.6952(5) 0.2243(3)
H30A* H 0.1412(8) 0.6802(5) 0.2541(3)
C22A* C 0.0258(8) 0.6401(5) 0.2189(3)
H31A* H 0.0261(8) 0.5866(5) 0.2441(3)
C23A* C -0.0440(8) 0.6647(5) 0.1760(3)
H32A* H -0.0939(8) 0.6283(5) 0.1730(3)
C24A* C -0.0424(6) 0.7407(4) 0.1379(3)
N3A* N 0.0342(5) 0.8720(3) 0.1020(2)
Na2A* Na -0.1583(2) 0.9742(2) 0.11243(10)
O1A* O -0.1016(4) 1.1004(3) 0.0892(2)
Si1A* Si -0.1181(2) 1.16528(12) 0.13092(8)
C1A* C 0.0289(6) 1.1843(5) 0.1418(3)
H1A* H 0.0758(19) 1.2057(27) 0.1054(3)
H2A* H 0.0106(6) 1.2267(21) 0.1659(15)
H3A* H 0.0773(19) 1.1305(7) 0.1599(17)
C2A* C -0.1978(7) 1.1225(5) 0.2032(3)
H4A* H -0.1407(14) 1.0746(19) 0.2221(8)
H5A* H -0.2244(37) 1.1680(9) 0.2253(7)
H6A* H -0.2696(24) 1.1028(27) 0.1999(3)
N1A* N -0.2104(5) 1.2619(3) 0.1026(2)
C3A* C -0.2389(6) 1.3328(4) 0.1312(3)
C4A* C -0.1647(7) 1.3923(4) 0.1185(3)
H7A* H -0.0931(7) 1.3862(4) 0.0905(3)
C5A* C -0.1943(8) 1.4611(5) 0.1465(3)
H8A* H -0.1428(8) 1.5014(5) 0.1370(3)
C6A* C -0.2960(8) 1.4713(5) 0.1872(3)
H9A* H -0.3156(8) 1.5187(5) 0.2055(3)
C7A* C -0.3697(8) 1.4127(5) 0.2014(3)
H10A* H -0.4400(8) 1.4190(5) 0.2300(3)
C8A* C -0.3417(7) 1.3434(5) 0.1738(3)
H11A* H -0.3932(7) 1.3031(5) 0.1841(3)
Si2A* Si -0.2861(2) 1.26817(12) 0.04669(8)
C9A* C -0.3622(7) 1.3826(4) 0.0249(3)
H12A* H -0.4103(33) 1.3877(6) -0.0044(13)
H13A* H -0.4168(32) 1.4031(9) 0.0575(5)
H14A* H -0.2994(7) 1.4171(6) 0.0103(18)
C10A* C -0.4069(6) 1.2029(5) 0.0730(3)
H15A* H -0.3682(8) 1.1433(7) 0.0869(17)
H16A* H -0.4661(24) 1.2257(18) 0.1037(13)
H17A* H -0.4498(28) 1.2055(24) 0.0423(6)
N2A* N -0.1327(5) 0.8447(3) 0.0056(2)
C13A* C -0.1661(6) 0.7692(4) 0.0066(3)
C14A* C -0.2833(6) 0.7632(4) 0.0008(3)
H24A* H -0.3443(6) 0.8141(4) -0.0060(3)
C15A* C -0.3122(7) 0.6847(5) 0.0048(3)
H25A* H -0.3927(7) 0.6837(5) 0.0006(3)
C16A* C -0.2287(7) 0.6087(5) 0.0146(3)
H26A* H -0.2503(7) 0.5552(5) 0.0185(3)
C17A* C -0.1092(7) 0.6137(5) 0.0185(3)
H27A* H -0.0482(7) 0.5625(5) 0.0245(3)
C18A* C -0.0789(7) 0.6918(4) 0.0139(3)
H28A* H 0.0030(7) 0.6929(4) 0.0156(3)
Si3A* Si -0.2218(2) 0.94666(12) -0.00435(8)
C11A* C -0.3686(6) 0.9634(5) 0.0481(3)
H18A* H -0.3515(10) 0.9366(25) 0.0861(4)
H19A* H -0.4287(16) 0.9374(25) 0.0393(12)
H20A* H -0.4019(23) 1.0249(5) 0.0461(14)
C12A* C -0.2648(6) 0.9854(4) -0.0760(3)
H21A* H -0.3203(30) 1.0419(12) -0.0778(6)
H22A* H -0.3062(34) 0.9451(14) -0.0836(7)
H23A* H -0.1904(7) 0.9897(25) -0.1042(3)
O3A* O -0.1269(4) 0.9996(2) 0.0057(2)
O6A* O -0.2712(4) 0.9167(3) 0.1983(2)
C25A* C -0.3522(7) 0.8600(5) 0.2040(3)
H34A* H -0.3196(7) 0.8212(5) 0.1767(3)
H35A* H -0.4349(7) 0.8931(5) 0.1970(3)
C26A* C -0.3590(9) 0.8095(6) 0.2635(4)
H36A* H -0.4359(9) 0.8330(6) 0.2874(4)
H37A* H -0.3566(9) 0.7487(6) 0.2644(4)
C27A* C -0.2543(11) 0.8173(7) 0.2828(4)
H38A* H -0.1865(11) 0.7668(7) 0.2783(4)
H39A* H -0.2752(11) 0.8212(7) 0.3231(4)
C28A* C -0.2173(8) 0.8948(5) 0.2490(3)
H40A* H -0.2469(8) 0.9420(5) 0.2702(3)
H41A* H -0.1265(8) 0.8850(5) 0.2393(3)
Yb1A* Yb -0.05050(3) 1.11587(2) -0.00334(1)
H33A* H -0.0899(6) 0.7550(4) 0.1086(3)
O4A* O 0.2302(5) 0.5205(3) 0.1161(2)
C29A* C 0.1441(10) 0.4691(6) 0.1209(5)
H42A* H 0.1155(10) 0.4783(6) 0.0846(5)
H43A* H 0.0719(10) 0.4839(6) 0.1500(5)
C30A* C 0.2091(10) 0.3775(6) 0.1373(4)
H44A* H 0.2564(10) 0.3539(6) 0.1039(4)
H45A* H 0.1506(10) 0.3410(6) 0.1585(4)
C31A* C 0.2990(17) 0.3863(12) 0.1766(8)
H48A* H 0.2611(17) 0.3751(12) 0.2168(8)
H49A* H 0.3789(17) 0.3452(12) 0.1713(8)
C33A* C 0.3156(15) 0.4714(11) 0.1594(7)
H52A* H 0.4024(15) 0.4718(11) 0.1421(7)
H53A* H 0.2952(15) 0.4995(11) 0.1923(7)
O5A* O 0.3904(5) 0.6885(3) 0.1019(2)
C35A* C 0.4825(8) 0.6382(5) 0.1358(4)
H56A* H 0.5452(8) 0.5988(5) 0.1143(4)
H57A* H 0.4437(8) 0.6039(5) 0.1703(4)
C36A* C 0.5415(8) 0.7006(5) 0.1508(4)
H58A* H 0.6187(8) 0.7078(5) 0.1245(4)
H59A* H 0.5589(8) 0.6818(5) 0.1898(4)
C37A* C 0.4423(7) 0.7829(5) 0.1448(4)
H60A* H 0.3794(7) 0.7844(5) 0.1793(4)
H61A* H 0.4783(7) 0.8342(5) 0.1362(4)
C38A* C 0.3888(7) 0.7765(5) 0.0956(3)
H62A* H 0.3036(7) 0.8108(5) 0.0967(3)
H63A* H 0.4392(7) 0.7973(5) 0.0595(3)
O8A* O 1.2132(4) -0.2264(3) 0.5004(2)
Na3A* Na 1.2396(2) -0.2803(2) 0.58998(11)
C57A* C 1.0255(6) -0.2055(4) 0.6407(3)
C58A* C 1.0844(7) -0.2274(5) 0.6883(3)
H92A* H 1.1330(7) -0.1912(5) 0.6930(3)
C59A* C 1.0721(8) -0.3013(5) 0.7286(3)
H93A* H 1.1143(8) -0.3157(5) 0.7597(3)
C60A* C 1.0007(9) -0.3531(5) 0.7240(4)
H94A* H 0.9930(9) -0.4033(5) 0.7517(4)
C61A* C 0.9381(8) -0.3316(5) 0.6780(3)
H95A* H 0.8883(8) -0.3678(5) 0.6746(3)
C62A* C 0.9482(7) -0.2586(4) 0.6378(3)
N6A* N 1.0397(5) -0.1348(3) 0.5981(2)
O10A* O 1.4072(5) -0.2685(4) 0.6225(2)
C63A* C 1.5148(15) -0.2722(12) 0.5818(7)
H97A* H 1.5153(15) -0.2159(12) 0.5562(7)
H98A* H 1.5211(15) -0.3155(12) 0.5591(7)
C65A* C 1.6250(8) -0.2983(6) 0.6166(3)
H101A* H 1.6609(8) -0.3605(6) 0.6213(3)
H102A* H 1.6905(8) -0.2664(6) 0.5979(3)
C66A* C 1.5648(8) -0.2738(6) 0.6720(4)
H105A* H 1.6034(8) -0.2315(6) 0.6800(4)
H106A* H 1.5708(8) -0.3247(6) 0.7029(4)
C67A* C 1.4324(8) -0.2354(7) 0.6654(4)
H107A* H 1.3771(8) -0.2507(7) 0.7012(4)
H108A* H 1.4192(8) -0.1722(7) 0.6549(4)
O11A* O 1.2684(5) -0.4254(3) 0.6164(2)
C68A* C 1.2046(12) -0.4774(7) 0.6018(5)
H109A* H 1.2483(12) -0.4958(7) 0.5662(5)
H110A* H 1.1209(12) -0.4448(7) 0.5962(5)
C69A* C 1.1970(13) -0.5505(8) 0.6458(5)
H111A* H 1.1953(13) -0.6008(8) 0.6310(5)
H112A* H 1.1231(13) -0.5391(8) 0.6747(5)
C70A* C 1.3106(22) -0.5633(15) 0.6684(10)
H115A* H 1.3795(22) -0.6008(15) 0.6482(10)
H116A* H 1.2993(22) -0.5896(15) 0.709(1)
C72A* C 1.3348(10) -0.4757(6) 0.6593(4)
H119A* H 1.3059(10) -0.4525(6) 0.6943(4)
H120A* H 1.4239(10) -0.4769(6) 0.6474(4)
Na4A* Na 0.8370(2) -0.0385(2) 0.60973(11)
O7A* O 0.8785(4) 0.0917(3) 0.5940(2)
Si4A* Si 0.8550(2) 0.15468(13) 0.63823(8)
C39A* C 0.7639(7) 0.1118(5) 0.7073(3)
H64A* H 0.8096(21) 0.0556(15) 0.7237(10)
H65A* H 0.7499(40) 0.1513(17) 0.7331(8)
H66A* H 0.6845(19) 0.1061(30) 0.7012(4)
C40A* C 0.9994(7) 0.1692(5) 0.6544(3)
H67A* H 1.0492(21) 0.1931(28) 0.6195(4)
H68A* H 0.9790(7) 0.2084(24) 0.6807(15)
H69A* H 1.0459(21) 0.1137(7) 0.6713(18)
N4A* N 0.7692(5) 0.2535(4) 0.6085(2)
C41A* C 0.7500(7) 0.3249(4) 0.6348(3)
C42A* C 0.8325(8) 0.3787(5) 0.6200(3)
H70A* H 0.9028(8) 0.3672(5) 0.5921(3)
C43A* C 0.8154(9) 0.4489(5) 0.6448(3)
H71A* H 0.8742(9) 0.4841(5) 0.6341(3)
C44A* C 0.7126(9) 0.4674(5) 0.6851(4)
H72A* H 0.6994(9) 0.5159(5) 0.7018(4)
C45A* C 0.6310(8) 0.4151(6) 0.7004(3)
H73A* H 0.5611(8) 0.4269(6) 0.7286(3)
C46A* C 0.6480(7) 0.3445(5) 0.6756(3)
H74A* H 0.5891(7) 0.3093(5) 0.6867(3)
Si5A* Si 0.6938(2) 0.26048(12) 0.55258(8)
C47A* C 0.5710(7) 0.1956(5) 0.5776(3)
H75A* H 0.6082(10) 0.1364(9) 0.5933(18)
H76A* H 0.5087(24) 0.2202(19) 0.6067(15)
H77A* H 0.5323(30) 0.1964(25) 0.5459(5)
C48A* C 0.6155(7) 0.3756(5) 0.5323(3)
H78A* H 0.5727(36) 0.3822(7) 0.5008(13)
H79A* H 0.5559(31) 0.3934(10) 0.5645(7)
H80A* H 0.6770(9) 0.4113(6) 0.5209(19)
N5A* N 0.8859(5) -0.1570(3) 0.4936(2)
C51A* C 0.8637(6) -0.2358(4) 0.4933(3)
C52A* C 0.7607(6) -0.2447(5) 0.4726(3)
H87A* H 0.7068(6) -0.1948(5) 0.4567(3)
C53A* C 0.7382(7) -0.3237(5) 0.4752(3)
H88A* H 0.6685(7) -0.3276(5) 0.4616(3)
C54A* C 0.8157(7) -0.3975(5) 0.4972(3)
H89A* H 0.7972(7) -0.4518(5) 0.5006(3)
C55A* C 0.9198(7) -0.3921(5) 0.5143(3)
H90A* H 0.9750(7) -0.4429(5) 0.5281(3)
C56A* C 0.9447(7) -0.3130(4) 0.5114(3)
H91A* H 1.0189(7) -0.3107(4) 0.5219(3)
Si6A* Si 0.7879(2) -0.05868(12) 0.48939(8)
C49A* C 0.6420(6) -0.0559(5) 0.5435(3)
H81A* H 0.6018(23) 0.0037(5) 0.5456(15)
H82A* H 0.5862(19) -0.0832(27) 0.5326(11)
H83A* H 0.6624(8) -0.0868(26) 0.5804(5)
C50A* C 0.7384(7) -0.0077(5) 0.4191(3)
H84A* H 0.8106(9) -0.0114(26) 0.3893(3)
H85A* H 0.6803(33) -0.0378(19) 0.4127(9)
H86A* H 0.6984(37) 0.0525(9) 0.4190(7)
O9A* O 0.8761(4) -0.0048(3) 0.5041(2)
O12A* O 0.7069(4) -0.0876(3) 0.6927(2)
C73A* C 0.7596(8) -0.1348(6) 0.7421(3)
H123A* H 0.8340(8) -0.1152(6) 0.7434(3)
H124A* H 0.7827(8) -0.1968(6) 0.7417(3)
C74A* C 0.6623(9) -0.1176(7) 0.7921(3)
H125A* H 0.6644(9) -0.1691(7) 0.8224(3)
H126A* H 0.6735(9) -0.0699(7) 0.8069(3)
C75A* C 0.5487(9) -0.0951(9) 0.7706(4)
H127A* H 0.4868(9) -0.0543(9) 0.7913(4)
H128A* H 0.5157(9) -0.1468(9) 0.7747(4)
C76A* C 0.5765(7) -0.0550(6) 0.7099(3)
H129A* H 0.5273(7) -0.0713(6) 0.6875(3)
H130A* H 0.5580(7) 0.0081(6) 0.7049(3)
Yb2A* Yb 0.93931(3) 0.11400(2) 0.50155(1)
H96A* H 0.9028(7) -0.2439(4) 0.6077(3)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.75
H 0.23
N 0.78
Na 1.68
O 0.68
Si 1.15
Yb 1.44
|
1100621.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 03:51:51 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100621.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100621
loop_
_publ_author_name
'Kraut, S.'
'Magull, J.'
'Schaller, U.'
'Karl, M.'
'Harms, K.'
'Dehnicke, K.'
_publ_section_title
;
Amidoliganden zum Aufbau von mehrkernigen Lanthanoidkomplexen
;
_journal_coden_ASTM ZAACAB
_journal_issue 7
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1193
_journal_page_last 1201
_journal_paper_doi
10.1002/(sici)1521-3749(199807)624:7<1193::aid-zaac1193>3.0.co;2-n
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C40 H96 Li4 N6 O6 Si4 Yb2'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 64.807(10)
_cell_angle_beta 68.864(10)
_cell_angle_gamma 80.748(10)
_cell_formula_units_Z 1
_cell_length_a 10.9406(10)
_cell_length_b 11.839(1)
_cell_length_c 13.142(1)
_cod_database_code 1100621
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C1 C -0.1775(5) 0.2369(5) 0.6784(5)
C2 C -0.0872(6) 0.3493(5) 0.6119(5)
H1 H -0.0585(27) 0.370(2) 0.5262(6)
H2 H -0.0107(17) 0.3295(12) 0.6387(22)
H3 H -0.1345(12) 0.4208(10) 0.6279(25)
C3 C -0.2631(11) 0.227(1) 0.7953(9)
H4 H -0.3182(11) 0.1531(10) 0.8330(9)
H5 H -0.3188(11) 0.3018(10) 0.7877(9)
H6 H -0.2102(11) 0.2195(10) 0.8443(9)
C4 C -0.265(1) 0.2728(10) 0.5926(9)
H7 H -0.2081(10) 0.2797(10) 0.5130(9)
H8 H -0.3098(10) 0.3527(10) 0.5872(9)
H9 H -0.3301(10) 0.2076(10) 0.6253(9)
C5? C -0.1566(14) 0.1853(13) 0.8084(12)
H10? H -0.0651(14) 0.1589(13) 0.8003(12)
H11? H -0.2143(14) 0.1142(13) 0.8650(12)
H12? H -0.1777(14) 0.2521(13) 0.8376(12)
C6? C -0.3157(14) 0.2722(14) 0.7039(14)
H13? H -0.3694(14) 0.1968(14) 0.7466(14)
H14? H -0.3331(14) 0.3232(14) 0.6291(14)
H15? H -0.3375(14) 0.3204(14) 0.7532(14)
C7 C -0.2410(5) -0.0859(5) 0.3613(5)
H16 H -0.2802(31) -0.0521(5) 0.2977(21)
H17 H -0.3049(26) -0.1385(19) 0.4356(10)
H18 H -0.1634(8) -0.1360(19) 0.3399(30)
C8 C -0.3500(5) 0.1210(5) 0.4426(5)
H19 H -0.3317(5) 0.1972(19) 0.4466(31)
H20 H -0.3982(17) 0.0625(14) 0.5226(14)
H21 H -0.4029(16) 0.1421(32) 0.3905(18)
C9 C 0.0744(5) -0.1951(5) 0.8643(4)
C10 C 0.0089(6) -0.1023(6) 0.9202(5)
H22 H 0.0040(33) -0.1386(15) 1.0039(10)
H23 H 0.0602(21) -0.0255(14) 0.8777(22)
H24 H -0.0798(14) -0.0831(27) 0.9151(30)
C11 C 0.2118(5) -0.2248(5) 0.8745(5)
H25 H 0.2056(6) -0.2587(32) 0.9585(6)
H26 H 0.2542(14) -0.2864(25) 0.8409(29)
H27 H 0.2638(12) -0.1483(8) 0.8307(27)
C12 C -0.0052(5) -0.3154(5) 0.9352(5)
H28 H -0.0110(29) -0.3471(18) 1.0189(7)
H29 H -0.0936(12) -0.2982(8) 0.9291(25)
H30 H 0.0379(18) -0.3779(12) 0.903(2)
C13 C -0.2048(5) -0.4723(5) 0.8581(4)
H31 H -0.2917(6) -0.5031(13) 0.9148(18)
H32 H -0.1491(26) -0.4691(7) 0.9007(20)
H33 H -0.1652(30) -0.5286(8) 0.8175(5)
C14 C -0.3265(5) -0.3361(5) 0.6704(5)
H34 H -0.3960(21) -0.3954(25) 0.7303(6)
H35 H -0.2724(8) -0.3697(31) 0.6117(22)
H36 H -0.3657(27) -0.2565(8) 0.6305(26)
C15 C -0.3938(5) -0.1754(5) 0.8765(4)
C16 C -0.4740(5) -0.0715(5) 0.8091(5)
H37 H -0.5578(17) -0.0609(25) 0.8657(6)
H38 H -0.4903(32) -0.0941(17) 0.7516(24)
H39 H -0.4252(17) 0.0068(10) 0.7670(28)
C17 C -0.4761(5) -0.2941(5) 0.9480(5)
H40 H -0.5576(18) -0.2783(12) 1.0039(25)
H41 H -0.4266(16) -0.3614(11) 0.9923(27)
H42 H -0.4968(32) -0.3186(21) 0.8936(6)
C18 C -0.3662(5) -0.1379(6) 0.9631(5)
H43 H -0.4490(6) -0.1180(35) 1.0147(23)
H44 H -0.3097(31) -0.0644(22) 0.9186(5)
H45 H -0.3222(34) -0.2070(14) 1.0117(23)
C19 C 0.1533(6) -0.5479(6) 0.6996(6)
H46 H 0.1434(6) -0.5182(6) 0.6203(6)
H47 H 0.0715(6) -0.5901(6) 0.7609(6)
C20 C 0.2672(9) -0.6353(10) 0.7075(14)
H48 H 0.2428(9) -0.7106(10) 0.7828(14)
H49 H 0.2975(9) -0.6615(10) 0.6400(14)
C21 C 0.3689(8) -0.5673(8) 0.7032(9)
H50 H 0.4261(8) -0.5237(8) 0.6202(9)
H51 H 0.4234(8) -0.6243(8) 0.7506(9)
C22 C 0.2985(7) -0.4781(7) 0.7539(8)
H52 H 0.3516(7) -0.4026(7) 0.7210(8)
H53 H 0.2756(7) -0.5157(7) 0.8416(8)
O1 O -0.1128(3) -0.0111(3) 0.4800(3)
O2 O -0.0754(3) -0.2618(3) 0.6483(3)
O3 O 0.1791(4) -0.4474(4) 0.7186(4)
Yb1 Yb -0.09937(2) -0.06569(2) 0.66247(2)
Si1 Si -0.19188(12) 0.04713(13) 0.38186(12)
Si2 Si -0.22139(13) -0.31076(12) 0.74486(12)
N1 N -0.1218(5) 0.1284(4) 0.6577(5)
N2 N 0.0757(4) -0.1455(4) 0.7387(3)
N3 N -0.2682(4) -0.1922(4) 0.7911(3)
Li1 Li 0.0439(9) 0.1798(8) 0.5155(7)
Li2 Li 0.0669(8) -0.3001(9) 0.7072(8)
Yb1A* Yb 0.09937(2) 0.06569(2) 0.33753(2)
O1A* O 0.1128(3) 0.0111(3) 0.5200(3)
Si1A* Si 0.19188(12) -0.04713(13) 0.61814(12)
C7A* C 0.2410(5) 0.0859(5) 0.6387(5)
H16A* H 0.2802(31) 0.0521(5) 0.7023(21)
H17A* H 0.3049(26) 0.1385(19) 0.5644(10)
H18A* H 0.1634(8) 0.1360(19) 0.6601(30)
C8A* C 0.3500(5) -0.1210(5) 0.5574(5)
H19A* H 0.3317(5) -0.1972(19) 0.5534(31)
H20A* H 0.3982(17) -0.0625(14) 0.4774(14)
H21A* H 0.4029(16) -0.1421(32) 0.6095(18)
O2A* O 0.0754(3) 0.2618(3) 0.3517(3)
N1A* N 0.1218(5) -0.1284(4) 0.3423(5)
C1A* C 0.1775(5) -0.2369(5) 0.3216(5)
C2A* C 0.0872(6) -0.3493(5) 0.3881(5)
H1A* H 0.0585(27) -0.370(2) 0.4738(6)
H2A* H 0.0107(17) -0.3295(12) 0.3613(22)
H3A* H 0.1345(12) -0.4208(10) 0.3721(25)
C3A* C 0.2631(11) -0.227(1) 0.2047(9)
H4A* H 0.3182(11) -0.1531(10) 0.1670(9)
H5A* H 0.3188(11) -0.3018(10) 0.2123(9)
H6A* H 0.2102(11) -0.2195(10) 0.1557(9)
C4A* C 0.265(1) -0.2728(10) 0.4074(9)
H7A* H 0.2081(10) -0.2797(10) 0.4870(9)
H8A* H 0.3098(10) -0.3527(10) 0.4128(9)
H9A* H 0.3301(10) -0.2076(10) 0.3747(9)
Li1A* Li -0.0439(9) -0.1798(8) 0.4845(7)
N2A* N -0.0757(4) 0.1455(4) 0.2613(3)
C9A* C -0.0744(5) 0.1951(5) 0.1357(4)
C10A* C -0.0089(6) 0.1023(6) 0.0798(5)
H22A* H -0.0040(33) 0.1386(15) -0.0039(10)
H23A* H -0.0602(21) 0.0255(14) 0.1223(22)
H24A* H 0.0798(14) 0.0831(27) 0.0849(30)
C11A* C -0.2118(5) 0.2248(5) 0.1255(5)
H25A* H -0.2056(6) 0.2587(32) 0.0415(6)
H26A* H -0.2542(14) 0.2864(25) 0.1591(29)
H27A* H -0.2638(12) 0.1483(8) 0.1693(27)
C12A* C 0.0052(5) 0.3154(5) 0.0648(5)
H28A* H 0.0110(29) 0.3471(18) -0.0189(7)
H29A* H 0.0936(12) 0.2982(8) 0.0709(25)
H30A* H -0.0379(18) 0.3779(12) 0.097(2)
N3A* N 0.2682(4) 0.1922(4) 0.2089(3)
C15A* C 0.3938(5) 0.1754(5) 0.1235(4)
C16A* C 0.4740(5) 0.0715(5) 0.1909(5)
H37A* H 0.5578(17) 0.0609(25) 0.1343(6)
H38A* H 0.4903(32) 0.0941(17) 0.2484(24)
H39A* H 0.4252(17) -0.0068(10) 0.2330(28)
C17A* C 0.4761(5) 0.2941(5) 0.0520(5)
H40A* H 0.5576(18) 0.2783(12) -0.0039(25)
H41A* H 0.4266(16) 0.3614(11) 0.0077(27)
H42A* H 0.4968(32) 0.3186(21) 0.1064(6)
C18A* C 0.3662(5) 0.1379(6) 0.0369(5)
H43A* H 0.4490(6) 0.1180(35) -0.0147(23)
H44A* H 0.3097(31) 0.0644(22) 0.0814(5)
H45A* H 0.3222(34) 0.2070(14) -0.0117(23)
Si2A* Si 0.22139(13) 0.31076(12) 0.25514(12)
C13A* C 0.2048(5) 0.4723(5) 0.1419(4)
H31A* H 0.2917(6) 0.5031(13) 0.0852(18)
H32A* H 0.1491(26) 0.4691(7) 0.0993(20)
H33A* H 0.1652(30) 0.5286(8) 0.1825(5)
C14A* C 0.3265(5) 0.3361(5) 0.3296(5)
H34A* H 0.3960(21) 0.3954(25) 0.2697(6)
H35A* H 0.2724(8) 0.3697(31) 0.3883(22)
H36A* H 0.3657(27) 0.2565(8) 0.3695(26)
Li2A* Li -0.0669(8) 0.3001(9) 0.2928(8)
O3A* O -0.1791(4) 0.4474(4) 0.2814(4)
C19A* C -0.1533(6) 0.5479(6) 0.3004(6)
H46A* H -0.1434(6) 0.5182(6) 0.3797(6)
H47A* H -0.0715(6) 0.5901(6) 0.2391(6)
C20A* C -0.2672(9) 0.6353(10) 0.2925(14)
H48A* H -0.2428(9) 0.7106(10) 0.2172(14)
H49A* H -0.2975(9) 0.6615(10) 0.3600(14)
C21A* C -0.3689(8) 0.5673(8) 0.2968(9)
H50A* H -0.4261(8) 0.5237(8) 0.3798(9)
H51A* H -0.4234(8) 0.6243(8) 0.2494(9)
C22A* C -0.2985(7) 0.4781(7) 0.2461(8)
H52A* H -0.3516(7) 0.4026(7) 0.2790(8)
H53A* H -0.2756(7) 0.5157(7) 0.1584(8)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 0.98
N 0.69
O 0.68
Si 1.08
Yb 1.50
|
1100622.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 12:25:08 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100622.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100622
loop_
_publ_author_name
'Chitsaz, Soheila'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Asymmetrisch substituierte Iminiumsalze [Et~3~PNAsPh~3~]X und ihre
Reaktion mit Acetonitril. Kristallstrukturen von [Et~3~PNAsPh~3~]X
(X = Cl, Br), [(Ph~3~As)~2~CCN]Br und [(Ph~3~As)~2~CCN(SnBr~5~)]
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1341
_journal_page_last 1346
_journal_paper_doi
10.1002/(sici)1521-3749(199808)624:8<1341::aid-zaac1341>3.0.co;2-v
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C24 H30 As Cl N P'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 92.06(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.202(1)
_cell_length_b 8.904(1)
_cell_length_c 25.621(2)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C24 H30 As1 Cl1 N1 P1'
_cod_database_code 1100622
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
As1 As 0.13927(4) 0.39848(4) 0.10400(1)
Cl1 Cl 0.51513(10) 0.93228(14) 0.14801(4)
N1 N 0.1831(3) 0.3193(4) 0.16351(11)
P1 P 0.28024(9) 0.36173(12) 0.21164(4)
C1 C 0.1013(3) 0.6093(4) 0.10670(12)
C2 C -0.0295(4) 0.6574(5) 0.10678(14)
H1 H -0.0992(4) 0.5877(5) 0.10119(14)
C3 C -0.0557(4) 0.8077(5) 0.11511(15)
H2 H -0.1439(4) 0.8420(5) 0.11503(15)
C4 C 0.0449(5) 0.9073(5) 0.1235(2)
H3 H 0.0256(5) 1.0099(5) 0.1299(2)
C5 C 0.1748(4) 0.8612(5) 0.12263(15)
H4 H 0.2438(4) 0.9317(5) 0.12798(15)
C6 C 0.2026(4) 0.7117(5) 0.11395(14)
H5 H 0.2911(4) 0.6791(5) 0.11294(14)
C7 C 0.2632(3) 0.3614(4) 0.05103(13)
C8 C 0.3403(4) 0.2348(5) 0.0548(2)
H6 H 0.3387(4) 0.1723(5) 0.0849(2)
C9 C 0.4206(4) 0.2003(6) 0.0139(2)
H7 H 0.4748(4) 0.1136(6) 0.0159(2)
C10 C 0.4222(5) 0.2918(8) -0.0298(2)
H8 H 0.4751(5) 0.2654(8) -0.0581(2)
C11 C 0.3483(5) 0.4194(7) -0.0324(2)
H9 H 0.3522(5) 0.4835(7) -0.0619(2)
C12 C 0.2675(4) 0.4554(5) 0.00807(14)
H10 H 0.2155(4) 0.5438(5) 0.00636(14)
C13 C -0.0176(3) 0.2934(4) 0.08318(13)
C14 C -0.0306(4) 0.2243(5) 0.03472(14)
H11 H 0.0349(4) 0.2369(5) 0.00962(14)
C15 C -0.1402(5) 0.1369(5) 0.0234(2)
H12 H -0.1501(5) 0.0897(5) -0.0097(2)
C16 C -0.2355(4) 0.1176(5) 0.0599(2)
H13 H -0.3096(4) 0.0564(5) 0.0518(2)
C17 C -0.2238(4) 0.1866(5) 0.1081(2)
H14 H -0.2897(4) 0.1741(5) 0.1330(2)
C18 C -0.1142(4) 0.2746(5) 0.11956(15)
H15 H -0.1050(4) 0.3225(5) 0.15263(15)
C19 C 0.4516(4) 0.3365(6) 0.2002(2)
H16 H 0.5016(4) 0.3472(6) 0.2338(2)
H17 H 0.4652(4) 0.2329(6) 0.1875(2)
C20 C 0.5076(4) 0.4471(6) 0.1606(2)
H18 H 0.6009(4) 0.4261(6) 0.1566(2)
H19 H 0.4969(4) 0.5501(6) 0.1732(2)
H20 H 0.4605(4) 0.4355(6) 0.1268(2)
C21 C 0.2653(5) 0.5480(6) 0.2376(2)
H21 H 0.3190(5) 0.5545(6) 0.2705(2)
H22 H 0.3022(5) 0.6199(6) 0.2126(2)
C22 C 0.1258(4) 0.5961(6) 0.2487(2)
H23 H 0.1267(4) 0.6985(6) 0.2626(2)
H24 H 0.0889(4) 0.5276(6) 0.2742(2)
H25 H 0.0720(4) 0.5930(6) 0.2162(2)
C23 C 0.2428(5) 0.2351(6) 0.2635(2)
H26 H 0.3092(5) 0.2481(6) 0.2923(2)
H27 H 0.1564(5) 0.2627(6) 0.2771(2)
C24 C 0.2393(5) 0.0717(5) 0.2478(2)
H28 H 0.2184(5) 0.0099(5) 0.2780(2)
H29 H 0.3252(5) 0.0422(5) 0.2352(2)
H30 H 0.1722(5) 0.0569(5) 0.2199(2)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
As 1.21
Cl 0.99
N 0.68
P 1.05
|
1100623.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 12:25:08 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100623.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100623
loop_
_publ_author_name
'Chitsaz, Soheila'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Asymmetrisch substituierte Iminiumsalze [Et~3~PNAsPh~3~]X und ihre
Reaktion mit Acetonitril. Kristallstrukturen von [Et~3~PNAsPh~3~]X
(X = Cl, Br), [(Ph~3~As)~2~CCN]Br und [(Ph~3~As)~2~CCN(SnBr~5~)]
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1341
_journal_page_last 1346
_journal_paper_doi
10.1002/(sici)1521-3749(199808)624:8<1341::aid-zaac1341>3.0.co;2-v
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C24 H30 As Br N P'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 92.40(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.262(1)
_cell_length_b 8.929(1)
_cell_length_c 25.702(2)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C24 H30 As1 Br1 N1 P1'
_cod_database_code 1100623
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
As1 As 0.13250(2) 0.39956(3) 0.10381(1)
Br1 Br 0.50781(3) 0.92580(3) 0.14561(1)
N1 N 0.1770(2) 0.3213(2) 0.16349(9)
P1 P 0.27489(6) 0.36457(7) 0.21095(3)
C1 C 0.0895(2) 0.6089(3) 0.10624(10)
C2 C -0.0402(3) 0.6526(3) 0.10571(11)
H1 H -0.0979(35) 0.5871(36) 0.1003(14)
C3 C -0.0711(3) 0.8014(3) 0.11335(12)
H2 H -0.1582(31) 0.8313(33) 0.1137(12)
C4 C 0.0271(3) 0.9055(3) 0.12237(12)
H3 H 0.0084(37) 1.0034(44) 0.1280(15)
C5 C 0.1571(3) 0.8622(3) 0.12236(12)
H4 H 0.2288(33) 0.9376(35) 0.1286(12)
C6 C 0.1891(3) 0.7137(3) 0.11405(11)
H5 H 0.2770(28) 0.6844(28) 0.1148(11)
C7 C 0.2569(2) 0.3652(3) 0.05164(10)
C8 C 0.3319(3) 0.2359(3) 0.05547(13)
H6 H 0.3263(34) 0.1706(41) 0.0870(14)
C9 C 0.4149(3) 0.2051(4) 0.0153(2)
H7 H 0.4578(41) 0.1193(45) 0.0188(16)
C10 C 0.4222(3) 0.2998(5) -0.0268(2)
H8 H 0.4794(43) 0.2809(48) -0.0546(17)
C11 C 0.3488(3) 0.4287(5) -0.02931(14)
H9 H 0.3517(38) 0.4977(44) -0.0574(16)
C12 C 0.2650(3) 0.4621(4) 0.00988(12)
H10 H 0.2255(42) 0.5467(46) 0.0101(16)
C13 C -0.0214(2) 0.2915(2) 0.0828(1)
C14 C -0.0332(3) 0.2216(3) 0.03461(11)
H11 H 0.0410(29) 0.2301(32) 0.0109(12)
C15 C -0.1417(3) 0.1338(3) 0.02233(14)
H12 H -0.1477(35) 0.0929(37) -0.0063(15)
C16 C -0.2380(3) 0.1172(3) 0.05789(15)
H13 H -0.3138(34) 0.0527(37) 0.0505(13)
C17 C -0.2276(3) 0.1881(3) 0.10560(14)
H14 H -0.2927(34) 0.1804(35) 0.1261(13)
C18 C -0.1199(3) 0.2756(3) 0.11828(12)
H15 H -0.1113(27) 0.3172(32) 0.1508(12)
C19 C 0.4467(3) 0.3389(4) 0.19894(15)
H16 H 0.4960(53) 0.3555(59) 0.2400(22)
H17 H 0.4542(39) 0.2258(48) 0.1876(16)
C20 C 0.5015(3) 0.4494(4) 0.16029(14)
H18 H 0.5896(43) 0.4444(43) 0.1565(16)
H19 H 0.4794(47) 0.5546(54) 0.1811(19)
H20 H 0.4550(48) 0.442(5) 0.1245(21)
C21 C 0.2627(4) 0.5518(4) 0.23673(15)
H21 H 0.3219(50) 0.5571(51) 0.2748(21)
H22 H 0.3182(42) 0.6163(46) 0.2082(18)
C22 C 0.1241(4) 0.5991(5) 0.2484(2)
H23 H 0.1125(52) 0.6916(67) 0.2604(21)
H24 H 0.0952(55) 0.5320(65) 0.2710(23)
H25 H 0.0670(37) 0.5871(37) 0.2181(16)
C23 C 0.2392(3) 0.2382(4) 0.26304(13)
H26 H 0.3115(44) 0.2665(49) 0.2933(18)
H27 H 0.1449(35) 0.2733(39) 0.2765(13)
C24 C 0.2369(4) 0.0752(4) 0.2481(2)
H28 H 0.2117(43) 0.0144(54) 0.2752(18)
H29 H 0.3240(48) 0.0594(50) 0.2359(17)
H30 H 0.1706(37) 0.0562(36) 0.2225(15)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
As 1.21
Br 1.21
N 0.68
P 1.05
|
1100624.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 12:25:08 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100624.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100624
loop_
_publ_author_name
'Chitsaz, Soheila'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Asymmetrisch substituierte Iminiumsalze [Et~3~PNAsPh~3~]X und ihre
Reaktion mit Acetonitril. Kristallstrukturen von [Et~3~PNAsPh~3~]X
(X = Cl, Br), [(Ph~3~As)~2~CCN]Br und [(Ph~3~As)~2~CCN(SnBr~5~)]
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1341
_journal_page_last 1346
_journal_paper_doi
10.1002/(sici)1521-3749(199808)624:8<1341::aid-zaac1341>3.0.co;2-v
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C38 H30 As2 Br N'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 100.883(9)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.2230(9)
_cell_length_b 15.9892(11)
_cell_length_c 19.6389(18)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C38 H30 As2 Br1 N1'
_cod_database_code 1100624
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
As1 As 0.56037(5) 0.88706(3) 0.21611(2)
C1 C 0.5769(5) 0.9107(3) 0.3124(2)
Br1 Br 0.23569(6) 0.28587(3) -0.00084(2)
As2 As 0.35680(5) 0.73709(3) 0.14325(2)
C2 C 0.5750(5) 0.8456(3) 0.3601(2)
H1 H 0.56500 0.78930 0.34460
C3 C 0.5880(6) 0.8639(4) 0.4300(2)
H2 H 0.58430 0.82020 0.46240
C4 C 0.6061(6) 0.9455(4) 0.4527(3)
H3 H 0.61860 0.95680 0.50100
C5 C 0.6065(5) 1.0118(4) 0.4064(2)
H4 H 0.61630 1.06780 0.42260
C6 C 0.5922(5) 0.9938(3) 0.3363(2)
H5 H 0.59270 1.03810 0.30400
C7 C 0.7269(5) 0.9093(3) 0.1902(2)
C8 C 0.8231(5) 0.9591(3) 0.2310(2)
H6 H 0.80720 0.98130 0.27360
C9 C 0.9407(6) 0.9760(4) 0.2096(2)
H7 H 1.00720 1.00880 0.23790
C10 C 0.9624(5) 0.9451(3) 0.1464(2)
H8 H 1.04280 0.95820 0.13120
C11 C 0.8692(5) 0.8961(3) 0.1061(2)
H9 H 0.88600 0.87500 0.06330
C12 C 0.7502(5) 0.8766(3) 0.1267(2)
H10 H 0.68590 0.84210 0.09880
C13 C 0.4327(5) 0.9642(3) 0.1688(2)
C14 C 0.4466(6) 0.9958(3) 0.1033(2)
H11 H 0.51480 0.97540 0.08090
C15 C 0.3595(6) 1.0567(3) 0.0726(3)
H12 H 0.36560 1.07640 0.02760
C16 C 0.2649(6) 1.0893(3) 0.1055(3)
H13 H 0.20860 1.13300 0.08420
C17 C 0.2504(5) 1.0593(3) 0.1700(2)
H14 H 0.18400 1.08170 0.19270
C18 C 0.3342(5) 0.9959(3) 0.2008(2)
H15 H 0.32370 0.97420 0.24450
C19 C 0.3093(5) 0.7934(3) 0.0566(2)
C20 C 0.3949(5) 0.7856(3) 0.0072(2)
H16 H 0.47560 0.75470 0.01800
C21 C 0.3578(6) 0.8239(3) -0.0567(2)
H17 H 0.41230 0.81730 -0.09050
C22 C 0.2444(7) 0.8709(4) -0.0722(2)
H18 H 0.22190 0.89730 -0.11620
C23 C 0.1620(6) 0.8804(4) -0.0243(2)
H19 H 0.08300 0.91290 -0.03510
C24 C 0.1969(5) 0.8415(3) 0.0404(2)
H20 H 0.14150 0.84860 0.07380
C25 C 0.3867(5) 0.6219(3) 0.12511(19)
C26 C 0.5011(5) 0.5986(3) 0.10151(19)
H21 H 0.56550 0.63950 0.09570
C27 C 0.5210(6) 0.5147(3) 0.0863(2)
H22 H 0.59980 0.49820 0.07080
C28 C 0.4259(6) 0.4558(3) 0.0938(2)
H23 H 0.43920 0.39890 0.08290
C29 C 0.3124(6) 0.4786(3) 0.1169(2)
H24 H 0.24730 0.43770 0.12150
C30 C 0.2927(5) 0.5612(3) 0.1336(2)
H25 H 0.21540 0.57660 0.15090
C31 C 0.2080(5) 0.7445(3) 0.18994(19)
C32 C 0.0817(5) 0.7219(3) 0.1580(2)
H26 H 0.06550 0.70610 0.11060
C33 C -0.0224(5) 0.7220(3) 0.1940(2)
H27 H -0.10980 0.70680 0.17160
C34 C 0.0032(5) 0.7447(3) 0.2637(2)
H28 H -0.06760 0.74500 0.28880
C35 C 0.1293(5) 0.7667(3) 0.2969(2)
H29 H 0.14490 0.78210 0.34440
C36 C 0.2344(5) 0.7665(3) 0.26067(19)
H30 H 0.32200 0.78090 0.28330
N1 N 0.6914(5) 0.6703(3) 0.2520(2)
C37 C 0.5135(5) 0.7756(3) 0.19568(19)
C38 C 0.6111(5) 0.7173(3) 0.2265(2)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
As 1.21
Br 1.21
N 0.68
|
1100625.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 12:25:08 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176951 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100625.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100625
loop_
_publ_author_name
'Chitsaz, Soheila'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Asymmetrisch substituierte Iminiumsalze [Et~3~PNAsPh~3~]X und ihre
Reaktion mit Acetonitril. Kristallstrukturen von [Et~3~PNAsPh~3~]X
(X = Cl, Br), [(Ph~3~As)~2~CCN]Br und [(Ph~3~As)~2~CCN(SnBr~5~)]
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1341
_journal_page_last 1346
_journal_paper_doi
10.1002/(sici)1521-3749(199808)624:8<1341::aid-zaac1341>3.0.co;2-v
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C38 H30 As2 Br5 N Sn'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 101.54(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.676(1)
_cell_length_b 22.562(1)
_cell_length_c 17.987(2)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C38 H30 As2 Br5 N1 Sn1'
_cod_database_code 1100625
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Sn1 Sn 0.45475(8) 0.25766(3) 0.30565(4)
Br1 Br 0.41117(11) 0.24045(4) 0.43949(5)
Br2 Br 0.71054(11) 0.22222(4) 0.34639(6)
Br3 Br 0.52096(12) 0.36697(4) 0.33649(6)
Br4 Br 0.48670(12) 0.26628(5) 0.16902(6)
Br5 Br 0.18824(11) 0.27638(4) 0.25465(5)
C1 C 0.1887(9) 0.0841(4) 0.2711(5)
C2 C 0.2989(11) 0.1255(4) 0.2830(5)
N1 N 0.3934(9) 0.1589(3) 0.2898(4)
As1 As 0.12218(11) 0.05596(4) 0.35368(5)
As2 As 0.11729(10) 0.06837(4) 0.16775(5)
C3 C 0.1235(9) 0.1164(3) 0.4267(4)
C4 C 0.0708(10) 0.1721(4) 0.4048(5)
H1 H 0.0413(10) 0.1812(4) 0.3525(5)
C5 C 0.0610(11) 0.2151(4) 0.4592(5)
H2 H 0.0221(11) 0.2529(4) 0.4440(5)
C6 C 0.1064(11) 0.2030(4) 0.5332(5)
H3 H 0.0972(11) 0.2322(4) 0.5699(5)
C7 C 0.1681(13) 0.1475(4) 0.5575(5)
H4 H 0.2038(13) 0.1397(4) 0.6097(5)
C8 C 0.1744(11) 0.1057(4) 0.5037(6)
H5 H 0.2146(11) 0.0681(4) 0.5191(6)
C9 C 0.2326(13) -0.0092(4) 0.3977(5)
C10 C 0.3576(13) -0.0226(4) 0.3778(6)
H6 H 0.3892(13) 0.0014(4) 0.3411(6)
C11 C 0.4381(16) -0.0688(6) 0.4084(7)
H7 H 0.5253(16) -0.0769(6) 0.3938(7)
C12 C 0.3934(18) -0.1030(6) 0.4596(9)
H8 H 0.4492(18) -0.1360(6) 0.4799(9)
C13 C 0.2750(17) -0.0926(4) 0.4829(7)
H9 H 0.2484(17) -0.1173(4) 0.5204(7)
C14 C 0.1883(12) -0.0454(4) 0.4528(5)
H10 H 0.1022(12) -0.0378(4) 0.4688(5)
C15 C -0.0666(11) 0.0293(4) 0.3225(5)
C16 C -0.0998(11) -0.0300(3) 0.3093(5)
H11 H -0.0273(11) -0.0591(3) 0.3189(5)
C17 C -0.2364(11) -0.0470(4) 0.2824(5)
H12 H -0.2572(11) -0.0876(4) 0.2716(5)
C18 C -0.3449(12) -0.0059(4) 0.2705(5)
H13 H -0.4397(12) -0.0182(4) 0.2531(5)
C19 C -0.3130(11) 0.0535(4) 0.2844(6)
H14 H -0.3859(11) 0.0824(4) 0.2768(6)
C20 C -0.1759(12) 0.0699(5) 0.3091(6)
H15 H -0.1547(12) 0.1108(5) 0.3175(6)
C21 C 0.0341(11) -0.0074(4) 0.1543(5)
C22 C 0.1077(11) -0.0584(4) 0.1829(5)
H16 H 0.2005(11) -0.0555(4) 0.2125(5)
C23 C 0.0439(14) -0.1135(4) 0.1677(6)
H17 H 0.0929(14) -0.1483(4) 0.1876(6)
C24 C -0.0919(13) -0.1179(4) 0.1231(6)
H18 H -0.1322(13) -0.1558(4) 0.1101(6)
C25 C -0.1657(12) -0.0687(5) 0.0988(6)
H19 H -0.2608(12) -0.0715(5) 0.0723(6)
C26 C -0.1021(11) -0.0146(4) 0.1126(5)
H20 H -0.1534(11) 0.0197(4) 0.0927(5)
C27 C 0.2735(10) 0.0713(4) 0.1198(4)
C28 C 0.3216(12) 0.1255(4) 0.0988(5)
H21 H 0.2710(12) 0.1608(4) 0.1043(5)
C29 C 0.4429(12) 0.1279(4) 0.0699(5)
H22 H 0.4736(12) 0.1652(4) 0.0547(5)
C30 C 0.5192(12) 0.0796(5) 0.0625(5)
H23 H 0.6038(12) 0.0823(5) 0.0435(5)
C31 C 0.4714(14) 0.0264(5) 0.0831(6)
H24 H 0.5235(14) -0.0085(5) 0.0778(6)
C32 C 0.3506(12) 0.0220(4) 0.1110(6)
H25 H 0.3197(12) -0.0157(4) 0.1245(6)
C33 C -0.0179(9) 0.1250(4) 0.1203(5)
C34 C -0.075(1) 0.1656(4) 0.1650(5)
H26 H -0.0482(10) 0.1643(4) 0.2188(5)
C35 C -0.1713(12) 0.2077(4) 0.1298(6)
H27 H -0.2055(12) 0.2374(4) 0.1590(6)
C36 C -0.2156(12) 0.2060(5) 0.0537(6)
H28 H -0.2849(12) 0.2334(5) 0.0299(6)
C37 C -0.1621(11) 0.1652(4) 0.0099(6)
H29 H -0.1938(11) 0.1651(4) -0.0436(6)
C38 C -0.0639(10) 0.1248(4) 0.0431(5)
H30 H -0.0275(10) 0.0966(4) 0.0128(5)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
As 1.21
Br 1.21
N 0.68
Sn 1.46
|
1100626.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 11:12:28 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176946 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100626.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100626
loop_
_publ_author_name
'Riese, Ulrike'
'Harms, Klaus'
'Neum\"uller, Bernhard'
'Dehnicke, Kurt'
_publ_section_title
;
Cobalt(II)-organische Phosphaniminato-Komplexe mit Heterocuban-Struktur.
Kristallstrukturen von [CoBr(NPR~3~)]~4~ mit R = Me, Et,
[Co(C\\tb C-CMe3)(NPMe3)]~4~ und [Co(C\\tb C-SiMe~3~)(NPEt~3~)]~4~
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1279
_journal_page_last 1284
_journal_paper_doi
10.1002/(SICI)1521-3749(199808)624:8<1279::AID-ZAAC1279>3.0.CO;2-K
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C14 H39 Br4 Co4 N5 P4'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 102.498(8)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.8662(7)
_cell_length_b 20.7898(11)
_cell_length_c 17.8309(13)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100626
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Co1 Co 0.22693(6) 0.13323(3) 0.29197(4)
Br1 Br 0.13160(6) 0.12019(4) 0.40180(4)
P1 P 0.08385(13) 0.01258(7) 0.19260(9)
N1 N 0.1800(4) 0.07440(18) 0.1988(2)
Co2 Co 0.16035(6) 0.15493(3) 0.13298(4)
Br2 Br -0.03027(5) 0.17022(3) 0.02922(3)
N2 N 0.3653(4) 0.15342(19) 0.1266(2)
P2 P 0.42635(15) 0.15839(8) 0.05177(9)
Co3 Co 0.38559(6) 0.07535(3) 0.19816(4)
Br3 Br 0.51644(6) -0.01909(3) 0.18686(4)
P3 P 0.55306(12) 0.11733(7) 0.36845(8)
N3 N 0.4330(4) 0.12950(18) 0.2946(2)
Co4 Co 0.40389(6) 0.20851(3) 0.22417(4)
Br4 Br 0.56034(5) 0.29643(3) 0.24907(4)
P4 P 0.11062(12) 0.27452(6) 0.24247(8)
N4 N 0.1982(3) 0.21400(18) 0.2259(2)
C1 C 0.1488(6) -0.0429(3) 0.2676(4)
H1 H 0.14920 -0.02280 0.31730
H2 H 0.24370 -0.05540 0.26530
H3 H 0.08950 -0.08120 0.26140
C2 C 0.0749(8) -0.0306(3) 0.1049(4)
H4 H 0.02140 -0.00570 0.06200
H5 H 0.02940 -0.07220 0.10780
H6 H 0.16900 -0.03780 0.09700
C3 C -0.0893(6) 0.0328(4) 0.1979(5)
H7 H -0.08870 0.05420 0.24690
H8 H -0.14550 -0.00640 0.19410
H9 H -0.12910 0.06190 0.15550
C4 C 0.3491(10) 0.1019(5) -0.0197(5)
H10 H 0.36580 0.05820 0.00090
H11 H 0.39010 0.10660 -0.06480
H12 H 0.24890 0.10980 -0.03450
C5 C 0.3998(10) 0.2360(4) 0.0067(5)
H13 H 0.43400 0.26950 0.04470
H14 H 0.30050 0.24260 -0.01440
H15 H 0.45030 0.23830 -0.03490
C6 C 0.6090(7) 0.1432(5) 0.0714(5)
H16 H 0.65750 0.17600 0.10670
H17 H 0.64180 0.14460 0.02330
H18 H 0.62790 0.10060 0.09480
C7 C 0.5432(6) 0.0390(3) 0.4078(4)
H19 H 0.45460 0.03420 0.42360
H20 H 0.61990 0.03320 0.45240
H21 H 0.54980 0.00650 0.36890
C8 C 0.5466(6) 0.1728(3) 0.4435(3)
H22 H 0.45840 0.16800 0.45960
H23 H 0.55430 0.21680 0.42490
H24 H 0.62370 0.16430 0.48720
C9 C 0.7208(5) 0.1237(3) 0.3465(4)
H25 H 0.72960 0.09160 0.30760
H26 H 0.79240 0.11600 0.39310
H27 H 0.73260 0.16680 0.32680
C10 C -0.0624(5) 0.2528(3) 0.2505(4)
H28 H -0.11170 0.23320 0.20230
H29 H -0.11230 0.29140 0.26090
H30 H -0.05750 0.22200 0.29260
C11 C 0.1891(6) 0.3134(3) 0.3309(3)
H31 H 0.28360 0.32690 0.32920
H32 H 0.19270 0.28340 0.37370
H33 H 0.13410 0.35120 0.33830
C12 C 0.0890(6) 0.3327(3) 0.1667(4)
H34 H 0.18040 0.34680 0.15990
H35 H 0.03760 0.36980 0.18000
H36 H 0.03730 0.31340 0.11890
N5 N 0.8594(8) 0.0885(4) 0.5426(4)
C13 C 0.9724(9) 0.0789(4) 0.5670(4)
C14 C 1.1145(9) 0.0667(5) 0.5990(5)
H37 H 1.12570 0.05430 0.65310
H38 H 1.16890 0.10560 0.59550
H39 H 1.14740 0.03170 0.57070
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Br 1.21
Co 1.16
N 0.68
P 1.05
|
1100627.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 11:12:28 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176946 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100627.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100627
loop_
_publ_author_name
'Riese, Ulrike'
'Harms, Klaus'
'Neum\"uller, Bernhard'
'Dehnicke, Kurt'
_publ_section_title
;
Cobalt(II)-organische Phosphaniminato-Komplexe mit Heterocuban-Struktur.
Kristallstrukturen von [CoBr(NPR~3~)]~4~ mit R = Me, Et,
[Co(C\\tb C-CMe3)(NPMe3)]~4~ und [Co(C\\tb C-SiMe~3~)(NPEt~3~)]~4~
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1279
_journal_page_last 1284
_journal_paper_doi
10.1002/(SICI)1521-3749(199808)624:8<1279::AID-ZAAC1279>3.0.CO;2-K
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C24 H60 Br4 Co4 N4 P4'
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 115.45(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 21.035(2)
_cell_length_b 11.112(2)
_cell_length_c 19.743(2)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100627
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2+y,z
3 x,-y,1/2+z
4 1/2+x,1/2-y,1/2+z
5 -x,-y,-z
6 -1/2-x,-1/2-y,-z
7 -x,y,-1/2-z
8 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Co1 Co -0.05013(6) 0.16058(11) 0.17563(6)
Co2 Co 0.05305(6) 0.33844(11) 0.22554(6)
Br1 Br -0.11010(5) 0.02420(9) 0.07592(5)
Br2 Br 0.11880(5) 0.47068(9) 0.18623(5)
N1 N 0.0580(3) 0.1551(6) 0.2249(3)
P1 P 0.10596(10) 0.0672(2) 0.20331(11)
C1 C 0.0854(5) 0.0668(8) 0.1054(5)
H1 H 0.1077(5) -0.0038(8) 0.0950(5)
H2 H 0.0344(5) 0.0571(8) 0.0771(5)
C2 C 0.1076(7) 0.1772(11) 0.0760(6)
H3 H 0.0941(7) 0.1678(11) 0.0227(6)
H4 H 0.1583(7) 0.1867(11) 0.1022(6)
H5 H 0.0847(7) 0.2477(11) 0.0842(6)
C3 C 0.1986(4) 0.1051(9) 0.2512(5)
H6 H 0.2245(4) 0.0536(9) 0.2314(5)
H7 H 0.2046(4) 0.1884(9) 0.2388(5)
C4 C 0.2318(5) 0.0925(10) 0.3357(5)
H8 H 0.2811(5) 0.1147(10) 0.3558(5)
H9 H 0.2277(5) 0.0097(10) 0.3490(5)
H10 H 0.2077(5) 0.1449(10) 0.3564(5)
C5 C 0.0971(5) -0.0856(8) 0.2273(5)
H11 H 0.1031(5) -0.0873(8) 0.2793(5)
H12 H 0.0490(5) -0.1124(8) 0.1954(5)
C6 C 0.1480(7) -0.1754(10) 0.2196(7)
H13 H 0.1389(7) -0.2548(10) 0.2338(7)
H14 H 0.1959(7) -0.1517(10) 0.2521(7)
H15 H 0.1417(7) -0.1769(10) 0.1680(7)
N2 N -0.0548(3) 0.3435(6) 0.1704(3)
P2 P -0.10081(10) 0.4302(2) 0.10243(10)
C7 C -0.1919(4) 0.3864(8) 0.0580(4)
H16 H -0.2154(4) 0.4328(8) 0.0115(4)
H17 H -0.1945(4) 0.3013(8) 0.0441(4)
C8 C -0.2329(4) 0.404(1) 0.1055(5)
H18 H -0.2812(4) 0.3781(10) 0.0771(5)
H19 H -0.2321(4) 0.4884(10) 0.1184(5)
H20 H -0.2112(4) 0.3566(10) 0.1510(5)
C9 C -0.0998(5) 0.5819(8) 0.1309(5)
H21 H -0.1113(5) 0.5824(8) 0.1740(5)
H22 H -0.0517(5) 0.6129(8) 0.1483(5)
C10 C -0.1459(9) 0.6693(13) 0.0743(9)
H23 H -0.1412(9) 0.7491(13) 0.0960(9)
H24 H -0.1940(9) 0.6417(13) 0.0577(9)
H25 H -0.1342(9) 0.6723(13) 0.0319(9)
C11? C -0.0423(28) 0.6563(55) 0.1545(28)
H26? H -0.0521(28) 0.7359(55) 0.1678(28)
H27? H -0.0273(28) 0.6628(55) 0.1145(28)
H28? H -0.0053(28) 0.6188(55) 0.1979(28)
C12 C -0.0715(5) 0.4341(8) 0.0290(5)
H29 H -0.1013(5) 0.4912(8) -0.0094(5)
H30 H -0.0233(5) 0.4656(8) 0.0502(5)
C13 C -0.0725(5) 0.3175(9) -0.0081(5)
H31 H -0.0559(5) 0.3294(9) -0.0465(5)
H32 H -0.1202(5) 0.2863(9) -0.0309(5)
H33 H -0.0420(5) 0.2606(9) 0.0289(5)
Co1F* Co 0.05013(6) 0.16058(11) 0.32437(6)
Br1F* Br 0.11010(5) 0.02420(9) 0.42408(5)
N1F* N -0.0580(3) 0.1551(6) 0.2751(3)
N2F* N 0.0548(3) 0.3435(6) 0.3296(3)
Co2F* Co -0.05305(6) 0.33844(11) 0.27446(6)
Br2F* Br -0.11880(5) 0.47068(9) 0.31377(5)
P1F* P -0.10596(10) 0.0672(2) 0.29669(11)
C1F* C -0.0854(5) 0.0668(8) 0.3946(5)
H1F* H -0.1077(5) -0.0038(8) 0.4050(5)
H2F* H -0.0344(5) 0.0571(8) 0.4229(5)
C2F* C -0.1076(7) 0.1772(11) 0.4240(6)
H3F* H -0.0941(7) 0.1678(11) 0.4773(6)
H4F* H -0.1583(7) 0.1867(11) 0.3978(6)
H5F* H -0.0847(7) 0.2477(11) 0.4158(6)
C3F* C -0.1986(4) 0.1051(9) 0.2488(5)
H6F* H -0.2245(4) 0.0536(9) 0.2686(5)
H7F* H -0.2046(4) 0.1884(9) 0.2612(5)
C4F* C -0.2318(5) 0.0925(10) 0.1643(5)
H8F* H -0.2811(5) 0.1147(10) 0.1442(5)
H9F* H -0.2277(5) 0.0097(10) 0.1510(5)
H10F* H -0.2077(5) 0.1449(10) 0.1436(5)
C5F* C -0.0971(5) -0.0856(8) 0.2727(5)
H11F* H -0.1031(5) -0.0873(8) 0.2207(5)
H12F* H -0.0490(5) -0.1124(8) 0.3046(5)
C6F* C -0.1480(7) -0.1754(10) 0.2804(7)
H13F* H -0.1389(7) -0.2548(10) 0.2662(7)
H14F* H -0.1959(7) -0.1517(10) 0.2479(7)
H15F* H -0.1417(7) -0.1769(10) 0.3320(7)
P2F* P 0.10081(10) 0.4302(2) 0.39757(10)
C7F* C 0.1919(4) 0.3864(8) 0.4420(4)
H16F* H 0.2154(4) 0.4328(8) 0.4885(4)
H17F* H 0.1945(4) 0.3013(8) 0.4559(4)
C8F* C 0.2329(4) 0.404(1) 0.3945(5)
H18F* H 0.2812(4) 0.3781(10) 0.4229(5)
H19F* H 0.2321(4) 0.4884(10) 0.3816(5)
H20F* H 0.2112(4) 0.3566(10) 0.3490(5)
C9F* C 0.0998(5) 0.5819(8) 0.3691(5)
H21F* H 0.1113(5) 0.5824(8) 0.3260(5)
H22F* H 0.0517(5) 0.6129(8) 0.3517(5)
C10F* C 0.1459(9) 0.6693(13) 0.4257(9)
H23F* H 0.1412(9) 0.7491(13) 0.4040(9)
H24F* H 0.1940(9) 0.6417(13) 0.4423(9)
H25F* H 0.1342(9) 0.6723(13) 0.4681(9)
C12F* C 0.0715(5) 0.4341(8) 0.4710(5)
H29F* H 0.1013(5) 0.4912(8) 0.5094(5)
H30F* H 0.0233(5) 0.4656(8) 0.4498(5)
C13F* C 0.0725(5) 0.3175(9) 0.5081(5)
H31F* H 0.0559(5) 0.3294(9) 0.5465(5)
H32F* H 0.1202(5) 0.2863(9) 0.5309(5)
H33F* H 0.0420(5) 0.2606(9) 0.4711(5)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Br 1.21
Co 1.15
N 0.68
P 1.05
|
1100628.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 11:12:28 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176946 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100628.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100628
loop_
_publ_author_name
'Riese, Ulrike'
'Harms, Klaus'
'Neum\"uller, Bernhard'
'Dehnicke, Kurt'
_publ_section_title
;
Cobalt(II)-organische Phosphaniminato-Komplexe mit Heterocuban-Struktur.
Kristallstrukturen von [CoBr(NPR~3~)]~4~ mit R = Me, Et,
[Co(C\\tb C-CMe3)(NPMe3)]~4~ und [Co(C\\tb C-SiMe~3~)(NPEt~3~)]~4~
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1279
_journal_page_last 1284
_journal_paper_doi
10.1002/(SICI)1521-3749(199808)624:8<1279::AID-ZAAC1279>3.0.CO;2-K
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C36 H72 Co4 N4 P4'
_space_group_IT_number 68
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-C 2a 2ac'
_symmetry_space_group_name_H-M 'C c c a :2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 18.5424(11)
_cell_length_b 27.4587(13)
_cell_length_c 9.6347(5)
_cod_original_sg_symbol_H-M 'C c c a'
_cod_database_code 1100628
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2+y,z
3 1/2+x,y,-z
4 x,-y,1/2+z
5 1/2-x,y,1/2+z
6 x,1/2+y,-z
7 1/2+x,1/2-y,1/2+z
8 -x,1/2+y,1/2+z
9 -x,-y,-z
10 -1/2-x,-1/2-y,-z
11 -1/2-x,-y,z
12 -x,y,-1/2-z
13 -1/2+x,-y,-1/2-z
14 -x,-1/2-y,z
15 -1/2-x,-1/2+y,-1/2-z
16 x,-1/2-y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Co1 Co 0.05307(2) 0.28735(1) 0.14578(5)
P1 P 0.11023(6) 0.31888(4) 0.44715(12)
N1 N 0.05718(15) 0.28635(9) 0.3595(3)
C1 C 0.1012(2) 0.34075(13) 0.0451(4)
C2 C 0.1184(2) 0.37999(13) -0.0011(4)
C3 C 0.1354(2) 0.42936(14) -0.0511(5)
C4? C 0.1744(16) 0.4328(9) -0.185(2)
H1? H 0.13970 0.43110 -0.26210
H2? H 0.20880 0.40590 -0.19300
H3? H 0.20040 0.46380 -0.18990
C5? C 0.0729(7) 0.4649(4) -0.029(2)
H4? H 0.03020 0.45320 -0.07880
H5? H 0.08640 0.49710 -0.06450
H6? H 0.06200 0.46730 0.07030
C6? C 0.1962(7) 0.4488(4) 0.0537(15)
H7? H 0.24070 0.43020 0.03980
H8? H 0.17960 0.44470 0.14950
H9? H 0.20540 0.48340 0.03580
C7 C 0.0947(2) 0.38277(13) 0.4226(5)
H10 H 0.04400 0.39020 0.44140
H11 H 0.10630 0.39170 0.32670
H12 H 0.12540 0.40130 0.48640
C8 C 0.2027(3) 0.3089(2) 0.4004(10)
H13 H 0.21240 0.27380 0.39690
H14 H 0.23420 0.32410 0.46970
H15 H 0.21210 0.32330 0.30910
C9 C 0.1025(7) 0.3078(3) 0.6273(6)
H16 H 0.05390 0.31660 0.65850
H17 H 0.13810 0.32750 0.67740
H18 H 0.11110 0.27320 0.64600
C10 C 0.0752(5) 0.4416(4) -0.1616(11)
H19 H 0.07570 0.41690 -0.23510
H20 H 0.08470 0.47370 -0.20210
H21 H 0.02790 0.44180 -0.11630
C11 C 0.1297(8) 0.4654(3) 0.0625(10)
H22 H 0.08190 0.46300 0.10550
H23 H 0.13660 0.49820 0.02510
H24 H 0.16690 0.45870 0.13230
C12 C 0.2041(8) 0.4275(6) -0.1331(18)
H25 H 0.19970 0.40290 -0.20650
H26 H 0.24420 0.41880 -0.07150
H27 H 0.21330 0.45940 -0.17490
Co1K* Co -0.05307(2) 0.28735(1) 0.35422(5)
N1K* N -0.05718(15) 0.28635(9) 0.1405(3)
N1O* N 0.05718(15) 0.21365(9) 0.1405(3)
Co1O* Co 0.05307(2) 0.21265(1) 0.35422(5)
N1M* N -0.05718(15) 0.21365(9) 0.3595(3)
Co1M* Co -0.05307(2) 0.21265(1) 0.14578(5)
P1O* P 0.11023(6) 0.18112(4) 0.05285(12)
C7O* C 0.0947(2) 0.11723(13) 0.0774(5)
H10O* H 0.04400 0.10980 0.05860
H11O* H 0.10630 0.10830 0.17330
H12O* H 0.12540 0.09870 0.01360
C8O* C 0.2027(3) 0.1911(2) 0.0996(10)
H13O* H 0.21240 0.22620 0.10310
H14O* H 0.23420 0.17590 0.03030
H15O* H 0.21210 0.17670 0.19090
C9O* C 0.1025(7) 0.1922(3) -0.1273(6)
H16O* H 0.05390 0.18340 -0.15850
H17O* H 0.13810 0.17250 -0.17740
H18O* H 0.11110 0.22680 -0.14600
P1K* P -0.11023(6) 0.31888(4) 0.05285(12)
C7K* C -0.0947(2) 0.38277(13) 0.0774(5)
H10K* H -0.04400 0.39020 0.05860
H11K* H -0.10630 0.39170 0.17330
H12K* H -0.12540 0.40130 0.01360
C8K* C -0.2027(3) 0.3089(2) 0.0996(10)
H13K* H -0.21240 0.27380 0.10310
H14K* H -0.23420 0.32410 0.03030
H15K* H -0.21210 0.32330 0.19090
C9K* C -0.1025(7) 0.3078(3) -0.1273(6)
H16K* H -0.05390 0.31660 -0.15850
H17K* H -0.13810 0.32750 -0.17740
H18K* H -0.11110 0.27320 -0.14600
C1M* C -0.1012(2) 0.15925(13) 0.0451(4)
C2M* C -0.1184(2) 0.12001(13) -0.0011(4)
C3M* C -0.1354(2) 0.07064(14) -0.0511(5)
C10M* C -0.0752(5) 0.0584(4) -0.1616(11)
H19M* H -0.07570 0.08310 -0.23510
H20M* H -0.08470 0.02630 -0.20210
H21M* H -0.02790 0.05820 -0.11630
C11M* C -0.1297(8) 0.0346(3) 0.0625(10)
H22M* H -0.08190 0.03700 0.10550
H23M* H -0.13660 0.00180 0.02510
H24M* H -0.16690 0.04130 0.13230
C12M* C -0.2041(8) 0.0725(6) -0.1331(18)
H25M* H -0.19970 0.09710 -0.20650
H26M* H -0.24420 0.08120 -0.07150
H27M* H -0.21330 0.04060 -0.17490
C1K* C -0.1012(2) 0.34075(13) 0.4549(4)
C2K* C -0.1184(2) 0.37999(13) 0.5011(4)
C3K* C -0.1354(2) 0.42936(14) 0.5511(5)
C10K* C -0.0752(5) 0.4416(4) 0.6616(11)
H19K* H -0.07570 0.41690 0.73510
H20K* H -0.08470 0.47370 0.70210
H21K* H -0.02790 0.44180 0.61630
C11K* C -0.1297(8) 0.4654(3) 0.4375(10)
H22K* H -0.08190 0.46300 0.39450
H23K* H -0.13660 0.49820 0.47490
H24K* H -0.16690 0.45870 0.36770
C12K* C -0.2041(8) 0.4275(6) 0.6331(18)
H25K* H -0.19970 0.40290 0.70650
H26K* H -0.24420 0.41880 0.57150
H27K* H -0.21330 0.45940 0.67490
P1M* P -0.11023(6) 0.18112(4) 0.44715(12)
C7M* C -0.0947(2) 0.11723(13) 0.4226(5)
H10M* H -0.04400 0.10980 0.44140
H11M* H -0.10630 0.10830 0.32670
H12M* H -0.12540 0.09870 0.48640
C8M* C -0.2027(3) 0.1911(2) 0.4004(10)
H13M* H -0.21240 0.22620 0.39690
H14M* H -0.23420 0.17590 0.46970
H15M* H -0.21210 0.17670 0.30910
C9M* C -0.1025(7) 0.1922(3) 0.6273(6)
H16M* H -0.05390 0.18340 0.65850
H17M* H -0.13810 0.17250 0.67740
H18M* H -0.11110 0.22680 0.64600
C1O* C 0.1012(2) 0.15925(13) 0.4549(4)
C2O* C 0.1184(2) 0.12001(13) 0.5011(4)
C3O* C 0.1354(2) 0.07064(14) 0.5511(5)
C10O* C 0.0752(5) 0.0584(4) 0.6616(11)
H19O* H 0.07570 0.08310 0.73510
H20O* H 0.08470 0.02630 0.70210
H21O* H 0.02790 0.05820 0.61630
C11O* C 0.1297(8) 0.0346(3) 0.4375(10)
H22O* H 0.08190 0.03700 0.39450
H23O* H 0.13660 0.00180 0.47490
H24O* H 0.16690 0.04130 0.36770
C12O* C 0.2041(8) 0.0725(6) 0.6331(18)
H25O* H 0.19970 0.09710 0.70650
H26O* H 0.24420 0.08120 0.57150
H27O* H 0.21330 0.04060 0.67490
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Co 1.20
N 0.68
P 1.05
|
1100629.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 11:12:28 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176946 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100629.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100629
loop_
_publ_author_name
'Riese, Ulrike'
'Harms, Klaus'
'Neum\"uller, Bernhard'
'Dehnicke, Kurt'
_publ_section_title
;
Cobalt(II)-organische Phosphaniminato-Komplexe mit Heterocuban-Struktur.
Kristallstrukturen von [CoBr(NPR~3~)]~4~ mit R = Me, Et,
[Co(C\\tb C-CMe3)(NPMe3)]~4~ und [Co(C\\tb C-SiMe~3~)(NPEt~3~)]~4~
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1279
_journal_page_last 1284
_journal_paper_doi
10.1002/(SICI)1521-3749(199808)624:8<1279::AID-ZAAC1279>3.0.CO;2-K
_journal_volume 624
_journal_year 1998
_chemical_formula_sum 'C44 H96 Co4 N4 P4 Si4'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 94.550(8)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.9708(8)
_cell_length_b 26.193(2)
_cell_length_c 22.3454(17)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100629
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Co1 Co 0.40432(6) 0.35152(3) 0.80550(3)
Si1 Si 0.24358(16) 0.50617(6) 0.89809(7)
P1 P 0.30231(14) 0.39511(6) 0.67693(6)
N1 N 0.3895(3) 0.35455(16) 0.71267(16)
C1 C 0.3213(5) 0.4042(2) 0.8489(2)
Co2 Co 0.57624(6) 0.35140(3) 0.71839(3)
Si2 Si 0.81770(17) 0.48572(6) 0.62543(7)
P2 P 0.31631(15) 0.23673(6) 0.84474(6)
N2 N 0.3913(4) 0.27383(17) 0.80458(16)
C2 C 0.2813(5) 0.4434(2) 0.8717(2)
Co3 Co 0.38858(7) 0.27724(3) 0.71264(3)
Si3 Si 0.19130(15) 0.14448(7) 0.57995(7)
P3 P 0.68747(15) 0.38478(6) 0.85204(6)
N3 N 0.5904(4) 0.35241(17) 0.81022(16)
C3 C 0.6772(5) 0.3968(2) 0.6736(2)
Co4 Co 0.57934(7) 0.27537(3) 0.80641(3)
Si4 Si 0.81581(17) 0.15416(7) 0.94176(7)
P4 P 0.66290(15) 0.24078(6) 0.67643(7)
N4 N 0.5758(4) 0.27342(16) 0.71513(17)
C4 C 0.7379(5) 0.4305(2) 0.6502(2)
C5 C 0.2898(5) 0.2320(2) 0.6584(2)
C6 C 0.2398(5) 0.1988(2) 0.6250(2)
C7 C 0.6808(6) 0.2315(2) 0.8601(3)
C8 C 0.7400(6) 0.2023(2) 0.8943(3)
C9 C 0.1449(6) 0.5036(3) 0.9619(3)
H1 H 0.18880 0.48640 0.99600
H2 H 0.06980 0.48480 0.94970
H3 H 0.12390 0.53840 0.97350
C10 C 0.3862(6) 0.5407(3) 0.9224(3)
H4 H 0.42620 0.52390 0.95790
H5 H 0.36670 0.57600 0.93230
H6 H 0.44110 0.54030 0.88990
C11 C 0.1633(6) 0.5413(2) 0.8343(3)
H7 H 0.08720 0.52340 0.82120
H8 H 0.21590 0.54290 0.80090
H9 H 0.14430 0.57600 0.84710
C12 C 0.8938(6) 0.5181(3) 0.6926(2)
H10 H 0.83180 0.52950 0.71890
H11 H 0.93990 0.54770 0.67980
H12 H 0.94980 0.49420 0.71440
C13 C 0.9355(6) 0.4670(2) 0.5738(2)
H13 H 0.89560 0.45970 0.53390
H14 H 0.97880 0.43650 0.58950
H15 H 0.99390 0.49510 0.57090
C14 C 0.7075(8) 0.5293(3) 0.5859(3)
H16 H 0.64260 0.53770 0.61200
H17 H 0.67160 0.51290 0.54930
H18 H 0.74940 0.56070 0.57530
C15 C 0.3193(6) 0.1252(3) 0.5350(3)
H19 H 0.34960 0.15510 0.51450
H20 H 0.29020 0.09960 0.50520
H21 H 0.38550 0.11060 0.56170
C16 C 0.1539(7) 0.0912(2) 0.6303(3)
H22 H 0.09240 0.10260 0.65690
H23 H 0.22800 0.08050 0.65450
H24 H 0.12150 0.06230 0.60610
C17 C 0.0539(6) 0.1584(3) 0.5290(3)
H25 H -0.01740 0.16190 0.55250
H26 H 0.04000 0.13040 0.50010
H27 H 0.06620 0.19030 0.50730
C18 C 0.9164(7) 0.1164(3) 0.8964(3)
H28 H 0.97480 0.13910 0.87880
H29 H 0.86680 0.09880 0.86420
H30 H 0.96090 0.09110 0.92200
C19 C 0.6955(6) 0.1133(3) 0.9711(3)
H31 H 0.63490 0.13480 0.98880
H32 H 0.73290 0.09010 1.00170
H33 H 0.65530 0.09320 0.93810
C20 C 0.9122(7) 0.1839(3) 1.0047(3)
H34 H 0.95530 0.21350 0.98970
H35 H 0.97190 0.15890 1.02160
H36 H 0.86010 0.19500 1.03590
C21 C 0.3545(6) 0.4596(2) 0.6915(2)
H37 H 0.35320 0.46610 0.73510
H38 H 0.44090 0.46170 0.68170
C22 C 0.2843(7) 0.5027(2) 0.6582(3)
H39 H 0.32550 0.53530 0.66750
H40 H 0.20080 0.50410 0.67090
H41 H 0.28130 0.49650 0.61490
C23 C 0.2920(6) 0.3862(2) 0.5970(2)
H42 H 0.27220 0.34990 0.58820
H43 H 0.22310 0.40700 0.57910
C24 C 0.4060(6) 0.4001(3) 0.5664(3)
H44 H 0.39560 0.39000 0.52410
H45 H 0.47660 0.38220 0.58610
H46 H 0.41960 0.43700 0.56920
C25 C 0.1486(5) 0.3935(3) 0.6987(3)
H47 H 0.15150 0.39760 0.74280
H48 H 0.10430 0.42330 0.68050
C26 C 0.0757(5) 0.3462(3) 0.6819(3)
H49 H -0.00720 0.34990 0.69480
H50 H 0.11520 0.31650 0.70170
H51 H 0.07150 0.34150 0.63830
C27 C 0.3360(6) 0.2529(2) 0.9226(2)
H52 H 0.42380 0.24910 0.93580
H53 H 0.31510 0.28940 0.92660
C28 C 0.2621(6) 0.2223(3) 0.9665(2)
H54 H 0.28450 0.23370 1.00770
H55 H 0.28050 0.18580 0.96300
H56 H 0.17450 0.22790 0.95660
C29 C 0.1552(6) 0.2371(3) 0.8240(3)
H57 H 0.14180 0.23040 0.78040
H58 H 0.11700 0.20880 0.84520
C30 C 0.0921(6) 0.2859(3) 0.8379(3)
H59 H 0.00760 0.28500 0.82000
H60 H 0.13530 0.31470 0.82120
H61 H 0.09200 0.28990 0.88150
C31 C 0.3645(7) 0.1702(2) 0.8414(3)
H62 H 0.45470 0.16890 0.84840
H63 H 0.33020 0.15150 0.87470
C32 C 0.3287(8) 0.1433(3) 0.7852(3)
H64 H 0.37210 0.11060 0.78460
H65 H 0.34970 0.16420 0.75110
H66 H 0.24030 0.13710 0.78220
C33 C 0.7184(6) 0.3577(3) 0.9267(2)
H67 H 0.76430 0.32550 0.92310
H68 H 0.77180 0.38160 0.95100
C34 C 0.6103(6) 0.3472(3) 0.9589(2)
H69 H 0.63580 0.33730 1.00030
H70 H 0.56350 0.31930 0.93890
H71 H 0.55920 0.37780 0.95910
C35 C 0.6415(6) 0.4488(2) 0.8639(3)
H72 H 0.56370 0.44830 0.88350
H73 H 0.70370 0.46530 0.89200
C36 C 0.6248(7) 0.4798(3) 0.8098(3)
H74 H 0.58770 0.51260 0.81940
H75 H 0.57110 0.46190 0.77960
H76 H 0.70430 0.48590 0.79400
C37 C 0.8346(5) 0.3867(2) 0.8212(3)
H77 H 0.86380 0.35110 0.81750
H78 H 0.82290 0.40090 0.78010
C38 C 0.9351(6) 0.4172(3) 0.8560(3)
H79 H 1.01060 0.41510 0.83550
H80 H 0.94940 0.40330 0.89670
H81 H 0.90980 0.45300 0.85830
C39 C 0.6196(6) 0.1750(2) 0.6692(3)
H82 H 0.53310 0.17320 0.65290
H83 H 0.66990 0.15860 0.63980
C40 C 0.6335(8) 0.1456(3) 0.7267(3)
H84 H 0.61140 0.10980 0.71900
H85 H 0.57970 0.16010 0.75530
H86 H 0.71860 0.14750 0.74370
C41 C 0.6674(6) 0.2637(3) 0.6004(2)
H87 H 0.70490 0.29810 0.60160
H88 H 0.72110 0.24080 0.57890
C42 C 0.5453(6) 0.2667(3) 0.5652(3)
H89 H 0.55610 0.27960 0.52480
H90 H 0.49180 0.28990 0.58540
H91 H 0.50840 0.23260 0.56240
C43 C 0.8184(5) 0.2431(2) 0.7069(3)
H92 H 0.84370 0.27940 0.70910
H93 H 0.82160 0.23000 0.74850
C44 C 0.9128(6) 0.2138(3) 0.6736(3)
H94 H 0.99360 0.21740 0.69530
H95 H 0.91510 0.22760 0.63300
H96 H 0.89040 0.17760 0.67140
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Co 1.17
N 0.68
P 1.05
Si 1.20
|
1100630.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-29 14:35:10 +0300 (Tue, 29 Mar 2016) $
#$Revision: 180580 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100630.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100630
loop_
_publ_author_name
'Bosold, F.'
'Marsch, M.'
'Harms, K.'
'Boche, G.'
_publ_section_title
;
Crystal structure of
1-lithio-1-phenyl-2,2-dimethylhydrazine-pentamethyldiethylenetriamine,
[(C6H5)(CH3)2N2]Li(C9H23N3)
;
_journal_coden_ASTM ZKNSFT
_journal_issue 1-4
_journal_name_full
;
Zeitschrift f\"ur Kristallographie - New Crystal Structures
;
_journal_page_first 619
_journal_page_last 620
_journal_paper_doi 10.1524/ncrs.1998.213.14.647
_journal_volume 213
_journal_year 1998
_chemical_formula_sum 'C17 H34 Li N5'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 97.467(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.305(2)
_cell_length_b 15.119(2)
_cell_length_c 14.411(3)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C17 H34 Li1 N5'
_cod_database_code 1100630
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
N1 N 0.2329(4) 0.8414(2) 0.8481(3)
N2 N 0.3068(5) 0.8911(2) 0.9259(3)
C1 C 0.0862(5) 0.8620(3) 0.8271(4)
C2 C 0.0054(6) 0.8264(3) 0.7460(4)
H1 H 0.0562(6) 0.7894(3) 0.7069(4)
C3 C -0.1450(6) 0.8406(3) 0.7211(5)
H2 H -0.1935(6) 0.8141(3) 0.6651(5)
C4 C -0.2244(6) 0.8933(3) 0.7775(5)
H3 H -0.3262(6) 0.9041(3) 0.7610(5)
C5 C -0.1492(6) 0.9297(3) 0.8559(5)
H4 H -0.2023(6) 0.9664(3) 0.8939(5)
C6 C 0.0034(5) 0.9166(3) 0.8833(4)
H5 H 0.0517(5) 0.9429(3) 0.9395(4)
C7 C 0.3029(6) 0.8417(4) 1.0107(4)
H6 H 0.2042(6) 0.8324(4) 1.0211(4)
H7 H 0.3497(6) 0.7856(4) 1.0059(4)
H8 H 0.3531(6) 0.8745(4) 1.0620(4)
C8 C 0.4616(5) 0.9031(3) 0.9110(4)
H9 H 0.4648(5) 0.9357(3) 0.8541(4)
H10 H 0.5113(5) 0.9357(3) 0.9626(4)
H11 H 0.5079(5) 0.8468(3) 0.9065(4)
Li1 Li 0.2816(8) 0.7169(5) 0.8104(6)
N3 N 0.3574(4) 0.7057(2) 0.6773(3)
N4 N 0.4509(5) 0.6235(3) 0.8593(3)
N5 N 0.1264(5) 0.6162(3) 0.8448(3)
C9 C 0.5055(6) 0.6648(4) 0.7059(5)
H12 H 0.5662(6) 0.7087(4) 0.7394(5)
H13 H 0.5497(6) 0.6470(4) 0.6523(5)
C10 C 0.4967(7) 0.5915(4) 0.7719(4)
H14 H 0.4221(7) 0.5525(4) 0.7437(4)
H15 H 0.5863(7) 0.5593(4) 0.7825(4)
C11 C 0.3684(7) 0.5521(3) 0.9055(5)
H16 H 0.3599(7) 0.5688(3) 0.9688(5)
H17 H 0.4227(7) 0.4980(3) 0.9072(5)
C12 C 0.2145(7) 0.5372(3) 0.8553(5)
H18 H 0.2240(7) 0.5134(3) 0.7946(5)
H19 H 0.1657(7) 0.4937(3) 0.8885(5)
C13 C 0.2691(7) 0.6542(4) 0.6060(4)
H20 H 0.3142(7) 0.6537(4) 0.5497(4)
H21 H 0.2626(7) 0.5948(4) 0.6286(4)
H22 H 0.1735(7) 0.6790(4) 0.5930(4)
C14 C 0.3774(6) 0.7948(3) 0.6418(4)
H23 H 0.4116(6) 0.7912(3) 0.5819(4)
H24 H 0.2872(6) 0.8266(3) 0.6357(4)
H25 H 0.4477(6) 0.8253(3) 0.6850(4)
C15 C 0.5809(7) 0.6500(4) 0.9242(5)
H26 H 0.6441(7) 0.6003(4) 0.9387(5)
H27 H 0.6316(7) 0.6953(4) 0.8947(5)
H28 H 0.5508(7) 0.6728(4) 0.9807(5)
C16 C -0.0091(7) 0.5993(4) 0.7777(6)
H29 H -0.0647(7) 0.5539(4) 0.8031(6)
H30 H -0.0669(7) 0.6519(4) 0.7675(6)
H31 H 0.0189(7) 0.5796(4) 0.7194(6)
C17 C 0.0758(8) 0.6444(3) 0.9314(4)
H32 H 0.0066(8) 0.6042(3) 0.9518(4)
H33 H 0.1609(8) 0.6461(3) 0.9769(4)
H34 H 0.0341(8) 0.7025(3) 0.9245(4)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 1.12
N 0.68
|
1100631.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-10 18:53:46 +0200 (Thu, 10 Mar 2016) $
#$Revision: 178098 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100631.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100631
loop_
_publ_author_name
'Bosold, F.'
'Marsch, M.'
'Harms, K.'
'Boche, G.'
_publ_section_title
;
Crystal structure of 1-lithio-1-phenyl-2,2-dimethylhydrazinetetrahydrofuran,
[(C~6~H~5~)(CH~3~)~2~N~2~]Li·C~4~H~8~O
;
_journal_issue 1-4
_journal_name_full 'Zeitschrift f\"ur Kristallographie'
_journal_page_first 621
_journal_page_last 622
_journal_paper_doi 10.1524/ncrs.1998.213.14.649
_journal_volume 213
_journal_year 1998
_chemical_formula_sum 'C12 H19 Li N2 O'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 100.51(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.810(3)
_cell_length_b 7.671(1)
_cell_length_c 16.541(6)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C12 H19 Li1 N2 O1'
_cod_database_code 1100631
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
N1 N -0.2931(2) -0.1184(3) 1.24072(13)
N2 N -0.1918(2) -0.0631(3) 1.19144(14)
C1 C -0.4226(3) -0.0618(4) 1.2083(2)
C2 C -0.4655(3) 0.0221(4) 1.1309(2)
H1 H -0.3996(3) 0.0360(4) 1.0949(2)
C3 C -0.5993(3) 0.0840(4) 1.1070(2)
H2 H -0.6242(3) 0.1419(4) 1.0549(2)
C4 C -0.6982(3) 0.0650(4) 1.1554(2)
H3 H -0.7899(3) 0.1113(4) 1.1386(2)
C5 C -0.6609(3) -0.0229(4) 1.2299(2)
H4 H -0.7292(3) -0.0410(4) 1.2639(2)
C6 C -0.5291(3) -0.0846(4) 1.2549(2)
H5 H -0.5067(3) -0.1454(4) 1.3063(2)
C7 C -0.0573(3) -0.0531(5) 1.2479(2)
H6 H -0.0237(3) -0.1692(5) 1.2607(2)
H7 H 0.0081(3) 0.0099(5) 1.2225(2)
H8 H -0.0687(3) 0.0052(5) 1.2976(2)
C8 C -0.1837(3) -0.1962(4) 1.1285(2)
H9 H -0.1583(3) -0.3061(4) 1.1548(2)
H10 H -0.2725(3) -0.2067(4) 1.0932(2)
H11 H -0.1155(3) -0.1628(4) 1.0966(2)
Li1 Li -0.2580(5) -0.3005(6) 1.3267(3)
O1 O -0.2730(2) -0.2260(3) 1.43824(12)
C9 C -0.3711(3) -0.2667(5) 1.4891(2)
H12 H -0.3597(3) -0.3853(5) 1.5077(2)
H13 H -0.4639(3) -0.2521(5) 1.4591(2)
C10 C -0.3422(4) -0.1445(6) 1.5607(2)
H14 H -0.3421(4) -0.2058(6) 1.6114(2)
H15 H -0.4121(4) -0.0555(6) 1.5551(2)
C11 C -0.2110(6) -0.0708(9) 1.5592(3)
H16 H -0.1452(6) -0.1131(9) 1.6052(3)
H17 H -0.2162(6) 0.0537(9) 1.5636(3)
C12 C -0.1662(4) -0.1163(5) 1.4830(2)
H18 H -0.1548(4) -0.0138(5) 1.4516(2)
H19 H -0.0797(4) -0.1781(5) 1.4941(2)
Li1C* Li -0.2420(5) 0.1995(6) 1.1733(3)
N2C* N -0.3082(2) -0.5631(3) 1.30856(14)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 1.01
N 0.68
O 0.68
|
1100632.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-29 15:07:46 +0300 (Tue, 29 Mar 2016) $
#$Revision: 180581 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100632.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100632
loop_
_publ_author_name
'Bosold, F.'
'Marsch, M.'
'Harms, K.'
'Boche, G.'
_publ_section_title
;
Crystal structure of
bis(1-lithio-1,2-diphenylhydrazine)-1,2-dilithio-1,2-diphenylhydrazine-tetrakis(diethyl ether),
[(C~6~H~5~)~2~N~2~Li]~2~[(C~6~H~5~)~2~N~2~Li~2~](C~4~H~10~O)~4~
;
_journal_coden_ASTM ZKNSFT
_journal_issue 1-4
_journal_name_full
;
Zeitschrift f\"ur Kristallographie - New Crystal Structures
;
_journal_page_first 623
_journal_page_last 624
_journal_paper_doi 10.1524/ncrs.1998.213.14.651
_journal_volume 213
_journal_year 1998
_chemical_formula_sum 'C52 H72 Li4 N6 O4'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 117.74(1)
_cell_angle_beta 107.02(1)
_cell_angle_gamma 98.30(1)
_cell_formula_units_Z 1
_cell_length_a 11.158(2)
_cell_length_b 11.798(1)
_cell_length_c 12.107(2)
_cod_database_code 1100632
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
N1 N 0.0095(2) 0.3896(2) 0.7081(2)
N2 N -0.0967(2) 0.4138(2) 0.6304(2)
H1 H -0.1138(25) 0.4814(27) 0.6822(27)
C1 C 0.1047(2) 0.3701(2) 0.6558(2)
C2 C 0.2135(3) 0.3452(3) 0.7224(3)
H2 H 0.2167(3) 0.3396(3) 0.7997(3)
C3 C 0.3151(3) 0.3282(3) 0.6791(3)
H3 H 0.3887(3) 0.3120(3) 0.7273(3)
C4 C 0.3114(3) 0.3343(3) 0.5670(3)
H4 H 0.3826(3) 0.3230(3) 0.5379(3)
C5 C 0.2056(3) 0.3574(3) 0.5000(3)
H5 H 0.2026(3) 0.3610(3) 0.4216(3)
C6 C 0.1032(3) 0.3748(3) 0.5408(3)
H6 H 0.0297(3) 0.3903(3) 0.4915(3)
C7 C -0.2067(2) 0.3056(3) 0.5197(3)
C8 C -0.2006(3) 0.1752(3) 0.4496(3)
H7 H -0.1196(3) 0.1585(3) 0.4813(3)
C9 C -0.3109(3) 0.0704(3) 0.3347(3)
H8 H -0.3061(3) -0.0193(3) 0.2873(3)
C10 C -0.4268(3) 0.0932(4) 0.2888(3)
H9 H -0.5021(3) 0.0212(4) 0.2083(3)
C11 C -0.4336(3) 0.2219(5) 0.3581(4)
H10 H -0.5151(3) 0.2381(5) 0.3271(4)
C12 C -0.3258(3) 0.3283(3) 0.4737(3)
H11 H -0.3313(3) 0.4176(3) 0.5221(3)
N3 N -0.0729(2) 0.4759(2) 0.9694(2)
C13 C -0.1205(2) 0.5605(2) 0.9324(2)
C14 C -0.2600(2) 0.5256(3) 0.8673(3)
H12 H -0.3161(2) 0.4458(3) 0.8529(3)
C15 C -0.3166(3) 0.6002(3) 0.8229(3)
H13 H -0.4116(3) 0.5723(3) 0.7786(3)
C16 C -0.2395(3) 0.7157(3) 0.8408(3)
H14 H -0.2799(3) 0.7675(3) 0.8091(3)
C17 C -0.1045(3) 0.7538(3) 0.9051(3)
H15 H -0.0498(3) 0.8345(3) 0.9198(3)
C18 C -0.0445(2) 0.6791(3) 0.9506(2)
H16 H 0.0506(2) 0.7082(3) 0.9948(2)
O1 O 0.2605(2) 0.6942(2) 0.9073(2)
C19 C -0.2886(3) 0.0483(3) 0.6539(4)
H17 H -0.3010(3) 0.0039(3) 0.7010(4)
H18 H -0.3213(3) -0.0192(3) 0.5580(4)
C20 C -0.3628(3) 0.1452(3) 0.6748(4)
H19 H -0.4560(3) 0.0998(3) 0.6407(4)
H20 H -0.3289(3) 0.2121(3) 0.7709(4)
H21 H -0.3493(3) 0.1888(3) 0.6273(4)
O2 O -0.1529(2) 0.1185(2) 0.7060(2)
C21 C -0.0823(9) 0.0178(9) 0.6894(10)
H22 H -0.1234(9) -0.0603(9) 0.5976(10)
H23 H -0.0864(9) -0.0116(9) 0.7504(10)
C22 C 0.0576(6) 0.0835(6) 0.7270(7)
H24 H 0.1036(6) 0.0190(6) 0.7182(7)
H25 H 0.0615(6) 0.1118(6) 0.6652(7)
H26 H 0.0989(6) 0.1609(6) 0.8192(7)
C23? C -0.0324(10) -0.0168(10) 0.7366(9)
H27? H 0.0178(10) -0.0768(10) 0.7114(9)
H28? H 0.0211(10) 0.0624(10) 0.8261(9)
H29? H -0.1104(10) -0.0625(10) 0.7375(9)
C24? C -0.0747(3) 0.0404(3) 0.6557(3)
H30? H 0.0009(3) 0.0888(3) 0.6539(3)
H31? H -0.1306(3) -0.0362(3) 0.5652(3)
C25 C 0.1964(3) 0.7505(3) 0.8336(3)
H32 H 0.1018(3) 0.7085(3) 0.7944(3)
H33 H 0.2236(3) 0.7325(3) 0.7606(3)
C26 C 0.2307(3) 0.9008(3) 0.9264(4)
H34 H 0.1877(3) 0.9378(3) 0.8765(4)
H35 H 0.2024(3) 0.9183(3) 0.9988(4)
H36 H 0.3252(3) 0.9426(3) 0.9647(4)
C27 C 0.3907(2) 0.6985(3) 0.9090(3)
H37 H 0.4372(2) 0.7862(3) 0.9307(3)
H38 H 0.3835(2) 0.6313(3) 0.8206(3)
C28 C 0.4666(3) 0.6736(3) 1.0148(3)
H39 H 0.5539(3) 0.6770(3) 1.0173(3)
H40 H 0.4737(3) 0.7415(3) 1.1028(3)
H41 H 0.4197(3) 0.5856(3) 0.9920(3)
Li1 Li -0.0706(4) 0.3154(4) 0.7972(4)
Li2 Li 0.1344(4) 0.5508(4) 0.8990(4)
N3A* N 0.0729(2) 0.5241(2) 1.0306(2)
C13A* C 0.1205(2) 0.4395(2) 1.0676(2)
C14A* C 0.2600(2) 0.4744(3) 1.1327(3)
H12A* H 0.3161(2) 0.5542(3) 1.1471(3)
C15A* C 0.3166(3) 0.3998(3) 1.1771(3)
H13A* H 0.4116(3) 0.4277(3) 1.2214(3)
C16A* C 0.2395(3) 0.2843(3) 1.1592(3)
H14A* H 0.2799(3) 0.2325(3) 1.1909(3)
C17A* C 0.1045(3) 0.2462(3) 1.0949(3)
H15A* H 0.0498(3) 0.1655(3) 1.0802(3)
C18A* C 0.0445(2) 0.3209(3) 1.0494(2)
H16A* H -0.0506(2) 0.2918(3) 1.0052(2)
Li1A* Li 0.0706(4) 0.6846(4) 1.2028(4)
N1A* N -0.0095(2) 0.6104(2) 1.2919(2)
N2A* N 0.0967(2) 0.5862(2) 1.3696(2)
H1A* H 0.1138(25) 0.5186(27) 1.3178(27)
C7A* C 0.2067(2) 0.6944(3) 1.4803(3)
C8A* C 0.2006(3) 0.8248(3) 1.5504(3)
H7A* H 0.1196(3) 0.8415(3) 1.5187(3)
C9A* C 0.3109(3) 0.9296(3) 1.6653(3)
H8A* H 0.3061(3) 1.0193(3) 1.7127(3)
C10A* C 0.4268(3) 0.9068(4) 1.7112(3)
H9A* H 0.5021(3) 0.9788(4) 1.7917(3)
C11A* C 0.4336(3) 0.7781(5) 1.6419(4)
H10A* H 0.5151(3) 0.7619(5) 1.6729(4)
C12A* C 0.3258(3) 0.6717(3) 1.5263(3)
H11A* H 0.3313(3) 0.5824(3) 1.4779(3)
C1A* C -0.1047(2) 0.6299(2) 1.3442(2)
C2A* C -0.2135(3) 0.6548(3) 1.2776(3)
H2A* H -0.2167(3) 0.6604(3) 1.2003(3)
C3A* C -0.3151(3) 0.6718(3) 1.3209(3)
H3A* H -0.3887(3) 0.6880(3) 1.2727(3)
C4A* C -0.3114(3) 0.6657(3) 1.4330(3)
H4A* H -0.3826(3) 0.6770(3) 1.4621(3)
C5A* C -0.2056(3) 0.6426(3) 1.5000(3)
H5A* H -0.2026(3) 0.6390(3) 1.5784(3)
C6A* C -0.1032(3) 0.6252(3) 1.4592(3)
H6A* H -0.0297(3) 0.6097(3) 1.5085(3)
Li2A* Li -0.1344(4) 0.4492(4) 1.1010(4)
O1A* O -0.2605(2) 0.3058(2) 1.0927(2)
C25A* C -0.1964(3) 0.2495(3) 1.1664(3)
H32A* H -0.1018(3) 0.2915(3) 1.2056(3)
H33A* H -0.2236(3) 0.2675(3) 1.2394(3)
C26A* C -0.2307(3) 0.0992(3) 1.0736(4)
H34A* H -0.1877(3) 0.0622(3) 1.1235(4)
H35A* H -0.2024(3) 0.0817(3) 1.0012(4)
H36A* H -0.3252(3) 0.0574(3) 1.0353(4)
C27A* C -0.3907(2) 0.3015(3) 1.0910(3)
H37A* H -0.4372(2) 0.2138(3) 1.0693(3)
H38A* H -0.3835(2) 0.3687(3) 1.1794(3)
C28A* C -0.4666(3) 0.3264(3) 0.9852(3)
H39A* H -0.5539(3) 0.3230(3) 0.9827(3)
H40A* H -0.4737(3) 0.2585(3) 0.8972(3)
H41A* H -0.4197(3) 0.4144(3) 1.0080(3)
O2A* O 0.1529(2) 0.8815(2) 1.2940(2)
C19A* C 0.2886(3) 0.9517(3) 1.3461(4)
H17A* H 0.3010(3) 0.9961(3) 1.2990(4)
H18A* H 0.3213(3) 1.0192(3) 1.4420(4)
C20A* C 0.3628(3) 0.8548(3) 1.3252(4)
H19A* H 0.4560(3) 0.9002(3) 1.3593(4)
H20A* H 0.3289(3) 0.7879(3) 1.2291(4)
H21A* H 0.3493(3) 0.8112(3) 1.3727(4)
C21A* C 0.0823(9) 0.9822(9) 1.3106(10)
H22A* H 0.1234(9) 1.0603(9) 1.4024(10)
H23A* H 0.0864(9) 1.0116(9) 1.2496(10)
C22A* C -0.0576(6) 0.9165(6) 1.2730(7)
H24A* H -0.1036(6) 0.9810(6) 1.2818(7)
H25A* H -0.0615(6) 0.8882(6) 1.3348(7)
H26A* H -0.0989(6) 0.8391(6) 1.1808(7)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Li 1.01
N 0.68
O 0.68
|
1100633.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-09 16:37:21 +0200 (Wed, 09 Mar 2016) $
#$Revision: 178051 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100633.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100633
loop_
_publ_author_name
'Aurich, Hans G\"unter'
'Geiger, Michael'
'Gentes, Christian'
'Harms, Klaus'
'K\"oster, Heiner'
_publ_section_title
;
Formation of enantiopure tricyclic compounds by intramolecular
1,3-dipolar cycloaddition of nitrones
;
_journal_coden_ASTM TETRAB
_journal_issue 13
_journal_name_full Tetrahedron
_journal_page_first 3181
_journal_page_last 3196
_journal_paper_doi 10.1016/s0040-4020(98)00064-7
_journal_volume 54
_journal_year 1998
_chemical_formula_sum 'C10 H17 N O2'
_space_group_IT_number 18
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 18
_symmetry_space_group_name_Hall 'P 2 2ab'
_symmetry_space_group_name_H-M 'P 21 21 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.061(1)
_cell_length_b 14.753(1)
_cell_length_c 5.643(1)
_cod_original_formula_sum 'C10 H17 N1 O2'
_cod_database_code 1100633
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 1/2+x,1/2-y,-z
4 1/2-x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C1 C 0.8784(2) 0.1783(2) 0.2308(4)
O1 O 0.83801(15) 0.22147(11) 0.4423(3)
N1 N 0.8264(2) 0.31647(14) 0.3901(4)
C2 C 0.7886(2) 0.3190(2) 0.1423(4)
C3 C 0.6613(2) 0.3236(2) 0.1179(5)
O2 O 0.62566(14) 0.23178(11) 0.1065(3)
C4 C 0.7050(2) 0.1863(2) -0.0389(4)
C5 C 0.6924(3) 0.0854(2) -0.0045(5)
C6 C 0.7363(3) 0.0537(2) 0.2346(6)
C7 C 0.8580(3) 0.0778(2) 0.2550(6)
C8 C 0.8180(2) 0.2265(2) 0.0304(4)
C9 C 0.9348(5) 0.3593(2) 0.4211(6)
C10 C 0.5997(2) 0.3716(2) 0.3101(6)
H1 H 0.9583(2) 0.1893(2) 0.2161(4)
H2 H 0.8241(2) 0.3687(2) 0.0557(4)
H3 H 0.6436(2) 0.3528(2) -0.0333(5)
H4 H 0.6900(2) 0.2010(2) -0.2052(4)
H5 H 0.7321(3) 0.0540(2) -0.1296(5)
H6 H 0.6146(3) 0.0694(2) -0.0174(5)
H7 H 0.6949(3) 0.0826(2) 0.3612(6)
H8 H 0.7269(3) -0.0114(2) 0.2492(6)
H9 H 0.8856(3) 0.0576(2) 0.4075(6)
H10 H 0.8991(3) 0.0461(2) 0.1328(6)
H11 H 0.8660(2) 0.2339(2) -0.1084(4)
H12 H 0.9275(4) 0.4238(2) 0.4034(40)
H13 H 0.9853(6) 0.3365(12) 0.3039(27)
H14 H 0.9628(9) 0.3458(13) 0.5764(16)
H15 H 0.6242(14) 0.4334(5) 0.3187(27)
H16 H 0.6134(15) 0.342(1) 0.4588(8)
H17 H 0.5217(3) 0.3701(13) 0.2762(21)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100634.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-09 16:37:21 +0200 (Wed, 09 Mar 2016) $
#$Revision: 178051 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100634.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100634
loop_
_publ_author_name
'Aurich, Hans G\"unter'
'Geiger, Michael'
'Gentes, Christian'
'Harms, Klaus'
'K\"oster, Heiner'
_publ_section_title
;
Formation of enantiopure tricyclic compounds by intramolecular
1,3-dipolar cycloaddition of nitrones
;
_journal_coden_ASTM TETRAB
_journal_issue 13
_journal_name_full Tetrahedron
_journal_page_first 3181
_journal_page_last 3196
_journal_paper_doi 10.1016/s0040-4020(98)00064-7
_journal_volume 54
_journal_year 1998
_chemical_formula_sum 'C17 H24 N2 O'
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 19
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 9.750(2)
_cell_length_b 10.525(2)
_cell_length_c 15.035(3)
_cod_original_formula_sum 'C17 H24 N2 O1'
_cod_database_code 1100634
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 1/2+x,1/2-y,-z
4 -x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
C1 C 0.8886(2) 0.1642(2) 0.14217(14)
O1 O 0.94360(13) 0.20889(14) 0.05915(10)
N1 N 0.8289(2) 0.2314(2) 0.00017(13)
C2 C 0.7327(2) 0.1282(2) 0.02051(14)
C3 C 0.7532(2) 0.0122(2) -0.03937(14)
N2 N 0.8437(2) -0.07004(15) 0.01338(11)
C4 C 0.7965(2) -0.0615(2) 0.10550(14)
C5 C 0.9016(2) -0.1103(2) 0.1719(2)
C6 C 1.0330(3) -0.0325(3) 0.1679(2)
C7 C 1.0046(3) 0.1033(3) 0.1932(2)
C8 C 0.7661(2) 0.0811(2) 0.11585(13)
C9 C 0.7715(3) 0.3559(2) 0.0220(2)
C10 C 0.6149(3) -0.0467(3) -0.0636(2)
C11 C 0.8635(2) -0.1981(2) -0.0207(2)
C12 C 0.9430(2) -0.2003(2) -0.10678(15)
C13 C 1.0504(3) -0.1183(2) -0.1209(2)
C14 C 1.1256(3) -0.1230(2) -0.1987(2)
C15 C 1.0946(3) -0.2097(3) -0.2638(2)
C16 C 0.9900(3) -0.2934(3) -0.2501(2)
C17 C 0.9139(2) -0.2883(3) -0.1722(2)
H1 H 0.8545(2) 0.2381(2) 0.17644(14)
H2 H 0.6368(2) 0.1588(2) 0.01699(14)
H3 H 0.8012(2) 0.0385(2) -0.09441(14)
H4 H 0.7102(2) -0.1102(2) 0.11215(14)
H5 H 0.9225(2) -0.1995(2) 0.1589(2)
H6 H 0.8632(2) -0.1059(2) 0.2321(2)
H7 H 1.1010(3) -0.0687(3) 0.2087(2)
H8 H 1.0709(3) -0.0356(3) 0.1076(2)
H9 H 1.0882(3) 0.1532(3) 0.1837(2)
H10 H 0.9830(3) 0.1065(3) 0.2569(2)
H11 H 0.6875(2) 0.0952(2) 0.15638(13)
H12 H 0.8397(8) 0.4211(3) 0.0111(13)
H13 H 0.745(2) 0.3575(7) 0.0842(4)
H14 H 0.6916(13) 0.3717(9) -0.0148(10)
H15 H 0.5605(9) 0.0147(7) -0.0963(13)
H16 H 0.5668(10) -0.0707(19) -0.0097(2)
H17 H 0.6296(3) -0.1214(12) -0.1001(12)
H18 H 0.7737(2) -0.2376(2) -0.0302(2)
H19 H 0.9126(2) -0.2486(2) 0.0239(2)
H20 H 1.0730(3) -0.0582(2) -0.0770(2)
H21 H 1.1989(3) -0.0662(2) -0.2071(2)
H22 H 1.1447(3) -0.2114(3) -0.3172(2)
H23 H 0.9694(3) -0.3547(3) -0.2935(2)
H24 H 0.8412(2) -0.3457(3) -0.1638(2)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100635.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 18:52:13 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177956 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100635.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100635
loop_
_publ_author_name
'Anfang, S.'
'Gr\"ob, T.'
'Harms, K.'
'Seybert, G.'
'Massa, W.'
'Greiner, A.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe von Seltenerdelementen. Die Kristallstrukturen
von [Yb~2~Cp~3~(NPPh~3~)~3~], [YCp(NPPh~3~)(\m-OSiMe~2~NPPh~3~)]~2~ und
[M(NPPh~3~)~2~(\m-OSiMe~2~NPPh~3~)]~2~ mit M = Y und Sm
;
_journal_coden_ASTM ZAACAB
_journal_issue 11
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1853
_journal_page_last 1859
_journal_paper_doi
10.1002/(sici)1521-3749(199911)625:11<1853::aid-zaac1853>3.0.co;2-4
_journal_volume 625
_journal_year 1999
_chemical_formula_sum 'C90 H84 N3 P3 Yb2'
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 61
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.2760(19)
_cell_length_b 19.7754(10)
_cell_length_c 28.4888(17)
_cod_database_code 1100635
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,y,1/2-z
3 x,1/2-y,1/2+z
4 1/2-x,1/2+y,z
5 -x,-y,-z
6 -1/2-x,-y,-1/2+z
7 -x,-1/2+y,-1/2-z
8 -1/2+x,-1/2-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Yb1 Yb 0.10624(1) 0.27356(2) 0.36447(1)
P1 P 0.12510(8) 0.43142(11) 0.42728(7)
N1 N 0.1185(2) 0.3696(3) 0.3973(2)
C1 C 0.1881(3) 0.4633(4) 0.4314(3)
Yb2 Yb 0.10716(1) 0.30602(2) 0.24728(1)
P2 P -0.00569(7) 0.3000(1) 0.30810(7)
N2 N 0.0511(2) 0.2944(3) 0.3064(2)
C2 C 0.2132(3) 0.4748(4) 0.3899(3)
H1 H 0.19760 0.46640 0.36060
P3 P 0.21193(7) 0.23702(10) 0.30442(7)
N3 N 0.1584(2) 0.2634(3) 0.30268(19)
C3 C 0.2613(3) 0.4988(5) 0.3910(4)
H2 H 0.27870 0.50570 0.36260
C4 C 0.2831(4) 0.5123(5) 0.4329(4)
H3 H 0.31560 0.52950 0.43340
C5 C 0.2592(3) 0.5018(5) 0.4735(3)
H4 H 0.27540 0.51010 0.50250
C6 C 0.2110(3) 0.4787(4) 0.4733(3)
H5 H 0.19380 0.47350 0.50210
C7 C 0.0929(3) 0.5073(4) 0.4085(3)
C8 C 0.1027(4) 0.5708(4) 0.4281(3)
H6 H 0.12530 0.57410 0.45340
C9 C 0.0803(4) 0.6284(5) 0.4117(3)
H7 H 0.08810 0.67120 0.42490
C10 C 0.0466(4) 0.6236(5) 0.3759(3)
H8 H 0.03080 0.66330 0.36470
C11 C 0.0356(3) 0.5615(5) 0.3560(3)
H9 H 0.01210 0.55830 0.33150
C12 C 0.0591(3) 0.5039(4) 0.3724(3)
H10 H 0.05190 0.46140 0.35850
C13 C 0.1064(3) 0.4175(4) 0.4878(3)
C14 C 0.1255(4) 0.3611(5) 0.5105(3)
H11 H 0.14870 0.33370 0.49440
C15 C 0.1118(4) 0.3440(6) 0.5555(3)
H12 H 0.12530 0.30520 0.57040
C16 C 0.0785(5) 0.3839(8) 0.5784(4)
H13 H 0.06900 0.37240 0.60950
C17 C 0.0585(4) 0.4399(7) 0.5576(4)
H14 H 0.03540 0.46690 0.57410
C18 C 0.0723(4) 0.4570(5) 0.5123(3)
H15 H 0.05860 0.49580 0.49780
C19 C -0.0302(3) 0.3744(4) 0.2783(3)
C20 C -0.0500(3) 0.4285(4) 0.3034(3)
H16 H -0.05360 0.42540 0.33650
C21 C -0.0643(3) 0.4867(4) 0.2801(4)
H17 H -0.07750 0.52350 0.29740
C22 C -0.0596(3) 0.4918(5) 0.2319(4)
H18 H -0.06980 0.53170 0.21610
C23 C -0.0401(3) 0.4383(5) 0.2067(3)
H19 H -0.03620 0.44170 0.17360
C24 C -0.0265(3) 0.3802(5) 0.2300(3)
H20 H -0.01420 0.34300 0.21240
C25 C -0.0381(3) 0.2292(4) 0.2815(3)
C26 C -0.0788(3) 0.2376(5) 0.2526(3)
H21 H -0.09090 0.28160 0.24580
C27 C -0.1020(3) 0.1800(5) 0.2336(3)
H22 H -0.12860 0.18520 0.21240
C28 C -0.0860(3) 0.1161(5) 0.2457(4)
H23 H -0.10260 0.07740 0.23400
C29 C -0.0462(3) 0.1084(5) 0.2744(3)
H24 H -0.03500 0.06430 0.28230
C30 C -0.0224(3) 0.1645(4) 0.2921(3)
H25 H 0.00530 0.15850 0.31180
C31 C -0.0315(3) 0.3039(4) 0.3674(3)
C32 C -0.0067(3) 0.3366(4) 0.4027(3)
H26 H 0.02390 0.35740 0.39620
C33 C -0.0259(4) 0.3396(5) 0.4475(3)
H27 H -0.00880 0.36290 0.47170
C34 C -0.0699(4) 0.3087(6) 0.4569(4)
H28 H -0.08300 0.31020 0.48770
C35 C -0.0952(4) 0.2756(6) 0.4218(4)
H29 H -0.12530 0.25340 0.42870
C36 C -0.0770(3) 0.2748(5) 0.3775(3)
H30 H -0.09530 0.25410 0.35300
C37 C 0.2211(3) 0.1514(4) 0.2832(3)
C38 C 0.1818(3) 0.1067(4) 0.2818(3)
H31 H 0.15040 0.12100 0.29230
C39 C 0.1882(3) 0.0416(4) 0.2653(3)
H32 H 0.16120 0.01120 0.26500
C40 C 0.2329(3) 0.0203(4) 0.2494(3)
H33 H 0.23650 -0.02400 0.23700
C41 C 0.2726(3) 0.0628(4) 0.2515(4)
H34 H 0.30400 0.04730 0.24210
C42 C 0.2665(3) 0.1287(4) 0.2673(3)
H35 H 0.29370 0.15870 0.26740
C43 C 0.2564(3) 0.2848(4) 0.2688(3)
C44 C 0.2511(3) 0.2848(4) 0.2198(3)
H36 H 0.22500 0.26040 0.20560
C45 C 0.2830(3) 0.3191(5) 0.1926(4)
H37 H 0.27940 0.31720 0.15950
C46 C 0.3207(3) 0.3567(5) 0.2113(4)
H38 H 0.34240 0.38140 0.19160
C47 C 0.3259(3) 0.3576(4) 0.2588(4)
H39 H 0.35150 0.38360 0.27230
C48 C 0.2949(3) 0.3216(4) 0.2880(3)
H40 H 0.29990 0.32210 0.32100
C49 C 0.2385(3) 0.2387(4) 0.3628(3)
C50 C 0.2646(3) 0.1840(5) 0.3819(3)
H41 H 0.26810 0.14330 0.36450
C51 C 0.2850(4) 0.1895(6) 0.4260(4)
H42 H 0.30220 0.15230 0.43930
C52 C 0.2807(4) 0.2489(6) 0.4509(4)
H43 H 0.29590 0.25310 0.48080
C53 C 0.2542(3) 0.3027(5) 0.4326(3)
H44 H 0.25080 0.34340 0.45000
C54 C 0.2334(3) 0.2965(4) 0.3895(3)
H45 H 0.21460 0.33310 0.37740
C55 C 0.0502(3) 0.2289(4) 0.1939(3)
H46 H 0.01610 0.22940 0.20090
C56 C 0.0739(3) 0.2725(5) 0.1628(3)
H47 H 0.05920 0.30790 0.14520
C57 C 0.1233(3) 0.2541(4) 0.1625(3)
H48 H 0.14840 0.27520 0.14470
C58 C 0.1295(3) 0.1986(4) 0.1934(3)
H49 H 0.15920 0.17520 0.19970
C59 C 0.0840(3) 0.1850(4) 0.2126(3)
H50 H 0.07730 0.15090 0.23520
C60 C 0.0847(3) 0.1436(4) 0.3805(3)
H51 H 0.07510 0.11790 0.35390
C61 C 0.1328(3) 0.1509(4) 0.3971(3)
H52 H 0.16130 0.13010 0.38450
C62 C 0.1308(4) 0.1946(5) 0.4356(3)
H53 H 0.15820 0.20980 0.45340
C63 C 0.0818(4) 0.2126(5) 0.4439(3)
H54 H 0.07030 0.24140 0.46820
C64 C 0.0530(3) 0.1808(5) 0.4101(3)
H55 H 0.01840 0.18350 0.40740
C65 C 0.0874(3) 0.4378(4) 0.2497(3)
H56 H 0.05540 0.45060 0.25930
C66 C 0.1025(4) 0.4265(5) 0.2039(3)
H57 H 0.08280 0.43020 0.17650
C67 C 0.1526(4) 0.4084(5) 0.2054(4)
H58 H 0.17270 0.39740 0.17920
C68 C 0.1669(3) 0.4096(4) 0.2513(4)
H59 H 0.19900 0.39990 0.26240
C69 C 0.1273(3) 0.4271(4) 0.2792(3)
H60 H 0.12740 0.43120 0.31240
C70? C 0.1426(5) 0.6035(5) 0.0796(5)
C71? C 0.1814(7) 0.6212(6) 0.0480(3)
H61? H 0.18110 0.61650 0.01480
C72? C 0.2172(5) 0.6450(6) 0.0735(6)
H62? H 0.24290 0.65190 0.05140
C73? C 0.2346(7) 0.6623(7) 0.1089(8)
H63? H 0.26530 0.68100 0.11770
C74? C 0.1869(9) 0.6425(7) 0.1360(4)
H64? H 0.19020 0.65370 0.16830
C75? C 0.1445(8) 0.6157(7) 0.1284(5)
H65? H 0.11970 0.60630 0.15090
C76? C 0.1108(6) 0.5883(8) 0.0617(9)
H66? H 0.11810 0.58380 0.02810
H67? H 0.08510 0.62230 0.06610
H68? H 0.09970 0.54470 0.07400
C77? C 0.2840(4) 0.4649(5) 0.1054(3)
C78? C 0.2309(4) 0.4554(5) 0.1021(3)
H69? H 0.21280 0.48840 0.11900
C79? C 0.1985(4) 0.4038(7) 0.0772(4)
H70? H 0.16370 0.40420 0.07520
C80? C 0.2292(5) 0.3576(5) 0.0588(4)
H71? H 0.21790 0.31750 0.04410
C81? C 0.2810(4) 0.3738(5) 0.0633(3)
H72? H 0.29800 0.33990 0.04620
C82? C 0.3152(3) 0.4145(6) 0.0803(4)
H73? H 0.34980 0.41230 0.07750
C83? C 0.3188(5) 0.4995(7) 0.1173(5)
H74? H 0.30700 0.53870 0.13510
H75? H 0.33650 0.51490 0.08940
H76? H 0.34080 0.47260 0.13710
C84 C 0.0126(4) 0.8811(7) 0.4397(4)
C85 C 0.0415(6) 0.8330(5) 0.4252(4)
H77 H 0.02940 0.78840 0.42970
C86 C 0.0906(6) 0.8373(7) 0.4029(5)
H78 H 0.10600 0.79960 0.38840
C87 C 0.1112(4) 0.8978(9) 0.4048(5)
H79 H 0.14440 0.90610 0.39650
C88 C 0.0765(5) 0.9525(6) 0.4215(4)
H80 H 0.09250 0.99510 0.42040
C89 C 0.0295(5) 0.9608(6) 0.4377(4)
H81 H 0.01200 1.00080 0.44540
C90 C -0.0320(4) 0.8961(11) 0.4545(6)
H82 H -0.05120 0.85450 0.45770
H83 H -0.04800 0.92620 0.43180
H84 H -0.03000 0.91880 0.48510
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.81
H 0.23
N 0.68
P 1.05
Yb 1.49
|
1100636.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 18:52:13 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177956 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100636.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100636
loop_
_publ_author_name
'Anfang, S.'
'Gr\"ob, T.'
'Harms, K.'
'Seybert, G.'
'Massa, W.'
'Greiner, A.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe von Seltenerdelementen. Die Kristallstrukturen
von [Yb~2~Cp~3~(NPPh~3~)~3~], [YCp(NPPh~3~)(\m-OSiMe~2~NPPh~3~)]~2~ und
[M(NPPh~3~)~2~(\m-OSiMe~2~NPPh~3~)]~2~ mit M = Y und Sm
;
_journal_coden_ASTM ZAACAB
_journal_issue 11
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1853
_journal_page_last 1859
_journal_paper_doi
10.1002/(sici)1521-3749(199911)625:11<1853::aid-zaac1853>3.0.co;2-4
_journal_volume 625
_journal_year 1999
_chemical_formula_sum 'C114 H114 N4 O2 P4 Si2 Y2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 93.196(10)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 14.6903(11)
_cell_length_b 12.3408(9)
_cell_length_c 27.615(2)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100636
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Y1 Y 0.37573(3) -0.00092(8) 0.00705(3)
P1 P 0.30687(9) 0.17536(18) 0.11284(8)
N1 N 0.3752(2) 0.0983(5) 0.0861(2)
C1 C 0.2689(4) -0.1356(7) 0.0564(3)
H1 H 0.24230 -0.10280 0.08340
Si1 Si 0.49025(9) 0.07538(18) 0.09910(8)
O1 O 0.51851(18) 0.0274(4) 0.04752(16)
P2 P 0.24760(9) 0.18967(18) -0.07241(8)
N2 N 0.2928(2) 0.1154(5) -0.0327(2)
C2 C 0.3538(4) -0.1903(6) 0.0569(3)
H2 H 0.39300 -0.20340 0.08480
C3 C 0.3703(4) -0.2217(6) 0.0097(3)
H3 H 0.42360 -0.25730 0.00000
C4 C 0.2941(4) -0.1919(7) -0.0215(3)
H4 H 0.28580 -0.20410 -0.05550
C5 C 0.2323(4) -0.1391(7) 0.0097(3)
H5 H 0.17430 -0.11070 -0.00070
C6 C 0.5122(3) -0.0241(7) 0.1480(3)
H6 H 0.50660 0.01140 0.17950
H7 H 0.57390 -0.05340 0.14620
H8 H 0.46770 -0.08310 0.14440
C7 C 0.5550(3) 0.2010(7) 0.1170(3)
H9 H 0.61720 0.18160 0.12830
H10 H 0.52460 0.23780 0.14310
H11 H 0.55690 0.24940 0.08890
C8 C 0.1893(3) 0.1266(7) 0.1081(3)
C9 C 0.1516(4) 0.1134(7) 0.0610(3)
H12 H 0.18820 0.12520 0.03420
C10 C 0.0594(4) 0.0827(7) 0.0529(3)
H13 H 0.03290 0.07290 0.02110
C11 C 0.0090(4) 0.0674(8) 0.0935(4)
H14 H -0.05380 0.04950 0.08880
C12 C 0.0459(4) 0.0771(9) 0.1397(4)
H15 H 0.01020 0.06200 0.16660
C13 C 0.1377(4) 0.1098(7) 0.1472(3)
H16 H 0.16350 0.12010 0.17920
C14 C 0.2955(3) 0.3099(7) 0.0881(3)
C15 C 0.3535(4) 0.3466(7) 0.0529(3)
H17 H 0.39940 0.29970 0.04200
C16 C 0.3448(4) 0.4498(8) 0.0339(3)
H18 H 0.38480 0.47360 0.01020
C17 C 0.2770(4) 0.5192(8) 0.0496(3)
H19 H 0.27150 0.59050 0.03680
C18 C 0.2175(4) 0.4837(9) 0.0839(3)
H20 H 0.17170 0.53070 0.09480
C19 C 0.2260(4) 0.3808(8) 0.1017(3)
H21 H 0.18360 0.35600 0.12400
C20 C 0.3380(4) 0.1917(8) 0.1760(3)
C21 C 0.3673(5) 0.2917(9) 0.1958(4)
H22 H 0.36710 0.35430 0.17580
C22 C 0.3960(6) 0.2994(12) 0.2439(5)
H23 H 0.41630 0.36720 0.25680
C23 C 0.3957(6) 0.2107(15) 0.2730(5)
H24 H 0.41570 0.21700 0.30620
C24 C 0.3669(5) 0.1119(11) 0.2549(4)
H25 H 0.36600 0.05060 0.27570
C25 C 0.3392(4) 0.1020(9) 0.2068(3)
H26 H 0.32080 0.03320 0.19430
C26 C 0.2249(4) 0.1270(8) -0.1306(3)
C27 C 0.2327(4) 0.0164(9) -0.1347(4)
H27 H 0.24830 -0.02540 -0.10660
C28 C 0.2180(4) -0.0360(9) -0.1795(5)
H28 H 0.22370 -0.11250 -0.18170
C29 C 0.1955(6) 0.0237(15) -0.2201(5)
H29 H 0.18540 -0.01120 -0.25060
C30 C 0.1875(7) 0.1350(14) -0.2169(5)
H30 H 0.17200 0.17750 -0.24480
C31 C 0.2026(5) 0.1827(10) -0.1718(4)
H31 H 0.19700 0.25920 -0.16960
C32 C 0.3145(3) 0.3098(7) -0.0854(3)
C33 C 0.2784(4) 0.4094(7) -0.1014(3)
H32 H 0.21430 0.41690 -0.10680
C34 C 0.3343(4) 0.4973(9) -0.1094(3)
H33 H 0.30830 0.56450 -0.11970
C35 C 0.4280(4) 0.4869(9) -0.1025(3)
H34 H 0.46670 0.54640 -0.10880
C36 C 0.4649(4) 0.3888(8) -0.0863(3)
H35 H 0.52910 0.38220 -0.08090
C37 C 0.4098(3) 0.3006(7) -0.0780(3)
H36 H 0.43630 0.23400 -0.06720
C38 C 0.1368(3) 0.2467(7) -0.0583(3)
C39 C 0.0558(3) 0.2032(7) -0.0802(3)
H37 H 0.05740 0.15160 -0.10570
C40 C -0.0292(4) 0.2393(9) -0.0627(4)
H38 H -0.08470 0.21220 -0.07730
C41 C -0.0317(4) 0.3101(9) -0.0264(4)
H39 H -0.08900 0.33060 -0.01500
C42 C 0.0475(4) 0.3546(8) -0.0048(3)
H40 H 0.04570 0.40730 0.02020
C43 C 0.1319(4) 0.3171(7) -0.0221(3)
H41 H 0.18710 0.34370 -0.00710
C44 C 0.3261(8) -0.1875(11) -0.2951(5)
C45 C 0.3541(8) -0.2271(13) -0.2504(5)
H42 H 0.40440 -0.19600 -0.23220
C46 C 0.3094(11) -0.3093(15) -0.2335(5)
H43 H 0.32840 -0.33600 -0.20230
C47 C 0.2345(10) -0.3614(13) -0.2586(8)
H44 H 0.20400 -0.42110 -0.24500
C48 C 0.2088(11) -0.3207(17) -0.3033(7)
H45 H 0.15870 -0.35190 -0.32150
C49 C 0.2544(9) -0.2362(13) -0.3217(6)
H46 H 0.23710 -0.21000 -0.35330
C50 C 0.3704(6) -0.0942(9) -0.3149(4)
H47 H 0.32540 -0.05080 -0.33390
H48 H 0.41800 -0.11840 -0.33600
H49 H 0.39790 -0.05020 -0.28840
C51 C 0.0141(6) 0.4867(9) -0.1839(4)
C52 C 0.0220(6) 0.5829(9) -0.2094(5)
H50 H 0.00570 0.59270 -0.24290
C53 C 0.0557(12) 0.659(2) -0.1797(8)
H51 H 0.06840 0.72470 -0.19570
C54 C 0.0773(12) 0.6624(19) -0.1279(8)
H52 H 0.09760 0.72550 -0.11080
C55 C 0.0656(16) 0.569(2) -0.1075(9)
H53 H 0.07610 0.56060 -0.07350
C56 C 0.0387(10) 0.4851(18) -0.1350(6)
H54 H 0.03620 0.41680 -0.11930
C57 C -0.0032(11) 0.3880(15) -0.2055(10)
H55 H -0.00950 0.33270 -0.18040
H56 H 0.04730 0.36860 -0.22550
H57 H -0.05980 0.39220 -0.22590
O1B* O 0.48149(18) -0.0274(4) -0.04752(16)
Y1B* Y 0.62427(3) 0.00092(8) -0.00705(3)
N1B* N 0.6248(2) -0.0983(5) -0.0861(2)
P1B* P 0.69313(9) -0.17536(18) -0.11284(8)
C8B* C 0.8107(3) -0.1266(7) -0.1081(3)
C9B* C 0.8484(4) -0.1134(7) -0.0610(3)
H12B* H 0.81180 -0.12520 -0.03420
C10B* C 0.9406(4) -0.0827(7) -0.0529(3)
H13B* H 0.96710 -0.07290 -0.02110
C11B* C 0.9910(4) -0.0674(8) -0.0935(4)
H14B* H 1.05380 -0.04950 -0.08880
C12B* C 0.9541(4) -0.0771(9) -0.1397(4)
H15B* H 0.98980 -0.06200 -0.16660
C13B* C 0.8623(4) -0.1098(7) -0.1472(3)
H16B* H 0.83650 -0.12010 -0.17920
C14B* C 0.7045(3) -0.3099(7) -0.0881(3)
C15B* C 0.6465(4) -0.3466(7) -0.0529(3)
H17B* H 0.60060 -0.29970 -0.04200
C16B* C 0.6552(4) -0.4498(8) -0.0339(3)
H18B* H 0.61520 -0.47360 -0.01020
C17B* C 0.7230(4) -0.5192(8) -0.0496(3)
H19B* H 0.72850 -0.59050 -0.03680
C18B* C 0.7825(4) -0.4837(9) -0.0839(3)
H20B* H 0.82830 -0.53070 -0.09480
C19B* C 0.7740(4) -0.3808(8) -0.1017(3)
H21B* H 0.81640 -0.35600 -0.12400
C20B* C 0.6620(4) -0.1917(8) -0.1760(3)
C21B* C 0.6327(5) -0.2917(9) -0.1958(4)
H22B* H 0.63290 -0.35430 -0.17580
C22B* C 0.6040(6) -0.2994(12) -0.2439(5)
H23B* H 0.58370 -0.36720 -0.25680
C23B* C 0.6043(6) -0.2107(15) -0.2730(5)
H24B* H 0.58430 -0.21700 -0.30620
C24B* C 0.6331(5) -0.1119(11) -0.2549(4)
H25B* H 0.63400 -0.05060 -0.27570
C25B* C 0.6608(4) -0.1020(9) -0.2068(3)
H26B* H 0.67920 -0.03320 -0.19430
Si1B* Si 0.50975(9) -0.07538(18) -0.09910(8)
C6B* C 0.4878(3) 0.0241(7) -0.1480(3)
H6B* H 0.49340 -0.01140 -0.17950
H7B* H 0.42610 0.05340 -0.14620
H8B* H 0.53230 0.08310 -0.14440
C7B* C 0.4450(3) -0.2010(7) -0.1170(3)
H9B* H 0.38280 -0.18160 -0.12830
H10B* H 0.47540 -0.23780 -0.14310
H11B* H 0.44310 -0.24940 -0.08890
C1B* C 0.7311(4) 0.1356(7) -0.0564(3)
H1B* H 0.75770 0.10280 -0.08340
C2B* C 0.6462(4) 0.1903(6) -0.0569(3)
N2B* N 0.7072(2) -0.1154(5) 0.0327(2)
P2B* P 0.75240(9) -0.18967(18) 0.07241(8)
C26B* C 0.7751(4) -0.1270(8) 0.1306(3)
C27B* C 0.7673(4) -0.0164(9) 0.1347(4)
H27B* H 0.75170 0.02540 0.10660
C28B* C 0.7820(4) 0.0360(9) 0.1795(5)
H28B* H 0.77630 0.11250 0.18170
C29B* C 0.8045(6) -0.0237(15) 0.2201(5)
H29B* H 0.81460 0.01120 0.25060
C30B* C 0.8125(7) -0.1350(14) 0.2169(5)
H30B* H 0.82800 -0.17750 0.24480
C31B* C 0.7974(5) -0.1827(10) 0.1718(4)
H31B* H 0.80300 -0.25920 0.16960
C32B* C 0.6855(3) -0.3098(7) 0.0854(3)
C33B* C 0.7216(4) -0.4094(7) 0.1014(3)
H32B* H 0.78570 -0.41690 0.10680
C34B* C 0.6657(4) -0.4973(9) 0.1094(3)
H33B* H 0.69170 -0.56450 0.11970
C35B* C 0.5720(4) -0.4869(9) 0.1025(3)
H34B* H 0.53330 -0.54640 0.10880
C36B* C 0.5351(4) -0.3888(8) 0.0863(3)
H35B* H 0.47090 -0.38220 0.08090
C37B* C 0.5902(3) -0.3006(7) 0.0780(3)
H36B* H 0.56370 -0.23400 0.06720
C38B* C 0.8632(3) -0.2467(7) 0.0583(3)
C39B* C 0.9442(3) -0.2032(7) 0.0802(3)
H37B* H 0.94260 -0.15160 0.10570
C40B* C 1.0292(4) -0.2393(9) 0.0627(4)
H38B* H 1.08470 -0.21220 0.07730
C41B* C 1.0317(4) -0.3101(9) 0.0264(4)
H39B* H 1.08900 -0.33060 0.01500
C42B* C 0.9525(4) -0.3546(8) 0.0048(3)
H40B* H 0.95430 -0.40730 -0.02020
C43B* C 0.8681(4) -0.3171(7) 0.0221(3)
H41B* H 0.81290 -0.34370 0.00710
C3B* C 0.6297(4) 0.2217(6) -0.0097(3)
H2B* H 0.60700 0.20340 -0.08480
H3B* H 0.57640 0.25730 0.00000
C4B* C 0.7059(4) 0.1919(7) 0.0215(3)
C5B* C 0.7677(4) 0.1391(7) -0.0097(3)
H4B* H 0.71420 0.20410 0.05550
H5B* H 0.82570 0.11070 0.00070
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.84
H 0.23
N 0.68
O 0.68
P 1.05
Si 1.20
Y 1.51
|
1100637.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 18:52:13 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177956 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100637.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100637
loop_
_publ_author_name
'Anfang, S.'
'Gr\"ob, T.'
'Harms, K.'
'Seybert, G.'
'Massa, W.'
'Greiner, A.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe von Seltenerdelementen. Die Kristallstrukturen
von [Yb~2~Cp~3~(NPPh~3~)~3~], [YCp(NPPh~3~)(\m-OSiMe~2~NPPh~3~)]~2~ und
[M(NPPh~3~)~2~(\m-OSiMe~2~NPPh~3~)]~2~ mit M = Y und Sm
;
_journal_coden_ASTM ZAACAB
_journal_issue 11
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1853
_journal_page_last 1859
_journal_paper_doi
10.1002/(sici)1521-3749(199911)625:11<1853::aid-zaac1853>3.0.co;2-4
_journal_volume 625
_journal_year 1999
_chemical_formula_sum 'C126 H118 N6 O2 P6 Si2 Y2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 98.716(9)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 18.0406(15)
_cell_length_b 14.0182(8)
_cell_length_c 22.2165(16)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100637
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Y1 Y 1.06083(3) -0.53138(4) 0.94497(2)
P1 P 1.24972(8) -0.62492(12) 0.99396(7)
P2 P 1.05799(8) -0.36790(13) 0.81717(7)
P3 P 0.98295(8) -0.73138(11) 0.83677(7)
Si1 Si 0.93767(8) -0.68285(11) 0.95677(7)
N1 N 1.1691(2) -0.5877(3) 0.9834(2)
N2 N 1.0642(2) -0.4498(4) 0.8632(2)
N3 N 0.9923(2) -0.6756(3) 0.89925(18)
O1 O 0.96243(18) -0.5846(2) 0.99250(16)
C1 C 1.2556(3) -0.7556(4) 1.0007(3)
C2 C 1.1885(4) -0.8033(6) 0.9958(4)
H1 H 1.14280 -0.76830 0.98960
C3 C 1.1865(5) -0.9015(7) 0.9997(5)
H2 H 1.13950 -0.93330 0.99570
C4 C 1.2491(6) -0.9518(6) 1.0089(3)
H3 H 1.24670 -1.01920 1.01250
C5 C 1.3164(5) -0.9085(6) 1.0133(3)
H4 H 1.36140 -0.94480 1.01910
C6 C 1.3189(4) -0.8084(5) 1.0092(3)
H5 H 1.36620 -0.77730 1.01240
C7 C 1.3060(3) -0.5814(4) 1.0639(3)
C8 C 1.2680(4) -0.5411(6) 1.1064(3)
H6 H 1.21490 -0.53600 1.09780
C9 C 1.3047(4) -0.5076(6) 1.1613(3)
H7 H 1.27630 -0.48100 1.18990
C10 C 1.3794(5) -0.5118(5) 1.1754(4)
H8 H 1.40410 -0.48730 1.21300
C11 C 1.4185(4) -0.5515(6) 1.1351(4)
H9 H 1.47160 -0.55520 1.14440
C12 C 1.3824(4) -0.5871(6) 1.0801(4)
H10 H 1.41140 -0.61640 1.05290
C13 C 1.3039(3) -0.5960(5) 0.9327(3)
C14 C 1.3768(4) -0.6248(5) 0.9278(4)
H11 H 1.40420 -0.66170 0.95950
C15 C 1.4100(4) -0.6007(6) 0.8779(4)
H12 H 1.45940 -0.62200 0.87540
C16 C 1.3730(4) -0.5474(7) 0.8328(4)
H13 H 1.39650 -0.53000 0.79890
C17 C 1.3021(4) -0.5186(8) 0.8359(3)
H14 H 1.27530 -0.48250 0.80350
C18 C 1.2685(3) -0.5415(7) 0.8858(3)
H15 H 1.21930 -0.51880 0.88770
C19 C 1.0821(3) -0.4006(5) 0.7438(3)
C20 C 1.0835(4) -0.4968(5) 0.7315(3)
H16 H 1.07320 -0.54140 0.76130
C21 C 1.0999(5) -0.5293(7) 0.6757(4)
H17 H 1.09970 -0.59590 0.66760
C22 C 1.1161(4) -0.4677(8) 0.6330(3)
H18 H 1.12650 -0.49040 0.59480
C23 C 1.1175(5) -0.3733(8) 0.6450(4)
H19 H 1.12940 -0.32930 0.61540
C24 C 1.1016(4) -0.3403(6) 0.7000(3)
H20 H 1.10410 -0.27370 0.70800
C25 C 1.1176(4) -0.2637(6) 0.8393(3)
C26 C 1.1828(4) -0.2777(7) 0.8786(4)
H21 H 1.19560 -0.34010 0.89340
C27 C 1.2311(5) -0.2009(10) 0.8972(5)
H22 H 1.27600 -0.21040 0.92490
C28 C 1.2114(7) -0.1107(10) 0.8740(6)
H23 H 1.24380 -0.05840 0.88590
C29 C 1.1488(7) -0.0962(8) 0.8360(4)
H24 H 1.13600 -0.03400 0.82090
C30 C 1.1019(5) -0.1733(7) 0.8185(4)
H25 H 1.05710 -0.16250 0.79080
C31 C 0.9651(3) -0.3165(4) 0.7988(3)
C32 C 0.9352(4) -0.2750(5) 0.7435(4)
H26 H 0.96590 -0.27060 0.71250
C33 C 0.8639(5) -0.2405(6) 0.7319(5)
H27 H 0.84560 -0.21350 0.69330
C34 C 0.8201(5) -0.2447(6) 0.7745(6)
H28 H 0.77040 -0.22060 0.76610
C35 C 0.8453(4) -0.2834(6) 0.8311(5)
H29 H 0.81360 -0.28580 0.86150
C36 C 0.9183(3) -0.3191(5) 0.8425(3)
H30 H 0.93620 -0.34580 0.88130
C37 C 0.9456(4) -0.8494(5) 0.8417(3)
C38 C 0.8705(5) -0.8701(6) 0.8276(4)
H31 H 0.83670 -0.82210 0.81040
C39 C 0.8439(10) -0.9592(11) 0.8380(6)
H32 H 0.79150 -0.97120 0.82950
C40 C 0.8894(15) -1.0282(11) 0.8596(8)
H33 H 0.86980 -1.09040 0.86330
C41 C 0.9629(10) -1.0127(7) 0.8763(6)
H34 H 0.99480 -1.06150 0.89530
C42 C 0.9916(6) -0.9215(6) 0.8650(4)
H35 H 1.04410 -0.91040 0.87400
C43 C 1.0700(3) -0.7482(5) 0.8091(3)
C44 C 1.1355(4) -0.7296(8) 0.8395(5)
H36 H 1.13770 -0.70210 0.87880
C45 C 1.2023(5) -0.7471(12) 0.8184(7)
H37 H 1.24860 -0.73390 0.84360
C46 C 1.2017(5) -0.7821(8) 0.7634(6)
H38 H 1.24730 -0.79600 0.74860
C47 C 1.1386(5) -0.7970(8) 0.7302(4)
H39 H 1.13760 -0.81990 0.68980
C48 C 1.0722(4) -0.7805(7) 0.7516(4)
H40 H 1.02640 -0.79190 0.72540
C49 C 0.9222(3) -0.6738(4) 0.7761(3)
C50 C 0.8955(4) -0.7191(5) 0.7212(3)
H41 H 0.90510 -0.78520 0.71680
C51 C 0.8556(4) -0.6698(7) 0.6735(3)
H42 H 0.83740 -0.70190 0.63660
C52 C 0.8423(4) -0.5747(7) 0.6793(3)
H43 H 0.81640 -0.54010 0.64580
C53 C 0.8660(3) -0.5295(6) 0.7328(3)
H44 H 0.85460 -0.46400 0.73740
C54 C 0.9065(3) -0.5786(5) 0.7805(3)
H45 H 0.92390 -0.54580 0.81740
C55 C 0.8356(3) -0.6840(5) 0.9298(3)
H46 H 0.82030 -0.74780 0.91460
H47 H 0.82350 -0.63730 0.89690
H48 H 0.80870 -0.66740 0.96350
C56 C 0.9620(4) -0.7885(4) 1.0060(3)
H49 H 0.95120 -0.84680 0.98190
H50 H 0.93220 -0.78800 1.03940
H51 H 1.01550 -0.78660 1.02280
C57 C 1.5805(6) 0.1924(10) 0.9596(5)
C58 C 1.5419(5) 0.1578(8) 1.0047(8)
H52 H 1.52200 0.09420 1.00190
C59 C 1.5321(5) 0.2154(14) 1.0538(6)
H53 H 1.50550 0.19150 1.08490
C60 C 1.5609(8) 0.3075(13) 1.0579(6)
H54 H 1.55420 0.34730 1.09180
C61 C 1.5995(7) 0.3421(8) 1.0128(9)
H55 H 1.61940 0.40570 1.01560
C62 C 1.6093(5) 0.2845(12) 0.9637(6)
H56 H 1.63590 0.30840 0.93260
C63 C 1.5925(11) 0.1451(17) 0.9182(6)
H57 H 1.56910 0.08230 0.92040
H58 H 1.64670 0.13740 0.91980
H59 H 1.57150 0.17640 0.87990
O1B* O 1.03757(18) -0.4154(2) 1.00750(16)
Y1B* Y 0.93917(3) -0.46862(4) 1.05503(2)
N1B* N 0.8309(2) -0.4123(3) 1.0166(2)
P1B* P 0.75028(8) -0.37508(12) 1.00604(7)
C1B* C 0.7444(3) -0.2444(4) 0.9993(3)
C2B* C 0.8115(4) -0.1967(6) 1.0042(4)
H1B* H 0.85720 -0.23170 1.01040
C3B* C 0.8135(5) -0.0985(7) 1.0003(5)
H2B* H 0.86050 -0.06670 1.00430
C4B* C 0.7509(6) -0.0482(6) 0.9911(3)
H3B* H 0.75330 0.01920 0.98750
C5B* C 0.6836(5) -0.0915(6) 0.9867(3)
H4B* H 0.63860 -0.05520 0.98090
C6B* C 0.6811(4) -0.1916(5) 0.9908(3)
H5B* H 0.63380 -0.22270 0.98760
C7B* C 0.6940(3) -0.4186(4) 0.9361(3)
C8B* C 0.7320(4) -0.4589(6) 0.8936(3)
H6B* H 0.78510 -0.46400 0.90220
C9B* C 0.6953(4) -0.4924(6) 0.8387(3)
H7B* H 0.72370 -0.51900 0.81010
C10B* C 0.6206(5) -0.4882(5) 0.8246(4)
H8B* H 0.59590 -0.51270 0.78700
C11B* C 0.5815(4) -0.4485(6) 0.8649(4)
H9B* H 0.52840 -0.44480 0.85560
C12B* C 0.6176(4) -0.4129(6) 0.9199(4)
H10B* H 0.58860 -0.38360 0.94710
C13B* C 0.6961(3) -0.4040(5) 1.0673(3)
C14B* C 0.6232(4) -0.3752(5) 1.0722(4)
H11B* H 0.59580 -0.33830 1.04050
C15B* C 0.5900(4) -0.3993(6) 1.1221(4)
H12B* H 0.54060 -0.37800 1.12460
C16B* C 0.6270(4) -0.4526(7) 1.1672(4)
H13B* H 0.60350 -0.47000 1.20110
C17B* C 0.6979(4) -0.4814(8) 1.1641(3)
H14B* H 0.72470 -0.51750 1.19650
C18B* C 0.7315(3) -0.4585(7) 1.1142(3)
H15B* H 0.78070 -0.48120 1.11230
N2B* N 0.9358(2) -0.5502(4) 1.1368(2)
P2B* P 0.94201(8) -0.63210(13) 1.18283(7)
C19B* C 0.9179(3) -0.5994(5) 1.2562(3)
C20B* C 0.9165(4) -0.5032(5) 1.2685(3)
H16B* H 0.92680 -0.45860 1.23870
C21B* C 0.9001(5) -0.4707(7) 1.3243(4)
H17B* H 0.90030 -0.40410 1.33240
C22B* C 0.8839(4) -0.5323(8) 1.3670(3)
H18B* H 0.87350 -0.50960 1.40520
C23B* C 0.8825(5) -0.6267(8) 1.3550(4)
H19B* H 0.87060 -0.67070 1.38460
C24B* C 0.8984(4) -0.6597(6) 1.3000(3)
H20B* H 0.89590 -0.72630 1.29200
C25B* C 0.8824(4) -0.7363(6) 1.1607(3)
C26B* C 0.8172(4) -0.7223(7) 1.1214(4)
H21B* H 0.80440 -0.65990 1.10660
C27B* C 0.7689(5) -0.7991(10) 1.1028(5)
H22B* H 0.72400 -0.78960 1.07510
C28B* C 0.7886(7) -0.8893(10) 1.1260(6)
H23B* H 0.75620 -0.94160 1.11410
C29B* C 0.8512(7) -0.9038(8) 1.1640(4)
H24B* H 0.86400 -0.96600 1.17910
C30B* C 0.8981(5) -0.8267(7) 1.1815(4)
H25B* H 0.94290 -0.83750 1.20920
C31B* C 1.0349(3) -0.6835(4) 1.2012(3)
C32B* C 1.0648(4) -0.7250(5) 1.2565(4)
H26B* H 1.03410 -0.72940 1.28750
C33B* C 1.1361(5) -0.7595(6) 1.2681(5)
H27B* H 1.15440 -0.78650 1.30670
C34B* C 1.1799(5) -0.7553(6) 1.2255(6)
H28B* H 1.22960 -0.77940 1.23390
C35B* C 1.1547(4) -0.7166(6) 1.1689(5)
H29B* H 1.18640 -0.71420 1.13850
C36B* C 1.0817(3) -0.6809(5) 1.1575(3)
H30B* H 1.06380 -0.65420 1.11870
N3B* N 1.0077(2) -0.3244(3) 1.10075(18)
P3B* P 1.01705(8) -0.26862(11) 1.16323(7)
C37B* C 1.0544(4) -0.1506(5) 1.1583(3)
C38B* C 1.1295(5) -0.1299(6) 1.1724(4)
H31B* H 1.16330 -0.17790 1.18960
C39B* C 1.1561(10) -0.0408(11) 1.1620(6)
H32B* H 1.20850 -0.02880 1.17050
C40B* C 1.1106(15) 0.0282(11) 1.1404(8)
H33B* H 1.13020 0.09040 1.13670
C41B* C 1.0371(10) 0.0127(7) 1.1237(6)
H34B* H 1.00520 0.06150 1.10470
C42B* C 1.0084(6) -0.0785(6) 1.1350(4)
H35B* H 0.95590 -0.08960 1.12600
C43B* C 0.9300(3) -0.2518(5) 1.1909(3)
C44B* C 0.8645(4) -0.2704(8) 1.1605(5)
H36B* H 0.86230 -0.29790 1.12120
C45B* C 0.7977(5) -0.2529(12) 1.1816(7)
H37B* H 0.75140 -0.26610 1.15640
C46B* C 0.7983(5) -0.2179(8) 1.2366(6)
H38B* H 0.75270 -0.20400 1.25140
C47B* C 0.8614(5) -0.2030(8) 1.2698(4)
H39B* H 0.86240 -0.18010 1.31020
C48B* C 0.9278(4) -0.2195(7) 1.2484(4)
H40B* H 0.97360 -0.20810 1.27460
C49B* C 1.0778(3) -0.3262(4) 1.2239(3)
C50B* C 1.1045(4) -0.2809(5) 1.2788(3)
H41B* H 1.09490 -0.21480 1.28320
C51B* C 1.1444(4) -0.3302(7) 1.3265(3)
H42B* H 1.16260 -0.29810 1.36340
C52B* C 1.1577(4) -0.4253(7) 1.3207(3)
H43B* H 1.18360 -0.45990 1.35420
C53B* C 1.1340(3) -0.4705(6) 1.2672(3)
H44B* H 1.14540 -0.53600 1.26260
C54B* C 1.0935(3) -0.4214(5) 1.2195(3)
H45B* H 1.07610 -0.45420 1.18260
Si1B* Si 1.06233(8) -0.31715(11) 1.04323(7)
C55B* C 1.1644(3) -0.3160(5) 1.0702(3)
H46B* H 1.17970 -0.25220 1.08540
H47B* H 1.17650 -0.36270 1.10310
H48B* H 1.19130 -0.33260 1.03650
C56B* C 1.0380(4) -0.2115(4) 0.9940(3)
H49B* H 1.04880 -0.15320 1.01810
H50B* H 1.06780 -0.21200 0.96060
H51B* H 0.98450 -0.21340 0.97720
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
P 1.05
Si 1.20
Y 1.51
|
1100638.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-06 18:52:13 +0200 (Sun, 06 Mar 2016) $
#$Revision: 177956 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100638.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100638
loop_
_publ_author_name
'Anfang, S.'
'Gr\"ob, T.'
'Harms, K.'
'Seybert, G.'
'Massa, W.'
'Greiner, A.'
'Dehnicke, K.'
_publ_section_title
;
Phosphaniminato-Komplexe von Seltenerdelementen. Die Kristallstrukturen
von [Yb~2~Cp~3~(NPPh~3~)~3~], [YCp(NPPh~3~)(\m-OSiMe~2~NPPh~3~)]~2~ und
[M(NPPh~3~)~2~(\m-OSiMe~2~NPPh~3~)]~2~ mit M = Y und Sm
;
_journal_coden_ASTM ZAACAB
_journal_issue 11
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1853
_journal_page_last 1859
_journal_paper_doi
10.1002/(sici)1521-3749(199911)625:11<1853::aid-zaac1853>3.0.co;2-4
_journal_volume 625
_journal_year 1999
_chemical_formula_sum 'C112 H102 N6 O2 P6 Si2 Sm2'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 112.457(8)
_cell_angle_beta 91.948(9)
_cell_angle_gamma 114.974(8)
_cell_formula_units_Z 1
_cell_length_a 13.6337(11)
_cell_length_b 13.6488(9)
_cell_length_c 16.5061(12)
_cod_database_code 1100638
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Si1 Si -0.13614(7) -0.92658(8) 0.42123(5)
O1 O -0.04529(17) -0.93632(19) 0.47921(13)
Sm1 Sm -0.04327(1) -1.11549(1) 0.37896(1)
P1 P 0.18138(7) -1.04658(8) 0.25691(5)
N1 N 0.0873(2) -1.0987(3) 0.30128(19)
C1 C 0.2073(3) -1.1559(3) 0.1672(2)
P2 P -0.19681(7) -1.43390(7) 0.32402(5)
N2 N -0.1656(2) -1.3045(3) 0.34032(19)
C2 C 0.1297(3) -1.2760(4) 0.1328(3)
H1 H 0.06620 -1.29990 0.15720
P3 P -0.27847(6) -1.12663(7) 0.23730(5)
N3 N -0.1775(2) -1.0543(2) 0.32086(16)
C3 C 0.1444(4) -1.3627(4) 0.0621(3)
H2 H 0.09100 -1.44510 0.03860
C4 C 0.2351(5) -1.3289(5) 0.0270(3)
H3 H 0.24360 -1.38790 -0.02180
C5 C 0.3145(4) -1.2106(5) 0.0611(3)
H4 H 0.37830 -1.18810 0.03700
C6 C 0.3008(3) -1.1242(4) 0.1313(2)
H5 H 0.35570 -1.04230 0.15520
C7 C 0.1573(3) -0.9619(3) 0.2024(2)
C8 C 0.1671(3) -0.9765(4) 0.1154(3)
H6 H 0.19470 -1.02890 0.08150
C9 C 0.1374(4) -0.9162(5) 0.0780(3)
H7 H 0.14490 -0.92770 0.01850
C10 C 0.0972(4) -0.8397(4) 0.1242(3)
H8 H 0.07780 -0.79760 0.09780
C11 C 0.0853(4) -0.8256(5) 0.2104(3)
H9 H 0.05670 -0.77380 0.24340
C12 C 0.1146(4) -0.8853(4) 0.2483(3)
H10 H 0.10570 -0.87450 0.30740
C13 C 0.3196(3) -0.9464(3) 0.3322(2)
C14 C 0.3629(4) -0.8239(4) 0.3736(3)
H11 H 0.32380 -0.78760 0.35840
C15 C 0.4651(5) -0.7511(5) 0.4386(3)
H12 H 0.49480 -0.66620 0.46650
C16 C 0.5211(4) -0.8030(6) 0.4614(3)
H13 H 0.58980 -0.75430 0.50520
C17 C 0.4779(3) -0.9254(6) 0.4207(3)
H14 H 0.51670 -0.96120 0.43710
C18 C 0.3784(3) -0.9978(4) 0.3559(3)
H15 H 0.35010 -1.08250 0.32770
C19 C -0.1030(3) -1.4905(3) 0.2733(2)
C20 C -0.1370(4) -1.6104(4) 0.2190(3)
H16 H -0.21280 -1.66790 0.20620
C21 C -0.0619(5) -1.6478(5) 0.1831(4)
H17 H -0.08640 -1.73040 0.14530
C22 C 0.0477(5) -1.5656(6) 0.2023(4)
H18 H 0.09940 -1.59130 0.17790
C23 C 0.0834(4) -1.4456(6) 0.2571(5)
H19 H 0.15960 -1.38870 0.27060
C24 C 0.0075(4) -1.4082(4) 0.2923(4)
H20 H 0.03190 -1.32560 0.32970
C25 C -0.3326(3) -1.5454(3) 0.2479(2)
C26 C -0.4184(3) -1.6277(3) 0.2688(3)
H21 H -0.40550 -1.63170 0.32410
C27 C -0.5217(3) -1.7033(4) 0.2094(3)
H22 H -0.57960 -1.75810 0.22460
C28 C -0.5408(4) -1.6996(4) 0.1290(3)
H23 H -0.61180 -1.75150 0.08850
C29 C -0.4563(4) -1.6200(5) 0.1067(3)
H24 H -0.46890 -1.61900 0.05020
C30 C -0.3542(3) -1.5424(4) 0.1664(2)
H25 H -0.29770 -1.48600 0.15160
C31 C -0.2051(3) -1.4617(3) 0.4238(2)
C32 C -0.2522(4) -1.4065(4) 0.4873(3)
H26 H -0.27960 -1.35780 0.47690
C33 C -0.2597(4) -1.4219(4) 0.5658(3)
H27 H -0.29480 -1.38680 0.60790
C34 C -0.2157(4) -1.4886(5) 0.5817(3)
H28 H -0.21800 -1.49680 0.63640
C35 C -0.1691(4) -1.5428(5) 0.5209(3)
H29 H -0.13990 -1.58950 0.53250
C36 C -0.1640(4) -1.5300(4) 0.4416(3)
H30 H -0.13190 -1.56880 0.39880
C37 C -0.3144(3) -1.0372(3) 0.1970(2)
C38 C -0.3090(4) -1.0428(4) 0.1118(3)
H31 H -0.28190 -1.09240 0.07290
C39 C -0.3429(5) -0.9768(5) 0.0828(3)
H32 H -0.33880 -0.98190 0.02410
C40 C -0.3821(4) -0.9046(4) 0.1373(3)
H33 H -0.40470 -0.85930 0.11700
C41 C -0.3883(4) -0.8984(4) 0.2220(3)
H34 H -0.41580 -0.84870 0.26030
C42 C -0.3554(3) -0.9631(4) 0.2517(2)
H35 H -0.36040 -0.95780 0.31040
C43 C -0.2505(3) -1.2248(3) 0.1421(2)
C44 C -0.3369(3) -1.3302(3) 0.0759(2)
H36 H -0.41150 -1.35260 0.08170
C45 C -0.3151(3) -1.4027(4) 0.0016(2)
H37 H -0.37470 -1.47370 -0.04400
C46 C -0.2075(3) -1.3719(4) -0.0061(2)
H38 H -0.19260 -1.42220 -0.05660
C47 C -0.1211(3) -1.2681(4) 0.0592(2)
H39 H -0.04660 -1.24700 0.05370
C48 C -0.1429(3) -1.1940(4) 0.1336(2)
H40 H -0.08320 -1.12210 0.17830
C49 C -0.4085(2) -1.2261(3) 0.2518(2)
C50 C -0.4056(3) -1.2958(3) 0.2941(2)
H41 H -0.33600 -1.28480 0.31960
C51 C -0.5027(3) -1.3807(4) 0.2994(3)
H42 H -0.50020 -1.42860 0.32790
C52 C -0.6041(3) -1.3961(4) 0.2631(3)
H43 H -0.67120 -1.45530 0.26620
C53 C -0.6083(3) -1.3266(4) 0.2229(3)
H44 H -0.67810 -1.33630 0.19950
C54 C -0.5112(3) -1.2424(4) 0.2160(2)
H45 H -0.51450 -1.19550 0.18680
C55 C -0.2498(3) -0.9271(4) 0.4808(2)
H46 H -0.30610 -1.01030 0.46350
H47 H -0.28410 -0.88520 0.46410
H48 H -0.21910 -0.88620 0.54600
C56 C -0.0721(3) -0.7877(3) 0.4038(3)
H49 H -0.00940 -0.78520 0.37570
H50 H -0.04550 -0.71700 0.46210
H51 H -0.12770 -0.78800 0.36440
O1A* O 0.04529(17) -1.06368(19) 0.52079(13)
Si1A* Si 0.13614(7) -1.07342(8) 0.57877(5)
N3A* N 0.1775(2) -0.9457(2) 0.67914(16)
Sm1A* Sm 0.04327(1) -0.88451(1) 0.62104(1)
N1A* N -0.0873(2) -0.9013(3) 0.69872(19)
P1A* P -0.18138(7) -0.95342(8) 0.74309(5)
C1A* C -0.2073(3) -0.8441(3) 0.8328(2)
C2A* C -0.1297(3) -0.7240(4) 0.8672(3)
H1A* H -0.06620 -0.70010 0.84280
C3A* C -0.1444(4) -0.6373(4) 0.9379(3)
H2A* H -0.09100 -0.55490 0.96140
C4A* C -0.2351(5) -0.6711(5) 0.9730(3)
H3A* H -0.24360 -0.61210 1.02180
C5A* C -0.3145(4) -0.7894(5) 0.9389(3)
H4A* H -0.37830 -0.81190 0.96300
C6A* C -0.3008(3) -0.8758(4) 0.8687(2)
H5A* H -0.35570 -0.95770 0.84480
C7A* C -0.1573(3) -1.0381(3) 0.7976(2)
C8A* C -0.1671(3) -1.0235(4) 0.8846(3)
H6A* H -0.19470 -0.97110 0.91850
C9A* C -0.1374(4) -1.0838(5) 0.9220(3)
H7A* H -0.14490 -1.07230 0.98150
C10A* C -0.0972(4) -1.1603(4) 0.8758(3)
H8A* H -0.07780 -1.20240 0.90220
C11A* C -0.0853(4) -1.1744(5) 0.7896(3)
H9A* H -0.05670 -1.22620 0.75660
C12A* C -0.1146(4) -1.1147(4) 0.7517(3)
H10A* H -0.10570 -1.12550 0.69260
C13A* C -0.3196(3) -1.0536(3) 0.6678(2)
C14A* C -0.3629(4) -1.1761(4) 0.6264(3)
H11A* H -0.32380 -1.21240 0.64160
C15A* C -0.4651(5) -1.2489(5) 0.5614(3)
H12A* H -0.49480 -1.33380 0.53350
C16A* C -0.5211(4) -1.1970(6) 0.5386(3)
H13A* H -0.58980 -1.24570 0.49480
C17A* C -0.4779(3) -1.0746(6) 0.5793(3)
H14A* H -0.51670 -1.03880 0.56290
C18A* C -0.3784(3) -1.0022(4) 0.6441(3)
H15A* H -0.35010 -0.91750 0.67230
N2A* N 0.1656(2) -0.6955(3) 0.65968(19)
P2A* P 0.19681(7) -0.56610(7) 0.67598(5)
C19A* C 0.1030(3) -0.5095(3) 0.7267(2)
C20A* C 0.1370(4) -0.3896(4) 0.7810(3)
H16A* H 0.21280 -0.33210 0.79380
C21A* C 0.0619(5) -0.3522(5) 0.8169(4)
H17A* H 0.08640 -0.26960 0.85470
C22A* C -0.0477(5) -0.4344(6) 0.7977(4)
H18A* H -0.09940 -0.40870 0.82210
C23A* C -0.0834(4) -0.5544(6) 0.7429(5)
H19A* H -0.15960 -0.61130 0.72940
C24A* C -0.0075(4) -0.5918(4) 0.7077(4)
H20A* H -0.03190 -0.67440 0.67030
C25A* C 0.3326(3) -0.4546(3) 0.7521(2)
C26A* C 0.4184(3) -0.3723(3) 0.7312(3)
H21A* H 0.40550 -0.36830 0.67590
C27A* C 0.5217(3) -0.2967(4) 0.7906(3)
H22A* H 0.57960 -0.24190 0.77540
C28A* C 0.5408(4) -0.3004(4) 0.8710(3)
H23A* H 0.61180 -0.24850 0.91150
C29A* C 0.4563(4) -0.3800(5) 0.8933(3)
H24A* H 0.46890 -0.38100 0.94980
C30A* C 0.3542(3) -0.4576(4) 0.8336(2)
H25A* H 0.29770 -0.51400 0.84840
C31A* C 0.2051(3) -0.5383(3) 0.5762(2)
C32A* C 0.2522(4) -0.5935(4) 0.5127(3)
H26A* H 0.27960 -0.64220 0.52310
C33A* C 0.2597(4) -0.5781(4) 0.4342(3)
H27A* H 0.29480 -0.61320 0.39210
C34A* C 0.2157(4) -0.5114(5) 0.4183(3)
H28A* H 0.21800 -0.50320 0.36360
C35A* C 0.1691(4) -0.4572(5) 0.4791(3)
H29A* H 0.13990 -0.41050 0.46750
C36A* C 0.1640(4) -0.4700(4) 0.5584(3)
H30A* H 0.13190 -0.43120 0.60120
P3A* P 0.27847(6) -0.87337(7) 0.76270(5)
C37A* C 0.3144(3) -0.9628(3) 0.8030(2)
C38A* C 0.3090(4) -0.9572(4) 0.8882(3)
H31A* H 0.28190 -0.90760 0.92710
C39A* C 0.3429(5) -1.0232(5) 0.9172(3)
H32A* H 0.33880 -1.01810 0.97590
C40A* C 0.3821(4) -1.0954(4) 0.8627(3)
H33A* H 0.40470 -1.14070 0.88300
C41A* C 0.3883(4) -1.1016(4) 0.7780(3)
H34A* H 0.41580 -1.15130 0.73970
C42A* C 0.3554(3) -1.0369(4) 0.7483(2)
H35A* H 0.36040 -1.04220 0.68960
C43A* C 0.2505(3) -0.7752(3) 0.8579(2)
C44A* C 0.3369(3) -0.6698(3) 0.9241(2)
H36A* H 0.41150 -0.64740 0.91830
C45A* C 0.3151(3) -0.5973(4) 0.9984(2)
H37A* H 0.37470 -0.52630 1.04400
C46A* C 0.2075(3) -0.6281(4) 1.0061(2)
H38A* H 0.19260 -0.57780 1.05660
C47A* C 0.1211(3) -0.7319(4) 0.9408(2)
H39A* H 0.04660 -0.75300 0.94630
C48A* C 0.1429(3) -0.8060(4) 0.8664(2)
H40A* H 0.08320 -0.87790 0.82170
C49A* C 0.4085(2) -0.7739(3) 0.7482(2)
C50A* C 0.4056(3) -0.7042(3) 0.7059(2)
H41A* H 0.33600 -0.71520 0.68040
C51A* C 0.5027(3) -0.6193(4) 0.7006(3)
H42A* H 0.50020 -0.57140 0.67210
C52A* C 0.6041(3) -0.6039(4) 0.7369(3)
H43A* H 0.67120 -0.54470 0.73380
C53A* C 0.6083(3) -0.6734(4) 0.7771(3)
H44A* H 0.67810 -0.66370 0.80050
C54A* C 0.5112(3) -0.7576(4) 0.7840(2)
H45A* H 0.51450 -0.80450 0.81320
C55A* C 0.2498(3) -1.0729(4) 0.5192(2)
H46A* H 0.30610 -0.98970 0.53650
H47A* H 0.28410 -1.11480 0.53590
H48A* H 0.21910 -1.11380 0.45400
C56A* C 0.0721(3) -1.2123(3) 0.5962(3)
H49A* H 0.00940 -1.21480 0.62430
H50A* H 0.04550 -1.28300 0.53790
H51A* H 0.12770 -1.21200 0.63560
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
P 1.05
Si 1.20
Sm 1.59
|
1100639.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 12:31:07 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176952 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100639.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100639
loop_
_publ_author_name
'Grebe, Jutta'
'Schlecht, Sabine'
'Weller, Frank'
'Harms, Klaus'
'Geiseler, Gertraud'
'Dehnicke, Kurt'
_publ_section_title
;
N-Chlortriphenylphosphanimin und seine Anwendung als Edukt zur Synthese
asymmetrischer PNP-Kationen. Kristallstrukturen von Ph~3~PNCl und
[Ph~3~PNPEt~3~]Cl
;
_journal_coden_ASTM ZAACAB
_journal_issue 4
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 633
_journal_page_last 636
_journal_paper_doi
10.1002/(sici)1521-3749(199904)625:4<633::aid-zaac633>3.0.co;2-2
_journal_volume 625
_journal_year 1999
_chemical_formula_sum 'C18 H15 Cl N P'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 93.919(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.4739(8)
_cell_length_b 10.0858(8)
_cell_length_c 14.5229(14)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C18 H15 Cl1 N1 P1'
_cod_database_code 1100639
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
P1 P 0.06642(4) 0.80385(4) 0.21166(3)
Cl1 Cl -0.00489(5) 1.06378(5) 0.17557(4)
N1 N -0.05318(13) 0.89696(15) 0.17919(10)
C1 C 0.12873(15) 0.81513(17) 0.33089(11)
C2 C 0.19639(17) 0.7097(2) 0.37283(12)
C3 C 0.24507(19) 0.7203(2) 0.46369(13)
C4 C 0.22523(19) 0.8340(2) 0.51323(13)
C5 C 0.1571(2) 0.9373(2) 0.47289(14)
C6 C 0.10852(19) 0.9287(2) 0.38175(13)
C7 C -0.00120(15) 0.64117(16) 0.19762(11)
C8 C 0.04176(17) 0.54984(19) 0.13501(13)
C9 C -0.0199(2) 0.4294(2) 0.12294(14)
C10 C -0.12340(19) 0.3998(2) 0.17267(15)
C11 C -0.16631(18) 0.4890(2) 0.23563(14)
C12 C -0.10499(17) 0.60924(19) 0.24845(12)
C13 C 0.20044(15) 0.81896(17) 0.14073(11)
C14 C 0.17383(18) 0.8522(2) 0.04846(12)
C15 C 0.27188(19) 0.8653(2) -0.00988(13)
C16 C 0.39697(19) 0.8439(2) 0.02265(14)
C17 C 0.42438(18) 0.8110(2) 0.11365(14)
C18 C 0.32743(16) 0.7996(2) 0.17335(13)
H1 H 0.065(2) 0.997(2) 0.3547(15)
H2 H 0.254(2) 0.837(2) 0.5749(15)
H3 H 0.2074(19) 0.631(2) 0.3404(14)
H4 H 0.292(2) 0.652(2) 0.4906(15)
H5 H 0.144(2) 1.012(2) 0.5049(16)
H6 H -0.133(2) 0.670(2) 0.2894(15)
H7 H 0.507(2) 0.793(2) 0.1340(16)
H8 H 0.465(2) 0.857(2) -0.0184(15)
H9 H 0.008(2) 0.373(2) 0.0806(15)
H10 H -0.165(2) 0.319(2) 0.1637(15)
H11 H 0.090(2) 0.871(2) 0.0265(14)
H12 H 0.3479(19) 0.7827(19) 0.2385(14)
H13 H 0.111(2) 0.570(2) 0.1031(14)
H14 H 0.252(2) 0.893(2) -0.0717(17)
H15 H -0.237(2) 0.468(2) 0.2684(16)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
N 0.68
P 1.05
|
1100640.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 12:31:07 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176952 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100640.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100640
loop_
_publ_author_name
'Grebe, Jutta'
'Schlecht, Sabine'
'Weller, Frank'
'Harms, Klaus'
'Geiseler, Gertraud'
'Dehnicke, Kurt'
_publ_section_title
;
N-Chlortriphenylphosphanimin und seine Anwendung als Edukt zur Synthese
asymmetrischer PNP-Kationen. Kristallstrukturen von Ph~3~PNCl und
[Ph~3~PNPEt~3~]Cl
;
_journal_coden_ASTM ZAACAB
_journal_issue 4
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 633
_journal_page_last 636
_journal_paper_doi
10.1002/(sici)1521-3749(199904)625:4<633::aid-zaac633>3.0.co;2-2
_journal_volume 625
_journal_year 1999
_chemical_formula_sum 'C24 H30 Cl N P2'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 91.94(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.035(1)
_cell_length_b 8.896(1)
_cell_length_c 25.643(1)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C24 H30 Cl1 N1 P2'
_cod_database_code 1100640
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 x,1/2-y,1/2+z
3 -x,-y,-z
4 -x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Cl1 Cl 0.48316(9) 0.92363(11) 0.34965(4)
N1 N 0.1948(3) 0.8322(3) 0.15908(10)
P1 P 0.28734(8) 0.86425(10) 0.20921(3)
P2 P 0.14381(8) 0.89185(9) 0.10432(3)
C1 C 0.2404(4) 0.7366(4) 0.25931(14)
H1 H 0.30450 0.74540 0.28880
H2 H 0.15270 0.76620 0.27160
C2 C 0.2341(4) 0.5743(4) 0.24216(16)
H3 H 0.21120 0.51150 0.27150
H4 H 0.32020 0.54400 0.22960
H5 H 0.16690 0.56310 0.21440
C3 C 0.2741(4) 1.0507(5) 0.23531(15)
H6 H 0.32700 1.05600 0.26810
H7 H 0.31310 1.12160 0.21090
C4 C 0.1316(4) 1.1003(5) 0.24560(16)
H8 H 0.13220 1.20350 0.25790
H9 H 0.09440 1.03570 0.27190
H10 H 0.07770 1.09320 0.21360
C5 C 0.4612(3) 0.8348(4) 0.19871(15)
H11 H 0.51040 0.84450 0.23220
H12 H 0.47350 0.73170 0.18630
C6 C 0.5213(3) 0.9422(5) 0.15999(15)
H13 H 0.61510 0.91900 0.15660
H14 H 0.51210 1.04460 0.17230
H15 H 0.47520 0.93160 0.12630
C7 C -0.0054(3) 0.7888(3) 0.08665(12)
C8 C -0.0262(3) 0.7248(4) 0.03765(12)
H16 H 0.03630 0.73970 0.01160
C9 C -0.1395(4) 0.6389(4) 0.02709(14)
H17 H -0.15400 0.59650 -0.00620
C10 C -0.2310(4) 0.6153(4) 0.06535(16)
H18 H -0.30640 0.55510 0.05830
C11 C -0.2119(3) 0.6797(4) 0.11355(16)
H19 H -0.27520 0.66550 0.13930
C12 C -0.0997(3) 0.7656(4) 0.12440(13)
H20 H -0.08690 0.80880 0.15760
C13 C 0.2588(3) 0.8590(4) 0.05332(12)
C14 C 0.2625(3) 0.9517(4) 0.00974(13)
H21 H 0.20930 1.03860 0.00770
C15 C 0.3448(4) 0.9154(6) -0.03058(15)
H22 H 0.34810 0.97880 -0.05990
C16 C 0.4219(4) 0.7874(7) -0.0282(2)
H23 H 0.47540 0.76150 -0.05620
C17 C 0.4199(4) 0.6972(6) 0.0157(2)
H24 H 0.47440 0.61130 0.01770
C18 C 0.3390(3) 0.7316(4) 0.05667(15)
H25 H 0.33820 0.66970 0.08640
C19 C 0.1025(3) 1.0882(3) 0.10451(12)
C20 C -0.0298(3) 1.1367(4) 0.10440(13)
H26 H -0.09940 1.06690 0.09920
C21 C -0.0590(4) 1.2871(4) 0.11193(13)
H27 H -0.14820 1.31940 0.11220
C22 C 0.0435(4) 1.3897(4) 0.11904(14)
H28 H 0.02350 1.49170 0.12430
C23 C 0.1749(4) 1.3439(4) 0.11859(14)
H29 H 0.24390 1.41460 0.12330
C24 C 0.2048(3) 1.1935(4) 0.11116(12)
H30 H 0.29420 1.16230 0.11060
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
N 0.68
P 1.05
|
1100641.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-05 02:54:16 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177585 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100641.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100641
loop_
_publ_author_name
'Elschenbroich, Christoph'
'M\"ockel, Reinhart'
'Vasil'kov, Alexander'
'Metz, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Chromium Sandwich Complexes of Polycyclic Aromatic Hydrocarbons:
Triphenylene and Fluoranthene as \h^6^ Ligands
;
_journal_coden_ASTM EJICFO
_journal_issue 10
_journal_name_full 'European Journal of Inorganic Chemistry'
_journal_page_first 1391
_journal_page_last 1401
_journal_paper_doi
10.1002/(sici)1099-0682(199810)1998:10<1391::aid-ejic1391>3.0.co;2-6
_journal_volume 1998
_journal_year 1998
_chemical_formula_sum 'C60 H44 B Cr'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 107.13(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 15.374(2)
_cell_length_b 16.636(2)
_cell_length_c 16.721(4)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C60 H44 B1 Cr1'
_cod_database_code 1100641
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,1/2-y,1/2+z
3 -x,-y,-z
4 -1/2-x,-1/2+y,-1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Cr1 Cr 0.89773(5) 0.03165(4) 0.17061(6)
C1 C 1.0111(3) -0.0358(3) 0.1562(3)
H1 H 1.03310 -0.08640 0.18010
C2 C 1.0435(3) 0.0345(3) 0.2012(3)
H2 H 1.08910 0.03160 0.25380
C3 C 1.0085(3) 0.1087(3) 0.1685(3)
H3 H 1.03060 0.15660 0.19860
C4 C 0.9404(3) 0.1131(3) 0.0909(3)
H4 H 0.91580 0.16390 0.06990
C5 C 0.9080(3) 0.0424(2) 0.0437(3)
C6 C 0.8358(3) 0.0463(2) -0.0373(3)
C7 C 0.7954(3) 0.1192(3) -0.0697(3)
H5 H 0.81450 0.16740 -0.03900
C8 C 0.7286(3) 0.1223(3) -0.1452(3)
H6 H 0.70040 0.17210 -0.16530
C9 C 0.7024(3) 0.0532(3) -0.1918(3)
H7 H 0.65720 0.05580 -0.24460
C10 C 0.7415(3) -0.0187(3) -0.1620(3)
H8 H 0.72350 -0.06580 -0.19480
C11 C 0.8081(3) -0.0245(2) -0.0833(3)
C12 C 0.8488(3) -0.1025(2) -0.0515(3)
C13 C 0.8239(3) -0.1740(3) -0.0969(3)
H9 H 0.77750 -0.17240 -0.14900
C14 C 0.8644(3) -0.2460(3) -0.0684(4)
H10 H 0.84630 -0.29330 -0.10090
C15 C 0.9317(3) -0.2498(3) 0.0079(4)
H11 H 0.96040 -0.29950 0.02750
C16 C 0.9566(3) -0.1817(3) 0.0545(3)
H12 H 1.00230 -0.18490 0.10700
C17 C 0.9165(3) -0.1072(2) 0.0270(3)
C18 C 0.9460(3) -0.0336(3) 0.0753(3)
C19 C 0.8736(3) -0.0256(3) 0.2760(3)
H13 H 0.91150 -0.06120 0.31570
C20 C 0.8818(4) 0.0561(3) 0.2911(4)
H14 H 0.92340 0.07560 0.34130
C21 C 0.8294(3) 0.1100(3) 0.2332(4)
H15 H 0.83580 0.16620 0.24330
C22 C 0.7669(3) 0.0807(3) 0.1598(4)
H16 H 0.73220 0.11770 0.11970
C23 C 0.7545(3) -0.0035(3) 0.1443(4)
C24 C 0.6909(3) -0.0343(3) 0.0664(3)
C25 C 0.6312(3) 0.0181(3) 0.0103(4)
H17 H 0.63090 0.07360 0.02340
C26 C 0.5732(3) -0.0103(4) -0.0634(4)
H18 H 0.53320 0.02530 -0.10140
C27 C 0.5739(4) -0.0911(4) -0.0815(4)
H19 H 0.53430 -0.11070 -0.13270
C28 C 0.6301(3) -0.1433(4) -0.0277(4)
H20 H 0.62900 -0.19870 -0.04190
C29 C 0.6896(3) -0.1164(3) 0.0484(3)
C30 C 0.7474(3) -0.1731(3) 0.1085(3)
C31 C 0.7468(3) -0.2559(3) 0.0926(4)
H21 H 0.70950 -0.27620 0.04070
C32 C 0.7994(4) -0.3086(3) 0.1509(5)
H22 H 0.80000 -0.36420 0.13820
C33 C 0.8507(4) -0.2805(3) 0.2271(4)
H23 H 0.88460 -0.31720 0.26820
C34 C 0.8536(3) -0.2000(3) 0.2447(4)
H24 H 0.89000 -0.18130 0.29760
C35 C 0.8036(3) -0.1449(3) 0.1857(3)
C36 C 0.8104(3) -0.0582(3) 0.2030(3)
B1 B 0.2420(4) 0.5877(3) 0.0264(4)
C37 C 0.1780(3) 0.6014(3) 0.0865(3)
C38 C 0.1841(4) 0.6655(3) 0.1410(4)
H25 H 0.23130 0.70390 0.14650
C39 C 0.1233(4) 0.6756(3) 0.1882(4)
H26 H 0.13010 0.72000 0.22530
C40 C 0.0535(4) 0.6214(4) 0.1811(4)
H27 H 0.01210 0.62810 0.21310
C41 C 0.0445(4) 0.5573(4) 0.1270(4)
H28 H -0.00330 0.51960 0.12120
C42 C 0.1044(3) 0.5486(3) 0.0821(4)
H29 H 0.09650 0.50400 0.04510
C43 C 0.1739(3) 0.5905(3) -0.0716(3)
C44 C 0.1027(3) 0.6466(3) -0.0917(3)
H30 H 0.09410 0.68010 -0.04860
C45 C 0.0445(3) 0.6550(3) -0.1720(4)
H31 H -0.00210 0.69450 -0.18340
C46 C 0.0538(3) 0.6063(3) -0.2355(3)
H32 H 0.01370 0.61180 -0.29050
C47 C 0.1219(3) 0.5495(3) -0.2184(3)
H33 H 0.12900 0.51550 -0.26160
C48 C 0.1808(3) 0.5422(3) -0.1366(3)
H34 H 0.22710 0.50250 -0.12560
C49 C 0.3009(3) 0.5036(3) 0.0490(3)
C50 C 0.3692(3) 0.4838(3) 0.0127(4)
H35 H 0.37900 0.51900 -0.02860
C51 C 0.4238(3) 0.4156(3) 0.0335(4)
H36 H 0.46820 0.40420 0.00590
C52 C 0.4121(4) 0.3649(3) 0.0949(4)
H37 H 0.44930 0.31850 0.11040
C53 C 0.3464(4) 0.3815(3) 0.1338(4)
H38 H 0.33820 0.34660 0.17590
C54 C 0.2920(3) 0.4499(3) 0.1108(3)
H39 H 0.24720 0.46050 0.13820
C55 C 0.3196(3) 0.6585(3) 0.0339(3)
C56 C 0.3313(3) 0.7041(3) -0.0311(3)
H40 H 0.28790 0.69870 -0.08460
C57 C 0.4033(3) 0.7577(3) -0.0227(4)
H41 H 0.40950 0.78610 -0.07000
C58 C 0.4658(3) 0.7691(3) 0.0555(4)
H42 H 0.51420 0.80650 0.06260
C59 C 0.4567(3) 0.7259(3) 0.1218(4)
H43 H 0.49950 0.73300 0.17540
C60 C 0.3856(3) 0.6715(3) 0.1122(3)
H44 H 0.38110 0.64220 0.15960
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
B 0.83
Cr 1.35
|
1100642.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-05 02:54:16 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177585 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100642.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100642
loop_
_publ_author_name
'Elschenbroich, Christoph'
'M\"ockel, Reinhart'
'Vasil'kov, Alexander'
'Metz, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Chromium Sandwich Complexes of Polycyclic Aromatic Hydrocarbons:
Triphenylene and Fluoranthene as \h^6^ Ligands
;
_journal_coden_ASTM EJICFO
_journal_issue 10
_journal_name_full 'European Journal of Inorganic Chemistry'
_journal_page_first 1391
_journal_page_last 1401
_journal_paper_doi
10.1002/(sici)1099-0682(199810)1998:10<1391::aid-ejic1391>3.0.co;2-6
_journal_volume 1998
_journal_year 1998
_chemical_formula_sum 'C33.5 H23 Cr I O0.5'
_space_group_IT_number 43
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 43
_symmetry_space_group_name_Hall 'F 2 -2d'
_symmetry_space_group_name_H-M 'F d d 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 16
_cell_length_a 21.637(1)
_cell_length_b 26.975(2)
_cell_length_c 17.521(1)
_cod_original_formula_sum 'C33.5 H23 Cr1 I1 O0.5'
_cod_database_code 1100642
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,z
3 1/4+x,1/4-y,1/4+z
4 1/4-x,1/4+y,1/4+z
5 x,1/2+y,1/2+z
6 -x,1/2-y,1/2+z
7 1/4+x,-1/4-y,-1/4+z
8 1/4-x,-1/4+y,-1/4+z
9 1/2+x,y,1/2+z
10 1/2-x,-y,1/2+z
11 -1/4+x,1/4-y,-1/4+z
12 -1/4-x,1/4+y,-1/4+z
13 1/2+x,1/2+y,z
14 1/2-x,1/2-y,z
15 -1/4+x,-1/4-y,1/4+z
16 -1/4-x,-1/4+y,1/4+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
I1 I 0.11187(3) 0.33042(2) 0.00817(4)
Cr1 Cr 0.04860(4) 0.24093(3) -0.30421(5)
C1 C -0.0426(3) 0.2097(2) -0.2845(4)
H1 H -0.06950 0.19360 -0.31770
C2 C 0.0032(3) 0.18296(19) -0.2432(4)
H2 H 0.00580 0.14880 -0.24940
C3 C 0.0447(3) 0.2067(2) -0.1936(4)
H3 H 0.07350 0.18810 -0.16670
C4 C 0.0430(3) 0.2589(2) -0.1839(3)
H4 H 0.07140 0.27450 -0.15210
C5 C -0.0023(2) 0.28674(17) -0.2230(3)
C6 C -0.0131(2) 0.34037(17) -0.2291(3)
C7 C 0.0146(3) 0.3808(2) -0.1980(4)
H5 H 0.04770 0.37750 -0.16450
C8 C -0.0085(3) 0.4278(2) -0.2183(4)
H6 H 0.01010 0.45580 -0.19760
C9 C -0.0567(3) 0.4337(2) -0.2666(4)
H7 H -0.07060 0.46550 -0.27800
C10 C -0.0865(3) 0.3921(2) -0.3003(4)
C11 C -0.1369(3) 0.3908(3) -0.3515(4)
H8 H -0.15520 0.42040 -0.36680
C12 C -0.1588(3) 0.3477(3) -0.3786(4)
H9 H -0.19240 0.34850 -0.41160
C13 C -0.1328(3) 0.3006(3) -0.3589(4)
H10 H -0.14830 0.27130 -0.37940
C14 C -0.0846(2) 0.3003(2) -0.3094(3)
C15 C -0.0460(2) 0.26209(19) -0.2729(3)
C16 C -0.0629(2) 0.34604(19) -0.2810(3)
C17 C 0.0502(3) 0.2250(2) -0.4258(3)
H11 H 0.01960 0.21230 -0.45750
C18 C 0.0915(3) 0.1931(2) -0.3860(4)
H12 H 0.08830 0.15900 -0.39250
C19 C 0.1372(3) 0.2123(2) -0.3367(4)
H13 H 0.16330 0.19060 -0.31100
C20 C 0.1441(3) 0.2641(2) -0.3255(4)
H14 H 0.17410 0.27640 -0.29260
C21 C 0.1044(2) 0.29636(17) -0.3654(3)
C22 C 0.1001(2) 0.35095(18) -0.3668(3)
C23 C 0.1340(3) 0.38842(19) -0.3354(3)
H15 H 0.16660 0.38180 -0.30240
C24 C 0.1177(3) 0.4378(2) -0.3545(4)
H16 H 0.14090 0.46360 -0.33410
C25 C 0.0698(3) 0.4488(2) -0.4014(4)
H17 H 0.06030 0.48180 -0.41130
C26 C 0.0335(2) 0.41064(18) -0.4358(3)
C27 C -0.0156(3) 0.4149(2) -0.4871(4)
H18 H -0.02920 0.44610 -0.50190
C28 C -0.0441(3) 0.3732(3) -0.5160(4)
H19 H -0.07650 0.37710 -0.55040
C29 C -0.0254(2) 0.3246(2) -0.4951(4)
H20 H -0.04590 0.29700 -0.51410
C30 C 0.0225(2) 0.31963(17) -0.4471(3)
C31 C 0.0574(2) 0.27731(18) -0.4155(3)
C32 C 0.0514(2) 0.36226(17) -0.4168(3)
C33 C 0.25000 0.25000 -0.1223(11)
O1 O 0.25000 0.25000 -0.1902(12)
C34 C 0.2174(6) 0.2122(6) -0.0833(9)
H21 H 0.24510 0.19510 -0.04940
H22 H 0.20080 0.18910 -0.11960
H23 H 0.18430 0.22670 -0.05430
C34M* C 0.2826(6) 0.2878(6) -0.0833(9)
H21M* H 0.25490 0.30490 -0.04940
H22M* H 0.29920 0.31090 -0.11960
H23M* H 0.31570 0.27330 -0.05430
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cr 1.35
I 1.40
O 0.68
|
1100643.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-05 02:54:16 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177585 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100643.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100643
loop_
_publ_author_name
'Elschenbroich, Christoph'
'M\"ockel, Reinhart'
'Vasil'kov, Alexander'
'Metz, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Chromium Sandwich Complexes of Polycyclic Aromatic Hydrocarbons:
Triphenylene and Fluoranthene as \h^6^ Ligands
;
_journal_coden_ASTM EJICFO
_journal_issue 10
_journal_name_full 'European Journal of Inorganic Chemistry'
_journal_page_first 1391
_journal_page_last 1401
_journal_paper_doi
10.1002/(sici)1099-0682(199810)1998:10<1391::aid-ejic1391>3.0.co;2-6
_journal_volume 1998
_journal_year 1998
_chemical_formula_sum 'C32 H20 Cr I'
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 62
_symmetry_space_group_name_Hall '-P 2ac 2n'
_symmetry_space_group_name_H-M 'P n m a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 22.3915(15)
_cell_length_b 10.1812(8)
_cell_length_c 10.4478(11)
_cod_original_formula_sum 'C32 H20 Cr1 I1'
_cod_database_code 1100643
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2+x,y,1/2-z
3 1/2-x,1/2+y,1/2+z
4 x,1/2-y,z
5 -x,-y,-z
6 -1/2-x,-y,-1/2+z
7 -1/2+x,-1/2-y,-1/2-z
8 -x,-1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
I1 I 0.92531(2) 0.75000 0.30596(4)
Cr1 Cr 0.94128(3) 0.25000 0.33108(6)
C1 C 0.99820(16) 0.3898(4) 0.2369(3)
H1 H 0.99720 0.48400 0.23970
C2 C 1.03130(16) 0.3191(3) 0.3274(3)
H2 H 1.05430 0.36560 0.39030
C3 C 0.8714(4) 0.25000 -0.1303(7)
C4 C 0.8546(3) 0.3757(11) -0.1751(6)
H3 H 0.82920 0.38000 -0.24890
C5 C 0.8735(3) 0.4878(10) -0.1171(6)
H4 H 0.86010 0.56980 -0.15210
C6 C 0.9117(2) 0.4871(6) -0.0077(4)
H5 H 0.92470 0.56680 0.03260
C7 C 0.92912(19) 0.3654(5) 0.0366(3)
C8 C 0.96708(16) 0.3216(4) 0.1424(3)
C9 C 0.9087(3) 0.25000 -0.0240(5)
C10 C 0.88654(16) 0.3901(4) 0.4301(3)
H6 H 0.88800 0.48430 0.42800
C11 C 0.92133(16) 0.3196(3) 0.5186(3)
H7 H 0.94530 0.36660 0.57960
C12 C 0.7453(2) 0.25000 0.0862(5)
C13 C 0.72821(18) 0.3748(5) 0.0404(3)
H8 H 0.69970 0.38110 -0.02810
C14 C 0.7515(2) 0.4873(5) 0.0918(4)
H9 H 0.73940 0.57060 0.05740
C15 C 0.79269(18) 0.4853(4) 0.1941(4)
H10 H 0.80870 0.56530 0.22860
C16 C 0.80909(15) 0.3652(4) 0.2425(3)
C17 C 0.84951(15) 0.3210(3) 0.3447(3)
C18 C 0.7853(2) 0.25000 0.1882(4)
C1C C 0.99820(16) 0.1102(4) 0.2369(3)
H1C H 0.99720 0.01600 0.23970
C2C C 1.03130(16) 0.1809(3) 0.3274(3)
C4C C 0.8546(3) 0.1243(11) -0.1751(6)
H3C H 0.82920 0.12000 -0.24890
C5C C 0.8735(3) 0.0122(10) -0.1171(6)
H4C H 0.86010 -0.06980 -0.15210
C6C C 0.9117(2) 0.0129(6) -0.0077(4)
H5C H 0.92470 -0.06680 0.03260
C7C C 0.92912(19) 0.1346(5) 0.0366(3)
C8C C 0.96708(16) 0.1784(4) 0.1424(3)
C10C C 0.88654(16) 0.1099(4) 0.4301(3)
H6C H 0.88800 0.01570 0.42800
C11C C 0.92133(16) 0.1804(3) 0.5186(3)
C13C C 0.72821(18) 0.1252(5) 0.0404(3)
H8C H 0.69970 0.11890 -0.02810
C14C C 0.7515(2) 0.0127(5) 0.0918(4)
H9C H 0.73940 -0.07060 0.05740
C15C C 0.79269(18) 0.0147(4) 0.1941(4)
H10C H 0.80870 -0.06530 0.22860
C16C C 0.80909(15) 0.1348(4) 0.2425(3)
C17C C 0.84951(15) 0.1790(3) 0.3447(3)
H7C H 0.94530 0.13340 0.57960
H2C H 1.05430 0.13440 0.39030
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cr 1.35
I 1.40
|
1100644.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 02:04:21 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177970 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100644.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100644
loop_
_publ_author_name
'Boche, Gernot'
'Bosold, Ferdinand'
'Hermann, Holger'
'Marsch, Michael'
'Harms, Klaus'
'Lohrenz, J. C. W.'
_publ_section_title
;
Crystal Structure of [2-ZnCl-benzoxazole·2 THF]~2~:
The Remarkable Difference between 2-ZnHal- and 2-Li-oxazoles
;
_journal_coden_ASTM CEUJED
_journal_issue 5
_journal_name_full 'Chemistry - A European Journal'
_journal_page_first 814
_journal_page_last 817
_journal_paper_doi
10.1002/(sici)1521-3765(19980515)4:5<814::aid-chem814>3.0.co;2-f
_journal_volume 4
_journal_year 1998
_chemical_formula_sum 'C30 H40 Cl2 N2 O6 Zn2'
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 86.610(9)
_cell_angle_beta 79.601(13)
_cell_angle_gamma 69.707(9)
_cell_formula_units_Z 1
_cell_length_a 8.6024(18)
_cell_length_b 10.1643(15)
_cell_length_c 10.2254(13)
_cod_database_code 1100644
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
Zn1 Zn 0.02775(3) 0.92287(2) 1.16590(2)
Cl1 Cl -0.11767(8) 0.88337(7) 1.35635(6)
O1 O 0.0957(2) 0.67561(16) 0.99701(16)
C1 C 0.0558(3) 0.8191(2) 0.9970(2)
N1 N -0.0316(2) 1.12909(19) 1.12118(18)
C2 C -0.0546(3) 1.2409(2) 1.2056(2)
C3 C 0.0940(3) 0.6385(2) 0.8692(2)
C4 C 0.1231(3) 0.5074(3) 0.8202(3)
C5 C 0.1101(4) 0.5020(3) 0.6877(3)
C6 C 0.0710(4) 0.6230(3) 0.6099(3)
C7 C -0.0416(3) 1.2459(3) 1.3389(2)
H1 H 0.149(4) 0.429(3) 0.875(3)
H2 H 0.127(4) 0.418(3) 0.652(3)
H3 H 0.058(3) 0.618(3) 0.521(3)
H4 H -0.011(4) 1.162(3) 1.394(3)
O2 O 0.2598(2) 0.8879(2) 1.21566(17)
C8 C 0.3072(4) 0.8560(3) 1.3456(3)
H5 H 0.29560 0.76650 1.37760
H6 H 0.23540 0.92980 1.40940
C9 C 0.4817(5) 0.8479(6) 1.3307(4)
H7 H 0.55150 0.75450 1.35610
H8 H 0.49130 0.91740 1.38840
C10 C 0.5396(4) 0.8759(4) 1.1893(3)
H9 H 0.61350 0.78890 1.14300
H10 H 0.60060 0.94220 1.18260
C11 C 0.3825(3) 0.9371(3) 1.1318(3)
H11 H 0.34510 1.03980 1.13270
H12 H 0.40050 0.90510 1.04000
O3 O 0.5090(5) 0.7559(3) 0.8312(3)
C12 C 0.6292(7) 0.5183(5) 0.7720(4)
H13 H 0.74790 0.46490 0.73990
H14 H 0.57230 0.45320 0.81100
C13 C 0.5478(6) 0.5992(5) 0.6624(4)
H15 H 0.44220 0.58370 0.65940
H16 H 0.62220 0.57210 0.57650
C14 C 0.5158(6) 0.7486(5) 0.6941(4)
H17 H 0.60640 0.77910 0.64570
H18 H 0.40920 0.80900 0.66900
C15 C 0.6122(7) 0.6266(5) 0.8711(4)
H19 H 0.56280 0.60260 0.95930
H20 H 0.72310 0.63060 0.87620
C2A* C 0.0546(3) 0.7591(2) 0.7944(2)
N1A* N 0.0316(2) 0.87091(19) 0.87882(18)
Zn1A* Zn -0.02775(3) 1.07713(2) 0.83410(2)
Cl1A* Cl 0.11767(8) 1.11663(7) 0.64365(6)
C1A* C -0.0558(3) 1.1809(2) 1.0030(2)
O1A* O -0.0957(2) 1.32439(16) 1.00299(16)
C3A* C -0.0940(3) 1.3615(2) 1.1308(2)
C6A* C -0.0710(4) 1.3770(3) 1.3901(3)
C5A* C -0.1101(4) 1.4980(3) 1.3123(3)
C4A* C -0.1231(3) 1.4926(3) 1.1798(3)
H1A* H -0.149(4) 1.571(3) 1.125(3)
H2A* H -0.127(4) 1.582(3) 1.348(3)
H3A* H -0.058(3) 1.382(3) 1.479(3)
O2A* O -0.2598(2) 1.1121(2) 0.78434(17)
C8A* C -0.3072(4) 1.1440(3) 0.6544(3)
H5A* H -0.29560 1.23350 0.62240
H6A* H -0.23540 1.07020 0.59060
C9A* C -0.4817(5) 1.1521(6) 0.6693(4)
H7A* H -0.55150 1.24550 0.64390
H8A* H -0.49130 1.08260 0.61160
C10A* C -0.5396(4) 1.1241(4) 0.8107(3)
H9A* H -0.61350 1.21110 0.85700
H10A* H -0.60060 1.05780 0.81740
C11A* C -0.3825(3) 1.0629(3) 0.8682(3)
H11A* H -0.34510 0.96020 0.86730
H12A* H -0.40050 1.09490 0.96000
C7A* C 0.0416(3) 0.7541(3) 0.6611(2)
H4A* H 0.011(4) 0.838(3) 0.606(3)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
N 0.68
O 0.68
Zn 1.45
|
1100645.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 04:14:33 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177980 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100645.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100645
loop_
_publ_author_name
'Schrey, Anna'
'Osterkamp, Frank'
'Straudi, Alrun'
'Rickert, Corry'
'Wagner, Holger'
'Koert, Ulrich'
'Herrschaft, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Synthesis of Enantiomerically Pure Amino Acids Containing
2,5-Disubstituted THF Rings in the Molecular Backbone
;
_journal_coden_ASTM EJOCFK
_journal_issue 11
_journal_name_full 'European Journal of Organic Chemistry'
_journal_page_first 2977
_journal_page_last 2990
_journal_paper_doi
10.1002/(sici)1099-0690(199911)1999:11<2977::aid-ejoc2977>3.0.co;2-3
_journal_volume 1999
_journal_year 1999
_chemical_formula_sum 'C15 H21 N O4 S'
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 19
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.0799(13)
_cell_length_b 12.9690(15)
_cell_length_c 14.4510(18)
_cod_original_formula_sum 'C15 H21 N1 O4 S1'
_cod_database_code 1100645
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 1/2+x,1/2-y,-z
4 -x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
S1 S 0.10804(6) 0.03883(4) 0.59882(3)
O1 O 0.06877(15) -0.22397(10) 0.60535(10)
O2 O -0.30836(16) -0.19219(9) 0.60284(9)
O3 O 0.26496(17) -0.01034(13) 0.61022(12)
O4 O 0.0423(2) 0.10072(12) 0.67154(9)
N1 N -0.02542(18) -0.05153(11) 0.57576(10)
C1 C -0.2128(2) -0.25140(14) 0.66802(14)
C2 C -0.0616(2) -0.29563(14) 0.62110(14)
C3 C 0.0354(3) -0.14885(14) 0.53695(13)
C4 C -0.2019(2) -0.02122(13) 0.56585(12)
C5 C -0.3145(2) -0.08498(14) 0.62827(13)
C6 C -0.1762(3) -0.18045(17) 0.74984(14)
C7 C 0.1188(2) 0.11784(14) 0.49989(13)
C8 C 0.2066(2) 0.08346(16) 0.42298(15)
C9 C 0.2074(3) 0.14182(16) 0.34342(15)
C10 C 0.1240(2) 0.23655(15) 0.33832(13)
C11 C 0.0380(3) 0.26939(15) 0.41583(15)
C12 C 0.0341(2) 0.21103(15) 0.49639(14)
C13 C 0.1274(3) 0.2998(2) 0.25163(17)
C14 C -0.2585(3) -0.02307(18) 0.46578(14)
C15 C -0.2728(3) -0.08153(16) 0.73092(13)
H1 H -0.286(3) -0.3132(19) 0.6896(17)
H2 H -0.212(3) 0.0495(16) 0.5881(14)
H3 H -0.441(3) -0.0612(16) 0.6136(14)
H4 H 0.261(3) 0.0188(19) 0.4249(17)
H5 H 0.267(3) 0.121(2) 0.2890(19)
H6 H -0.028(3) 0.3355(17) 0.4097(15)
H7 H -0.031(3) 0.233(2) 0.5524(18)
H8 H -0.099(3) -0.3229(16) 0.5596(15)
H9 H -0.009(3) -0.3526(19) 0.6606(16)
H10 H -0.049(3) -0.1741(18) 0.4913(15)
H11 H 0.142(3) -0.1330(18) 0.5059(16)
H12 H -0.055(4) -0.166(2) 0.7520(19)
H13 H -0.197(3) -0.2145(19) 0.8119(19)
H14 H 0.091(4) 0.259(2) 0.195(2)
H15 H 0.051(4) 0.366(2) 0.250(2)
H16 H 0.241(4) 0.326(2) 0.243(2)
H17 H -0.182(3) 0.014(2) 0.4254(19)
H18 H -0.373(4) 0.010(2) 0.4597(17)
H19 H -0.266(3) -0.0974(19) 0.4409(17)
H20 H -0.211(3) -0.022(2) 0.7437(17)
H21 H -0.384(3) -0.0795(18) 0.7679(16)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
S 1.02
|
1100646.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 04:14:33 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177980 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100646.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100646
loop_
_publ_author_name
'Schrey, Anna'
'Osterkamp, Frank'
'Straudi, Alrun'
'Rickert, Corry'
'Wagner, Holger'
'Koert, Ulrich'
'Herrschaft, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Synthesis of Enantiomerically Pure Amino Acids Containing
2,5-Disubstituted THF Rings in the Molecular Backbone
;
_journal_coden_ASTM EJOCFK
_journal_issue 11
_journal_name_full 'European Journal of Organic Chemistry'
_journal_page_first 2977
_journal_page_last 2990
_journal_paper_doi
10.1002/(sici)1099-0690(199911)1999:11<2977::aid-ejoc2977>3.0.co;2-3
_journal_volume 1999
_journal_year 1999
_chemical_formula_sum 'C14 H19 N O4 S'
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 19
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.455(1)
_cell_length_b 11.6555(10)
_cell_length_c 14.3828(10)
_cod_original_formula_sum 'C14 H19 N1 O4 S1'
_cod_database_code 1100646
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 -x,1/2+y,1/2-z
4 1/2+x,1/2-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
S1 S 0.84925(11) 0.02064(8) 0.63183(6)
N1 N 0.9936(3) -0.0705(2) 0.6373(2)
O1 O 0.7057(3) -0.0442(3) 0.6206(2)
C1 C 0.8756(5) 0.1023(3) 0.5295(2)
O2 O 0.8656(4) 0.0971(3) 0.70883(18)
C2 C 0.9596(5) 0.2035(3) 0.5315(3)
H1 H 1.00050 0.23160 0.58860
C3 C 0.9842(6) 0.2640(4) 0.4502(3)
H2 H 1.04310 0.33340 0.45200
O3 O 1.2567(3) -0.2070(2) 0.60523(19)
C4 C 0.9242(5) 0.2251(4) 0.3658(3)
O4 O 0.9428(5) -0.2676(3) 0.6681(3)
H3 H 1.0104(81) -0.2766(58) 0.6946(45)
C5 C 0.8383(6) 0.1231(4) 0.3657(3)
H4 H 0.79590 0.09530 0.30890
C6 C 0.8138(6) 0.0620(4) 0.4461(3)
H5 H 0.75490 -0.00740 0.44470
C7 C 0.9759(5) -0.1862(3) 0.5994(3)
H6 H 0.88500 -0.18520 0.55490
C8 C 1.1243(5) -0.2152(4) 0.5448(3)
H7 H 1.11640 -0.29430 0.51840
C9 C 1.1552(7) -0.1276(4) 0.4669(3)
H8 H 1.20470 -0.16460 0.41220
H9 H 1.05590 -0.08950 0.44730
C10 C 1.2673(6) -0.0428(4) 0.5122(3)
H10 H 1.22470 0.03620 0.50920
H11 H 1.37240 -0.04450 0.48190
C11 C 1.2778(5) -0.0846(3) 0.6128(3)
H12 H 1.38470 -0.06700 0.63900
C12 C 1.1505(5) -0.0358(3) 0.6749(2)
H13 H 1.15730 0.04970 0.67160
C13 C 1.1682(6) -0.0707(4) 0.7769(3)
H14 H 1.16350 -0.15450 0.78200
H15 H 1.08230 -0.03660 0.81340
H16 H 1.27010 -0.04330 0.80060
C14 C 0.9498(7) 0.2897(5) 0.2777(3)
H17 H 0.99960 0.23930 0.23180
H18 H 1.01880 0.35570 0.28970
H19 H 0.84790 0.31670 0.25380
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
S 1.02
|
1100647.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 04:14:33 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177980 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100647.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100647
loop_
_publ_author_name
'Schrey, Anna'
'Osterkamp, Frank'
'Straudi, Alrun'
'Rickert, Corry'
'Wagner, Holger'
'Koert, Ulrich'
'Herrschaft, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Synthesis of Enantiomerically Pure Amino Acids Containing
2,5-Disubstituted THF Rings in the Molecular Backbone
;
_journal_coden_ASTM EJOCFK
_journal_issue 11
_journal_name_full 'European Journal of Organic Chemistry'
_journal_page_first 2977
_journal_page_last 2990
_journal_paper_doi
10.1002/(sici)1099-0690(199911)1999:11<2977::aid-ejoc2977>3.0.co;2-3
_journal_volume 1999
_journal_year 1999
_chemical_formula_sum 'C12 H21 N O5'
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 95.90(1)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.623(1)
_cell_length_b 9.913(1)
_cell_length_c 9.624(1)
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C12 H21 N1 O5'
_cod_database_code 1100647
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
N1 N 0.1369(6) 1.0330(4) 0.6485(4)
H1 H 0.2304(74) 0.9931(63) 0.6244(55)
O1 O 0.4236(4) 1.1358(3) 0.5377(3)
O2 O 0.6262(5) 1.3227(4) 0.4299(5)
O3 O 0.7474(5) 1.1726(4) 0.2990(5)
H2 H 0.8133(83) 1.2292(77) 0.2768(68)
O4 O 0.0461(5) 0.8641(4) 0.7824(4)
O5 O -0.1014(4) 1.0631(4) 0.7593(3)
C1 C 0.6369(6) 1.2096(5) 0.3871(5)
C2 C 0.5235(6) 1.0955(5) 0.4297(5)
H3 H 0.5991(6) 1.0194(5) 0.4620(5)
C3 C 0.3923(6) 1.0492(6) 0.3078(6)
H4 H 0.4099(6) 1.0986(6) 0.2233(6)
H5 H 0.4052(6) 0.9536(6) 0.2903(6)
C4 C 0.2127(6) 1.0794(6) 0.3542(5)
H6 H 0.1563(6) 0.9975(6) 0.3826(5)
H7 H 0.1367(6) 1.1222(6) 0.2800(5)
C5 C 0.2526(6) 1.1746(5) 0.4774(5)
H8 H 0.2576(6) 1.2673(5) 0.4425(5)
C6 C 0.1291(6) 1.1697(5) 0.5911(5)
H9 H 0.0087(6) 1.1872(5) 0.5490(5)
C7 C 0.1781(8) 1.2761(6) 0.7022(7)
H10 H 0.1669(51) 1.3641(6) 0.6608(11)
H11 H 0.2977(20) 1.2624(25) 0.7415(30)
H12 H 0.1007(36) 1.2689(27) 0.7745(22)
C8 C 0.0276(7) 0.9796(6) 0.7336(5)
C9 C -0.2021(6) 1.0445(6) 0.8801(5)
C10 C -0.0771(7) 1.0367(8) 1.0104(6)
H13 H -0.0136(44) 0.9530(22) 1.0119(24)
H14 H -0.1422(10) 1.0417(49) 1.0905(6)
H15 H 0.0046(40) 1.1106(27) 1.0123(25)
C11 C -0.3080(8) 1.1738(7) 0.8777(7)
H16 H -0.3859(44) 1.1710(21) 0.9499(32)
H17 H -0.3759(47) 1.1831(24) 0.7885(19)
H18 H -0.2294(9) 1.2492(8) 0.8930(48)
C12 C -0.321(1) 0.9228(8) 0.8581(9)
H19 H -0.3942(55) 0.9165(34) 0.9332(33)
H20 H -0.2504(10) 0.8428(10) 0.8559(60)
H21 H -0.3938(53) 0.9318(28) 0.7711(30)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100648.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 04:14:33 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177980 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100648.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100648
loop_
_publ_author_name
'Schrey, Anna'
'Osterkamp, Frank'
'Straudi, Alrun'
'Rickert, Corry'
'Wagner, Holger'
'Koert, Ulrich'
'Herrschaft, Bernhard'
'Harms, Klaus'
_publ_section_title
;
Synthesis of Enantiomerically Pure Amino Acids Containing
2,5-Disubstituted THF Rings in the Molecular Backbone
;
_journal_coden_ASTM EJOCFK
_journal_issue 11
_journal_name_full 'European Journal of Organic Chemistry'
_journal_page_first 2977
_journal_page_last 2990
_journal_paper_doi
10.1002/(sici)1099-0690(199911)1999:11<2977::aid-ejoc2977>3.0.co;2-3
_journal_volume 1999
_journal_year 1999
_chemical_formula_sum 'C12 H21 N O5'
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 106.459(8)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.6269(7)
_cell_length_b 9.251(2)
_cell_length_c 9.789(1)
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C12 H21 N1 O5'
_cod_database_code 1100648
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O1 O 0.2111(2) 0.2642(3) 0.4335(3)
O2 O 0.3867(2) 0.1989(3) 0.3168(2)
O3 O 0.5877(2) 0.4181(2) 0.4540(2)
O4 O 0.7003(2) 0.0506(3) 0.1614(2)
O5 O 0.9590(2) 0.1202(3) 0.2661(2)
N1 N 0.7463(2) 0.2212(3) 0.3231(2)
C1 C 0.3531(3) 0.2664(3) 0.4096(2)
C2 C 0.4694(3) 0.3631(3) 0.5161(3)
C3 C 0.7459(3) 0.3658(3) 0.5292(3)
C4 C 0.8360(3) 0.3303(3) 0.4214(3)
C5 C 0.8137(3) 0.1309(3) 0.2513(3)
C6 C 0.7390(3) -0.0546(4) 0.0647(3)
C7 C 0.8353(7) -0.1734(5) 0.1500(6)
C8 C 0.5602(4) 0.2810(4) 0.6501(3)
C9 C 0.7174(3) 0.2396(4) 0.6187(3)
C10 C 0.8689(5) 0.4637(4) 0.3441(4)
C11 C 0.5743(5) -0.1110(8) -0.0159(4)
C12 C 0.8189(8) 0.0191(9) -0.0332(4)
H1 H 0.130(5) 0.217(6) 0.373(4)
H2 H 0.408(4) 0.439(5) 0.545(3)
H3 H 0.802(3) 0.446(3) 0.586(3)
H4 H 0.939(3) 0.288(3) 0.476(3)
H5 H 0.641(3) 0.219(4) 0.298(3)
H6 H 0.77630 -0.21540 0.20980
H7 H 0.93610 -0.13560 0.20820
H8 H 0.85590 -0.24590 0.08720
H9 H 0.51180 -0.03410 -0.07090
H10 H 0.52020 -0.14730 0.05020
H11 H 0.58620 -0.18750 -0.07850
H12 H 0.74940 0.09400 -0.08460
H13 H 0.83920 -0.05000 -0.09930
H14 H 0.91930 0.06070 0.02140
H15 H 0.584(5) 0.341(6) 0.724(4)
H16 H 0.498(4) 0.196(5) 0.670(4)
H17 H 0.807(4) 0.232(5) 0.696(4)
H18 H 0.707(4) 0.145(4) 0.563(3)
H19 H 0.925(4) 0.426(5) 0.273(4)
H20 H 0.773(5) 0.505(5) 0.295(4)
H21 H 0.932(5) 0.540(6) 0.408(4)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100649.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100649.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100649
loop_
_publ_author_name
'Chizuru, Sasaki'
'Soh-ichi, Kitoh'
'Kazuya, Yamada'
'Ko-Ki, Kunimoto'
'Shiro, Maeda'
'Akio, Kuwae'
'Kazuhiko, Hanai'
_publ_section_title
;
Crystal Structure of 2-Trifluoromethyl-4'-dimethylaminoazobenzene
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x1
_journal_page_last x2
_journal_paper_doi 10.2116/analscix.19.x1
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C15 H14 F3 N3 '
_chemical_formula_sum 'C15 H14 F3 N3'
_chemical_formula_weight 293.29
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 61
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 15.625(4)
_cell_length_b 23.028(6)
_cell_length_c 7.685(2)
_cell_measurement_reflns_used 5258
_cell_measurement_temperature 123.2
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.1
_cell_volume 2765(1)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9972
_diffrn_measurement_device_type 'Quantum CCD/Rigaku AFC-7'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.098
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -28
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 5258
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.114
_exptl_absorpt_correction_type none
_exptl_crystal_colour Orange-red
_exptl_crystal_density_diffrn 1.409
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plates
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_min 0.030
_refine_diff_density_max 0.33
_refine_diff_density_min -0.36
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.979
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 246
_refine_ls_number_reflns 2536
_refine_ls_R_factor_gt 0.0486
_refine_ls_shift/su_max 0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0701
_reflns_number_gt 1473
_reflns_number_total 3154
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C15 H14 F3 N3 '
_cod_database_code 1100649
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
1/2-x,-y,1/2+z
-x,-y,-z
1/2-x,1/2+y,z
x,1/2-y,1/2+z
1/2+x,y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F(1) F 0.2506(1) 0.26046(9) 0.5985(3) 0.0347(6) Uani 1.00 d . . .
F(2) F 0.1623(1) 0.20898(9) 0.7428(3) 0.0350(6) Uani 1.00 d . . .
F(3) F 0.2183(2) 0.1755(1) 0.5090(3) 0.0462(7) Uani 1.00 d . . .
N(1) N 0.2259(2) 0.0956(1) 0.8096(4) 0.0222(7) Uani 1.00 d . . .
N(2) N 0.2307(2) 0.0440(1) 0.8677(4) 0.0209(7) Uani 1.00 d . . .
N(3) N -0.0609(2) -0.0957(1) 0.8298(4) 0.0254(8) Uani 1.00 d . . .
C(1) C 0.2352(2) 0.2064(2) 0.6526(5) 0.0254(9) Uani 1.00 d . . .
C(2) C 0.3087(2) 0.1822(1) 0.7540(5) 0.0214(9) Uani 1.00 d . . .
C(3) C 0.3838(2) 0.2149(2) 0.7707(5) 0.0252(10) Uani 1.00 d . . .
C(4) C 0.4511(2) 0.1944(2) 0.8700(5) 0.0264(10) Uani 1.00 d . . .
C(5) C 0.4442(2) 0.1416(2) 0.9544(5) 0.026(1) Uani 1.00 d . . .
C(6) C 0.3715(2) 0.1084(2) 0.9392(5) 0.0242(10) Uani 1.00 d . . .
C(7) C 0.3036(2) 0.1277(2) 0.8361(5) 0.0219(9) Uani 1.00 d . . .
C(8) C 0.1561(2) 0.0107(1) 0.8460(4) 0.0201(9) Uani 1.00 d . . .
C(9) C 0.1569(2) -0.0446(2) 0.9221(5) 0.0226(9) Uani 1.00 d . . .
C(10) C 0.0856(2) -0.0801(2) 0.9161(5) 0.0229(9) Uani 1.00 d . . .
C(11) C 0.0105(2) -0.0618(1) 0.8340(4) 0.0204(9) Uani 1.00 d . . .
C(12) C 0.0106(2) -0.0063(2) 0.7539(5) 0.0234(9) Uani 1.00 d . . .
C(13) C 0.0816(2) 0.0290(1) 0.7612(5) 0.0227(9) Uani 1.00 d . . .
C(14) C -0.0606(3) -0.1522(2) 0.9101(7) 0.036(1) Uani 1.00 d . . .
C(15) C -0.1385(3) -0.0761(2) 0.7425(6) 0.028(1) Uani 1.00 d . . .
H(1) H 0.388(2) 0.250(2) 0.715(5) 0.030(9) Uiso 1.00 d . . .
H(2) H 0.500(2) 0.216(1) 0.880(5) 0.032(9) Uiso 1.00 d . . .
H(3) H 0.486(2) 0.129(2) 1.018(5) 0.031(9) Uiso 1.00 d . . .
H(4) H 0.367(2) 0.071(2) 1.001(5) 0.029(9) Uiso 1.00 d . . .
H(5) H 0.206(2) -0.058(1) 0.978(4) 0.027(7) Uiso 1.00 d . . .
H(6) H 0.088(2) -0.115(1) 0.965(5) 0.027(8) Uiso 1.00 d . . .
H(7) H -0.036(2) 0.006(2) 0.698(5) 0.028(9) Uiso 1.00 d . . .
H(8) H 0.080(2) 0.064(1) 0.711(4) 0.027(8) Uiso 1.00 d . . .
H(9) H -0.050(3) -0.148(2) 1.029(8) 0.04(1) Uiso 1.00 d . . .
H(10) H -0.018(3) -0.175(2) 0.860(5) 0.043(10) Uiso 1.00 d . . .
H(11) H -0.114(3) -0.170(2) 0.894(6) 0.04(1) Uiso 1.00 d . . .
H(12) H -0.156(2) -0.041(2) 0.790(5) 0.034(9) Uiso 1.00 d . . .
H(13) H -0.181(2) -0.104(2) 0.757(6) 0.034(9) Uiso 1.00 d . . .
H(14) H -0.128(2) -0.071(1) 0.625(5) 0.034(8) Uiso 1.00 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100650.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100650.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100650
loop_
_publ_author_name
'Azumaya, Isao'
'Okamoto, Iwao'
'Takayanagi, Hiroaki'
_publ_section_title
;
Spontaneous Optical Resolution of 1,2-Bis(formylamino)benzene in Crystals
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x3
_journal_page_last x4
_journal_paper_doi 10.2116/analscix.19.x3
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C8 H8 N2 O2'
_chemical_formula_sum 'C8 H8 N2 O2'
_chemical_formula_weight 164.16
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 19
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.21(1)
_cell_length_b 6.28(1)
_cell_length_c 8.73(1)
_cell_measurement_reflns_used 18
_cell_measurement_temperature 296.2
_cell_measurement_theta_max 29.1
_cell_measurement_theta_min 27.5
_cell_volume 778(2)
_diffrn_measured_fraction_theta_full 0.2951
_diffrn_measured_fraction_theta_max 0.2951
_diffrn_measurement_device_type 'Rigaku AFC5R'
_diffrn_measurement_method \w-2\q
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 845
_diffrn_reflns_theta_full 67.64
_diffrn_reflns_theta_max 67.64
_diffrn_standards_decay_% 0.13
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.864
_exptl_absorpt_correction_T_max 0.970
_exptl_absorpt_correction_T_min 0.825
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.400
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_size_max 0.200
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.150
_exptl_crystal_size_rad ?
_refine_diff_density_max 0.38
_refine_diff_density_min -0.27
_refine_ls_extinction_coef 0.6(1)
_refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref 1.307
_refine_ls_hydrogen_treatment noref
_refine_ls_number_parameters 110
_refine_ls_number_reflns 827
_refine_ls_R_factor_gt 0.0606
_refine_ls_shift/su_max 0.0002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00533|Fo|^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0984
_reflns_number_gt 783
_reflns_number_total 276
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P 21 21 21 '
_cod_original_formula_sum 'C8 H8 N2 O2 '
_cod_database_code 1100650
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O(1) O 0.6786(2) -0.0087(5) 0.0768(2) 0.0528(7) Uani 1.00 d . . .
O(2) O 0.8028(2) -0.4944(5) -0.1678(2) 0.0582(8) Uani 1.00 d . . .
N(1) N 0.7946(2) -0.0205(5) 0.2561(3) 0.0436(7) Uani 1.00 d . . .
N(2) N 0.8176(2) -0.3905(4) 0.0821(3) 0.0410(7) Uani 1.00 d . . .
C(1) C 0.8727(2) -0.0389(5) 0.1534(3) 0.0408(8) Uani 1.00 d . . .
C(2) C 0.8833(2) -0.2229(4) 0.0642(3) 0.0368(7) Uani 1.00 d . . .
C(3) C 0.9590(2) -0.2411(6) -0.0353(3) 0.0451(9) Uani 1.00 d . . .
C(4) C 1.0225(3) -0.0747(7) -0.0461(4) 0.059(1) Uani 1.00 d . . .
C(5) C 1.0122(2) 0.1054(6) 0.0413(5) 0.063(1) Uani 1.00 d . . .
C(6) C 0.9373(2) 0.1227(5) 0.1441(4) 0.0535(10) Uani 1.00 d . . .
C(7) C 0.7046(2) -0.0068(6) 0.2080(4) 0.0446(9) Uani 1.00 d . . .
C(8) C 0.7809(2) -0.5063(5) -0.0318(4) 0.0461(9) Uani 1.00 d . . .
H(1) H 0.9672 -0.3652 -0.0944 0.0466 Uiso 1.00 calc . . .
H(2) H 1.0732 -0.0813 -0.1145 0.0589 Uiso 1.00 calc . . .
H(3) H 1.0556 0.2150 0.0290 0.0652 Uiso 1.00 calc . . .
H(4) H 0.9331 0.2418 0.2094 0.0578 Uiso 1.00 calc . . .
H(5) H 0.8072 -0.0175 0.3628 0.0413 Uiso 1.00 calc . . .
H(6) H 0.6575 0.0028 0.2857 0.0478 Uiso 1.00 calc . . .
H(7) H 0.7966 -0.4214 0.1833 0.0393 Uiso 1.00 calc . . .
H(8) H 0.7347 -0.6107 -0.0056 0.0469 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.049 0.032
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.031 0.018
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100651.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100651.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100651
loop_
_publ_author_name
'Ryoichi, Nakagaki'
'Shigeru, Kohtani'
'Yuko, Nakamura'
'Michiyo, Okamura'
'Soh-ichi, Kitoh'
'Ko-Ki, Kunimoto'
_publ_section_title
;
Crystal Structure of 4-N,N-Dimethylamino-2,3,5,6-tetrafluorobenzonitrile
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x5
_journal_page_last x6
_journal_paper_doi 10.2116/analscix.19.x5
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C9 H6 F4 N2 '
_chemical_formula_sum 'C9 H6 F4 N2'
_chemical_formula_weight 218.15
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 92.92(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.373(2)
_cell_length_b 10.654(6)
_cell_length_c 20.05(1)
_cell_measurement_reflns_used 3349
_cell_measurement_temperature 116.0
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 6.1
_cell_volume 933.2(9)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.077
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 3349
_diffrn_reflns_theta_full 27.43
_diffrn_reflns_theta_max 27.43
_exptl_absorpt_coefficient_mu 0.151
_exptl_absorpt_correction_type none
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.553
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Plates
_exptl_crystal_F_000 440.00
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.31
_refine_diff_density_min -0.29
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.631
_refine_ls_hydrogen_treatment noref
_refine_ls_number_parameters 136
_refine_ls_number_reflns 1129
_refine_ls_R_factor_gt 0.0726
_refine_ls_shift/su_max 0.0001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0890
_reflns_number_gt 990
_reflns_number_total 1990
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C9 H6 F4 N2 '
_cod_database_code 1100651
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F(1) F 1.6646(3) 0.4427(1) 0.27086(7) 0.0337(4) Uani 1.00 d . . .
F(2) F 1.5085(3) 0.4265(1) 0.14148(7) 0.0347(4) Uani 1.00 d . . .
F(3) F 0.8015(3) 0.1003(1) 0.18985(7) 0.0324(4) Uani 1.00 d . . .
F(4) F 0.9724(3) 0.1176(1) 0.31805(7) 0.0332(4) Uani 1.00 d . . .
N(1) N 1.4913(6) 0.3017(3) 0.4234(1) 0.0539(7) Uani 1.00 d . . .
N(2) N 1.0683(5) 0.2490(2) 0.09234(9) 0.0341(5) Uani 1.00 d . . .
C(1) C 1.4169(6) 0.2936(2) 0.3676(1) 0.0376(6) Uani 1.00 d . . .
C(2) C 1.3242(5) 0.2809(2) 0.2986(1) 0.0288(5) Uani 1.00 d . . .
C(3) C 1.4437(5) 0.3606(2) 0.2504(1) 0.0261(5) Uani 1.00 d . . .
C(4) C 1.3627(5) 0.3516(2) 0.1834(1) 0.0273(5) Uani 1.00 d . . .
C(5) C 1.1441(5) 0.2622(2) 0.1582(1) 0.0268(5) Uani 1.00 d . . .
C(6) C 1.0214(5) 0.1842(2) 0.2082(1) 0.0266(4) Uani 1.00 d . . .
C(7) C 1.1099(5) 0.1935(2) 0.2741(1) 0.0267(5) Uani 1.00 d . . .
C(8) C 1.0566(7) 0.3559(2) 0.0461(1) 0.0390(6) Uani 1.00 d . . .
C(9) C 0.9904(7) 0.1278(2) 0.0624(1) 0.0408(6) Uani 1.00 d . . .
H(1) H 1.2540 0.3928 0.0449 0.0468 Uiso 1.00 calc . . .
H(2) H 0.9928 0.3277 0.0026 0.0468 Uiso 1.00 calc . . .
H(3) H 0.9153 0.4165 0.0607 0.0468 Uiso 1.00 calc . . .
H(4) H 0.8185 0.0936 0.0832 0.0490 Uiso 1.00 calc . . .
H(5) H 0.9423 0.1384 0.0160 0.0490 Uiso 1.00 calc . . .
H(6) H 1.1596 0.0723 0.0686 0.0490 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100652.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100652.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100652
loop_
_publ_author_name
'Fujii, Isao'
'Hirayama, Noriaki'
_publ_section_title
;
Structure of 7-\a-hydroxycholesterol
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x7
_journal_page_last x8
_journal_paper_doi 10.2116/analscix.19.x7
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C28 H50 O3'
_chemical_formula_weight 434.70
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 19
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.5558(5)
_cell_length_b 30.2416(6)
_cell_length_c 6.2872(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 296.2
_cell_measurement_theta_max 16.0
_cell_measurement_theta_min 14.0
_cell_volume 2767.6(2)
_diffrn_measured_fraction_theta_full 0.2869
_diffrn_measured_fraction_theta_max 0.2869
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_limit_h_max 0
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 35
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 0
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 2759
_diffrn_reflns_theta_full 65.00
_diffrn_reflns_theta_max 65.00
_exptl_absorpt_coefficient_mu 0.501
_exptl_absorpt_correction_type none
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.043
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.400
_exptl_crystal_size_min 0.250
_refine_diff_density_max 0.35
_refine_diff_density_min -0.28
_refine_ls_extinction_coef 0.015(5)
_refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref 1.546
_refine_ls_hydrogen_treatment noref
_refine_ls_number_parameters 281
_refine_ls_number_reflns 2725
_refine_ls_R_factor_gt 0.0676
_refine_ls_shift/su_max 0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.03600(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1447
_reflns_number_gt 1254
_reflns_number_total 902
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P 21 21 21 '
_cod_original_formula_sum 'C28 H50 O3 '
_cod_database_code 1100652
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O(3) O 0.4609(3) 0.2340(1) 0.8198(7) 0.126(2) Uani 1.00 d . . .
O(7) O 0.0651(2) 0.3071(1) 0.4651(6) 0.076(1) Uani 1.00 d . . .
O(100) O 0.5665(4) 0.2388(2) 0.1688(8) 0.145(2) Uani 1.00 d . . .
C(1) C 0.3306(4) 0.3409(2) 0.8603(9) 0.082(2) Uani 1.00 d . . .
C(2) C 0.4111(4) 0.3089(2) 0.895(1) 0.097(2) Uani 1.00 d . . .
C(3) C 0.3887(4) 0.2649(2) 0.799(1) 0.086(2) Uani 1.00 d . . .
C(4) C 0.3698(4) 0.2709(2) 0.563(1) 0.087(2) Uani 1.00 d . . .
C(5) C 0.2931(4) 0.3035(2) 0.5205(9) 0.061(2) Uani 1.00 d . . .
C(6) C 0.2237(4) 0.2935(2) 0.3995(9) 0.070(2) Uani 1.00 d . . .
C(7) C 0.1436(4) 0.3226(2) 0.3479(9) 0.068(2) Uani 1.00 d . . .
C(8) C 0.1652(4) 0.3699(2) 0.4012(9) 0.062(2) Uani 1.00 d . . .
C(9) C 0.2120(3) 0.3743(2) 0.6179(8) 0.060(2) Uani 1.00 d . . .
C(10) C 0.3029(4) 0.3486(2) 0.6249(9) 0.065(2) Uani 1.00 d . . .
C(11) C 0.2215(4) 0.4223(2) 0.6917(9) 0.075(2) Uani 1.00 d . . .
C(12) C 0.1338(4) 0.4499(2) 0.6700(9) 0.079(2) Uani 1.00 d . . .
C(13) C 0.0939(4) 0.4479(2) 0.4443(9) 0.067(2) Uani 1.00 d . . .
C(14) C 0.0802(4) 0.3989(2) 0.3899(8) 0.067(2) Uani 1.00 d . . .
C(15) C 0.0212(4) 0.3992(2) 0.1924(10) 0.079(2) Uani 1.00 d . . .
C(16) C -0.0375(4) 0.4414(2) 0.214(1) 0.096(2) Uani 1.00 d . . .
C(17) C -0.0032(4) 0.4665(2) 0.4115(10) 0.077(2) Uani 1.00 d . . .
C(18) C 0.1599(4) 0.4704(2) 0.283(1) 0.094(2) Uani 1.00 d . . .
C(19) C 0.3808(4) 0.3739(2) 0.509(1) 0.093(2) Uani 1.00 d . . .
C(20) C -0.0199(5) 0.5161(2) 0.396(1) 0.095(3) Uani 1.00 d . . .
C(21) C 0.0195(5) 0.5416(2) 0.589(1) 0.137(3) Uani 1.00 d . . .
C(22) C -0.1197(5) 0.5268(2) 0.372(1) 0.122(3) Uani 1.00 d . . .
C(23) C -0.1417(6) 0.5741(2) 0.301(2) 0.152(4) Uani 1.00 d . . .
C(24) C -0.2331(6) 0.5858(3) 0.278(2) 0.175(4) Uani 1.00 d . . .
C(25) C -0.2581(7) 0.6327(4) 0.216(3) 0.203(6) Uani 1.00 d . . .
C(26) C -0.241(1) 0.6383(5) -0.010(3) 0.324(9) Uani 1.00 d . . .
C(27) C -0.3381(9) 0.6458(4) 0.267(3) 0.314(8) Uani 1.00 d . . .
C(100) C 0.6195(6) 0.2756(3) 0.192(2) 0.193(5) Uani 1.00 d . . .
H(1) H 0.279 0.329 0.933 0.098 Uiso 1.00 calc . . .
H(2) H 0.347 0.369 0.922 0.098 Uiso 1.00 calc . . .
H(3) H 0.422 0.306 1.042 0.114 Uiso 1.00 calc . . .
H(4) H 0.464 0.321 0.828 0.114 Uiso 1.00 calc . . .
H(5) H 0.336 0.253 0.867 0.106 Uiso 1.00 calc . . .
H(6) H 0.498 0.242 0.941 0.101 Uiso 1.00 calc . . .
H(7) H 0.353 0.243 0.507 0.099 Uiso 1.00 calc . . .
H(8) H 0.424 0.281 0.496 0.099 Uiso 1.00 calc . . .
H(9) H 0.223 0.265 0.337 0.083 Uiso 1.00 calc . . .
H(10) H 0.016 0.290 0.382 0.101 Uiso 1.00 calc . . .
H(11) H 0.131 0.320 0.200 0.082 Uiso 1.00 calc . . .
H(12) H 0.207 0.381 0.296 0.075 Uiso 1.00 calc . . .
H(13) H 0.172 0.360 0.717 0.073 Uiso 1.00 calc . . .
H(14) H 0.268 0.436 0.612 0.092 Uiso 1.00 calc . . .
H(15) H 0.238 0.422 0.839 0.092 Uiso 1.00 calc . . .
H(16) H 0.088 0.439 0.766 0.093 Uiso 1.00 calc . . .
H(17) H 0.146 0.480 0.704 0.093 Uiso 1.00 calc . . .
H(18) H 0.041 0.388 0.499 0.078 Uiso 1.00 calc . . .
H(19) H -0.017 0.374 0.187 0.093 Uiso 1.00 calc . . .
H(20) H 0.058 0.400 0.068 0.093 Uiso 1.00 calc . . .
H(21) H -0.101 0.434 0.232 0.112 Uiso 1.00 calc . . .
H(22) H -0.031 0.459 0.091 0.112 Uiso 1.00 calc . . .
H(23) H -0.039 0.456 0.528 0.093 Uiso 1.00 calc . . .
H(24) H 0.159 0.502 0.305 0.108 Uiso 1.00 calc . . .
H(25) H 0.221 0.460 0.305 0.108 Uiso 1.00 calc . . .
H(26) H 0.141 0.464 0.143 0.108 Uiso 1.00 calc . . .
H(27) H 0.388 0.402 0.568 0.113 Uiso 1.00 calc . . .
H(28) H 0.437 0.358 0.520 0.113 Uiso 1.00 calc . . .
H(29) H 0.365 0.377 0.361 0.113 Uiso 1.00 calc . . .
H(30) H 0.011 0.527 0.275 0.119 Uiso 1.00 calc . . .
H(31) H -0.007 0.530 0.719 0.164 Uiso 1.00 calc . . .
H(32) H 0.004 0.572 0.579 0.164 Uiso 1.00 calc . . .
H(33) H 0.084 0.539 0.595 0.164 Uiso 1.00 calc . . .
H(34) H -0.145 0.507 0.269 0.142 Uiso 1.00 calc . . .
H(35) H -0.150 0.522 0.505 0.142 Uiso 1.00 calc . . .
H(36) H -0.113 0.578 0.167 0.183 Uiso 1.00 calc . . .
H(37) H -0.116 0.593 0.403 0.183 Uiso 1.00 calc . . .
H(38) H -0.258 0.568 0.167 0.202 Uiso 1.00 calc . . .
H(39) H -0.263 0.579 0.407 0.202 Uiso 1.00 calc . . .
H(40) H -0.218 0.653 0.292 0.263 Uiso 1.00 calc . . .
H(41) H -0.255 0.665 -0.057 0.396 Uiso 1.00 calc . . .
H(42) H -0.180 0.629 -0.037 0.396 Uiso 1.00 calc . . .
H(43) H -0.282 0.616 -0.079 0.396 Uiso 1.00 calc . . .
H(44) H -0.354 0.675 0.219 0.377 Uiso 1.00 calc . . .
H(45) H -0.351 0.645 0.418 0.377 Uiso 1.00 calc . . .
H(46) H -0.385 0.626 0.202 0.377 Uiso 1.00 calc . . .
H(47) H 0.622 0.285 0.337 0.233 Uiso 1.00 calc . . .
H(48) H 0.681 0.270 0.147 0.233 Uiso 1.00 calc . . .
H(49) H 0.596 0.299 0.108 0.233 Uiso 1.00 calc . . .
H(50) H 0.550 0.224 0.259 0.101 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.049 0.032
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
|
1100653.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100653.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100653
loop_
_publ_author_name
'Guillon, Jean'
'Leger, Jean-Michel'
'Sonnet, Pascal'
'Jarry, Christian'
_publ_section_title
;
Crystal Structure of 25-(2-tert-Butoxyethoxy)-27-hydroxycalix[4]arene-crown-6
in the Cone Conformation
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x9
_journal_page_last x10
_journal_paper_doi 10.2116/analscix.19.x9
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C44 H54 O9'
_chemical_formula_weight 726.87
_space_group_IT_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 84.74(2)
_cell_angle_beta 87.840(10)
_cell_angle_gamma 75.77(2)
_cell_formula_units_Z 2
_cell_length_a 10.2140(10)
_cell_length_b 12.734(5)
_cell_length_c 16.062(2)
_cell_measurement_temperature 296(2)
_cell_volume 2016.2(9)
_diffrn_ambient_temperature 296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0145
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 6795
_diffrn_reflns_theta_full 64.88
_diffrn_reflns_theta_max 64.88
_diffrn_reflns_theta_min 2.76
_exptl_absorpt_coefficient_mu 0.667
_exptl_absorpt_correction_T_max 0.9242
_exptl_absorpt_correction_T_min 0.6345
_exptl_crystal_density_diffrn 1.197
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 780
_exptl_crystal_size_max 0.75
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.325
_refine_diff_density_min -0.347
_refine_diff_density_rms 0.060
_refine_ls_extinction_coef 0.024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.069
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 480
_refine_ls_number_reflns 6795
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.069
_refine_ls_R_factor_all 0.1052
_refine_ls_R_factor_gt 0.0880
_refine_ls_shift/su_max 0.178
_refine_ls_shift/su_mean 0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1622P)^2^+0.8043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2599
_refine_ls_wR_factor_ref 0.2807
_reflns_number_gt 5105
_reflns_number_total 6795
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100653
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8106(3) 0.5230(2) 0.19518(17) 0.0592(7) Uani 1 1 d . . .
C2 C 0.7413(3) 0.5498(2) 0.11971(17) 0.0639(7) Uani 1 1 d . . .
C3 C 0.6419(3) 0.6466(3) 0.1121(2) 0.0760(9) Uani 1 1 d . . .
H3 H 0.5958 0.6672 0.0621 0.091 Uiso 1 1 calc R . .
C4 C 0.6103(3) 0.7127(3) 0.1765(2) 0.0823(10) Uani 1 1 d . . .
H4 H 0.5464 0.7787 0.1693 0.099 Uiso 1 1 calc R . .
C5 C 0.6733(3) 0.6807(2) 0.2513(2) 0.0737(8) Uani 1 1 d . . .
H5 H 0.6486 0.7239 0.2957 0.088 Uiso 1 1 calc R . .
C6 C 0.7733(3) 0.5855(2) 0.26231(18) 0.0616(7) Uani 1 1 d . . .
C7 C 0.8369(3) 0.5447(3) 0.34743(18) 0.0698(8) Uani 1 1 d . . .
H7A H 0.9342 0.5221 0.3406 0.084 Uiso 1 1 calc R . .
H7B H 0.8163 0.6036 0.3838 0.084 Uiso 1 1 calc R . .
C8 C 0.7849(3) 0.4502(3) 0.38756(17) 0.0656(7) Uani 1 1 d . . .
C9 C 0.6491(3) 0.4632(3) 0.4073(2) 0.0775(9) Uani 1 1 d . . .
H9 H 0.5903 0.5315 0.3981 0.093 Uiso 1 1 calc R . .
C10 C 0.5999(4) 0.3772(3) 0.4401(2) 0.0874(10) Uani 1 1 d . . .
H10 H 0.5086 0.3878 0.4540 0.105 Uiso 1 1 calc R . .
C11 C 0.6852(4) 0.2747(3) 0.4526(2) 0.0898(10) Uani 1 1 d . . .
H11 H 0.6504 0.2166 0.4739 0.108 Uiso 1 1 calc R . .
C12 C 0.8218(3) 0.2572(3) 0.4339(2) 0.0763(9) Uani 1 1 d . . .
C13 C 0.8701(3) 0.3464(3) 0.40360(17) 0.0656(8) Uani 1 1 d . . .
C14 C 0.9134(4) 0.1426(3) 0.4416(3) 0.0916(11) Uani 1 1 d . . .
H14A H 1.0063 0.1463 0.4303 0.110 Uiso 1 1 calc R . .
H14B H 0.9078 0.1103 0.4983 0.110 Uiso 1 1 calc R . .
C15 C 0.8740(3) 0.0715(3) 0.3810(2) 0.0788(9) Uani 1 1 d . . .
C16 C 0.8186(4) -0.0148(3) 0.4076(3) 0.0898(11) Uani 1 1 d . . .
H16 H 0.8092 -0.0321 0.4646 0.108 Uiso 1 1 calc R . .
C17 C 0.7772(5) -0.0758(3) 0.3526(3) 0.1003(12) Uani 1 1 d . . .
H17 H 0.7419 -0.1342 0.3725 0.120 Uiso 1 1 calc R . .
C18 C 0.7881(4) -0.0503(3) 0.2676(3) 0.0948(11) Uani 1 1 d . . .
H18 H 0.7579 -0.0907 0.2303 0.114 Uiso 1 1 calc R . .
C19 C 0.8442(4) 0.0358(3) 0.2370(2) 0.0818(9) Uani 1 1 d . . .
C20 C 0.8897(3) 0.0936(2) 0.2942(2) 0.0751(8) Uani 1 1 d . . .
C21 C 0.8503(5) 0.0691(3) 0.1449(2) 0.0952(12) Uani 1 1 d . . .
H21A H 0.8282 0.0144 0.1136 0.114 Uiso 1 1 calc R . .
H21B H 0.9413 0.0741 0.1292 0.114 Uiso 1 1 calc R . .
C22 C 0.7520(4) 0.1783(3) 0.1234(2) 0.0782(9) Uani 1 1 d . . .
C23 C 0.6158(4) 0.1936(3) 0.1407(2) 0.0916(11) Uani 1 1 d . . .
H23 H 0.5825 0.1346 0.1619 0.110 Uiso 1 1 calc R . .
C24 C 0.5275(4) 0.2948(4) 0.1272(3) 0.0944(11) Uani 1 1 d . . .
H24 H 0.4356 0.3030 0.1379 0.113 Uiso 1 1 calc R . .
C25 C 0.5756(4) 0.3833(3) 0.0979(2) 0.0812(9) Uani 1 1 d . . .
H25 H 0.5160 0.4515 0.0908 0.097 Uiso 1 1 calc R . .
C26 C 0.7113(3) 0.3727(3) 0.07890(17) 0.0679(8) Uani 1 1 d . . .
C27 C 0.7974(3) 0.2686(3) 0.08971(17) 0.0700(8) Uani 1 1 d . . .
C28 C 0.7644(3) 0.4712(3) 0.05220(18) 0.0729(8) Uani 1 1 d . . .
H28A H 0.7196 0.5078 0.0016 0.087 Uiso 1 1 calc R . .
H28B H 0.8604 0.4484 0.0398 0.087 Uiso 1 1 calc R . .
O29 O 0.9113(2) 0.42921(17) 0.20668(13) 0.0735(6) Uani 1 1 d . . .
C30 C 1.0378(3) 0.4280(4) 0.1658(3) 0.1127(16) Uani 1 1 d . . .
H30A H 1.0888 0.3528 0.1673 0.135 Uiso 1 1 calc R . .
H30B H 1.0196 0.4528 0.1075 0.135 Uiso 1 1 calc R . .
C31 C 1.1213(5) 0.4870(5) 0.1939(3) 0.131(2) Uani 1 1 d . . .
H31A H 1.2131 0.4463 0.1792 0.144 Uiso 1 1 d . . .
H31B H 1.1058 0.5535 0.1576 0.144 Uiso 1 1 d . . .
O32 O 1.1343(4) 0.5155(4) 0.2654(3) 0.0679(10) Uani 1 1 d . . .
C33 C 1.1886(4) 0.6202(4) 0.2685(3) 0.0983(12) Uani 1 1 d . . .
C34 C 1.3016(7) 0.6306(7) 0.2103(5) 0.179(3) Uani 1 1 d . . .
H34A H 1.2671 0.6551 0.1553 0.268 Uiso 1 1 calc R . .
H34B H 1.3650 0.5613 0.2089 0.268 Uiso 1 1 calc R . .
H34C H 1.3458 0.6823 0.2291 0.268 Uiso 1 1 calc R . .
C35 C 1.2275(7) 0.5826(6) 0.3554(4) 0.157(2) Uani 1 1 d . . .
H35A H 1.1482 0.5790 0.3886 0.236 Uiso 1 1 calc R . .
H35B H 1.2713 0.6325 0.3774 0.236 Uiso 1 1 calc R . .
H35C H 1.2883 0.5118 0.3571 0.236 Uiso 1 1 calc R . .
C36 C 1.0881(7) 0.7290(6) 0.2712(5) 0.181(3) Uani 1 1 d . . .
H36A H 1.0596 0.7567 0.2154 0.272 Uiso 1 1 calc R . .
H36B H 1.1298 0.7790 0.2949 0.272 Uiso 1 1 calc R . .
H36C H 1.0112 0.7204 0.3048 0.272 Uiso 1 1 calc R . .
O37 O 1.0072(2) 0.32995(18) 0.38423(12) 0.0714(6) Uani 1 1 d . . .
C38 C 1.0871(3) 0.3340(3) 0.4547(2) 0.0810(9) Uani 1 1 d . . .
H38A H 1.0637 0.2884 0.5018 0.097 Uiso 1 1 calc R . .
H38B H 1.0684 0.4080 0.4706 0.097 Uiso 1 1 calc R . .
C39 C 1.2313(4) 0.2963(4) 0.4338(3) 0.0941(11) Uani 1 1 d . . .
H39A H 1.2517 0.3326 0.3809 0.113 Uiso 1 1 calc R . .
H39B H 1.2854 0.3131 0.4767 0.113 Uiso 1 1 calc R . .
O40 O 1.2613(3) 0.1841(3) 0.4282(2) 0.1074(9) Uani 1 1 d . . .
C41 C 1.3965(6) 0.1350(7) 0.4055(6) 0.188(3) Uani 1 1 d . . .
H41A H 1.4553 0.1262 0.4530 0.226 Uiso 1 1 calc R . .
H41B H 1.4285 0.1793 0.3607 0.226 Uiso 1 1 calc R . .
C42 C 1.3944(11) 0.0213(10) 0.3758(7) 0.263(6) Uani 1 1 d . . .
H42A H 1.4817 -0.0301 0.3819 0.316 Uiso 1 1 calc R . .
H42B H 1.3258 -0.0091 0.4053 0.316 Uiso 1 1 calc R . .
O43 O 1.3619(11) 0.0527(18) 0.2910(7) 0.500(15) Uani 1 1 d . . .
C44 C 1.2819(12) -0.0162(16) 0.2879(11) 0.343(12) Uani 1 1 d . . .
H44A H 1.1970 0.0086 0.3176 0.412 Uiso 1 1 calc R . .
H44B H 1.3261 -0.0890 0.3106 0.412 Uiso 1 1 calc R . .
C45 C 1.2610(11) -0.0120(9) 0.1940(6) 0.215(4) Uani 1 1 d . . .
H45A H 1.2080 -0.0631 0.1839 0.258 Uiso 1 1 calc R . .
H45B H 1.2093 0.0602 0.1749 0.258 Uiso 1 1 calc R . .
O46 O 1.3727(6) -0.0346(5) 0.1501(4) 0.198(2) Uani 1 1 d . . .
C47 C 1.3521(11) -0.0427(7) 0.0601(6) 0.212(4) Uani 1 1 d . . .
H47A H 1.2860 -0.0847 0.0550 0.254 Uiso 1 1 calc R . .
H47B H 1.4364 -0.0812 0.0355 0.254 Uiso 1 1 calc R . .
C48 C 1.3049(8) 0.0666(7) 0.0122(5) 0.172(3) Uani 1 1 d . . .
H48A H 1.3447 0.1191 0.0354 0.206 Uiso 1 1 calc R . .
H48B H 1.3341 0.0618 -0.0458 0.206 Uiso 1 1 calc R . .
O49 O 1.1706(4) 0.0997(3) 0.0165(2) 0.1170(10) Uani 1 1 d . . .
C50 C 1.1157(5) 0.2032(3) -0.0257(3) 0.1008(12) Uani 1 1 d . . .
H50A H 1.1393 0.2025 -0.0847 0.121 Uiso 1 1 calc R . .
H50B H 1.1511 0.2582 -0.0027 0.121 Uiso 1 1 calc R . .
C51 C 0.9665(4) 0.2273(3) -0.0140(2) 0.0901(11) Uani 1 1 d . . .
H51A H 0.9237 0.2876 -0.0530 0.108 Uiso 1 1 calc R . .
H51B H 0.9339 0.1644 -0.0243 0.108 Uiso 1 1 calc R . .
O52 O 0.9338(2) 0.25473(19) 0.07045(13) 0.0762(6) Uani 1 1 d . . .
O53 O 0.9516(2) 0.17318(18) 0.26351(15) 0.0825(7) Uani 1 1 d . . .
H53 H 0.8975 0.2326 0.2636 0.124 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0540(14) 0.0639(16) 0.0593(15) -0.0065(12) -0.0030(11) -0.0130(12)
C2 0.0679(17) 0.0690(17) 0.0564(16) 0.0020(13) -0.0049(12) -0.0218(14)
C3 0.079(2) 0.0713(19) 0.075(2) 0.0139(16) -0.0128(15) -0.0185(15)
C4 0.077(2) 0.0613(18) 0.102(3) 0.0038(17) -0.0084(18) -0.0070(15)
C5 0.0724(19) 0.0607(17) 0.089(2) -0.0156(15) 0.0049(16) -0.0150(14)
C6 0.0588(15) 0.0642(16) 0.0647(16) -0.0122(13) -0.0008(12) -0.0182(12)
C7 0.0731(18) 0.0767(19) 0.0631(17) -0.0236(14) -0.0062(13) -0.0178(15)
C8 0.0673(17) 0.0805(19) 0.0491(14) -0.0180(13) -0.0069(12) -0.0131(14)
C9 0.0697(19) 0.086(2) 0.074(2) -0.0145(16) -0.0031(15) -0.0116(16)
C10 0.067(2) 0.108(3) 0.087(2) -0.010(2) 0.0024(16) -0.0204(19)
C11 0.085(2) 0.103(3) 0.085(2) 0.003(2) -0.0109(18) -0.033(2)
C12 0.078(2) 0.091(2) 0.0599(17) -0.0042(15) -0.0178(14) -0.0196(17)
C13 0.0649(17) 0.084(2) 0.0480(14) -0.0129(13) -0.0106(12) -0.0145(14)
C14 0.093(2) 0.087(2) 0.090(2) 0.0156(19) -0.0316(19) -0.0170(19)
C15 0.0723(19) 0.0663(18) 0.091(2) 0.0085(16) -0.0137(16) -0.0073(15)
C16 0.096(3) 0.072(2) 0.094(3) 0.0177(18) -0.0113(19) -0.0138(18)
C17 0.113(3) 0.068(2) 0.119(3) 0.008(2) -0.001(2) -0.026(2)
C18 0.109(3) 0.0606(19) 0.115(3) -0.0156(19) 0.004(2) -0.0189(18)
C19 0.090(2) 0.0582(17) 0.093(2) -0.0144(16) 0.0112(18) -0.0096(15)
C20 0.0729(19) 0.0561(16) 0.092(2) -0.0038(15) 0.0045(16) -0.0093(14)
C21 0.125(3) 0.072(2) 0.090(3) -0.0284(18) 0.024(2) -0.022(2)
C22 0.096(2) 0.081(2) 0.0646(18) -0.0236(15) 0.0083(16) -0.0300(18)
C23 0.106(3) 0.091(3) 0.091(2) -0.0186(19) 0.007(2) -0.047(2)
C24 0.080(2) 0.112(3) 0.099(3) -0.012(2) -0.0041(19) -0.036(2)
C25 0.077(2) 0.094(2) 0.074(2) -0.0053(17) -0.0134(16) -0.0224(18)
C26 0.0784(19) 0.082(2) 0.0466(14) -0.0103(13) -0.0100(12) -0.0237(15)
C27 0.082(2) 0.086(2) 0.0482(15) -0.0202(14) 0.0004(13) -0.0274(16)
C28 0.083(2) 0.088(2) 0.0476(15) 0.0006(14) -0.0070(13) -0.0210(16)
O29 0.0641(12) 0.0765(13) 0.0738(13) -0.0229(10) -0.0147(9) 0.0021(10)
C30 0.0549(19) 0.159(4) 0.129(3) -0.083(3) 0.0032(19) -0.010(2)
C31 0.129(4) 0.182(5) 0.112(4) -0.072(3) 0.057(3) -0.084(4)
O32 0.068(2) 0.086(3) 0.054(2) -0.007(2) -0.0055(18) -0.024(2)
C33 0.078(2) 0.127(3) 0.101(3) -0.032(2) -0.004(2) -0.038(2)
C34 0.137(5) 0.239(8) 0.197(7) -0.089(6) 0.058(5) -0.099(5)
C35 0.163(5) 0.185(6) 0.140(5) 0.010(4) -0.037(4) -0.075(5)
C36 0.157(6) 0.170(6) 0.180(7) -0.005(5) 0.003(5) 0.024(5)
O37 0.0670(12) 0.0904(14) 0.0523(11) -0.0100(9) -0.0087(9) -0.0077(10)
C38 0.073(2) 0.104(2) 0.0680(19) -0.0154(17) -0.0165(15) -0.0202(17)
C39 0.082(2) 0.115(3) 0.090(3) -0.005(2) -0.0111(18) -0.034(2)
O40 0.0773(16) 0.118(2) 0.117(2) 0.0085(17) -0.0010(14) -0.0099(15)
C41 0.084(3) 0.199(7) 0.273(10) -0.071(7) -0.041(4) 0.006(4)
C42 0.238(11) 0.276(13) 0.203(10) -0.085(9) -0.016(8) 0.101(9)
O43 0.227(9) 1.10(4) 0.189(8) -0.239(15) 0.045(7) -0.128(15)
C44 0.154(9) 0.47(2) 0.306(19) 0.171(18) -0.046(10) 0.040(12)
C45 0.201(9) 0.236(10) 0.161(7) -0.033(7) -0.032(7) 0.047(7)
O46 0.153(4) 0.201(5) 0.195(5) -0.037(4) -0.015(4) 0.051(4)
C47 0.238(10) 0.178(7) 0.168(7) 0.012(6) -0.031(7) 0.044(7)
C48 0.153(6) 0.194(7) 0.157(6) -0.040(5) 0.007(5) -0.013(5)
O49 0.116(2) 0.097(2) 0.125(2) -0.0244(17) 0.0058(18) 0.0024(17)
C50 0.121(3) 0.095(3) 0.084(2) -0.019(2) 0.026(2) -0.023(2)
C51 0.105(3) 0.105(3) 0.0575(18) -0.0175(17) 0.0159(17) -0.019(2)
O52 0.0827(14) 0.0898(15) 0.0585(12) -0.0199(10) 0.0046(10) -0.0216(11)
O53 0.0916(16) 0.0736(14) 0.0841(15) -0.0079(12) 0.0091(12) -0.0250(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O29 C1 C6 118.1(2) . . ?
O29 C1 C2 120.6(2) . . ?
C6 C1 C2 121.2(3) . . ?
C3 C2 C1 117.5(3) . . ?
C3 C2 C28 121.2(3) . . ?
C1 C2 C28 121.1(3) . . ?
C4 C3 C2 121.6(3) . . ?
C5 C4 C3 119.6(3) . . ?
C4 C5 C6 121.3(3) . . ?
C5 C6 C1 118.7(3) . . ?
C5 C6 C7 121.6(3) . . ?
C1 C6 C7 119.6(3) . . ?
C8 C7 C6 111.4(2) . . ?
C9 C8 C13 117.5(3) . . ?
C9 C8 C7 120.6(3) . . ?
C13 C8 C7 121.9(3) . . ?
C10 C9 C8 121.1(3) . . ?
C9 C10 C11 120.3(3) . . ?
C12 C11 C10 121.0(4) . . ?
C11 C12 C13 117.7(3) . . ?
C11 C12 C14 120.6(3) . . ?
C13 C12 C14 121.6(3) . . ?
C12 C13 O37 118.3(3) . . ?
C12 C13 C8 122.3(3) . . ?
O37 C13 C8 119.2(3) . . ?
C15 C14 C12 111.5(3) . . ?
C16 C15 C20 117.3(3) . . ?
C16 C15 C14 122.3(4) . . ?
C20 C15 C14 120.4(3) . . ?
C17 C16 C15 122.2(4) . . ?
C16 C17 C18 119.8(4) . . ?
C17 C18 C19 120.5(4) . . ?
C20 C19 C18 118.3(4) . . ?
C20 C19 C21 120.1(3) . . ?
C18 C19 C21 121.6(4) . . ?
O53 C20 C19 117.7(3) . . ?
O53 C20 C15 120.6(3) . . ?
C19 C20 C15 121.8(3) . . ?
C19 C21 C22 110.7(3) . . ?
C23 C22 C27 117.5(3) . . ?
C23 C22 C21 121.2(3) . . ?
C27 C22 C21 121.2(3) . . ?
C22 C23 C24 121.3(4) . . ?
C25 C24 C23 120.1(4) . . ?
C24 C25 C26 121.1(4) . . ?
C25 C26 C27 117.6(3) . . ?
C25 C26 C28 120.7(3) . . ?
C27 C26 C28 121.6(3) . . ?
O52 C27 C26 119.2(3) . . ?
O52 C27 C22 118.5(3) . . ?
C26 C27 C22 122.2(3) . . ?
C26 C28 C2 111.4(2) . . ?
C1 O29 C30 117.3(3) . . ?
C31 C30 O29 120.1(3) . . ?
O32 C31 C30 131.0(5) . . ?
C31 O32 C33 116.2(5) . . ?
C35 C33 C34 115.2(5) . . ?
C35 C33 C36 106.5(5) . . ?
C34 C33 C36 109.8(6) . . ?
C35 C33 O32 87.9(4) . . ?
C34 C33 O32 116.5(4) . . ?
C36 C33 O32 118.8(4) . . ?
C13 O37 C38 113.1(2) . . ?
O37 C38 C39 110.0(3) . . ?
O40 C39 C38 108.6(3) . . ?
C39 O40 C41 115.8(5) . . ?
O40 C41 C42 105.9(6) . . ?
O43 C42 C41 99.5(12) . . ?
O43 C42 C44 41.7(9) . . ?
C41 C42 C44 130.0(8) . . ?
C44 O43 C42 93.9(16) . . ?
O43 C44 C45 101.4(12) . . ?
O43 C44 C42 44.4(9) . . ?
C45 C44 C42 144.3(12) . . ?
O46 C45 C44 114.1(9) . . ?
C45 O46 C47 113.9(7) . . ?
O46 C47 C48 112.8(8) . . ?
O49 C48 C47 110.2(8) . . ?
C48 O49 C50 114.7(5) . . ?
O49 C50 C51 107.5(4) . . ?
O52 C51 C50 108.6(3) . . ?
C27 O52 C51 112.7(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O29 1.375(3) . ?
C1 C6 1.385(4) . ?
C1 C2 1.399(4) . ?
C2 C3 1.389(4) . ?
C2 C28 1.515(4) . ?
C3 C4 1.373(5) . ?
C4 C5 1.365(5) . ?
C5 C6 1.382(4) . ?
C6 C7 1.527(4) . ?
C7 C8 1.514(5) . ?
C8 C9 1.384(4) . ?
C8 C13 1.400(4) . ?
C9 C10 1.369(5) . ?
C10 C11 1.382(5) . ?
C11 C12 1.383(5) . ?
C12 C13 1.388(5) . ?
C12 C14 1.525(5) . ?
C13 O37 1.391(4) . ?
C14 C15 1.516(5) . ?
C15 C16 1.382(5) . ?
C15 C20 1.408(5) . ?
C16 C17 1.370(6) . ?
C17 C18 1.382(6) . ?
C18 C19 1.400(5) . ?
C19 C20 1.388(5) . ?
C19 C21 1.504(5) . ?
C20 O53 1.368(4) . ?
C21 C22 1.521(5) . ?
C22 C23 1.378(5) . ?
C22 C27 1.400(5) . ?
C23 C24 1.384(6) . ?
C24 C25 1.375(5) . ?
C25 C26 1.384(5) . ?
C26 C27 1.398(5) . ?
C26 C28 1.507(5) . ?
C27 O52 1.387(4) . ?
O29 C30 1.425(5) . ?
C30 C31 1.379(6) . ?
C31 O32 1.257(6) . ?
O32 C33 1.570(6) . ?
C33 C35 1.470(7) . ?
C33 C34 1.481(7) . ?
C33 C36 1.512(8) . ?
O37 C38 1.432(3) . ?
C38 C39 1.469(5) . ?
C39 O40 1.396(5) . ?
O40 C41 1.417(7) . ?
C41 C42 1.571(13) . ?
C42 O43 1.412(15) . ?
C42 C44 2.01(2) . ?
O43 C44 1.34(2) . ?
C44 C45 1.525(17) . ?
C45 O46 1.303(10) . ?
O46 C47 1.484(9) . ?
C47 C48 1.504(10) . ?
C48 O49 1.334(7) . ?
O49 C50 1.419(5) . ?
C50 C51 1.487(6) . ?
C51 O52 1.438(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O29 C1 C2 C3 -179.1(3) . . . . ?
C6 C1 C2 C3 5.8(4) . . . . ?
O29 C1 C2 C28 6.5(4) . . . . ?
C6 C1 C2 C28 -168.6(3) . . . . ?
C1 C2 C3 C4 -1.5(5) . . . . ?
C28 C2 C3 C4 172.9(3) . . . . ?
C2 C3 C4 C5 -2.9(5) . . . . ?
C3 C4 C5 C6 3.1(5) . . . . ?
C4 C5 C6 C1 1.1(5) . . . . ?
C4 C5 C6 C7 -175.3(3) . . . . ?
O29 C1 C6 C5 179.2(3) . . . . ?
C2 C1 C6 C5 -5.6(4) . . . . ?
O29 C1 C6 C7 -4.4(4) . . . . ?
C2 C1 C6 C7 170.8(3) . . . . ?
C5 C6 C7 C8 104.6(3) . . . . ?
C1 C6 C7 C8 -71.7(3) . . . . ?
C6 C7 C8 C9 -61.8(3) . . . . ?
C6 C7 C8 C13 116.1(3) . . . . ?
C13 C8 C9 C10 -1.0(4) . . . . ?
C7 C8 C9 C10 177.0(3) . . . . ?
C8 C9 C10 C11 -1.3(5) . . . . ?
C9 C10 C11 C12 1.3(6) . . . . ?
C10 C11 C12 C13 1.0(5) . . . . ?
C10 C11 C12 C14 -175.3(3) . . . . ?
C11 C12 C13 O37 -179.7(3) . . . . ?
C14 C12 C13 O37 -3.5(4) . . . . ?
C11 C12 C13 C8 -3.4(4) . . . . ?
C14 C12 C13 C8 172.9(3) . . . . ?
C9 C8 C13 C12 3.4(4) . . . . ?
C7 C8 C13 C12 -174.6(3) . . . . ?
C9 C8 C13 O37 179.7(2) . . . . ?
C7 C8 C13 O37 1.7(4) . . . . ?
C11 C12 C14 C15 63.4(4) . . . . ?
C13 C12 C14 C15 -112.7(4) . . . . ?
C12 C14 C15 C16 -111.5(4) . . . . ?
C12 C14 C15 C20 66.8(4) . . . . ?
C20 C15 C16 C17 -1.5(5) . . . . ?
C14 C15 C16 C17 176.9(3) . . . . ?
C15 C16 C17 C18 -1.2(6) . . . . ?
C16 C17 C18 C19 1.6(6) . . . . ?
C17 C18 C19 C20 0.7(6) . . . . ?
C17 C18 C19 C21 -176.6(4) . . . . ?
C18 C19 C20 O53 176.2(3) . . . . ?
C21 C19 C20 O53 -6.5(5) . . . . ?
C18 C19 C20 C15 -3.5(5) . . . . ?
C21 C19 C20 C15 173.9(3) . . . . ?
C16 C15 C20 O53 -175.8(3) . . . . ?
C14 C15 C20 O53 5.8(5) . . . . ?
C16 C15 C20 C19 3.9(5) . . . . ?
C14 C15 C20 C19 -174.6(3) . . . . ?
C20 C19 C21 C22 -67.9(5) . . . . ?
C18 C19 C21 C22 109.4(4) . . . . ?
C19 C21 C22 C23 -58.2(5) . . . . ?
C19 C21 C22 C27 118.1(4) . . . . ?
C27 C22 C23 C24 -1.5(5) . . . . ?
C21 C22 C23 C24 174.9(3) . . . . ?
C22 C23 C24 C25 -1.7(6) . . . . ?
C23 C24 C25 C26 2.1(6) . . . . ?
C24 C25 C26 C27 0.6(5) . . . . ?
C24 C25 C26 C28 -176.0(3) . . . . ?
C25 C26 C27 O52 179.3(2) . . . . ?
C28 C26 C27 O52 -4.1(4) . . . . ?
C25 C26 C27 C22 -4.0(4) . . . . ?
C28 C26 C27 C22 172.6(3) . . . . ?
C23 C22 C27 O52 -178.9(3) . . . . ?
C21 C22 C27 O52 4.7(4) . . . . ?
C23 C22 C27 C26 4.4(4) . . . . ?
C21 C22 C27 C26 -172.1(3) . . . . ?
C25 C26 C28 C2 60.8(4) . . . . ?
C27 C26 C28 C2 -115.7(3) . . . . ?
C3 C2 C28 C26 -105.9(3) . . . . ?
C1 C2 C28 C26 68.3(4) . . . . ?
C6 C1 O29 C30 -109.7(3) . . . . ?
C2 C1 O29 C30 75.1(3) . . . . ?
C1 O29 C30 C31 72.2(6) . . . . ?
O29 C30 C31 O32 27.8(11) . . . . ?
C30 C31 O32 C33 -154.3(6) . . . . ?
C31 O32 C33 C35 -159.7(5) . . . . ?
C31 O32 C33 C34 -42.4(7) . . . . ?
C31 O32 C33 C36 92.6(6) . . . . ?
C12 C13 O37 C38 -86.3(3) . . . . ?
C8 C13 O37 C38 97.3(3) . . . . ?
C13 O37 C38 C39 169.5(3) . . . . ?
O37 C38 C39 O40 -71.5(4) . . . . ?
C38 C39 O40 C41 178.0(5) . . . . ?
C39 O40 C41 C42 -162.4(6) . . . . ?
O40 C41 C42 O43 86.5(9) . . . . ?
O40 C41 C42 C44 54.5(14) . . . . ?
C41 C42 O43 C44 -142.4(12) . . . . ?
C42 O43 C44 C45 -167.9(8) . . . . ?
C41 C42 C44 O43 51.8(16) . . . . ?
O43 C42 C44 C45 20.6(16) . . . . ?
C41 C42 C44 C45 72(2) . . . . ?
O43 C44 C45 O46 55.1(16) . . . . ?
C42 C44 C45 O46 41(2) . . . . ?
C44 C45 O46 C47 173.5(11) . . . . ?
C45 O46 C47 C48 76.6(11) . . . . ?
O46 C47 C48 O49 -87.0(9) . . . . ?
C47 C48 O49 C50 179.0(6) . . . . ?
C48 O49 C50 C51 -179.5(4) . . . . ?
O49 C50 C51 O52 74.2(4) . . . . ?
C26 C27 O52 C51 -92.6(3) . . . . ?
C22 C27 O52 C51 90.6(3) . . . . ?
C50 C51 O52 C27 -174.3(3) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21122561
|
1100654.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100654.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100654
loop_
_publ_author_name
'Yoon, I.'
'Park, K.-M.'
'Bark, K.-M.'
'Yang, M. S.'
'Lee, S. S.'
_publ_section_title
;
Crystal Structure of a Fluoroquinolone Antibiotic, Enoxacin
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x11
_journal_page_last x12
_journal_paper_doi 10.2116/analscix.19.x11
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C31 H44 F2 N8 O10'
_chemical_formula_sum 'C31 H44 F2 N8 O10'
_chemical_name_common Enoxacin
_chemical_name_systematic
'1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazin-yl)-1,8-naphthyridine-3-carboxylic acid'
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_cell_angle_alpha 90
_cell_angle_beta 100.903(1)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.4053(6)
_cell_length_b 22.1236(16)
_cell_length_c 17.1548(12)
_cell_volume 3132.4(4)
_exptl_crystal_density_diffrn 1.541
_refine_ls_R_factor_gt 0.0683
_refine_ls_wR_factor_gt 0.224
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100654
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,-1/2-y,-1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
F(1A) F 0.2144(2) 0.741(1) 0.6097(1) 0.016(1)
O(1A) O 0.4005(3) 0.9103(1) 0.4559(1) 0.02(1)
O(2A) O 0.5291(3) 0.9661(1) 0.3337(1) 0.024(1)
O(3A) O 0.6991(3) 0.9088(1) 0.2819(1) 0.025(1)
N(1A) N 0.5439(3) 0.7515(1) 0.3661(1) 0.013(1)
N(2A) N 0.435(3) 0.6952(1) 0.4579(1) 0.012(1)
N(3A) N 0.3256(3) 0.6348(1) 0.545(1) 0.014(1)
N(4A) N 0.2705(3) 0.5148(1) 0.5968(2) 0.018(1)
C(1A) C 0.5931(3) 0.9164(1) 0.3239(2) 0.015(1)
C(2A) C 0.5798(3) 0.8057(1) 0.337(2) 0.014(1)
C(3A) C 0.5394(3) 0.8609(1) 0.3636(2) 0.014(1)
C(4A) C 0.4499(3) 0.8635(1) 0.428(2) 0.015(1)
C(5A) C 0.3367(3) 0.8009(1) 0.5253(2) 0.013(1)
C(6A) C 0.3055(3) 0.7453(1) 0.5524(2) 0.012(1)
C(7A) C 0.3586(3) 0.6915(1) 0.5193(2) 0.013(1)
C(8A) C 0.4629(3) 0.7502(1) 0.4297(2) 0.012(1)
C(9A) C 0.4201(3) 0.8045(1) 0.4612(2) 0.013(1)
C(10A) C 0.5836(3) 0.6953(1) 0.3267(2) 0.015(1)
C(11A) C 0.4594(4) 0.6824(2) 0.2526(2) 0.024(1)
C(12A) C 0.3434(4) 0.6211(1) 0.6304(2) 0.016(1)
C(13A) C 0.233(4) 0.569(1) 0.642(2) 0.019(1)
C(14A) C 0.2617(4) 0.5291(1) 0.5113(2) 0.016(1)
C(15A) C 0.37(4) 0.5824(1) 0.5009(2) 0.016(1)
F(1B) F 0.2795(2) 0.2569(1) 0.8614(1) 0.023(1)
O(1B) O 0.1149(3) 0.0891(1) 1.0277(1) 0.021(1)
O(2B) O 0.0306(3) 0.0394(1) 1.1671(1) 0.027(1)
O(3B) O -0.1673(3) 0.093(1) 1.2043(1) 0.019(1)
N(1B) N -0.0068(3) 0.2509(1) 1.1207(1) 0.014(1)
N(2B) N 0.0864(3) 0.3048(1) 1.0229(1) 0.014(1)
N(3B) N 0.184(3) 0.3661(1) 0.9342(1) 0.016(1)
N(4B) N 0.2592(3) 0.4865(1) 0.8912(2) 0.019(1)
C(1B) C -0.0518(4) 0.0871(1) 1.168(2) 0.016(1)
C(2B) C -0.0417(3) 0.1972(1) 1.1514(2) 0.014(1)
C(3B) C -0.0068(3) 0.1415(1) 1.1239(2) 0.015(1)
C(4B) C 0.0726(3) 0.1372(1) 1.056(2) 0.014(1)
C(5B) C 0.1719(3) 0.1993(1) 0.9529(2) 0.015(1)
C(6B) C 0.2001(3) 0.2545(1) 0.9239(2) 0.016(1)
C(7B) C 0.1548(3) 0.3093(1) 0.9589(2) 0.015(1)
C(8B) C 0.0619(3) 0.2504(1) 1.0527(2) 0.013(1)
C(9B) C 0.0989(3) 0.1955(1) 1.0201(2) 0.014(1)
C(10B) C -0.0319(3) 0.3105(1) 1.1565(2) 0.015(1)
C(11B) C -0.1022(4) 0.3064(1) 1.2309(2) 0.021(1)
C(12B) C 0.1881(4) 0.3815(1) 0.8514(2) 0.018(1)
C(13B) C 0.3085(4) 0.4325(1) 0.8491(2) 0.02(1)
C(14B) C 0.2437(4) 0.4716(1) 0.9745(2) 0.019(1)
C(15B) C 0.1302(4) 0.4183(1) 0.9765(2) 0.018(1)
O(1W) O -0.0068(3) 0.4611(1) 0.2126(1) 0.025(1)
O(2W) O 0.2479(3) 0.5677(1) 0.1404(1) 0.028(1)
O(3W) O 0.2388(10) 0.4281(4) 0.3667(4) 0.155(3)
O(7) O 0.392(5) 0.5004(2) 0.338(2) 0.062(1)
C(31) C 0.4774(6) 0.5357(2) 0.3073(3) 0.055(1)
loop_
_atom_type_symbol
C
H
O
N
F
|
1100655.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100655.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100655
loop_
_publ_author_name
'Hansongnern, Kanidtha'
'Tempiam, Sansanee'
'Liou, Jian-Cheng'
'Liao, Fen-Ling'
'Lu, Tian-Huey'
_publ_section_title
;
Crystal Structure of 2-(4'-N,N-Diethylaminophenylazo)pyrimidine
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x13
_journal_page_last x14
_journal_paper_doi 10.2116/analscix.19.x13
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C14 H17 N5'
_chemical_formula_weight 255.33
_space_group_IT_number 56
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ab 2ac'
_symmetry_space_group_name_H-M 'P c c n'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 15.878(4)
_cell_length_b 22.125(5)
_cell_length_c 7.9029(19)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 18
_cell_measurement_theta_min 12
_cell_volume 2776.3(12)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type '4-circle diffractometer'
_diffrn_measurement_method 'scintillation counter'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0750
_diffrn_reflns_av_sigmaI/netI 0.1017
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 14980
_diffrn_reflns_theta_full 28.44
_diffrn_reflns_theta_max 28.44
_diffrn_reflns_theta_min 1.58
_exptl_absorpt_coefficient_mu 0.078
_exptl_crystal_colour Red
_exptl_crystal_density_diffrn 1.222
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Parallelepiped
_exptl_crystal_F_000 1088
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.160
_refine_diff_density_min -0.117
_refine_diff_density_rms 0.028
_refine_ls_extinction_coef 0.0015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 0.822
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 191
_refine_ls_number_reflns 3300
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 0.825
_refine_ls_R_factor_all 0.1696
_refine_ls_R_factor_gt 0.0595
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1081
_refine_ls_wR_factor_ref 0.1253
_reflns_number_gt 1175
_reflns_number_total 3300
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1100655
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.56660(12) 0.10769(9) 1.1067(2) 0.0624(6) Uani 1 1 d . . .
N2 N 0.54785(12) 0.15089(8) 1.0052(2) 0.0609(5) Uani 1 1 d . . .
N3 N 0.66951(12) 0.09207(8) 1.3101(3) 0.0620(6) Uani 1 1 d . . .
N4 N 0.59497(12) 0.18669(9) 1.3065(2) 0.0706(6) Uani 1 1 d . . .
N5 N 0.34185(16) 0.10362(10) 0.4484(3) 0.0950(8) Uani 1 1 d D . .
C1 C 0.61267(15) 0.13087(11) 1.2481(3) 0.0582(6) Uani 1 1 d . . .
C2 C 0.71315(16) 0.11348(12) 1.4425(3) 0.0734(8) Uani 1 1 d . . .
H2 H 0.7545 0.0889 1.4894 0.088 Uiso 1 1 calc R . .
C3 C 0.70070(17) 0.16891(12) 1.5124(3) 0.0777(8) Uani 1 1 d . . .
H3 H 0.7322 0.1823 1.6043 0.093 Uiso 1 1 calc R . .
C4 C 0.63912(17) 0.20419(11) 1.4403(3) 0.0737(8) Uani 1 1 d . . .
H4 H 0.6280 0.2419 1.4873 0.088 Uiso 1 1 calc R . .
C5 C 0.49742(14) 0.13354(10) 0.8664(3) 0.0573(6) Uani 1 1 d . . .
C6 C 0.46186(14) 0.07683(10) 0.8400(3) 0.0603(6) Uani 1 1 d . A .
H6 H 0.4715 0.0460 0.9176 0.072 Uiso 1 1 calc R . .
C7 C 0.41260(14) 0.06597(11) 0.7001(3) 0.0610(6) Uani 1 1 d . . .
H7 H 0.3905 0.0275 0.6827 0.073 Uiso 1 1 calc R A .
C8 C 0.39480(17) 0.11296(11) 0.5811(3) 0.0673(7) Uani 1 1 d . A .
C9 C 0.43112(16) 0.16985(12) 0.6112(3) 0.0739(8) Uani 1 1 d . . .
H9 H 0.4208 0.2014 0.5361 0.089 Uiso 1 1 calc R A .
C10 C 0.48199(15) 0.17984(11) 0.7509(3) 0.0683(7) Uani 1 1 d . A .
H10 H 0.5060 0.2177 0.7678 0.082 Uiso 1 1 calc R . .
C11 C 0.30885(16) 0.04469(12) 0.4062(4) 0.0815(8) Uani 1 1 d . A .
H11A H 0.2579 0.0497 0.3398 0.098 Uiso 1 1 calc R . .
H11B H 0.2937 0.0238 0.5098 0.098 Uiso 1 1 calc R . .
C12 C 0.3699(2) 0.00614(13) 0.3082(4) 0.1074(10) Uani 1 1 d . . .
H12A H 0.3444 -0.0321 0.2832 0.161 Uiso 1 1 calc R A .
H12B H 0.4198 -0.0002 0.3745 0.161 Uiso 1 1 calc R . .
H12C H 0.3846 0.0262 0.2045 0.161 Uiso 1 1 calc R . .
C13 C 0.2971(4) 0.1540(3) 0.3624(8) 0.0925(19) Uani 0.60 1 d PD A 1
H13A H 0.2934 0.1895 0.4338 0.111 Uiso 0.60 1 calc PR A 1
H13B H 0.2411 0.1422 0.3263 0.111 Uiso 0.60 1 calc PR A 1
C14 C 0.3549(5) 0.1639(4) 0.2146(8) 0.088(2) Uani 0.60 1 d PD A 1
H14A H 0.3339 0.1966 0.1467 0.132 Uiso 0.60 1 calc PR A 1
H14B H 0.3575 0.1278 0.1476 0.132 Uiso 0.60 1 calc PR A 1
H14C H 0.4103 0.1737 0.2550 0.132 Uiso 0.60 1 calc PR A 1
C13A C 0.3525(10) 0.1445(5) 0.2940(13) 0.097(4) Uani 0.40 1 d PD A 2
H13C H 0.3427 0.1215 0.1914 0.116 Uiso 0.40 1 calc PR A 2
H13D H 0.4095 0.1602 0.2904 0.116 Uiso 0.40 1 calc PR A 2
C14A C 0.2887(5) 0.1978(3) 0.3048(11) 0.088(2) Uani 0.40 1 d PD A 2
H14D H 0.2952 0.2235 0.2077 0.132 Uiso 0.40 1 calc PR A 2
H14E H 0.2991 0.2207 0.4057 0.132 Uiso 0.40 1 calc PR A 2
H14F H 0.2323 0.1821 0.3076 0.132 Uiso 0.40 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0668(13) 0.0653(13) 0.0550(12) -0.0022(11) -0.0050(11) 0.0021(10)
N2 0.0671(13) 0.0647(14) 0.0509(12) -0.0007(11) -0.0038(10) 0.0045(10)
N3 0.0737(14) 0.0529(13) 0.0593(13) 0.0035(10) -0.0109(12) 0.0067(10)
N4 0.0763(15) 0.0731(15) 0.0624(13) -0.0123(11) -0.0222(12) 0.0156(12)
N5 0.130(2) 0.0646(16) 0.0907(18) -0.0020(13) -0.0613(17) -0.0002(15)
C1 0.0712(17) 0.0582(16) 0.0452(13) 0.0050(12) -0.0027(13) 0.0034(13)
C2 0.0787(19) 0.0661(18) 0.0753(18) -0.0006(15) -0.0229(15) 0.0071(14)
C3 0.102(2) 0.0635(18) 0.0675(18) -0.0082(15) -0.0289(16) 0.0124(15)
C4 0.094(2) 0.0657(17) 0.0619(16) -0.0097(13) -0.0176(16) 0.0113(15)
C5 0.0648(16) 0.0571(15) 0.0499(14) 0.0027(12) -0.0128(13) 0.0014(13)
C6 0.0701(17) 0.0619(16) 0.0491(14) 0.0002(12) -0.0015(13) 0.0077(13)
C7 0.0694(16) 0.0559(15) 0.0577(15) -0.0049(13) -0.0033(14) 0.0015(12)
C8 0.0836(18) 0.0584(17) 0.0597(16) -0.0094(13) -0.0166(15) 0.0046(14)
C9 0.100(2) 0.0646(18) 0.0566(15) 0.0055(14) -0.0222(15) -0.0013(15)
C10 0.0888(19) 0.0603(16) 0.0559(14) 0.0017(13) -0.0112(15) -0.0096(13)
C11 0.0744(18) 0.088(2) 0.0818(19) -0.0231(16) -0.0178(15) -0.0022(15)
C12 0.128(3) 0.090(2) 0.104(2) -0.0260(18) 0.036(2) 0.0023(19)
C13 0.097(5) 0.097(5) 0.084(5) -0.009(4) 0.000(4) 0.004(4)
C14 0.093(4) 0.089(5) 0.082(5) 0.001(4) 0.007(5) -0.006(4)
C13A 0.126(10) 0.104(10) 0.059(8) 0.004(6) -0.003(8) 0.001(8)
C14A 0.092(6) 0.081(5) 0.090(6) 0.010(5) 0.007(5) 0.014(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 C1 109.89(19) . . ?
N1 N2 C5 114.52(19) . . ?
C1 N3 C2 114.0(2) . . ?
C4 N4 C1 115.5(2) . . ?
C8 N5 C11 122.7(2) . . ?
C8 N5 C13 122.3(3) . . ?
C11 N5 C13 113.4(3) . . ?
C8 N5 C13A 117.2(6) . . ?
C11 N5 C13A 113.0(5) . . ?
C13 N5 C13A 40.9(5) . . ?
N3 C1 N4 127.1(2) . . ?
N3 C1 N1 113.6(2) . . ?
N4 C1 N1 119.3(2) . . ?
N3 C2 C3 124.1(2) . . ?
C2 C3 C4 116.5(2) . . ?
N4 C4 C3 122.7(2) . . ?
C6 C5 C10 119.6(2) . . ?
C6 C5 N2 126.3(2) . . ?
C10 C5 N2 114.1(2) . . ?
C7 C6 C5 120.6(2) . . ?
C6 C7 C8 120.9(2) . . ?
N5 C8 C9 121.4(2) . . ?
N5 C8 C7 121.3(2) . . ?
C9 C8 C7 117.3(2) . . ?
C10 C9 C8 121.1(2) . . ?
C9 C10 C5 120.5(2) . . ?
N5 C11 C12 113.4(2) . . ?
N5 C13 C14 100.0(6) . . ?
N5 C13A C14A 109.4(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N2 1.283(2) . ?
N1 C1 1.431(3) . ?
N2 C5 1.411(3) . ?
N3 C1 1.338(3) . ?
N3 C2 1.342(3) . ?
N4 C4 1.326(3) . ?
N4 C1 1.348(3) . ?
N5 C8 1.360(3) . ?
N5 C11 1.444(3) . ?
N5 C13 1.485(6) . ?
N5 C13A 1.529(9) . ?
C2 C3 1.360(3) . ?
C3 C4 1.375(3) . ?
C5 C6 1.392(3) . ?
C5 C10 1.394(3) . ?
C6 C7 1.375(3) . ?
C7 C8 1.430(3) . ?
C8 C9 1.405(3) . ?
C9 C10 1.386(3) . ?
C11 C12 1.506(3) . ?
C13 C14 1.502(8) . ?
C13A C14A 1.557(13) . ?
|
1100656.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100656.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100656
loop_
_publ_author_name
'Kitoh, Soh-ichi'
'Senda, Hitoshi'
'Kunimoto, Ko-Ki'
_publ_section_title
;
Crystal Structures of Chiral and Racemic
4-Methyl-5-phenyl-1,3-oxazolidine-2-thione
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x15
_journal_page_last x16
_journal_paper_doi 10.2116/analscix.19.x15
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C10 H11 N O S '
_chemical_formula_sum 'C10 H11 N O S'
_chemical_formula_weight 193.26
_space_group_IT_number 18
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 18
_symmetry_space_group_name_Hall 'P 2 2ab'
_symmetry_space_group_name_H-M 'P 21 21 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 10.104(2)
_cell_length_b 32.447(1)
_cell_length_c 6.014(1)
_cell_measurement_temperature 123.2
_cell_volume 1971.7(5)
_diffrn_measured_fraction_theta_full 0.9514
_diffrn_measured_fraction_theta_max 0.9514
_diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.018
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 40
_diffrn_reflns_limit_k_min -41
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 10642
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.286
_exptl_absorpt_correction_type none
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.302
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_size_max 0.230
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.160
_refine_diff_density_max 0.14
_refine_diff_density_min -0.10
_refine_ls_abs_structure_Flack 0.55(7)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.115
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 324
_refine_ls_number_reflns 2414
_refine_ls_R_factor_gt 0.0268
_refine_ls_shift/su_max 0.0006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0398
_reflns_number_gt 2361
_reflns_number_total 2518
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P 21 21 2 '
_cod_original_formula_sum 'C10 H11 N O S '
_cod_database_code 1100656
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
1/2+x,1/2-y,-z
1/2-x,1/2+y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S(1A) S 0.02684(5) 0.37822(1) 0.95014(8) 0.0265(1) Uani 1.00 d . . .
S(1B) S 0.09851(5) 0.44542(1) -0.63999(8) 0.0239(1) Uani 1.00 d . . .
O(1A) O 0.0458(2) 0.30292(4) 0.7925(2) 0.0278(3) Uani 1.00 d . . .
O(1B) O 0.2110(1) 0.51306(4) -0.4849(2) 0.0221(3) Uani 1.00 d . . .
N(1A) N 0.0856(2) 0.35023(5) 0.5406(3) 0.0254(4) Uani 1.00 d . . .
N(1B) N 0.1375(2) 0.47237(5) -0.2223(3) 0.0208(4) Uani 1.00 d . . .
C(1A) C 0.0541(2) 0.34394(5) 0.7502(3) 0.0224(4) Uani 1.00 d . . .
C(2A) C 0.1179(2) 0.31241(5) 0.4189(3) 0.0244(4) Uani 1.00 d . . .
C(3A) C 0.0559(2) 0.28048(5) 0.5818(3) 0.0237(4) Uani 1.00 d . . .
C(4A) C 0.2657(2) 0.30891(7) 0.3784(4) 0.0331(5) Uani 1.00 d . . .
C(5A) C 0.1312(2) 0.24108(5) 0.6150(3) 0.0233(4) Uani 1.00 d . . .
C(6A) C 0.1267(2) 0.21121(6) 0.4483(4) 0.0299(5) Uani 1.00 d . . .
C(7A) C 0.1975(2) 0.17452(6) 0.4729(4) 0.0331(5) Uani 1.00 d . . .
C(8A) C 0.2701(2) 0.16741(6) 0.6626(4) 0.0314(5) Uani 1.00 d . . .
C(9A) C 0.2737(2) 0.19662(7) 0.8296(4) 0.0352(5) Uani 1.00 d . . .
C(10A) C 0.2048(2) 0.23360(6) 0.8061(4) 0.0305(5) Uani 1.00 d . . .
C(1B) C 0.1496(2) 0.47706(5) -0.4380(3) 0.0204(4) Uani 1.00 d . . .
C(2B) C 0.2052(2) 0.50428(5) -0.0941(3) 0.0198(4) Uani 1.00 d . . .
C(3B) C 0.2169(2) 0.53711(5) -0.2791(3) 0.0200(4) Uani 1.00 d . . .
C(4B) C 0.3362(2) 0.48814(6) -0.0049(3) 0.0228(4) Uani 1.00 d . . .
C(5B) C 0.3397(2) 0.56344(5) -0.2708(3) 0.0209(4) Uani 1.00 d . . .
C(6B) C 0.3585(2) 0.58804(6) -0.0833(3) 0.0251(4) Uani 1.00 d . . .
C(7B) C 0.4726(2) 0.61176(6) -0.0609(4) 0.0302(5) Uani 1.00 d . . .
C(8B) C 0.5673(2) 0.61145(6) -0.2271(4) 0.0311(5) Uani 1.00 d . . .
C(9B) C 0.5473(2) 0.58795(6) -0.4165(4) 0.0302(5) Uani 1.00 d . . .
C(10B) C 0.4345(2) 0.56376(5) -0.4386(3) 0.0247(4) Uani 1.00 d . . .
H(1A) H 0.101(3) 0.374(1) 0.491(6) 0.051(8) Uiso 1.00 d . . .
H(2A) H 0.076(2) 0.3110(8) 0.279(4) 0.022(6) Uiso 1.00 d . . .
H(3A) H -0.034(3) 0.2761(7) 0.521(4) 0.024(6) Uiso 1.00 d . . .
H(4A) H 0.295(3) 0.3310(9) 0.289(5) 0.040(7) Uiso 1.00 d . . .
H(5A) H 0.311(3) 0.3080(9) 0.518(5) 0.035(7) Uiso 1.00 d . . .
H(6A) H 0.293(3) 0.2823(9) 0.288(5) 0.039(7) Uiso 1.00 d . . .
H(7A) H 0.073(3) 0.2164(9) 0.311(5) 0.042(7) Uiso 1.00 d . . .
H(8A) H 0.195(3) 0.1554(9) 0.357(6) 0.044(7) Uiso 1.00 d . . .
H(9A) H 0.316(3) 0.1416(8) 0.687(5) 0.033(6) Uiso 1.00 d . . .
H(10A) H 0.313(3) 0.1916(10) 0.972(6) 0.046(8) Uiso 1.00 d . . .
H(11A) H 0.212(3) 0.2531(8) 0.922(5) 0.036(7) Uiso 1.00 d . . .
H(1B) H 0.120(3) 0.4549(10) -0.179(5) 0.033(7) Uiso 1.00 d . . .
H(2B) H 0.153(3) 0.5152(7) 0.024(4) 0.025(6) Uiso 1.00 d . . .
H(3B) H 0.133(3) 0.5557(8) -0.288(5) 0.033(6) Uiso 1.00 d . . .
H(4B) H 0.320(2) 0.4634(7) 0.093(4) 0.023(5) Uiso 1.00 d . . .
H(5B) H 0.395(2) 0.4814(8) -0.132(5) 0.029(6) Uiso 1.00 d . . .
H(6B) H 0.380(2) 0.5070(8) 0.083(4) 0.029(6) Uiso 1.00 d . . .
H(7B) H 0.299(3) 0.5893(9) 0.018(5) 0.040(7) Uiso 1.00 d . . .
H(8B) H 0.484(3) 0.6273(8) 0.071(4) 0.031(6) Uiso 1.00 d . . .
H(9B) H 0.647(3) 0.6264(9) -0.216(5) 0.038(7) Uiso 1.00 d . . .
H(10B) H 0.614(3) 0.5876(8) -0.528(5) 0.032(6) Uiso 1.00 d . . .
H(11B) H 0.419(2) 0.5466(7) -0.552(4) 0.023(5) Uiso 1.00 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100657.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100657.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100657
loop_
_publ_author_name
'Kitoh, Soh-ichi'
'Senda, Hitoshi'
'Kunimoto, Ko-Ki'
_publ_section_title
;
Crystal Structures of Chiral and Racemic
4-Methyl-5-phenyl-1,3-oxazolidine-2-thione
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x15
_journal_page_last x16
_journal_paper_doi 10.2116/analscix.19.x15
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C10 H11 N O S '
_chemical_formula_sum 'C10 H11 N O S'
_chemical_formula_weight 193.26
_chemical_melting_point ?
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 15
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 99.433(1)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 27.238(4)
_cell_length_b 6.0517(8)
_cell_length_c 11.726(3)
_cell_measurement_temperature 123.2
_cell_volume 1906.7(6)
_diffrn_measured_fraction_theta_full 0.9575
_diffrn_measured_fraction_theta_max 0.9575
_diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.022
_diffrn_reflns_limit_h_max 35
_diffrn_reflns_limit_h_min -32
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8854
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.296
_exptl_absorpt_correction_type none
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.346
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_size_max 0.180
_exptl_crystal_size_mid 0.130
_exptl_crystal_size_min 0.110
_refine_diff_density_max 0.27
_refine_diff_density_min -0.15
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.930
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 162
_refine_ls_number_reflns 1765
_refine_ls_R_factor_gt 0.0279
_refine_ls_shift/su_max 0.0009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0341
_reflns_number_gt 1657
_reflns_number_total 2096
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C10 H11 N O S '
_cod_database_code 1100657
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,1/2-z
-x,-y,-z
x,-y,1/2+z
1/2+x,1/2+y,z
1/2-x,1/2+y,1/2-z
1/2-x,1/2-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S(1) S 0.47541(1) 0.19665(6) 0.06028(3) 0.02594(9) Uani 1.00 d . . .
O(1) O 0.42012(3) 0.3229(2) 0.21174(8) 0.0236(2) Uani 1.00 d . . .
N(1) N 0.45340(4) 0.6025(2) 0.1329(1) 0.0230(3) Uani 1.00 d . . .
C(1) C 0.44953(4) 0.3849(2) 0.1354(1) 0.0215(3) Uani 1.00 d . . .
C(2) C 0.41972(5) 0.7130(2) 0.2008(1) 0.0214(3) Uani 1.00 d . . .
C(3) C 0.41173(5) 0.5176(2) 0.2803(1) 0.0217(3) Uani 1.00 d . . .
C(4) C 0.37326(5) 0.7964(3) 0.1230(1) 0.0258(3) Uani 1.00 d . . .
C(5) C 0.36193(5) 0.4990(2) 0.3200(1) 0.0207(3) Uani 1.00 d . . .
C(6) C 0.34871(5) 0.6625(2) 0.3932(1) 0.0253(3) Uani 1.00 d . . .
C(7) C 0.30426(5) 0.6459(3) 0.4361(1) 0.0292(4) Uani 1.00 d . . .
C(8) C 0.27307(5) 0.4668(3) 0.4074(1) 0.0269(3) Uani 1.00 d . . .
C(9) C 0.28574(5) 0.3056(3) 0.3341(1) 0.0279(3) Uani 1.00 d . . .
C(10) C 0.33011(5) 0.3219(2) 0.2902(1) 0.0258(3) Uani 1.00 d . . .
H(1) H 0.4686(6) 0.666(3) 0.084(2) 0.033(5) Uiso 1.00 d . . .
H(2) H 0.4363(5) 0.831(3) 0.245(1) 0.026(3) Uiso 1.00 d . . .
H(3) H 0.4370(6) 0.522(3) 0.347(1) 0.026(4) Uiso 1.00 d . . .
H(4) H 0.3571(6) 0.676(3) 0.080(2) 0.031(4) Uiso 1.00 d . . .
H(5) H 0.3823(6) 0.904(3) 0.071(2) 0.031(5) Uiso 1.00 d . . .
H(6) H 0.3514(6) 0.861(3) 0.169(2) 0.031(4) Uiso 1.00 d . . .
H(7) H 0.3701(6) 0.785(3) 0.414(1) 0.030(4) Uiso 1.00 d . . .
H(8) H 0.2952(6) 0.758(3) 0.485(2) 0.035(5) Uiso 1.00 d . . .
H(9) H 0.2430(6) 0.455(3) 0.438(2) 0.032(4) Uiso 1.00 d . . .
H(10) H 0.2642(7) 0.183(3) 0.314(2) 0.033(5) Uiso 1.00 d . . .
H(11) H 0.3386(7) 0.211(4) 0.239(2) 0.031(5) Uiso 1.00 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100658.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100658.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100658
loop_
_publ_author_name
'Doreswamy, Beeranahally H.'
Basappa
'Mahendra, Madegowda'
'Mantelingu, Kempegowda'
'Anandalwar, Sridhar M.'
'Prasad, Javaregowda S.'
'Rangappa, Kanchugarakoppal S.'
_publ_section_title
;
Microwave-Assisted Synthesis and Crystal Structure of
2-Butyl-4-chloro-1H-imidazole-5-carboxaldehyde
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x31
_journal_page_last x32
_journal_paper_doi 10.2116/analscix.19.x31
_journal_volume 19
_journal_year 2003
_chemical_formula_iupac 2-Butyl-4-chloro-1H-imidazole-5-carboxaldehy
_chemical_formula_moiety 'C8 H11 Cl N2 O'
_chemical_formula_sum 'C8 H11 Cl N2 O'
_chemical_formula_weight 186.64
_chemical_name_common imidazole
_chemical_name_systematic
;
2-Butyl-4-chloro-1H-imidazole-5-carboxaldehyde
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 101.94
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.251
_cell_length_b 13.195(1)
_cell_length_c 9.835(1)
_cell_measurement_temperature 293(2)
_cell_volume 920.62(12)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0257
_diffrn_reflns_av_sigmaI/netI 0.0303
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 3617
_diffrn_reflns_theta_full 27.93
_diffrn_reflns_theta_max 27.93
_diffrn_reflns_theta_min 2.62
_exptl_absorpt_coefficient_mu 0.369
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.347
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description '0.25 x 0.2 x 0.25 mm'
_exptl_crystal_F_000 392
_refine_diff_density_max 0.657
_refine_diff_density_min -0.431
_refine_diff_density_rms 0.125
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 0.13(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 111
_refine_ls_number_reflns 1977
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0798
_refine_ls_R_factor_gt 0.0651
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+0.1028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1890
_refine_ls_wR_factor_ref 0.2167
_reflns_number_gt 1552
_reflns_number_total 1977
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M P21/c
_cod_database_code 1100658
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.76028(10) 0.54189(5) 0.15677(7) 0.0694(4) Uani 1 1 d . . .
N6 N 0.9265(3) 0.70522(13) -0.1187(2) 0.0474(5) Uani 1 1 d . . .
H6 H 0.9436 0.7217 -0.1998 0.057 Uiso 1 1 calc R . .
N8 N 0.9356(3) 0.71213(13) 0.1070(2) 0.0505(5) Uani 1 1 d . . .
C9 C 1.0789(4) 0.85854(15) 0.0039(3) 0.0558(6) Uani 1 1 d . . .
H9A H 1.0060 0.9090 0.0415 0.067 Uiso 1 1 calc R . .
H9B H 1.0855 0.8793 -0.0895 0.067 Uiso 1 1 calc R . .
C2 C 0.8477(3) 0.62639(15) 0.0535(2) 0.0493(5) Uani 1 1 d . . .
C3 C 0.8389(3) 0.61811(15) -0.0863(2) 0.0487(6) Uani 1 1 d . . .
C7 C 0.9802(3) 0.75943(15) -0.0026(2) 0.0477(5) Uani 1 1 d . . .
O5 O 0.7653(3) 0.54495(14) -0.3082(3) 0.0740(6) Uani 1 1 d . . .
C11 C 1.4124(4) 0.7833(2) 0.0407(3) 0.0656(7) Uani 1 1 d . . .
H11A H 1.5257 0.7754 0.1122 0.079 Uiso 1 1 calc R . .
H11B H 1.3531 0.7173 0.0241 0.079 Uiso 1 1 calc R . .
C4 C 0.7611(4) 0.54124(17) -0.1863(3) 0.0594(7) Uani 1 1 d . . .
H4 H 0.7041 0.4853 -0.1547 0.071 Uiso 1 1 calc R . .
C10 C 1.2784(4) 0.85528(18) 0.0933(3) 0.0609(7) Uani 1 1 d . . .
H10A H 1.3311 0.9231 0.0982 0.073 Uiso 1 1 calc R . .
H10B H 1.2707 0.8353 0.1869 0.073 Uiso 1 1 calc R . .
C12 C 1.4663(5) 0.8192(3) -0.0901(4) 0.0828(9) Uani 1 1 d . . .
H12A H 1.3555 0.8241 -0.1627 0.124 Uiso 1 1 calc R . .
H12B H 1.5529 0.7720 -0.1170 0.124 Uiso 1 1 calc R . .
H12C H 1.5250 0.8846 -0.0746 0.124 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0831(6) 0.0584(5) 0.0714(6) 0.0143(2) 0.0267(4) -0.0104(3)
N6 0.0577(11) 0.0413(9) 0.0459(11) 0.0009(6) 0.0168(7) 0.0013(7)
N8 0.0617(11) 0.0415(9) 0.0503(12) 0.0017(7) 0.0161(8) -0.0003(7)
C9 0.0690(15) 0.0357(11) 0.0659(16) 0.0009(8) 0.0211(11) -0.0004(9)
C2 0.0543(12) 0.0392(10) 0.0566(14) 0.0044(8) 0.0167(9) 0.0022(8)
C3 0.0552(12) 0.0394(10) 0.0540(14) 0.0006(8) 0.0167(9) 0.0009(8)
C7 0.0547(12) 0.0369(10) 0.0538(13) 0.0021(8) 0.0163(9) 0.0032(8)
O5 0.0928(16) 0.0676(13) 0.0625(13) -0.0145(8) 0.0183(10) -0.0105(9)
C11 0.0635(15) 0.0582(14) 0.0737(18) 0.0014(11) 0.0107(12) 0.0021(11)
C4 0.0621(14) 0.0477(13) 0.0696(18) -0.0077(9) 0.0167(11) -0.0047(9)
C10 0.0716(16) 0.0506(13) 0.0619(16) -0.0090(10) 0.0173(11) -0.0073(11)
C12 0.083(2) 0.083(2) 0.087(2) -0.0026(16) 0.0290(16) 0.0158(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N6 C3 108.33(19) . . ?
C7 N8 C2 104.50(19) . . ?
C7 C9 C10 112.9(2) . . ?
N8 C2 C3 112.21(19) . . ?
N8 C2 Cl1 121.11(18) . . ?
C3 C2 Cl1 126.68(17) . . ?
C2 C3 N6 103.75(18) . . ?
C2 C3 C4 132.1(2) . . ?
N6 C3 C4 124.1(2) . . ?
N6 C7 N8 111.21(19) . . ?
N6 C7 C9 124.1(2) . . ?
N8 C7 C9 124.7(2) . . ?
C12 C11 C10 113.1(2) . . ?
O5 C4 C3 124.2(2) . . ?
C11 C10 C9 114.6(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C2 1.715(2) . ?
N6 C7 1.336(3) . ?
N6 C3 1.382(3) . ?
N8 C7 1.341(3) . ?
N8 C2 1.350(3) . ?
C9 C7 1.486(3) . ?
C9 C10 1.530(4) . ?
C2 C3 1.368(3) . ?
C3 C4 1.444(3) . ?
O5 C4 1.206(4) . ?
C11 C12 1.497(5) . ?
C11 C10 1.523(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 49824
|
1100659.cif | #------------------------------------------------------------------------------
#$Date: 2016-01-27 04:56:07 +0200 (Wed, 27 Jan 2016) $
#$Revision: 175113 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100659.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100659
loop_
_publ_author_name
'Lakshmi, S.'
'Sridhar, M. A.'
'Prasad, J. S.'
'Srinivasan, V.'
'Kandhaswamy, M. A.'
'Dhandapani, M.'
_publ_section_title
;
Synthesis and Structural Analysis of Tetrathioureacopper(I) Chloride
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x19
_journal_page_last x20
_journal_paper_doi 10.2116/analscix.19.x19
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C3 H12 Cl Cu N6 S3'
_chemical_formula_sum 'C3 H12 Cl Cu N6 S3'
_chemical_name_common
;
Tetrathiourea Copper (II) chloride
;
_chemical_name_systematic
;
Tetrathiourea Copper (II) chloride
;
_space_group_IT_number 92
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 92
_symmetry_space_group_name_Hall 'P 4abw 2nw'
_symmetry_space_group_name_H-M 'P 41 21 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 13.4090(5)
_cell_length_b 13.4090(5)
_cell_length_c 13.8100(4)
_cell_volume 2483.1(1)
_exptl_crystal_density_diffrn 1.751
_refine_ls_R_factor_gt 0.0362
_cod_database_code 1100659
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -y+1/2,x+1/2,z+1/4
3 -x,-y,z+1/2
4 y+1/2,-x+1/2,z-1/4
5 x+1/2,-y+1/2,-z-1/4
6 -x+1/2,y+1/2,-z+1/4
7 y,x,-z
8 -y,-x,-z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Cu1 Cu 0.97121(4) 0.35595(4) 0.08493(3) 0.0371(2)
S2 S 0.88974(7) 0.49322(6) 0.00024(6) 0.0294(2)
C3 C 0.9224(3) 0.6072(3) 0.0498(3) 0.0335(7)
N4 N 0.9771(4) 0.6106(3) 0.1281(3) 0.056(1)
N5 N 0.8927(3) 0.6906(3) 0.0109(3) 0.054(1)
S6 S 1.11754(8) 0.31439(9) 0.01150(8) 0.0440(3)
C7 C 1.0856(4) 0.2639(4) -0.1006(3) 0.049(1)
N8 N 1.1568(4) 0.2623(5) -0.1697(3) 0.085(2)
N9 N 0.9992(4) 0.2289(4) -0.1210(3) 0.064(1)
S10 S 0.84462(7) 0.23521(8) 0.07583(7) 0.0380(2)
C11 C 0.8950(3) 0.1222(3) 0.1087(3) 0.0381(8)
N12 N 0.9905(3) 0.1068(3) 0.1106(3) 0.059(1)
N13 N 0.8374(4) 0.0482(4) 0.1327(3) 0.069(1)
Cl14 Cl 1.0175(1) 0.14442(8) -0.34353(9) 0.0690(5)
loop_
_atom_type_symbol
C
H
Cl
Cu
N
S
|
1100660.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100660.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100660
loop_
_publ_author_name
'Akimoto, Toshio'
'Hirayama, Noriaki'
_publ_section_title
;
Crystal Structure of Ciclopirox Olamine
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x21
_journal_page_last x22
_journal_paper_doi 10.2116/analscix.19.x21
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C26 H41 N3 O5 '
_chemical_formula_sum 'C26 H41 N3 O5'
_chemical_formula_weight 475.63
_space_group_IT_number 88
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4ad'
_symmetry_space_group_name_H-M 'I 41/a :2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 16
_cell_length_a 26.0133(6)
_cell_length_b 26.0133(6)
_cell_length_c 15.8980(8)
_cell_measurement_reflns_used 46398
_cell_measurement_temperature 293.1
_cell_measurement_theta_max 68.1
_cell_measurement_theta_min 2.4
_cell_volume 10758.0(6)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9895
_diffrn_measured_fraction_theta_max 0.9895
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5419
_diffrn_reflns_av_R_equivalents 0.044
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_k_max 30
_diffrn_reflns_limit_k_min -31
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 110718
_diffrn_reflns_theta_full 67.76
_diffrn_reflns_theta_max 67.76
_exptl_absorpt_coefficient_mu 0.656
_exptl_absorpt_correction_T_max 0.906
_exptl_absorpt_correction_T_min 0.734
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.175
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 4128.00
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.45
_refine_diff_density_min -0.39
_refine_ls_extinction_coef 22(12)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref 1.293
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 352
_refine_ls_number_reflns 3341
_refine_ls_R_factor_gt 0.0680
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1410
_reflns_number_gt 3341
_reflns_number_total 5017
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_Hall 'I 4bw -1bw'
_cod_original_sg_symbol_H-M 'I 41/a (origin at -1)'
_cod_original_formula_sum 'C26 H41 N3 O5 '
_cod_database_code 1100660
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z+1/2
-x+1/2,-y+1/2,-z+1/2
-y+3/4,x+1/4,z+1/4
y+3/4,-x+1/4,-z+1/4
-y+5/4,x+3/4,z+3/4
y+5/4,-x+3/4,-z+3/4
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
-x,-y+1/2,z
x,y+1/2,-z
y+3/4,-x+3/4,z+3/4
-y+3/4,x+3/4,-z+3/4
y+5/4,-x+5/4,z+5/4
-y+5/4,x+5/4,-z+5/4
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O101 O 0.09022(7) -0.08376(8) 0.8439(1) 0.0541(7) Uani 1.00 1 d . . .
O102 O 0.09541(8) -0.0477(1) 0.9976(1) 0.0730(8) Uani 1.00 1 d . . .
O201 O 0.11305(7) 0.00397(8) 0.7969(1) 0.0480(6) Uani 1.00 1 d . . .
O202 O 0.19714(8) -0.04152(8) 0.7385(1) 0.0535(6) Uani 1.00 1 d . . .
O304 O -0.1643(1) 0.0434(1) 0.8758(2) 0.103(1) Uani 1.00 1 d . . .
N101 N 0.04657(9) -0.08433(9) 0.8943(1) 0.0469(8) Uani 1.00 1 d . . .
N201 N 0.12092(9) 0.00035(8) 0.7116(1) 0.0416(7) Uani 1.00 1 d . . .
N301 N -0.20318(9) -0.06001(9) 0.8322(1) 0.0511(8) Uani 1.00 1 d . . .
C102 C 0.0519(1) -0.0654(1) 0.9754(2) 0.054(1) Uani 1.00 1 d . . .
C103 C 0.0072(1) -0.0675(1) 1.0257(2) 0.056(1) Uani 1.00 1 d . . .
C104 C -0.0381(1) -0.0884(1) 0.9980(2) 0.051(1) Uani 1.00 1 d . . .
C105 C -0.0396(1) -0.1089(1) 0.9161(2) 0.052(1) Uani 1.00 1 d . . .
C106 C 0.0022(1) -0.1063(1) 0.8635(2) 0.0469(9) Uani 1.00 1 d . . .
C107 C -0.0858(1) -0.0897(1) 1.0511(2) 0.071(1) Uani 1.00 1 d . . .
C108 C 0.0021(1) -0.1239(1) 0.7728(2) 0.053(1) Uani 1.00 1 d . . .
C109 C -0.0036(1) -0.0774(1) 0.7140(2) 0.062(1) Uani 1.00 1 d . . .
C110 C -0.0019(2) -0.0929(1) 0.6216(2) 0.087(1) Uani 1.00 1 d . . .
C111 C -0.0421(2) -0.1324(2) 0.6018(3) 0.105(2) Uani 1.00 1 d . . .
C112 C -0.0373(2) -0.1790(2) 0.6590(3) 0.105(2) Uani 1.00 1 d . . .
C113 C -0.0398(2) -0.1635(1) 0.7526(2) 0.083(1) Uani 1.00 1 d . . .
C202 C 0.1645(1) -0.0258(1) 0.6847(2) 0.0442(9) Uani 1.00 1 d . . .
C203 C 0.1685(1) -0.0329(1) 0.5968(2) 0.049(1) Uani 1.00 1 d . . .
C204 C 0.1343(1) -0.0121(1) 0.5415(2) 0.052(1) Uani 1.00 1 d . . .
C205 C 0.0936(1) 0.0180(1) 0.5738(2) 0.055(1) Uani 1.00 1 d . . .
C206 C 0.0867(1) 0.0246(1) 0.6583(2) 0.0455(9) Uani 1.00 1 d . . .
C207 C 0.1395(1) -0.0201(1) 0.4475(2) 0.075(1) Uani 1.00 1 d . . .
C208 C 0.0481(1) 0.0604(1) 0.6978(2) 0.050(1) Uani 1.00 1 d . . .
C209 C 0.0739(1) 0.1128(1) 0.7120(2) 0.062(1) Uani 1.00 1 d . . .
C210 C 0.0371(1) 0.1529(1) 0.7492(2) 0.079(1) Uani 1.00 1 d . . .
C211 C -0.0116(2) 0.1579(1) 0.6970(3) 0.084(1) Uani 1.00 1 d . . .
C212 C -0.0372(1) 0.1061(2) 0.6887(3) 0.089(2) Uani 1.00 1 d . . .
C213 C -0.0015(1) 0.0670(1) 0.6467(3) 0.077(1) Uani 1.00 1 d . . .
C302 C -0.1554(2) -0.0342(2) 0.8004(3) 0.097(2) Uani 1.00 1 d . . .
C303 C -0.1545(2) 0.0194(2) 0.7999(3) 0.132(2) Uani 1.00 1 d . . .
H1 H 0.0084(1) -0.0535(1) 1.0808(2) 0.067(1) Uiso 1.00 1 c . . .
H2 H -0.0704(1) -0.1244(1) 0.8965(2) 0.062(1) Uiso 1.00 1 c . . .
H3 H 0.0704(1) 0.0341(1) 0.5358(2) 0.066(1) Uiso 1.00 1 c . . .
H4 H 0.1962(1) -0.0527(1) 0.5754(2) 0.059(1) Uiso 1.00 1 c . . .
H5 H -0.0354(2) -0.1930(1) 0.7872(2) 0.099(2) Uiso 1.00 1 c . . .
H6 H -0.0723(2) -0.1484(1) 0.7635(2) 0.099(2) Uiso 1.00 1 c . . .
H7 H -0.0361(1) -0.0621(1) 0.7246(2) 0.074(1) Uiso 1.00 1 c . . .
H8 H 0.0229(1) -0.0532(1) 0.7259(2) 0.074(1) Uiso 1.00 1 c . . .
H9 H -0.0058(2) -0.0635(1) 0.5867(2) 0.105(2) Uiso 1.00 1 c . . .
H10 H 0.0305(2) -0.1085(1) 0.6108(2) 0.105(2) Uiso 1.00 1 c . . .
H11 H -0.0745(2) -0.1170(2) 0.6134(3) 0.126(2) Uiso 1.00 1 c . . .
H12 H -0.0408(2) -0.1424(2) 0.5444(3) 0.126(2) Uiso 1.00 1 c . . .
H13 H -0.0044(2) -0.1936(2) 0.6485(3) 0.126(2) Uiso 1.00 1 c . . .
H14 H -0.0632(2) -0.2036(2) 0.6465(3) 0.126(2) Uiso 1.00 1 c . . .
H15 H 0.1027(1) 0.1085(1) 0.7480(2) 0.074(1) Uiso 1.00 1 c . . .
H16 H 0.0852(1) 0.1251(1) 0.6588(2) 0.074(1) Uiso 1.00 1 c . . .
H17 H 0.0275(1) 0.1418(1) 0.8039(2) 0.095(2) Uiso 1.00 1 c . . .
H18 H 0.0540(1) 0.1851(1) 0.7528(2) 0.095(2) Uiso 1.00 1 c . . .
H19 H -0.0343(2) 0.1819(1) 0.7224(3) 0.101(2) Uiso 1.00 1 c . . .
H20 H -0.0024(2) 0.1697(1) 0.6424(3) 0.101(2) Uiso 1.00 1 c . . .
H21 H -0.0680(1) 0.1094(2) 0.6571(3) 0.107(2) Uiso 1.00 1 c . . .
H22 H -0.0450(1) 0.0937(2) 0.7434(3) 0.107(2) Uiso 1.00 1 c . . .
H23 H 0.0076(1) 0.0799(1) 0.5928(3) 0.093(2) Uiso 1.00 1 c . . .
H24 H -0.0181(1) 0.0346(1) 0.6405(3) 0.093(2) Uiso 1.00 1 c . . .
H25 H 0.0344(1) -0.1395(1) 0.7613(2) 0.064(1) Uiso 1.00 1 c . . .
H26 H 0.0387(1) 0.0470(1) 0.7512(2) 0.060(1) Uiso 1.00 1 c . . .
H27 H -0.0786(1) -0.0750(1) 1.1044(2) 0.085(2) Uiso 1.00 1 c . . .
H28 H -0.1122(1) -0.0706(1) 1.0242(2) 0.085(2) Uiso 1.00 1 c . . .
H29 H -0.0967(1) -0.1243(1) 1.0582(2) 0.085(2) Uiso 1.00 1 c . . .
H30 H 0.099(1) -0.042(2) 0.819(2) 0.12(1) Uiso 1.00 1 c . . .
H34 H -0.1279(2) -0.0453(2) 0.8352(3) 0.117(2) Uiso 1.00 1 c . . .
H35 H -0.1497(2) -0.0455(2) 0.7444(3) 0.116(2) Uiso 1.00 1 c . . .
H36 H -0.1806(2) 0.0304(2) 0.7621(3) 0.158(3) Uiso 1.00 1 c . . .
H37 H -0.1220(2) 0.0308(2) 0.7802(3) 0.158(3) Uiso 1.00 1 c . . .
H38 H -0.20972(9) -0.04950(9) 0.8884(1) 0.062(1) Uiso 1.00 1 c . . .
H39 H -0.23114(9) -0.05008(9) 0.7973(1) 0.062(1) Uiso 1.00 1 c . . .
H40 H -0.19933(9) -0.09631(9) 0.8304(1) 0.062(1) Uiso 1.00 1 c . . .
H42 H -0.1323(1) 0.0480(1) 0.9036(2) 0.123(2) Uiso 1.00 1 c . . .
H31 H 0.1379(1) -0.0559(1) 0.4355(2) 0.091(2) Uiso 1.00 1 c . . .
H32 H 0.1125(1) -0.0029(1) 0.4189(2) 0.091(2) Uiso 1.00 1 c . . .
H33 H 0.1717(1) -0.0069(1) 0.4292(2) 0.091(2) Uiso 1.00 1 c . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.049 0.032
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.031 0.018
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100661.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100661.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100661
loop_
_publ_author_name
'Ayg\"un, Muhittin'
'Akkus, Nilg\"un'
'G\"uven, Kutalm\,s'
'Akg\"ung\"or, Kadir'
_publ_section_title
;
Crystal Structure of 4-Ethoxy-N-(o-hydroxyacetophenolidene)aniline
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x23
_journal_page_last x24
_journal_paper_doi 10.2116/analscix.19.x23
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C16 H17 N O2'
_chemical_formula_weight 255.31
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 97.020(10)
_cell_angle_beta 102.750(10)
_cell_angle_gamma 100.520(10)
_cell_formula_units_Z 2
_cell_length_a 8.2790(10)
_cell_length_b 14.843(2)
_cell_length_c 5.9590(10)
_cell_measurement_temperature 293(2)
_cell_volume 692.05(17)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.829
_diffrn_measured_fraction_theta_max 0.829
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0174
_diffrn_reflns_av_sigmaI/netI 0.0542
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 2829
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 27.50
_diffrn_reflns_theta_min 2.58
_exptl_absorpt_coefficient_mu 0.081
_exptl_absorpt_correction_type none
_exptl_crystal_density_diffrn 1.225
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 272
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.123
_refine_diff_density_min -0.161
_refine_diff_density_rms 0.031
_refine_ls_extinction_coef 0.017(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 241
_refine_ls_number_reflns 2639
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.009
_refine_ls_R_factor_all 0.1198
_refine_ls_R_factor_gt 0.0411
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+0.0179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1169
_refine_ls_wR_factor_ref 0.1595
_reflns_number_gt 1186
_reflns_number_total 2639
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100661
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.1323(3) 0.29361(13) 0.4971(3) 0.0719(6) Uani 1 1 d . . .
O1 O 0.0589(3) 0.40172(14) 0.2073(3) 0.0981(7) Uani 1 1 d . . .
O2 O 0.6035(2) 0.08800(11) 0.8431(3) 0.0761(5) Uani 1 1 d . . .
C1 C 0.8190(5) 0.0433(2) 1.1086(7) 0.0935(9) Uani 1 1 d . . .
C2 C 0.7002(4) 0.1073(2) 1.0802(5) 0.0778(7) Uani 1 1 d . . .
C3 C 0.4904(3) 0.14253(16) 0.7726(4) 0.0666(6) Uani 1 1 d . . .
C4 C 0.4007(3) 0.12008(19) 0.5403(4) 0.0755(7) Uani 1 1 d . . .
C5 C 0.2850(4) 0.17049(19) 0.4529(5) 0.0752(7) Uani 1 1 d . . .
C6 C 0.2520(3) 0.24247(15) 0.5946(4) 0.0672(6) Uani 1 1 d . . .
C7 C 0.3440(3) 0.26500(18) 0.8250(4) 0.0749(7) Uani 1 1 d . . .
C8 C 0.4636(4) 0.21618(17) 0.9143(5) 0.0732(7) Uani 1 1 d . . .
C9 C -0.0087(3) 0.29099(14) 0.5562(3) 0.0633(6) Uani 1 1 d . . .
C10 C -0.1219(3) 0.34887(14) 0.4514(3) 0.0654(6) Uani 1 1 d . . .
C11 C -0.0837(4) 0.40110(16) 0.2814(4) 0.0773(8) Uani 1 1 d . . .
C12 C -0.1957(6) 0.45501(19) 0.1845(5) 0.0981(11) Uani 1 1 d . . .
C13 C -0.3399(6) 0.4569(2) 0.2568(6) 0.0990(10) Uani 1 1 d . . .
C14 C -0.3813(5) 0.40694(18) 0.4225(5) 0.0891(8) Uani 1 1 d . . .
C15 C -0.2730(4) 0.35379(17) 0.5170(5) 0.0759(7) Uani 1 1 d . . .
C16 C -0.0651(4) 0.2297(2) 0.7202(5) 0.0771(8) Uani 1 1 d . . .
H1 H 0.121(3) 0.363(2) 0.284(5) 0.100(10) Uiso 1 1 d . . .
H1A H 0.895(4) 0.0510(19) 1.012(5) 0.107(10) Uiso 1 1 d . . .
H1B H 0.887(4) 0.049(2) 1.272(6) 0.112(10) Uiso 1 1 d . . .
H1C H 0.763(4) -0.023(3) 1.066(5) 0.123(11) Uiso 1 1 d . . .
H2A H 0.760(3) 0.1732(18) 1.116(4) 0.076(7) Uiso 1 1 d . . .
H2B H 0.620(3) 0.0944(17) 1.180(4) 0.092(8) Uiso 1 1 d . . .
H4 H 0.421(3) 0.0707(17) 0.438(4) 0.080(7) Uiso 1 1 d . . .
H5 H 0.222(3) 0.1562(16) 0.298(4) 0.083(7) Uiso 1 1 d . . .
H7 H 0.324(3) 0.3168(17) 0.931(4) 0.080(7) Uiso 1 1 d . . .
H8 H 0.525(3) 0.2310(17) 1.068(5) 0.084(8) Uiso 1 1 d . . .
H12 H -0.162(4) 0.487(2) 0.071(5) 0.111(10) Uiso 1 1 d . . .
H13 H -0.413(4) 0.494(2) 0.188(5) 0.116(10) Uiso 1 1 d . . .
H14 H -0.492(5) 0.404(2) 0.481(6) 0.151(14) Uiso 1 1 d . . .
H15 H -0.295(3) 0.3233(17) 0.632(4) 0.073(7) Uiso 1 1 d . . .
H16A H -0.060(4) 0.267(2) 0.868(6) 0.126(11) Uiso 1 1 d . . .
H16B H 0.007(4) 0.189(2) 0.748(5) 0.115(11) Uiso 1 1 d . . .
H16C H -0.182(4) 0.198(2) 0.658(4) 0.099(9) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0811(14) 0.0644(12) 0.0651(12) 0.0067(9) 0.0254(11) -0.0029(10)
O1 0.1181(17) 0.0959(15) 0.0728(12) 0.0305(11) 0.0258(12) -0.0087(12)
O2 0.0710(10) 0.0771(11) 0.0706(11) -0.0105(8) 0.0223(9) 0.0016(8)
C1 0.092(2) 0.086(2) 0.098(2) 0.0149(18) 0.025(2) 0.0082(19)
C2 0.0772(18) 0.0756(18) 0.0715(17) -0.0016(13) 0.0238(15) -0.0041(15)
C3 0.0605(14) 0.0658(14) 0.0679(15) -0.0054(12) 0.0276(12) -0.0033(11)
C4 0.0745(17) 0.0789(17) 0.0656(16) -0.0148(13) 0.0317(14) -0.0020(14)
C5 0.0738(17) 0.0835(17) 0.0588(15) -0.0055(13) 0.0226(13) -0.0030(14)
C6 0.0730(16) 0.0601(14) 0.0642(14) 0.0026(12) 0.0298(12) -0.0065(12)
C7 0.0813(18) 0.0683(16) 0.0672(16) -0.0107(13) 0.0247(14) 0.0032(13)
C8 0.0757(17) 0.0720(16) 0.0594(15) -0.0115(12) 0.0192(13) -0.0034(13)
C9 0.0813(17) 0.0498(12) 0.0520(12) -0.0013(10) 0.0222(12) -0.0037(11)
C10 0.0879(17) 0.0452(12) 0.0522(12) 0.0012(10) 0.0121(12) -0.0017(12)
C11 0.102(2) 0.0581(15) 0.0524(14) 0.0030(11) 0.0097(14) -0.0145(14)
C12 0.137(3) 0.0682(18) 0.0634(17) 0.0198(14) -0.0054(19) -0.0109(19)
C13 0.122(3) 0.0655(19) 0.084(2) 0.0054(16) -0.013(2) 0.0085(19)
C14 0.111(2) 0.0622(16) 0.0844(18) 0.0056(14) 0.0068(17) 0.0190(16)
C15 0.101(2) 0.0577(14) 0.0660(15) 0.0083(12) 0.0214(15) 0.0093(14)
C16 0.086(2) 0.0735(17) 0.0815(19) 0.0269(15) 0.0367(17) 0.0144(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 N1 C6 121.97(18) . . ?
C11 O1 H1 109.8(18) . . ?
C3 O2 C2 118.59(19) . . ?
C2 C1 H1A 112.3(16) . . ?
C2 C1 H1B 113.5(16) . . ?
H1A C1 H1B 108(2) . . ?
C2 C1 H1C 114.1(18) . . ?
H1A C1 H1C 104(2) . . ?
H1B C1 H1C 104(2) . . ?
O2 C2 C1 108.3(3) . . ?
O2 C2 H2A 108.1(13) . . ?
C1 C2 H2A 112.3(13) . . ?
O2 C2 H2B 107.8(14) . . ?
C1 C2 H2B 109.1(15) . . ?
H2A C2 H2B 111.2(19) . . ?
O2 C3 C8 124.8(2) . . ?
O2 C3 C4 115.6(2) . . ?
C8 C3 C4 119.6(3) . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 119.4(13) . . ?
C3 C4 H4 120.5(13) . . ?
C4 C5 C6 121.2(3) . . ?
C4 C5 H5 121.6(14) . . ?
C6 C5 H5 117.2(14) . . ?
C7 C6 C5 118.2(3) . . ?
C7 C6 N1 122.2(2) . . ?
C5 C6 N1 119.5(2) . . ?
C6 C7 C8 121.3(2) . . ?
C6 C7 H7 120.2(13) . . ?
C8 C7 H7 118.5(13) . . ?
C3 C8 C7 119.7(3) . . ?
C3 C8 H8 118.9(15) . . ?
C7 C8 H8 121.4(15) . . ?
N1 C9 C10 117.96(19) . . ?
N1 C9 C16 123.2(2) . . ?
C10 C9 C16 118.8(2) . . ?
C15 C10 C11 117.1(3) . . ?
C15 C10 C9 121.3(2) . . ?
C11 C10 C9 121.6(2) . . ?
O1 C11 C10 121.8(3) . . ?
O1 C11 C12 118.3(3) . . ?
C10 C11 C12 119.9(3) . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12 125.6(18) . . ?
C11 C12 H12 114.4(18) . . ?
C12 C13 C14 121.8(3) . . ?
C12 C13 H13 117.7(19) . . ?
C14 C13 H13 120.5(19) . . ?
C13 C14 C15 118.5(4) . . ?
C13 C14 H14 124.9(19) . . ?
C15 C14 H14 116.5(19) . . ?
C14 C15 C10 122.7(3) . . ?
C14 C15 H15 119.9(15) . . ?
C10 C15 H15 117.3(14) . . ?
C9 C16 H16A 110.3(18) . . ?
C9 C16 H16B 109.1(18) . . ?
H16A C16 H16B 108(2) . . ?
C9 C16 H16C 110.6(16) . . ?
H16A C16 H16C 106(2) . . ?
H16B C16 H16C 113(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C9 1.286(3) . ?
N1 C6 1.423(3) . ?
O1 C11 1.348(3) . ?
O1 H1 0.93(3) . ?
O2 C3 1.377(3) . ?
O2 C2 1.427(3) . ?
C1 C2 1.484(4) . ?
C1 H1A 0.94(3) . ?
C1 H1B 0.99(3) . ?
C1 H1C 0.99(4) . ?
C2 H2A 0.99(3) . ?
C2 H2B 0.99(3) . ?
C3 C8 1.380(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.373(4) . ?
C4 H4 0.96(3) . ?
C5 C6 1.385(3) . ?
C5 H5 0.93(2) . ?
C6 C7 1.382(3) . ?
C7 C8 1.383(4) . ?
C7 H7 0.99(2) . ?
C8 H8 0.92(3) . ?
C9 C10 1.474(3) . ?
C9 C16 1.505(3) . ?
C10 C15 1.402(3) . ?
C10 C11 1.404(3) . ?
C11 C12 1.407(4) . ?
C12 C13 1.360(4) . ?
C12 H12 0.93(3) . ?
C13 C14 1.370(5) . ?
C13 H13 0.95(3) . ?
C14 C15 1.374(4) . ?
C14 H14 1.05(4) . ?
C15 H15 0.90(2) . ?
C16 H16A 0.97(3) . ?
C16 H16B 0.93(3) . ?
C16 H16C 0.97(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 18299511
|
1100662.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100662.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100662
loop_
_publ_author_name
'Akimoto, Toshio'
'Hirayama, Noriaki'
_publ_section_title
;
Crystal Structure of Ketotifen Fumarate
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x25
_journal_page_last x26
_journal_paper_doi 10.2116/analscix.19.x25
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C23 H23 N O5 S'
_chemical_formula_sum 'C23 H23 N O5 S'
_chemical_formula_weight 425.50
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 74.054(2)
_cell_angle_beta 81.034(3)
_cell_angle_gamma 88.4315(7)
_cell_formula_units_Z 4
_cell_length_a 10.0901(6)
_cell_length_b 11.7760(7)
_cell_length_c 18.8200(7)
_cell_measurement_reflns_used 3320
_cell_measurement_temperature 296.1
_cell_measurement_theta_max 67.8
_cell_measurement_theta_min 5.9
_cell_volume 2123.6(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.8826
_diffrn_measured_fraction_theta_max 0.8826
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5418
_diffrn_reflns_av_R_equivalents 0.070
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 22422
_diffrn_reflns_theta_full 68.14
_diffrn_reflns_theta_max 68.14
_exptl_absorpt_coefficient_mu 1.648
_exptl_absorpt_correction_T_max 0.952
_exptl_absorpt_correction_T_min 0.562
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.331
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 896.00
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.03
_refine_diff_density_max 0.77
_refine_diff_density_min -0.40
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.970
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 593
_refine_ls_number_reflns 3154
_refine_ls_R_factor_gt 0.0680
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0047Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1720
_reflns_number_gt 3116
_reflns_number_total 6850
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C23 H23 N O5 S '
_cod_database_code 1100662
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S(101) S 0.7315(2) 0.5950(2) 0.5147(1) 0.0692(8) Uani 1.00 1 d . . .
S(201) S 0.7678(2) 0.1024(2) 0.5163(1) 0.0717(8) Uani 1.00 1 d . . .
O(110) O 0.4727(6) 0.4961(5) 0.6044(3) 0.077(2) Uani 1.00 1 d . . .
O(210) O 0.9698(6) -0.0156(6) 0.6082(4) 0.082(2) Uani 1.00 1 d . . .
O(301) O 0.4271(5) 0.8147(5) 0.9300(3) 0.068(2) Uani 1.00 1 d . . .
O(302) O 0.2477(6) 0.9035(5) 0.8918(4) 0.072(2) Uani 1.00 1 d . . .
O(303) O 0.3916(5) 0.4156(5) 0.8897(3) 0.069(2) Uani 1.00 1 d . . .
O(304) O 0.1966(5) 0.4927(4) 0.8621(3) 0.057(2) Uani 1.00 1 d . . .
O(401) O 0.9154(6) 0.3382(6) 0.9267(4) 0.096(3) Uani 1.00 1 d . . .
O(402) O 1.1134(6) 0.2827(5) 0.8790(3) 0.062(2) Uani 1.00 1 d . . .
O(403) O 1.0092(5) -0.1225(4) 0.8665(3) 0.056(2) Uani 1.00 1 d . . .
O(404) O 0.8089(5) -0.0600(5) 0.9049(3) 0.069(2) Uani 1.00 1 d . . .
N(115) N 0.8574(5) 0.6844(5) 0.8723(3) 0.042(2) Uani 1.00 1 d . . .
N(215) N 0.4532(5) 0.1988(5) 0.8762(3) 0.041(2) Uani 1.00 1 d . . .
C(102) C 0.8596(8) 0.6897(8) 0.5093(4) 0.065(3) Uani 1.00 1 d . . .
C(103) C 0.8411(7) 0.7425(7) 0.5651(4) 0.055(3) Uani 1.00 1 d . . .
C(104) C 0.7205(7) 0.7075(6) 0.6154(4) 0.043(2) Uani 1.00 1 d . . .
C(105) C 0.6490(7) 0.6265(7) 0.5943(4) 0.046(2) Uani 1.00 1 d . . .
C(106) C 0.6709(6) 0.7567(6) 0.6795(4) 0.038(2) Uani 1.00 1 d . . .
C(107) C 0.5316(7) 0.8015(7) 0.6802(4) 0.044(2) Uani 1.00 1 d . . .
C(108) C 0.4235(7) 0.7226(7) 0.6899(4) 0.051(3) Uani 1.00 1 d . . .
C(109) C 0.4540(8) 0.5917(7) 0.7006(4) 0.058(3) Uani 1.00 1 d . . .
C(110) C 0.5234(8) 0.5671(7) 0.6310(5) 0.054(3) Uani 1.00 1 d . . .
C(111) C 0.5046(8) 0.9192(8) 0.6680(5) 0.066(3) Uani 1.00 1 d . . .
C(112) C 0.3736(9) 0.9594(9) 0.6641(5) 0.081(4) Uani 1.00 1 d . . .
C(113) C 0.2719(7) 0.8824(8) 0.6741(5) 0.060(3) Uani 1.00 1 d . . .
C(114) C 0.2942(8) 0.764(1) 0.6866(4) 0.072(3) Uani 1.00 1 d . . .
C(116) C 0.9079(7) 0.6326(6) 0.8091(4) 0.047(2) Uani 1.00 1 d . . .
C(117) C 0.8869(6) 0.7153(6) 0.7345(4) 0.046(2) Uani 1.00 1 d . . .
C(118) C 0.7433(6) 0.7587(6) 0.7330(4) 0.041(2) Uani 1.00 1 d . . .
C(119) C 0.6903(7) 0.8025(7) 0.7997(4) 0.049(2) Uani 1.00 1 d . . .
C(120) C 0.7122(6) 0.7137(7) 0.8722(4) 0.051(2) Uani 1.00 1 d . . .
C(121) C 0.8821(8) 0.6054(7) 0.9451(4) 0.059(3) Uani 1.00 1 d . . .
C(202) C 0.6459(8) 0.2041(8) 0.5107(4) 0.068(3) Uani 1.00 1 d . . .
C(203) C 0.6337(8) 0.2568(7) 0.5670(4) 0.057(3) Uani 1.00 1 d . . .
C(204) C 0.7266(7) 0.2170(7) 0.6171(4) 0.047(2) Uani 1.00 1 d . . .
C(205) C 0.8089(7) 0.1290(7) 0.5966(4) 0.052(2) Uani 1.00 1 d . . .
C(206) C 0.7422(7) 0.2622(6) 0.6817(4) 0.042(2) Uani 1.00 1 d . . .
C(207) C 0.8827(7) 0.2994(7) 0.6823(4) 0.044(2) Uani 1.00 1 d . . .
C(208) C 0.9828(7) 0.2114(7) 0.6920(4) 0.049(2) Uani 1.00 1 d . . .
C(209) C 0.9424(8) 0.0825(7) 0.7034(4) 0.057(3) Uani 1.00 1 d . . .
C(210) C 0.9097(8) 0.0616(8) 0.6339(5) 0.060(3) Uani 1.00 1 d . . .
C(211) C 0.9181(8) 0.4138(8) 0.6706(5) 0.060(3) Uani 1.00 1 d . . .
C(212) C 1.0525(8) 0.4467(8) 0.6674(5) 0.070(3) Uani 1.00 1 d . . .
C(213) C 1.1475(6) 0.3616(7) 0.6777(4) 0.041(2) Uani 1.00 1 d . . .
C(214) C 1.1145(8) 0.2471(9) 0.6894(4) 0.066(3) Uani 1.00 1 d . . .
C(216) C 0.4323(7) 0.1558(7) 0.8108(4) 0.049(2) Uani 1.00 1 d . . .
C(217) C 0.4964(6) 0.2381(7) 0.7377(4) 0.048(2) Uani 1.00 1 d . . .
C(218) C 0.6415(7) 0.2686(6) 0.7362(4) 0.043(2) Uani 1.00 1 d . . .
C(219) C 0.6626(7) 0.3043(7) 0.8050(4) 0.049(2) Uani 1.00 1 d . . .
C(220) C 0.5998(6) 0.2150(7) 0.8761(4) 0.046(2) Uani 1.00 1 d . . .
C(221) C 0.3863(7) 0.1183(7) 0.9481(4) 0.059(3) Uani 1.00 1 d . . .
C(301) C 0.3247(8) 0.8111(7) 0.9048(4) 0.050(3) Uani 1.00 1 d . . .
C(302) C 0.2809(7) 0.7036(7) 0.8887(4) 0.047(2) Uani 1.00 1 d . . .
C(303) C 0.3462(7) 0.6050(7) 0.9006(4) 0.052(3) Uani 1.00 1 d . . .
C(304) C 0.3087(8) 0.4965(6) 0.8826(4) 0.045(2) Uani 1.00 1 d . . .
C(401) C 0.9859(8) 0.2645(8) 0.9087(5) 0.057(3) Uani 1.00 1 d . . .
C(402) C 0.9357(8) 0.1452(7) 0.9158(4) 0.050(3) Uani 1.00 1 d . . .
C(403) C 0.9948(7) 0.0673(6) 0.8848(4) 0.048(2) Uani 1.00 1 d . . .
C(404) C 0.9318(8) -0.0470(7) 0.8874(4) 0.044(2) Uani 1.00 1 d . . .
H(1) H 0.3564(9) 1.0415(9) 0.6542(5) 0.099(4) Uiso 1.00 1 c . . .
H(2) H 0.5756(8) 0.9738(8) 0.6625(5) 0.083(3) Uiso 1.00 1 c . . .
H(3) H 0.1829(7) 0.9104(8) 0.6728(5) 0.076(4) Uiso 1.00 1 c . . .
H(4) H 0.7346(7) 0.8748(7) 0.7955(4) 0.060(3) Uiso 1.00 1 c . . .
H(5) H 0.1994(7) 0.7056(7) 0.8691(4) 0.059(3) Uiso 1.00 1 c . . .
H(6) H 0.4259(7) 0.6031(7) 0.9219(4) 0.063(3) Uiso 1.00 1 c . . .
H(7) H 0.7562(7) 0.3099(7) 0.8055(4) 0.058(3) Uiso 1.00 1 c . . .
H(8) H 0.6231(7) 0.3791(7) 0.8030(4) 0.058(3) Uiso 1.00 1 c . . .
H(9) H 0.6105(6) 0.2430(7) 0.9177(4) 0.057(3) Uiso 1.00 1 c . . .
H(10) H 0.6436(6) 0.1415(7) 0.8802(4) 0.057(3) Uiso 1.00 1 c . . .
H(11) H 0.4936(6) 0.2002(7) 0.6994(4) 0.058(3) Uiso 1.00 1 c . . .
H(12) H 0.4467(6) 0.3089(7) 0.7277(4) 0.058(3) Uiso 1.00 1 c . . .
H(13) H 0.4691(7) 0.0793(7) 0.8162(4) 0.060(3) Uiso 1.00 1 c . . .
H(14) H 0.2217(8) 0.711(1) 0.6929(4) 0.089(4) Uiso 1.00 1 c . . .
H(15) H 0.8515(8) 0.4728(8) 0.6639(5) 0.073(3) Uiso 1.00 1 c . . .
H(16) H 1.0769(8) 0.5274(8) 0.6579(5) 0.086(3) Uiso 1.00 1 c . . .
H(17) H 1.2377(6) 0.3837(7) 0.6769(4) 0.049(3) Uiso 1.00 1 c . . .
H(18) H 1.1825(8) 0.1894(9) 0.6963(4) 0.081(3) Uiso 1.00 1 c . . .
H(19) H 0.5916(8) 0.2230(8) 0.4723(4) 0.085(3) Uiso 1.00 1 c . . .
H(20) H 0.5687(8) 0.3150(7) 0.5723(4) 0.069(3) Uiso 1.00 1 c . . .
H(21) H 0.8516(8) 0.1224(7) 0.9467(4) 0.061(3) Uiso 1.00 1 c . . .
H(22) H 0.3387(7) 0.1518(7) 0.8100(4) 0.060(3) Uiso 1.00 1 c . . .
H(23) H 0.9027(7) 0.7983(7) 0.5702(4) 0.065(3) Uiso 1.00 1 c . . .
H(24) H 0.5967(7) 0.8153(7) 0.8009(4) 0.060(3) Uiso 1.00 1 c . . .
H(25) H 1.0161(8) 0.0341(7) 0.7171(4) 0.068(3) Uiso 1.00 1 c . . .
H(26) H 0.8677(8) 0.0615(7) 0.7422(4) 0.068(3) Uiso 1.00 1 c . . .
H(27) H 0.6629(6) 0.6434(7) 0.8779(4) 0.061(3) Uiso 1.00 1 c . . .
H(28) H 0.6811(6) 0.7459(7) 0.9127(4) 0.061(3) Uiso 1.00 1 c . . .
H(29) H 1.0009(7) 0.6170(6) 0.8084(4) 0.058(3) Uiso 1.00 1 c . . .
H(30) H 0.9061(5) 0.7561(5) 0.8637(3) 0.050(2) Uiso 1.00 1 c . . .
H(31) H 0.9358(8) 0.7042(8) 0.4712(4) 0.077(3) Uiso 1.00 1 c . . .
H(32) H 0.5102(8) 0.5681(7) 0.7380(4) 0.069(3) Uiso 1.00 1 c . . .
H(33) H 0.8601(7) 0.5608(6) 0.8167(4) 0.058(3) Uiso 1.00 1 c . . .
H(34) H 0.9454(6) 0.7817(6) 0.7238(4) 0.057(3) Uiso 1.00 1 c . . .
H(35) H 0.9088(6) 0.6748(6) 0.6971(4) 0.057(3) Uiso 1.00 1 c . . .
H(36) H 0.8528(8) 0.6430(7) 0.9833(4) 0.070(3) Uiso 1.00 1 c . . .
H(37) H 0.8336(8) 0.5332(7) 0.9553(4) 0.069(3) Uiso 1.00 1 c . . .
H(38) H 0.9752(8) 0.5897(7) 0.9436(4) 0.069(3) Uiso 1.00 1 c . . .
H(39) H 0.3722(8) 0.5475(7) 0.7166(4) 0.069(3) Uiso 1.00 1 c . . .
H(40) H 1.0836(7) 0.0840(6) 0.8587(4) 0.058(3) Uiso 1.00 1 c . . .
H(41) H 0.4127(5) 0.2739(5) 0.8705(3) 0.047(2) Uiso 1.00 1 c . . .
H(42) H 0.3993(7) 0.1497(7) 0.9879(4) 0.068(3) Uiso 1.00 1 c . . .
H(43) H 0.2930(7) 0.1130(7) 0.9468(4) 0.068(3) Uiso 1.00 1 c . . .
H(44) H 0.4239(7) 0.0418(7) 0.9555(4) 0.068(3) Uiso 1.00 1 c . . .
H(45) H 0.186(5) 0.894(5) 0.878(3) 0.01(2) Uiso 1.00 1 c . . .
H(47) H 1.120(7) 0.369(7) 0.868(4) 0.07(3) Uiso 1.00 1 c . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.031 0.018
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.049 0.032
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
S S 0.333 0.557
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100663.cif | #------------------------------------------------------------------------------
#$Date: 2016-01-27 17:27:09 +0200 (Wed, 27 Jan 2016) $
#$Revision: 175153 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100663.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100663
loop_
_publ_author_name
'Kurosaki, Hiromasa'
'Tawada, Toshiaki'
'Kawasoe, Satomi'
'Ohashi, Yoko'
'Goto, Masafumi'
_publ_section_title
;
Crystal Structure of
Chloro{N-mercaptoethyl[bis(6-methyl-2-pyridylmethyl)amine]}zinc(II) complex
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x27
_journal_page_last x28
_journal_paper_doi 10.2116/analscix.19.x27
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C16 H24 Cl N3 S Zn'
_chemical_formula_sum 'C16 H24 Cl N3 S Zn'
_chemical_formula_weight 391.28
_space_group_IT_number 31
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 31
_symmetry_space_group_name_Hall 'P 2ac -2'
_symmetry_space_group_name_H-M 'P m n 21'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 13.5608(8)
_cell_length_b 7.2782(9)
_cell_length_c 8.6423(5)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293.2
_cell_measurement_theta_max 20.0
_cell_measurement_theta_min 19.8
_cell_volume 853.0(1)
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 1.0000
_diffrn_measurement_device_type 'Rigaku AFC7R'
_diffrn_measurement_method \w-2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.017
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 3215
_diffrn_reflns_theta_full 27.50
_diffrn_reflns_theta_max 27.50
_diffrn_standards_decay_% 0.17
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.718
_exptl_absorpt_correction_T_max 0.998
_exptl_absorpt_correction_T_min 0.965
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North, Phillips & Mathews,1968)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.523
_exptl_crystal_description prismatic
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.200
_refine_diff_density_max 0.90
_refine_diff_density_min -0.86
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 320.490
_refine_ls_hydrogen_treatment noref
_refine_ls_number_parameters 112
_refine_ls_number_reflns 1053
_refine_ls_R_factor_gt 0.0534
_refine_ls_shift/su_max 4.3196
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme unit
_refine_ls_wR_factor_ref 0.0308
_reflns_number_gt 1053
_reflns_number_total 1088
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_database_code 1100663
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,z
1/2-x,-y,1/2+z
1/2+x,-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn(1) Zn 0.0000 0.216969(6) 0.00609(1) 0.04226(1) Uani 1.00 d S . .
Cl(1) Cl 0.0000 0.16207(2) 0.25989(1) 0.06764(4) Uani 1.00 d S . .
S(1) S 0.0000 0.04347(1) -0.21237(1) 0.04916(3) Uani 1.00 d S . .
N(1) N 0.0000 0.47982(4) -0.10933(3) 0.03962(9) Uani 1.00 d S . .
N(2) N 0.16836(1) 0.29829(3) -0.00778(3) 0.03997(5) Uani 1.00 d . . .
C(1) C 0.09233(2) 0.58625(3) -0.07534(3) 0.05578(9) Uani 1.00 d . . .
C(2) C 0.18086(2) 0.46378(3) -0.06943(3) 0.04238(8) Uani 1.00 d . . .
C(3) C 0.27019(2) 0.52297(5) -0.12292(3) 0.05590(9) Uani 1.00 d . . .
C(4) C 0.34789(2) 0.40430(4) -0.10734(4) 0.0670(1) Uani 1.00 d . . .
C(5) C 0.34054(2) 0.24220(4) -0.04248(3) 0.05205(9) Uani 1.00 d . . .
C(6) C 0.24659(2) 0.18779(3) 0.00672(4) 0.04795(7) Uani 1.00 d . . .
C(7) C 0.23092(2) 0.00375(4) 0.08236(3) 0.0748(1) Uani 1.00 d . . .
C(8) C 0.0000 0.42876(6) -0.26741(5) 0.0746(2) Uani 1.00 d S . .
C(9) C 0.04035(3) 0.24814(9) -0.31103(5) 0.0749(2) Uani 0.50 d P . .
H(1) H 0.0978 0.6906 -0.1454 0.0616 Uiso 1.00 calc . . .
H(2) H 0.0806 0.6537 0.0293 0.0616 Uiso 1.00 calc . . .
H(3) H 0.2797 0.6497 -0.1647 0.0646 Uiso 1.00 calc . . .
H(4) H 0.4132 0.4552 -0.1423 0.0726 Uiso 1.00 calc . . .
H(5) H 0.3997 0.1650 -0.0255 0.0707 Uiso 1.00 calc . . .
H(6) H 0.2918 -0.0716 0.0946 0.0798 Uiso 1.00 calc . . .
H(7) H 0.2047 0.0063 0.1908 0.0798 Uiso 1.00 calc . . .
H(8) H 0.1855 -0.0760 0.0280 0.0798 Uiso 1.00 calc . . .
H(9) H 0.0357 0.5186 -0.3376 0.0775 Uiso 1.00 calc . . .
H(10) H -0.0667 0.4270 -0.3163 0.0775 Uiso 1.00 calc . . .
H(11) H 0.1114 0.2604 -0.3108 0.0600 Uiso 1.00 calc . . .
H(12) H 0.0269 0.2287 -0.4286 0.0600 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.284 1.430
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and=
6.1.1.1)
;
|
1100664.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100664.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100664
loop_
_publ_author_name
'Mahendra, M.'
'Doreswamy, B. H.'
'Khanum, S. A.'
'Shashikanth, S.'
'Sudha, B. S.'
'Sridhar, M. A.'
'Prasad, J. S.'
_publ_section_title
;
Synthesis and Crystal Structure of (2-Hydroxy-5-methyl phenyl)phenyl Methanone
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x29
_journal_page_last x30
_journal_paper_doi 10.2116/analscix.19.x29
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C14 H12 O2'
_chemical_formula_sum 'C14 H12 O2'
_chemical_formula_weight 212.24
_space_group_IT_number 61
_space_group_name_Hall '-P 2ac 2ab'
_space_group_name_H-M_alt 'P b c a'
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 61
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 5.8820(5)
_cell_length_b 12.1040(5)
_cell_length_c 30.580(3)
_cell_measurement_temperature 293
_cell_volume 2177.2(3)
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.562
_diffrn_measured_fraction_theta_max 0.562
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0122
_diffrn_reflns_av_sigmaI/netI 0.0190
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 46
_diffrn_reflns_limit_l_min -45
_diffrn_reflns_number 3987
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full 32.55
_diffrn_reflns_theta_max 32.55
_diffrn_reflns_theta_min 3.91
_exptl_absorpt_coefficient_mu 0.086
_exptl_crystal_density_diffrn 1.295
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 896
_refine_diff_density_max 0.256
_refine_diff_density_min -0.328
_refine_diff_density_rms 0.038
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 0.010(4)
_refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^
_refine_ls_extinction_method shelxl
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 146
_refine_ls_number_reflns 2221
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.057
_refine_ls_R_factor_all 0.0786
_refine_ls_R_factor_gt 0.0590
_refine_ls_shift/su_max 0.008
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1185P)^2^+0.6250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1965
_refine_ls_wR_factor_ref 0.2227
_reflns_number_gt 1543
_reflns_number_total 2221
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100664
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,y,1/2-z
1/2-x,1/2+y,z
x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
O8 O Uani -0.1156(4) 0.56852(17) 0.40456(6) 1.000 0.0731(9) . .
O11 O Uani -0.0139(4) 0.40350(16) 0.35583(7) 1.000 0.0762(9) . .
C1 C Uani 0.3417(5) 0.7221(2) 0.44091(6) 1.000 0.0523(9) . .
C2 C Uani 0.3888(5) 0.8151(2) 0.46580(6) 1.000 0.0611(9) . .
C3 C Uani 0.2328(6) 0.9007(2) 0.46817(7) 1.000 0.0636(12) . .
C4 C Uani 0.0309(6) 0.8933(2) 0.44640(8) 1.000 0.0663(12) . .
C5 C Uani -0.0224(5) 0.7992(2) 0.42282(7) 1.000 0.0576(9) . .
C6 C Uani 0.1356(5) 0.71385(17) 0.41974(6) 1.000 0.0465(8) . .
C7 C Uani 0.0676(5) 0.6123(2) 0.39536(6) 1.000 0.0515(9) . .
C9 C Uani 0.2171(5) 0.56701(18) 0.36161(6) 1.000 0.0495(8) . .
C10 C Uani 0.1674(6) 0.4615(2) 0.34371(6) 1.000 0.0595(12) . .
C12 C Uani 0.3118(6) 0.4186(2) 0.31227(7) 1.000 0.0695(12) . .
C13 C Uani 0.4912(6) 0.4793(2) 0.29716(7) 1.000 0.0728(12) . .
C14 C Uani 0.5388(5) 0.5860(2) 0.31250(6) 1.000 0.0580(9) . .
C15 C Uani 0.7256(6) 0.6537(3) 0.29407(8) 1.000 0.0759(13) . .
C16 C Uani 0.3998(5) 0.62634(18) 0.34521(6) 1.000 0.0503(8) . .
H1 H Uiso 0.45140 0.66380 0.43830 1.000 0.0630 . R
H2 H Uiso 0.53050 0.81970 0.48130 1.000 0.0730 . R
H3 H Uiso 0.26390 0.96600 0.48490 1.000 0.0760 . R
H4 H Uiso -0.07410 0.95400 0.44750 1.000 0.0800 . R
H5 H Uiso -0.16770 0.79100 0.40890 1.000 0.0690 . R
H11 H Uiso -0.14430 0.36140 0.36470 1.000 0.0910 . R
H12 H Uiso 0.28380 0.34590 0.30090 1.000 0.0830 . R
H13 H Uiso 0.58710 0.44620 0.27540 1.000 0.0870 . R
H15A H Uiso 0.80040 0.61220 0.27150 1.000 0.0910 . R
H15B H Uiso 0.83250 0.67100 0.31680 1.000 0.0910 . R
H15C H Uiso 0.66630 0.72100 0.28190 1.000 0.0910 . R
H16 H Uiso 0.43500 0.69780 0.35700 1.000 0.0600 . R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
|
1100665.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100665.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100665
loop_
_publ_author_name
'Doreswamy, Beeranahally H.'
Basappa
'Mahendra, Madegowda'
'Mantelingu, Kempegowda'
'Anandalwar, Sridhar M.'
'Prasad, Javaregowda S.'
'Rangappa, Kanchugarakoppal S.'
_publ_section_title
;
Microwave-Assisted Synthesis and Crystal Structure of
2-Butyl-4-chloro-1H-imidazole-5-carboxaldehyde
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x31
_journal_page_last x32
_journal_paper_doi 10.2116/analscix.19.x31
_journal_volume 19
_journal_year 2003
_chemical_formula_iupac 2-Butyl-4-chloro-1H-imidazole-5-carboxaldehy
_chemical_formula_moiety 'C8 H11 Cl N2 O'
_chemical_formula_sum 'C8 H11 Cl N2 O'
_chemical_formula_weight 186.64
_chemical_name_common imidazole
_chemical_name_systematic
;
2-Butyl-4-chloro-1H-imidazole-5-carboxaldehyde
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 101.94
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.251
_cell_length_b 13.195(1)
_cell_length_c 9.835(1)
_cell_volume 920.62(12)
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0257
_diffrn_reflns_av_sigmaI/netI 0.0303
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 3617
_diffrn_reflns_theta_full 27.93
_diffrn_reflns_theta_max 27.93
_diffrn_reflns_theta_min 2.62
_exptl_absorpt_coefficient_mu 0.369
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.347
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description '0.25 x 0.2 x 0.25 mm'
_exptl_crystal_F_000 392
_refine_diff_density_max 0.657
_refine_diff_density_min -0.431
_refine_diff_density_rms 0.125
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 0.13(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.064
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 111
_refine_ls_number_reflns 1977
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.064
_refine_ls_R_factor_all 0.0798
_refine_ls_R_factor_gt 0.0651
_refine_ls_shift/su_max 0.009
_refine_ls_shift/su_mean 0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+0.1028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1890
_refine_ls_wR_factor_ref 0.2167
_reflns_number_gt 1552
_reflns_number_total 1977
_reflns_threshold_expression I>2\s(I)
_cod_duplicate_entry 1100658
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100665
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_adp_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Cl1 Cl Uani 0.76028(10) 0.54189(5) 0.15677(7) 1.000 0.0694(3) . .
O5 O Uani 0.7653(3) 0.54495(14) -0.3082(3) 1.000 0.0740(8) . .
N6 N Uani 0.9265(3) 0.70522(13) -0.1187(2) 1.000 0.0474(6) . .
N8 N Uani 0.9356(3) 0.71213(13) 0.1070(2) 1.000 0.0505(6) . .
C2 C Uani 0.8477(3) 0.62639(15) 0.0535(2) 1.000 0.0493(7) . .
C3 C Uani 0.8389(3) 0.61811(15) -0.0863(2) 1.000 0.0488(7) . .
C4 C Uani 0.7611(4) 0.54124(17) -0.1863(3) 1.000 0.0594(9) . .
C7 C Uani 0.9802(3) 0.75943(15) -0.0026(2) 1.000 0.0477(7) . .
C9 C Uani 1.0789(4) 0.85854(15) 0.0039(3) 1.000 0.0558(8) . .
C10 C Uani 1.2784(4) 0.85528(18) 0.0933(3) 1.000 0.0609(9) . .
C11 C Uani 1.4124(4) 0.7833(2) 0.0407(3) 1.000 0.0656(9) . .
C12 C Uani 1.4663(5) 0.8192(3) -0.0901(4) 1.000 0.0827(12) . .
H4 H Uiso 0.70410 0.48530 -0.15470 1.000 0.0710 calc R
H6 H Uiso 0.94360 0.72170 -0.19980 1.000 0.0570 calc R
H9A H Uiso 1.00600 0.90900 0.04150 1.000 0.0670 calc R
H9B H Uiso 1.08550 0.87930 -0.08950 1.000 0.0670 calc R
H10A H Uiso 1.33110 0.92310 0.09820 1.000 0.0730 calc R
H10B H Uiso 1.27070 0.83530 0.18690 1.000 0.0730 calc R
H11A H Uiso 1.52570 0.77540 0.11220 1.000 0.0790 calc R
H11B H Uiso 1.35310 0.71730 0.02410 1.000 0.0790 calc R
H12A H Uiso 1.35550 0.82410 -0.16270 1.000 0.1240 calc R
H12B H Uiso 1.55290 0.77200 -0.11700 1.000 0.1240 calc R
H12C H Uiso 1.52500 0.88460 -0.07460 1.000 0.1240 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0831(6) 0.0584(5) 0.0714(6) 0.0143(2) 0.0267(4) -0.0104(3)
N6 0.0577(11) 0.0413(9) 0.0459(11) 0.0009(6) 0.0168(7) 0.0013(7)
N8 0.0617(11) 0.0415(9) 0.0503(12) 0.0017(7) 0.0161(8) -0.0003(7)
C9 0.0690(15) 0.0357(11) 0.0659(16) 0.0009(8) 0.0211(11) -0.0004(9)
C2 0.0543(12) 0.0392(10) 0.0566(14) 0.0044(8) 0.0167(9) 0.0022(8)
C3 0.0552(12) 0.0394(10) 0.0540(14) 0.0006(8) 0.0167(9) 0.0009(8)
C7 0.0547(12) 0.0369(10) 0.0538(13) 0.0021(8) 0.0163(9) 0.0032(8)
O5 0.0928(16) 0.0676(13) 0.0625(13) -0.0145(8) 0.0183(10) -0.0105(9)
C11 0.0635(15) 0.0582(14) 0.0737(18) 0.0014(11) 0.0107(12) 0.0021(11)
C4 0.0621(14) 0.0477(13) 0.0696(18) -0.0077(9) 0.0167(11) -0.0047(9)
C10 0.0716(16) 0.0506(13) 0.0619(16) -0.0090(10) 0.0173(11) -0.0073(11)
C12 0.083(2) 0.083(2) 0.087(2) -0.0026(16) 0.0290(16) 0.0158(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 N6 C3 108.33(19) . . ?
C7 N8 C2 104.50(19) . . ?
C7 C9 C10 112.9(2) . . ?
N8 C2 C3 112.21(19) . . ?
N8 C2 Cl1 121.11(18) . . ?
C3 C2 Cl1 126.68(17) . . ?
C2 C3 N6 103.75(18) . . ?
C2 C3 C4 132.1(2) . . ?
N6 C3 C4 124.1(2) . . ?
N6 C7 N8 111.21(19) . . ?
N6 C7 C9 124.1(2) . . ?
N8 C7 C9 124.7(2) . . ?
C12 C11 C10 113.1(2) . . ?
O5 C4 C3 124.2(2) . . ?
C11 C10 C9 114.6(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C2 1.715(2) . ?
N6 C7 1.336(3) . ?
N6 C3 1.382(3) . ?
N8 C7 1.341(3) . ?
N8 C2 1.350(3) . ?
C9 C7 1.486(3) . ?
C9 C10 1.530(4) . ?
C2 C3 1.368(3) . ?
C3 C4 1.444(3) . ?
O5 C4 1.206(4) . ?
C11 C12 1.497(5) . ?
C11 C10 1.523(4) . ?
|
1100666.cif | #------------------------------------------------------------------------------
#$Date: 2021-04-22 17:20:50 +0300 (Thu, 22 Apr 2021) $
#$Revision: 264417 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100666.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100666
loop_
_publ_author_name
'Mahendra, Madegowda'
'Doreswamy, Beeranahally H.'
'Sridhar, Mandayam A.'
'Prasad, Javaregowda S.'
'Narodia, Vishal P.'
'Naliapara, Yogesh T.'
'Shah, Anamik'
_publ_section_title
;
Crystal Structure of Ethyl-2H-1-benzopyran-2-oxo-3-carboxylate
;
_journal_coden_ASTM XSAOAF
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x33
_journal_page_last x34
_journal_paper_doi 10.2116/analscix.19.x33
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C12 H10 O4'
_chemical_formula_sum 'C12 H10 O4'
_chemical_formula_weight 218.20
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 108.110(6)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.9160(10)
_cell_length_b 15.736(2)
_cell_length_c 8.7370(8)
_cell_measurement_temperature 293
_cell_volume 1034.4(2)
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0215
_diffrn_reflns_av_sigmaI/netI 0.0261
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 2502
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full 23.25
_diffrn_reflns_theta_max 23.25
_diffrn_reflns_theta_min 2.77
_exptl_absorpt_coefficient_mu 0.106
_exptl_crystal_density_diffrn 1.401
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 456
_refine_diff_density_max 0.423
_refine_diff_density_min -0.477
_refine_diff_density_rms 0.154
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.111
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 145
_refine_ls_number_reflns 1470
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.111
_refine_ls_R_factor_all 0.0902
_refine_ls_R_factor_gt 0.0696
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1636P)^2^+0.1491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1966
_refine_ls_wR_factor_ref 0.2325
_reflns_number_gt 1124
_reflns_number_total 1470
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
Updated bibliographic information.
Antanas Vaitkus,
2021-04-22
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100666
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O Uani 0.7845(4) 0.12665(15) 0.7323(3) 1.000 0.0888(10) . .
O3 O Uani 0.6081(3) 0.01865(12) 0.7214(2) 1.000 0.0646(7) . .
O13 O Uani 0.9538(3) 0.19207(14) 1.0378(3) 1.000 0.0855(10) . .
O14 O Uani 1.0050(3) 0.09495(12) 1.2326(2) 1.000 0.0666(7) . .
C2 C Uani 0.7395(4) 0.07299(18) 0.8078(3) 1.000 0.0620(10) . .
C4 C Uani 0.5611(3) -0.05345(17) 0.7862(3) 1.000 0.0539(9) . .
C5 C Uani 0.4332(4) -0.10559(19) 0.6847(3) 1.000 0.0624(10) . .
C6 C Uani 0.3889(4) -0.17948(19) 0.7451(4) 1.000 0.0655(10) . .
C7 C Uani 0.4689(4) -0.20221(18) 0.9039(4) 1.000 0.0680(11) . .
C8 C Uani 0.5932(4) -0.1495(2) 1.0049(3) 1.000 0.0642(10) . .
C9 C Uani 0.6418(3) -0.07365(16) 0.9476(3) 1.000 0.0516(9) . .
C10 C Uani 0.7656(3) -0.01392(16) 1.0444(3) 1.000 0.0523(9) . .
C11 C Uani 0.8111(3) 0.05752(16) 0.9817(3) 1.000 0.0514(9) . .
C12 C Uani 0.9312(3) 0.12255(18) 1.0826(3) 1.000 0.0567(10) . .
C15 C Uani 1.1087(4) 0.1573(2) 1.3471(3) 1.000 0.0726(11) . .
C16 C Uani 1.1527(6) 0.1192(3) 1.5090(4) 1.000 0.1027(16) . .
H5 H Uiso 0.37690 -0.08940 0.57460 1.000 0.0750 . R
H6 H Uiso 0.30180 -0.21650 0.67590 1.000 0.0790 . R
H7 H Uiso 0.43750 -0.25440 0.94510 1.000 0.0820 . R
H8 H Uiso 0.64720 -0.16530 1.11550 1.000 0.0770 . R
H10 H Uiso 0.81790 -0.02580 1.15700 1.000 0.0630 . R
H15A H Uiso 1.21660 0.16860 1.32250 1.000 0.0870 . R
H15B H Uiso 1.04160 0.20890 1.33820 1.000 0.0870 . R
H16A H Uiso 1.22190 0.15860 1.58760 1.000 0.1230 . R
H16B H Uiso 1.21810 0.06730 1.51470 1.000 0.1230 . R
H16C H Uiso 1.04310 0.10760 1.53040 1.000 0.1230 . R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
|
1100667.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100667.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100667
loop_
_publ_author_name
'Haramura, Masayuki'
'Yanaka, Akito'
'Akimoto, Toshio'
'Hirayama, Noriaki'
_publ_section_title
;
Crystal Structure of Dichlorphenamide
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x35
_journal_page_last x36
_journal_paper_doi 10.2116/analscix.19.x35
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C6 H6 Cl2 N2 O4 S2'
_chemical_formula_sum 'C6 H6 Cl2 N2 O4 S2'
_chemical_formula_weight 305.15
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 15
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_cell_angle_alpha 90
_cell_angle_beta 94.716(9)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 17.202(2)
_cell_length_b 7.9139(9)
_cell_length_c 16.507(3)
_cell_measurement_reflns_used 5401
_cell_measurement_temperature 296.1
_cell_measurement_theta_max 67.8
_cell_measurement_theta_min 6.0
_cell_volume 2239.5(5)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9766
_diffrn_measured_fraction_theta_max 0.9766
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5419
_diffrn_reflns_av_R_equivalents 0.053
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 25216
_diffrn_reflns_theta_full 68.25
_diffrn_reflns_theta_max 68.25
_exptl_absorpt_coefficient_mu 8.761
_exptl_absorpt_correction_T_max 0.269
_exptl_absorpt_correction_T_min 0.106
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.810
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description chip
_exptl_crystal_F_000 1232.00
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.34
_refine_diff_density_min -0.29
_refine_ls_extinction_coef 14(2)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref 1.093
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 170
_refine_ls_number_reflns 1774
_refine_ls_R_factor_gt 0.0370
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0910
_reflns_number_gt 1771
_reflns_number_total 2171
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C6 H6 Cl2 N2 O4 S2 '
_cod_database_code 1100667
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.88071(4) -0.0571(1) 0.45887(5) 0.0558(2) Uani 1.00 1 d . . .
Cl2 Cl 0.71543(5) -0.0984(1) 0.36726(4) 0.0631(3) Uani 1.00 1 d . . .
S1 S 0.58151(3) 0.09935(8) 0.63672(4) 0.0357(2) Uani 1.00 1 d . . .
S2 S 0.89590(4) 0.09823(9) 0.64259(4) 0.0390(2) Uani 1.00 1 d . . .
O1 O 0.5205(1) 0.1544(3) 0.5786(1) 0.0488(6) Uani 1.00 1 d . . .
O2 O 0.6056(1) 0.2023(3) 0.7048(1) 0.0528(6) Uani 1.00 1 d . . .
O3 O 0.9420(1) 0.1939(3) 0.5914(1) 0.0590(7) Uani 1.00 1 d . . .
O4 O 0.8768(1) 0.1674(3) 0.7186(1) 0.0559(6) Uani 1.00 1 d . . .
N1 N 0.5555(2) -0.0772(4) 0.6690(2) 0.0558(9) Uani 1.00 1 d . . .
N2 N 0.9380(2) -0.0752(4) 0.6613(2) 0.0503(8) Uani 1.00 1 d . . .
C1 C 0.6658(1) 0.0663(3) 0.5842(1) 0.0321(7) Uani 1.00 1 d . . .
C2 C 0.7381(1) 0.0953(3) 0.6243(2) 0.0343(7) Uani 1.00 1 d . . .
C3 C 0.8048(1) 0.0602(3) 0.5861(1) 0.0331(7) Uani 1.00 1 d . . .
C4 C 0.7992(1) -0.0028(3) 0.5062(1) 0.0359(7) Uani 1.00 1 d . . .
C5 C 0.7253(1) -0.0268(4) 0.4663(1) 0.0375(7) Uani 1.00 1 d . . .
C6 C 0.6586(1) 0.0066(4) 0.5047(1) 0.0370(7) Uani 1.00 1 d . . .
H1 H 0.577(2) -0.125(5) 0.697(3) 0.06(1) Uiso 1.00 1 c . . .
H2 H 0.525(2) -0.134(5) 0.636(2) 0.07(1) Uiso 1.00 1 c . . .
H3 H 0.921(2) -0.137(5) 0.698(2) 0.07(1) Uiso 1.00 1 c . . .
H4 H 0.955(2) -0.123(5) 0.623(3) 0.08(1) Uiso 1.00 1 c . . .
H5 H 0.741(2) 0.137(4) 0.674(2) 0.045(8) Uiso 1.00 1 c . . .
H6 H 0.606(1) -0.023(3) 0.469(2) 0.032(6) Uiso 1.00 1 c . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
S S 0.333 0.557
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.049 0.032
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.364 0.702
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.031 0.018
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100668.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100668.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100668
loop_
_publ_author_name
'Haramura, Masayuki'
'Tanaka, Akito'
'Akimoto, Toshio'
'Hirayama, Noriaki'
_publ_section_title
;
Crystal Structure of Clobetasol Propionate
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x37
_journal_page_last x38
_journal_paper_doi 10.2116/analscix.19.x37
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C25 H32 Cl F O5'
_chemical_formula_sum 'C25 H32 Cl F O5'
_chemical_formula_weight 466.98
_space_group_IT_number 4
_space_group_name_Hall 'P 2yb'
_space_group_name_H-M_alt 'P 1 21 1'
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 4
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 95.739(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.6961(3)
_cell_length_b 14.6036(5)
_cell_length_c 10.4355(5)
_cell_measurement_reflns_used 3852
_cell_measurement_temperature 293.1
_cell_measurement_theta_max 66.9
_cell_measurement_theta_min 9.1
_cell_volume 1166.98(8)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9347
_diffrn_measured_fraction_theta_max 0.9347
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.5419
_diffrn_reflns_av_R_equivalents 0.042
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 13150
_diffrn_reflns_theta_full 68.15
_diffrn_reflns_theta_max 68.15
_exptl_absorpt_coefficient_mu 1.806
_exptl_absorpt_correction_T_max 0.791
_exptl_absorpt_correction_T_min 0.535
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.329
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 496.00
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.13
_refine_diff_density_max 0.33
_refine_diff_density_min -0.26
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1732 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.01(2)
_refine_ls_extinction_coef 127(8)
_refine_ls_extinction_method
'Larson (1970) Crystallographic Computing eq. 22'
_refine_ls_goodness_of_fit_ref 0.985
_refine_ls_hydrogen_treatment mixed
_refine_ls_number_parameters 353
_refine_ls_number_reflns 3024
_refine_ls_R_factor_gt 0.0380
_refine_ls_shift/su_max 0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0011Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0910
_reflns_number_gt 3005
_reflns_number_total 3818
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C25 H32 Cl F O5 '
_cod_database_code 1100668
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl(22) Cl 0.2346(2) -0.0883(1) -0.5901(1) 0.1111(5) Uani 1.00 1 d . . .
F(9) F -0.1850(2) -0.5253(1) -0.7459(1) 0.0444(5) Uani 1.00 1 d . . .
O(3) O -0.2906(3) -0.7697(2) -1.0474(3) 0.0656(8) Uani 1.00 1 d . . .
O(11) O -0.0471(4) -0.3359(2) -0.9218(2) 0.0606(7) Uani 1.00 1 d . . .
O(20) O -0.1133(4) -0.1009(2) -0.4840(3) 0.0844(9) Uani 1.00 1 d . . .
O(24) O -0.0035(3) -0.3327(2) -0.4285(2) 0.0600(6) Uani 1.00 1 d . . .
O(25) O 0.0114(4) -0.2519(2) -0.2450(3) 0.098(1) Uani 1.00 1 d . . .
C(1) C -0.1326(4) -0.5423(2) -1.0070(3) 0.0461(9) Uani 1.00 1 d . . .
C(2) C -0.1350(4) -0.6307(2) -1.0343(3) 0.051(1) Uani 1.00 1 d . . .
C(3) C -0.2867(4) -0.6869(2) -1.0201(3) 0.0494(9) Uani 1.00 1 d . . .
C(4) C -0.4363(4) -0.6416(2) -0.9727(3) 0.0486(9) Uani 1.00 1 d . . .
C(5) C -0.4368(4) -0.5527(2) -0.9427(3) 0.0431(8) Uani 1.00 1 d . . .
C(6) C -0.5885(4) -0.5068(2) -0.8880(3) 0.0514(9) Uani 1.00 1 d . . .
C(7) C -0.5290(4) -0.4604(2) -0.7604(3) 0.0472(9) Uani 1.00 1 d . . .
C(8) C -0.3719(4) -0.3975(2) -0.7679(3) 0.0391(8) Uani 1.00 1 d . . .
C(9) C -0.2228(3) -0.4485(2) -0.8263(3) 0.0344(7) Uani 1.00 1 d . . .
C(10) C -0.2822(4) -0.4908(2) -0.9608(3) 0.0394(8) Uani 1.00 1 d . . .
C(11) C -0.0453(4) -0.3970(2) -0.8176(3) 0.0440(9) Uani 1.00 1 d . . .
C(12) C 0.0019(4) -0.3513(2) -0.6872(3) 0.0454(9) Uani 1.00 1 d . . .
C(13) C -0.1484(4) -0.2961(2) -0.6385(3) 0.0417(8) Uani 1.00 1 d . . .
C(14) C -0.3043(4) -0.3605(2) -0.6359(3) 0.0413(8) Uani 1.00 1 d . . .
C(15) C -0.4275(4) -0.3097(2) -0.5557(3) 0.057(1) Uani 1.00 1 d . . .
C(16) C -0.3041(5) -0.2757(3) -0.4406(3) 0.068(1) Uani 1.00 1 d . . .
C(17) C -0.1197(4) -0.2647(2) -0.4924(3) 0.0501(9) Uani 1.00 1 d . . .
C(18) C -0.1940(6) -0.2125(2) -0.7223(4) 0.054(1) Uani 1.00 1 d . . .
C(19) C -0.3422(6) -0.4186(3) -1.0657(3) 0.057(1) Uani 1.00 1 d . . .
C(20) C -0.0321(5) -0.1702(3) -0.4826(3) 0.060(1) Uani 1.00 1 d . . .
C(21) C 0.1652(5) -0.1691(3) -0.4801(4) 0.068(1) Uani 1.00 1 d . . .
C(23) C -0.3772(7) -0.1968(5) -0.3670(6) 0.100(2) Uani 1.00 1 d . . .
C(25) C 0.0464(5) -0.3207(4) -0.3019(3) 0.077(1) Uani 1.00 1 d . . .
C(26) C 0.1413(8) -0.4026(4) -0.2451(4) 0.112(2) Uani 1.00 1 d . . .
C(27) C 0.2737(9) -0.4400(4) -0.3168(6) 0.130(2) Uani 1.00 1 d . . .
H(10) H -0.400(5) -0.145(3) -0.429(4) 0.07(1) Uiso 1.00 1 c . . .
H(11) H -0.480(6) -0.225(3) -0.326(4) 0.09(1) Uiso 1.00 1 c . . .
H(12) H -0.281(7) -0.173(3) -0.312(5) 0.11(2) Uiso 1.00 1 c . . .
H(18) H -0.222(6) -0.385(3) -1.089(4) 0.10(1) Uiso 1.00 1 c . . .
H(19) H -0.430(5) -0.375(3) -1.036(3) 0.07(1) Uiso 1.00 1 c . . .
H(20) H -0.377(4) -0.454(2) -1.146(3) 0.053(9) Uiso 1.00 1 c . . .
H(21) H -0.230(5) -0.228(3) -0.813(4) 0.08(1) Uiso 1.00 1 c . . .
H(22) H -0.282(5) -0.179(2) -0.695(3) 0.05(1) Uiso 1.00 1 c . . .
H(23) H -0.088(4) -0.174(2) -0.727(3) 0.046(8) Uiso 1.00 1 c . . .
H(26) H 0.047(6) -0.318(3) -0.922(4) 0.07(1) Uiso 1.00 1 c . . .
H(1) H -0.0341(4) -0.6578(2) -1.0638(3) 0.062(1) Uiso 1.00 1 c . . .
H(2) H -0.0290(4) -0.5091(2) -1.0177(3) 0.056(1) Uiso 1.00 1 c . . .
H(3) H -0.5383(4) -0.6766(2) -0.9633(3) 0.059(1) Uiso 1.00 1 c . . .
H(4) H -0.6362(4) -0.4621(2) -0.9475(3) 0.062(1) Uiso 1.00 1 c . . .
H(5) H -0.6750(4) -0.5513(2) -0.8747(3) 0.062(1) Uiso 1.00 1 c . . .
H(6) H -0.6231(4) -0.4249(2) -0.7349(3) 0.057(1) Uiso 1.00 1 c . . .
H(7) H -0.4989(4) -0.5063(2) -0.6977(3) 0.057(1) Uiso 1.00 1 c . . .
H(8) H -0.4829(4) -0.2601(2) -0.6025(3) 0.069(1) Uiso 1.00 1 c . . .
H(9) H -0.5138(4) -0.3498(2) -0.5283(3) 0.070(1) Uiso 1.00 1 c . . .
H(13) H 0.0371(4) -0.3972(2) -0.6256(3) 0.055(1) Uiso 1.00 1 c . . .
H(14) H 0.0966(4) -0.3107(2) -0.6956(3) 0.054(1) Uiso 1.00 1 c . . .
H(15) H 0.2039(5) -0.2282(3) -0.5026(4) 0.081(2) Uiso 1.00 1 c . . .
H(16) H 0.2147(5) -0.1539(3) -0.3957(4) 0.081(2) Uiso 1.00 1 c . . .
H(17) H 0.1918(8) -0.3881(4) -0.1608(4) 0.134(2) Uiso 1.00 1 c . . .
H(24) H 0.0571(8) -0.4497(4) -0.2406(4) 0.134(2) Uiso 1.00 1 c . . .
H(25) H 0.3224(9) -0.4935(4) -0.2757(6) 0.151(3) Uiso 1.00 1 c . . .
H(27) H 0.2266(9) -0.4546(4) -0.4019(6) 0.151(3) Uiso 1.00 1 c . . .
H(28) H 0.3621(9) -0.3948(4) -0.3197(6) 0.152(3) Uiso 1.00 1 c . . .
H(29) H -0.2921(5) -0.3253(3) -0.3814(3) 0.082(2) Uiso 1.00 1 c . . .
H(30) H -0.2632(4) -0.4120(2) -0.5863(3) 0.050(1) Uiso 1.00 1 c . . .
H(31) H -0.4068(4) -0.3472(2) -0.8221(3) 0.047(1) Uiso 1.00 1 c . . .
H(32) H 0.0421(4) -0.4416(2) -0.8281(3) 0.053(1) Uiso 1.00 1 c . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cl Cl 0.364 0.702
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.073 0.053
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.049 0.032
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100669.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100669.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100669
loop_
_publ_author_name
'Ooyama, Dai'
'Sato, Masahito'
_publ_section_title
'Crystal Structure of (2,2'-Bipyridine-N,N')(diphenyl-2-phosphinopyridine-P)-chloro(dicarbonyl)ruthenium(II) Hexafluorophosphate'
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x39
_journal_page_last x40
_journal_paper_doi 10.2116/analscix.19.x39
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C29 H22 Cl F6 N3 O2 P2 Ru'
_chemical_formula_weight 756.97
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 106.257(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.237(1)
_cell_length_b 18.754(2)
_cell_length_c 16.566(2)
_cell_measurement_reflns_used 8303
_cell_measurement_temperature 173.1
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.0
_cell_volume 3053.3(5)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.030
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 340
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_exptl_absorpt_coefficient_mu 0.775
_exptl_absorpt_correction_type none
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.647
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Platelet
_exptl_crystal_size_max 0.330
_exptl_crystal_size_mid 0.280
_exptl_crystal_size_min 0.050
_refine_diff_density_max 0.55
_refine_diff_density_min -0.54
_refine_ls_abs_structure_Flack 0.00000
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.354
_refine_ls_hydrogen_treatment noref
_refine_ls_number_parameters 397
_refine_ls_number_reflns 6879
_refine_ls_R_factor_gt 0.0341
_refine_ls_shift/su_max 0.0017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.03400(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0794
_reflns_number_gt 5781
_reflns_number_total 6983
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C29 H22 Cl F6 N3 O2 P2 Ru '
_cod_database_code 1100669
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.36748(2) 0.640750(8) 0.271533(9) 0.02366(4) Uani 1.00 d . . .
Cl1 Cl 0.33539(7) 0.69570(3) 0.39749(3) 0.0435(2) Uani 1.00 d . . .
P1 P 0.40409(5) 0.59098(3) 0.15104(3) 0.0246(1) Uani 1.00 d . . .
P2 P 0.51323(5) 0.93034(3) 0.14855(4) 0.0347(1) Uani 1.00 d . . .
F1 F 0.6289(1) 0.98348(7) 0.19779(9) 0.0555(4) Uani 1.00 d . . .
F2 F 0.3990(2) 0.87594(9) 0.09992(9) 0.0669(5) Uani 1.00 d . . .
F3 F 0.5864(2) 0.92139(9) 0.07595(9) 0.0601(5) Uani 1.00 d . . .
F4 F 0.4394(1) 0.93779(8) 0.22128(8) 0.0511(4) Uani 1.00 d . . .
F5 F 0.4272(1) 0.99541(8) 0.09982(9) 0.0617(5) Uani 1.00 d . . .
F6 F 0.6000(2) 0.86514(7) 0.19898(10) 0.0534(4) Uani 1.00 d . . .
O1 O 0.2653(2) 0.78121(9) 0.1876(1) 0.0569(6) Uani 1.00 d . . .
O2 O 0.0731(2) 0.5955(1) 0.2286(1) 0.0685(6) Uani 1.00 d . . .
N1 N 0.4442(2) 0.54957(8) 0.34350(9) 0.0228(4) Uani 1.00 d . . .
N2 N 0.5762(2) 0.66452(9) 0.31927(10) 0.0275(4) Uani 1.00 d . . .
N3 N 0.1566(2) 0.6380(1) 0.0586(1) 0.0500(6) Uani 1.00 d . . .
C1 C 0.3065(2) 0.7282(1) 0.2160(1) 0.0359(6) Uani 1.00 d . . .
C2 C 0.1827(2) 0.6112(1) 0.2415(1) 0.0402(6) Uani 1.00 d . . .
C3 C 0.3703(2) 0.4924(1) 0.3520(1) 0.0286(5) Uani 1.00 d . . .
C4 C 0.4271(2) 0.4339(1) 0.3995(1) 0.0361(6) Uani 1.00 d . . .
C5 C 0.5637(2) 0.4339(1) 0.4397(1) 0.0373(6) Uani 1.00 d . . .
C6 C 0.6410(2) 0.4929(1) 0.4324(1) 0.0326(5) Uani 1.00 d . . .
C7 C 0.5793(2) 0.5501(1) 0.3835(1) 0.0251(5) Uani 1.00 d . . .
C8 C 0.6530(2) 0.6136(1) 0.3688(1) 0.0265(5) Uani 1.00 d . . .
C9 C 0.7922(2) 0.6216(1) 0.4019(1) 0.0412(6) Uani 1.00 d . . .
C10 C 0.8529(3) 0.6844(2) 0.3849(2) 0.0556(8) Uani 1.00 d . . .
C11 C 0.7741(3) 0.7356(1) 0.3372(2) 0.0564(8) Uani 1.00 d . . .
C12 C 0.6365(2) 0.7244(1) 0.3045(1) 0.0415(6) Uani 1.00 d . . .
C13 C 0.4265(2) 0.4946(1) 0.1594(1) 0.0271(5) Uani 1.00 d . . .
C14 C 0.3174(2) 0.4495(1) 0.1239(1) 0.0375(6) Uani 1.00 d . . .
C15 C 0.3287(2) 0.3771(1) 0.1396(2) 0.0445(6) Uani 1.00 d . . .
C16 C 0.4469(2) 0.3491(1) 0.1908(1) 0.0380(6) Uani 1.00 d . . .
C17 C 0.5552(2) 0.3931(1) 0.2267(1) 0.0342(5) Uani 1.00 d . . .
C18 C 0.5453(2) 0.4660(1) 0.2112(1) 0.0267(5) Uani 1.00 d . . .
C19 C 0.5475(2) 0.6307(1) 0.1216(1) 0.0272(5) Uani 1.00 d . . .
C20 C 0.6666(2) 0.5956(1) 0.1239(1) 0.0410(6) Uani 1.00 d . . .
C21 C 0.7705(3) 0.6312(1) 0.1026(2) 0.0549(8) Uani 1.00 d . . .
C22 C 0.7568(3) 0.7013(1) 0.0790(2) 0.0489(7) Uani 1.00 d . . .
C23 C 0.6373(3) 0.7363(1) 0.0742(2) 0.0466(7) Uani 1.00 d . . .
C24 C 0.5327(2) 0.7019(1) 0.0953(1) 0.0411(6) Uani 1.00 d . . .
C25 C 0.2670(2) 0.6030(1) 0.0537(1) 0.0293(5) Uani 1.00 d . . .
C26 C 0.0568(3) 0.6473(2) -0.0138(2) 0.0626(8) Uani 1.00 d . . .
C27 C 0.0622(2) 0.6213(1) -0.0898(1) 0.0463(7) Uani 1.00 d . . .
C28 C 0.1755(2) 0.5858(1) -0.0939(1) 0.0475(7) Uani 1.00 d . . .
C29 C 0.2807(2) 0.5774(1) -0.0214(1) 0.0470(7) Uani 1.00 d . . .
H1 H 0.2756 0.4921 0.3240 0.0352 Uiso 1.00 calc . . .
H2 H 0.3719 0.3943 0.4044 0.0442 Uiso 1.00 calc . . .
H3 H 0.6049 0.3937 0.4721 0.0457 Uiso 1.00 calc . . .
H4 H 0.7356 0.4940 0.4607 0.0399 Uiso 1.00 calc . . .
H5 H 0.8453 0.5850 0.4354 0.0496 Uiso 1.00 calc . . .
H6 H 0.9484 0.6914 0.4065 0.0683 Uiso 1.00 calc . . .
H7 H 0.8139 0.7791 0.3266 0.0679 Uiso 1.00 calc . . .
H8 H 0.5825 0.7604 0.2704 0.0505 Uiso 1.00 calc . . .
H9 H 0.2349 0.4687 0.0889 0.0456 Uiso 1.00 calc . . .
H10 H 0.2540 0.3465 0.1149 0.0541 Uiso 1.00 calc . . .
H11 H 0.4543 0.2992 0.2013 0.0461 Uiso 1.00 calc . . .
H12 H 0.6368 0.3735 0.2623 0.0421 Uiso 1.00 calc . . .
H13 H 0.6201 0.4963 0.2361 0.0328 Uiso 1.00 calc . . .
H14 H 0.6776 0.5469 0.1404 0.0494 Uiso 1.00 calc . . .
H15 H 0.8525 0.6065 0.1042 0.0675 Uiso 1.00 calc . . .
H16 H 0.8298 0.7256 0.0658 0.0589 Uiso 1.00 calc . . .
H17 H 0.6269 0.7846 0.0564 0.0571 Uiso 1.00 calc . . .
H18 H 0.4502 0.7266 0.0919 0.0498 Uiso 1.00 calc . . .
H19 H -0.0217 0.6735 -0.0117 0.0768 Uiso 1.00 calc . . .
H20 H -0.0117 0.6280 -0.1388 0.0558 Uiso 1.00 calc . . .
H21 H 0.1821 0.5671 -0.1459 0.0580 Uiso 1.00 calc . . .
H22 H 0.3624 0.5542 -0.0235 0.0569 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ru Ru -1.259 0.836
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100670.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100670.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100670
loop_
_publ_author_name
'Miao, Qian'
'Jin, Zhi-Min'
'Xiong, Jing'
'Hu, Mao-Lin'
_publ_section_title
;
Crystal Structure of 4-(2-Aminothiazol-4-yl)-4-(hydroxyimino)acetic ester
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x41
_journal_page_last x42
_journal_paper_doi 10.2116/analscix.19.x41
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C7 H9 N3 O3 S'
_chemical_formula_sum 'C7 H9 N3 O3 S'
_chemical_formula_weight 215.23
_chemical_name_systematic
;
4-(2-Aminothiazol-4-yl)-4-(hydroxyimino)acetic ester
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 100.148(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.2822(17)
_cell_length_b 10.9006(18)
_cell_length_c 8.8072(15)
_cell_measurement_reflns_used 436
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 21.98
_cell_measurement_theta_min 2.37
_cell_volume 971.7(3)
_diffrn_ambient_temperature 273(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type 'Bruker SMART CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0337
_diffrn_reflns_av_sigmaI/netI 0.0404
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 5700
_diffrn_reflns_theta_full 28.23
_diffrn_reflns_theta_max 28.23
_diffrn_reflns_theta_min 2.01
_exptl_absorpt_coefficient_mu 0.319
_exptl_absorpt_correction_T_max 0.894
_exptl_absorpt_correction_T_min 0.836
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2000)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.471
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelike
_exptl_crystal_F_000 448
_exptl_crystal_size_max 0.61
_exptl_crystal_size_mid 0.47
_exptl_crystal_size_min 0.35
_refine_diff_density_max 0.564
_refine_diff_density_min -0.407
_refine_diff_density_rms 0.063
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.974
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 131
_refine_ls_number_reflns 2207
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.974
_refine_ls_R_factor_all 0.0635
_refine_ls_R_factor_gt 0.0501
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1298
_refine_ls_wR_factor_ref 0.1357
_reflns_number_gt 1674
_reflns_number_total 2207
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100670
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.37920(7) 0.87067(5) 0.18910(6) 0.0510(2) Uani 1 1 d . . .
O1 O 0.25265(17) 1.17935(13) 0.72514(16) 0.0523(4) Uani 1 1 d . . .
H1A H 0.2561 1.1148 0.7736 0.078 Uiso 1 1 calc R . .
O2 O 0.31065(16) 0.90647(13) 0.76041(17) 0.0490(4) Uani 1 1 d . . .
O3 O 0.11456(17) 0.92635(17) 0.6067(2) 0.0644(5) Uani 1 1 d . . .
N1 N 0.3776(2) 1.08344(17) 0.0350(2) 0.0529(5) Uani 1 1 d . . .
H1B H 0.3684 1.1616 0.0252 0.064 Uiso 1 1 calc R . .
H1C H 0.3972 1.0404 -0.0396 0.064 Uiso 1 1 calc R . .
N2 N 0.33149(18) 1.08630(15) 0.28580(18) 0.0392(4) Uani 1 1 d . . .
N3 N 0.2933(2) 1.15886(15) 0.58417(19) 0.0448(4) Uani 1 1 d . . .
C1 C 0.3613(2) 1.02880(18) 0.1664(2) 0.0388(5) Uani 1 1 d . . .
C2 C 0.3414(3) 0.88514(19) 0.3705(2) 0.0465(5) Uani 1 1 d . . .
C3 C 0.3206(2) 1.00357(17) 0.4024(2) 0.0382(5) Uani 1 1 d . . .
C4 C 0.2856(2) 1.04530(17) 0.5475(2) 0.0386(5) Uani 1 1 d . . .
C5 C 0.2403(2) 0.95120(17) 0.6524(2) 0.0395(5) Uani 1 1 d . . .
C6 C 0.0508(3) 0.8447(3) 0.7031(4) 0.0778(9) Uani 1 1 d . . .
H6A H -0.0291 0.8108 0.6424 0.093 Uiso 1 1 calc R . .
H6B H 0.1096 0.7772 0.7393 0.093 Uiso 1 1 calc R . .
C7 C 0.0179(4) 0.9110(4) 0.8342(5) 0.1100(13) Uani 1 1 d . . .
H7A H -0.0237 0.8562 0.8964 0.165 Uiso 1 1 calc R . .
H7B H -0.0414 0.9769 0.7982 0.165 Uiso 1 1 calc R . .
H7C H 0.0971 0.9437 0.8948 0.165 Uiso 1 1 calc R . .
H2 H 0.342(2) 0.824(2) 0.432(3) 0.051(6) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0878(5) 0.0326(3) 0.0362(3) -0.0033(2) 0.0209(3) 0.0029(2)
O1 0.0936(12) 0.0361(7) 0.0331(8) -0.0004(6) 0.0278(8) -0.0005(7)
O2 0.0672(10) 0.0418(8) 0.0375(8) 0.0092(6) 0.0076(7) 0.0006(7)
O3 0.0601(11) 0.0749(12) 0.0566(11) 0.0161(9) 0.0056(8) -0.0105(8)
N1 0.0922(15) 0.0411(10) 0.0291(9) 0.0021(7) 0.0207(9) 0.0083(9)
N2 0.0602(11) 0.0320(8) 0.0262(8) 0.0001(6) 0.0100(7) 0.0004(7)
N3 0.0713(12) 0.0381(9) 0.0274(8) -0.0016(7) 0.0153(8) -0.0006(8)
C1 0.0553(12) 0.0324(10) 0.0290(10) 0.0010(7) 0.0080(9) 0.0003(8)
C2 0.0795(16) 0.0313(10) 0.0311(10) 0.0032(8) 0.0161(10) 0.0008(10)
C3 0.0555(12) 0.0337(9) 0.0261(9) 0.0008(8) 0.0088(8) -0.0019(8)
C4 0.0568(12) 0.0324(10) 0.0267(9) 0.0023(7) 0.0081(9) 0.0011(8)
C5 0.0570(13) 0.0331(10) 0.0298(10) -0.0028(8) 0.0115(9) -0.0001(8)
C6 0.0675(18) 0.091(2) 0.077(2) 0.0176(17) 0.0190(16) -0.0212(15)
C7 0.088(2) 0.155(4) 0.096(3) -0.005(3) 0.040(2) -0.024(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 S1 C1 88.82(10) . . ?
C5 O3 C6 117.77(19) . . ?
C1 N2 C3 110.20(16) . . ?
C4 N3 O1 111.37(17) . . ?
N2 C1 N1 124.43(18) . . ?
N2 C1 S1 114.66(15) . . ?
N1 C1 S1 120.91(16) . . ?
C3 C2 S1 110.63(16) . . ?
C2 C3 N2 115.68(18) . . ?
C2 C3 C4 123.62(18) . . ?
N2 C3 C4 120.68(17) . . ?
N3 C4 C3 120.57(19) . . ?
N3 C4 C5 121.10(18) . . ?
C3 C4 C5 118.33(16) . . ?
O2 C5 O3 125.9(2) . . ?
O2 C5 C4 123.9(2) . . ?
O3 C5 C4 110.26(17) . . ?
C7 C6 O3 110.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C2 1.717(2) . ?
S1 C1 1.741(2) . ?
O1 N3 1.396(2) . ?
O2 C5 1.193(2) . ?
O3 C5 1.313(3) . ?
O3 C6 1.463(3) . ?
N1 C1 1.337(3) . ?
N2 C1 1.307(3) . ?
N2 C3 1.386(2) . ?
N3 C4 1.278(2) . ?
C2 C3 1.346(3) . ?
C3 C4 1.461(3) . ?
C4 C5 1.508(3) . ?
C6 C7 1.452(5) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O2 0.82 2.35 3.039(2) 142.4 .
O1 H1A N1 0.82 2.44 2.993(2) 125.4 1_556
N1 H1B N3 0.86 2.20 2.993(3) 153.5 4_585
N1 H1C O2 0.86 2.34 3.076(2) 143.7 1_554
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N2 C1 N1 179.47(19) . . . . ?
C3 N2 C1 S1 -0.4(2) . . . . ?
C2 S1 C1 N2 0.84(18) . . . . ?
C2 S1 C1 N1 -179.08(19) . . . . ?
C1 S1 C2 C3 -0.99(19) . . . . ?
S1 C2 C3 N2 1.0(3) . . . . ?
S1 C2 C3 C4 179.50(16) . . . . ?
C1 N2 C3 C2 -0.4(3) . . . . ?
C1 N2 C3 C4 -178.92(18) . . . . ?
O1 N3 C4 C3 178.65(17) . . . . ?
O1 N3 C4 C5 -1.4(3) . . . . ?
C2 C3 C4 N3 165.7(2) . . . . ?
N2 C3 C4 N3 -15.9(3) . . . . ?
C2 C3 C4 C5 -14.3(3) . . . . ?
N2 C3 C4 C5 164.17(18) . . . . ?
C6 O3 C5 O2 5.6(4) . . . . ?
C6 O3 C5 C4 -174.7(2) . . . . ?
N3 C4 C5 O2 -82.3(3) . . . . ?
C3 C4 C5 O2 97.7(2) . . . . ?
N3 C4 C5 O3 98.0(2) . . . . ?
C3 C4 C5 O3 -82.0(2) . . . . ?
C5 O3 C6 C7 79.2(3) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 4912241
|
1100671.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100671.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100671
loop_
_publ_author_name
'Shimo, Tetsuro'
'Kamimura, Kazutaka'
'Nogita, Rika'
'Yasutake, Mikio'
'Shinmyozu, Teruo'
'Somekawa, Kenichi'
_publ_section_title
;
Crystal Structure of 1:1 Complex Crystal between
4-(3-Chlorobenzyloxy)-6-methyl-2-pyrone and Maleimide
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x43
_journal_page_last x44
_journal_paper_doi 10.2116/analscix.19.x43
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C17 H14 Cl N O5 '
_chemical_formula_sum 'C17 H14 Cl N O5'
_chemical_formula_weight 347.75
_chemical_melting_point ?
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_Int_Tables_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 65.101(10)
_cell_angle_beta 87.60(2)
_cell_angle_gamma 71.910(9)
_cell_formula_units_Z 2
_cell_length_a 7.181(2)
_cell_length_b 11.123(4)
_cell_length_c 11.686(4)
_cell_measurement_reflns_used 5822
_cell_measurement_temperature 113.2
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2.1
_cell_volume 800.5(4)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.8655
_diffrn_measured_fraction_theta_max 0.8655
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.050
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 5022
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.265
_exptl_absorpt_correction_T_max 0.923
_exptl_absorpt_correction_T_min 0.534
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(Higashi, 1995)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.443
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.500
_exptl_crystal_size_min 0.300
_exptl_crystal_size_rad ?
_refine_diff_density_max 0.33
_refine_diff_density_min -0.38
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack ?
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.280
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 273
_refine_ls_number_reflns 2294
_refine_ls_R_factor_gt 0.0565
_refine_ls_shift/su_max 0.0139
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00308|Fo|^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0816
_reflns_number_gt 2294
_reflns_number_total 3172
_reflns_threshold_expression F^2^>3.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P -1 '
_cod_original_formula_sum 'C17 H14 Cl N O5 '
_cod_database_code 1100671
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl(1) Cl 1.3836(1) 0.22793(8) 0.03991(7) 0.0437(2) Uani 1.00 d . . .
O(1) O 0.6976(3) 0.3518(2) 0.7108(2) 0.0361(6) Uani 1.00 d . . .
O(2) O 0.7107(3) 0.5660(2) 0.6371(2) 0.0413(6) Uani 1.00 d . . .
O(3) O 0.7988(3) 0.3284(2) 0.3744(2) 0.0336(5) Uani 1.00 d . . .
O(4) O 1.1858(3) 0.2320(2) 0.7198(2) 0.0453(6) Uani 1.00 d . . .
O(5) O 1.2879(4) 0.0635(2) 0.4220(2) 0.0511(7) Uani 1.00 d . . .
N(1) N 1.2467(4) 0.1814(3) 0.5478(2) 0.0366(7) Uani 1.00 d . . .
C(1) C 0.7229(4) 0.4689(3) 0.6116(3) 0.0330(7) Uani 1.00 d . . .
C(2) C 0.7566(4) 0.4640(3) 0.4930(3) 0.0322(7) Uani 1.00 d . . .
C(3) C 0.7643(4) 0.3477(3) 0.4800(2) 0.0316(7) Uani 1.00 d . . .
C(4) C 0.7355(4) 0.2301(3) 0.5842(3) 0.0356(8) Uani 1.00 d . . .
C(5) C 0.7052(4) 0.2358(3) 0.6953(3) 0.0370(8) Uani 1.00 d . . .
C(6) C 0.6820(5) 0.1216(3) 0.8139(3) 0.0422(9) Uani 1.00 d . . .
C(7) C 0.8291(5) 0.4428(3) 0.2627(3) 0.0344(8) Uani 1.00 d . . .
C(8) C 0.8863(4) 0.3881(3) 0.1655(2) 0.0309(7) Uani 1.00 d . . .
C(9) C 0.7439(4) 0.3872(3) 0.0895(2) 0.0339(7) Uani 1.00 d . . .
C(10) C 0.7985(4) 0.3385(3) -0.0019(3) 0.0342(7) Uani 1.00 d . . .
C(11) C 0.9958(4) 0.2890(3) -0.0187(3) 0.0342(7) Uani 1.00 d . . .
C(12) C 1.1353(4) 0.2885(3) 0.0592(3) 0.0312(7) Uani 1.00 d . . .
C(13) C 1.0844(4) 0.3387(3) 0.1503(2) 0.0320(7) Uani 1.00 d . . .
C(14) C 1.2078(4) 0.1535(3) 0.6706(3) 0.0389(8) Uani 1.00 d . . .
C(15) C 1.2006(5) 0.0071(3) 0.7294(3) 0.0461(9) Uani 1.00 d . . .
C(16) C 1.2320(5) -0.0428(3) 0.6431(3) 0.0481(9) Uani 1.00 d . . .
C(17) C 1.2598(5) 0.0681(3) 0.5229(3) 0.0409(8) Uani 1.00 d . . .
H(1) H 0.781(5) 0.546(3) 0.432(3) 0.037(8) Uiso 1.00 calc . . .
H(2) H 0.738(4) 0.158(3) 0.580(3) 0.032(8) Uiso 1.00 calc . . .
H(3) H 0.695(5) 0.046(4) 0.800(3) 0.045(9) Uiso 1.00 calc . . .
H(4) H 0.783(6) 0.107(4) 0.875(4) 0.08(1) Uiso 1.00 calc . . .
H(5) H 0.557(6) 0.148(4) 0.842(4) 0.056(10) Uiso 1.00 calc . . .
H(6) H 0.932(4) 0.463(3) 0.283(3) 0.032(7) Uiso 1.00 calc . . .
H(7) H 0.705(5) 0.523(3) 0.237(3) 0.039(8) Uiso 1.00 calc . . .
H(8) H 0.603(5) 0.429(3) 0.096(3) 0.043(8) Uiso 1.00 calc . . .
H(9) H 0.707(5) 0.339(3) -0.062(3) 0.042(8) Uiso 1.00 calc . . .
H(10) H 1.038(4) 0.249(3) -0.084(3) 0.036(8) Uiso 1.00 calc . . .
H(11) H 1.176(5) 0.336(3) 0.207(3) 0.041(8) Uiso 1.00 calc . . .
H(12) H 1.262(5) 0.267(4) 0.490(3) 0.048(9) Uiso 1.00 calc . . .
H(13) H 1.164(5) -0.038(3) 0.816(3) 0.045(8) Uiso 1.00 calc . . .
H(14) H 1.220(5) -0.141(3) 0.651(3) 0.044(8) Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100672.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100672.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100672
loop_
_publ_author_name
'Sekine, Akiko'
'Jomoto, Kohei'
'Uekusa, Hidehiro'
'Ohashi, Yuji'
'Yagi, Minoru'
_publ_section_title
;
Crystal Structure of a Host-guest Complex of 4,4'-Ethylidenebisphenol
and 5-Chloro-2-methyl-4-isothiazoline-3-one
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x45
_journal_page_last x46
_journal_paper_doi 10.2116/analscix.19.x45
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C18 H18 Cl N O3 S'
_chemical_formula_weight 363.84
_chemical_name_common
;
5-chloro-2-methyl-4-isothiazoline-3-one and 4,4'-ethylidenebisphenol
;
_chemical_name_systematic
;
5-chloro-2-methyl-4-isothiazoline-3-one 4,4'-ethane-1,1-diyldiphenol
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yab'
_symmetry_space_group_name_H-M 'P 1 21/a 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 105.48(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.152(6)
_cell_length_b 10.127(5)
_cell_length_c 11.450(5)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 30.0
_cell_measurement_theta_min 25.0
_cell_volume 1805.0(13)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type AFC5R
_diffrn_measurement_method '\w-2\q scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Rigaku Rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0361
_diffrn_reflns_av_sigmaI/netI 0.0523
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 4293
_diffrn_reflns_theta_full 27.49
_diffrn_reflns_theta_max 27.49
_diffrn_reflns_theta_min 1.85
_diffrn_standards_decay_% -0.1
_diffrn_standards_number 150
_exptl_absorpt_coefficient_mu 0.342
_exptl_absorpt_correction_T_max 0.9713
_exptl_absorpt_correction_T_min 0.9392
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details North
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.339
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 760
_exptl_crystal_preparation
;
recrystallized from methanol solution
;
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.5
_refine_diff_density_max 0.305
_refine_diff_density_min -0.401
_refine_diff_density_rms 0.047
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 229
_refine_ls_number_reflns 4144
_refine_ls_number_restraints 3
_refine_ls_restrained_S_all 1.028
_refine_ls_R_factor_all 0.1098
_refine_ls_R_factor_gt 0.0520
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.6064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1251
_refine_ls_wR_factor_ref 0.1460
_reflns_number_gt 2436
_reflns_number_total 4144
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'PSI-SCAN' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P21/a
_cod_database_code 1100672
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl -0.00655(6) -0.30885(12) 0.36005(10) 0.0998(4) Uani 1 1 d . . .
S1 S 0.10699(5) -0.14801(8) 0.55241(8) 0.0631(2) Uani 1 1 d . . .
O1 O 0.21510(12) 0.05755(19) 1.30116(15) 0.0550(5) Uani 1 1 d . . .
H1O H 0.1636 0.0745 1.2828 0.083 Uiso 1 1 calc R . .
O2 O 0.29736(12) -0.07594(18) 0.51068(15) 0.0521(5) Uani 1 1 d . . .
H2O H 0.2745 -0.0324 0.4503 0.078 Uiso 1 1 calc R . .
O3 O -0.04798(13) -0.0823(3) 0.73878(18) 0.0769(7) Uani 1 1 d . . .
N1 N 0.06996(13) -0.0874(2) 0.6661(2) 0.0548(6) Uani 1 1 d . . .
C1 C 0.34221(17) 0.1568(3) 0.8211(2) 0.0490(6) Uani 1 1 d D . .
C2 C 0.30207(18) 0.2079(3) 0.7098(2) 0.0510(6) Uani 1 1 d . A .
H2 H 0.2855 0.2961 0.7042 0.061 Uiso 1 1 calc R . .
C3 C 0.28537(15) 0.1329(2) 0.6058(2) 0.0436(6) Uani 1 1 d . . .
H3 H 0.2572 0.1702 0.5317 0.052 Uiso 1 1 calc R A .
C4 C 0.31048(15) 0.0026(2) 0.6117(2) 0.0401(5) Uani 1 1 d . A .
C5 C 0.34969(18) -0.0532(3) 0.7229(2) 0.0524(7) Uani 1 1 d . . .
H5 H 0.3652 -0.1419 0.7282 0.063 Uiso 1 1 calc R A .
C6 C 0.36572(19) 0.0242(3) 0.8262(2) 0.0569(7) Uani 1 1 d . A .
H6 H 0.3928 -0.0133 0.9008 0.068 Uiso 1 1 calc R . .
C8 C 0.32621(19) 0.1898(3) 1.0328(2) 0.0523(7) Uani 1 1 d D . .
C9 C 0.37425(18) 0.1298(3) 1.1374(3) 0.0610(8) Uani 1 1 d . A .
H9 H 0.4331 0.1191 1.1488 0.073 Uiso 1 1 calc R . .
C10 C 0.33653(17) 0.0849(3) 1.2261(2) 0.0562(7) Uani 1 1 d . . .
H10 H 0.3701 0.0449 1.2959 0.067 Uiso 1 1 calc R A .
C11 C 0.24998(16) 0.0999(2) 1.2105(2) 0.0424(6) Uani 1 1 d . A .
C12 C 0.20052(17) 0.1589(3) 1.1057(2) 0.0508(6) Uani 1 1 d . . .
H12 H 0.1416 0.1688 1.0937 0.061 Uiso 1 1 calc R A .
C13 C 0.2393(2) 0.2027(3) 1.0195(2) 0.0588(7) Uani 1 1 d . A .
H13 H 0.2056 0.2426 0.9497 0.071 Uiso 1 1 calc R . .
C14 C 0.00907(18) -0.2208(3) 0.4914(3) 0.0602(7) Uani 1 1 d . . .
C15 C -0.04742(17) -0.1998(3) 0.5555(3) 0.0628(8) Uani 1 1 d . . .
H15 H -0.1031 -0.2333 0.5345 0.075 Uiso 1 1 calc R . .
C16 C -0.01287(17) -0.1195(3) 0.6610(3) 0.0561(7) Uani 1 1 d . . .
C17 C 0.1263(2) -0.0109(4) 0.7643(3) 0.0721(9) Uani 1 1 d . . .
H17A H 0.0924 0.0319 0.8105 0.108 Uiso 1 1 calc R . .
H17B H 0.1563 0.0544 0.7306 0.108 Uiso 1 1 calc R . .
H17C H 0.1670 -0.0689 0.8161 0.108 Uiso 1 1 calc R . .
C7 C 0.3603(3) 0.2495(4) 0.9306(3) 0.0501(10) Uani 0.834(8) 1 d PD A 1
H7 H 0.3305 0.3332 0.9053 0.060 Uiso 0.834(8) 1 calc PR A 1
C18 C 0.4571(3) 0.2767(6) 0.9717(3) 0.0762(17) Uani 0.834(8) 1 d PD A 1
H18A H 0.4698 0.3311 1.0429 0.114 Uiso 0.834(8) 1 calc PR A 1
H18B H 0.4744 0.3215 0.9082 0.114 Uiso 0.834(8) 1 calc PR A 1
H18C H 0.4876 0.1947 0.9896 0.114 Uiso 0.834(8) 1 calc PR A 1
C7B C 0.3890(4) 0.2007(18) 0.9518(5) 0.054(6) Uiso 0.166(8) 1 d PD A 2
H7B H 0.4412 0.1487 0.9847 0.064 Uiso 0.166(8) 1 calc PR A 2
C18B C 0.4087(15) 0.3474(17) 0.9526(18) 0.068(6) Uiso 0.166(8) 1 d PD A 2
H18D H 0.3559 0.3965 0.9332 0.102 Uiso 0.166(8) 1 calc PR A 2
H18E H 0.4396 0.3659 0.8936 0.102 Uiso 0.166(8) 1 calc PR A 2
H18F H 0.4430 0.3727 1.0315 0.102 Uiso 0.166(8) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0796(6) 0.1207(9) 0.1028(8) -0.0361(6) 0.0308(5) -0.0092(6)
S1 0.0447(4) 0.0727(5) 0.0791(5) 0.0022(4) 0.0293(4) -0.0031(4)
O1 0.0528(11) 0.0746(13) 0.0401(10) 0.0089(9) 0.0166(8) 0.0050(9)
O2 0.0670(12) 0.0521(11) 0.0368(9) -0.0045(8) 0.0130(8) 0.0010(9)
O3 0.0510(11) 0.128(2) 0.0586(13) 0.0093(13) 0.0263(10) 0.0033(12)
N1 0.0415(12) 0.0650(15) 0.0609(14) 0.0075(12) 0.0186(10) -0.0024(11)
C1 0.0590(15) 0.0537(16) 0.0397(13) -0.0061(12) 0.0227(12) -0.0159(13)
C2 0.0654(17) 0.0418(14) 0.0507(15) -0.0010(12) 0.0243(13) -0.0059(13)
C3 0.0470(13) 0.0448(14) 0.0397(13) 0.0057(11) 0.0125(11) -0.0020(11)
C4 0.0415(12) 0.0460(14) 0.0352(12) -0.0015(11) 0.0143(10) -0.0059(11)
C5 0.0686(18) 0.0474(15) 0.0412(14) 0.0061(12) 0.0149(12) 0.0075(13)
C6 0.0674(18) 0.0684(19) 0.0325(13) 0.0077(13) 0.0094(12) 0.0002(15)
C8 0.0638(17) 0.0579(17) 0.0378(13) -0.0140(12) 0.0178(12) -0.0146(14)
C9 0.0485(15) 0.076(2) 0.0622(18) -0.0057(16) 0.0217(14) -0.0027(15)
C10 0.0508(15) 0.0707(19) 0.0467(15) 0.0065(14) 0.0125(12) 0.0106(14)
C11 0.0507(14) 0.0453(14) 0.0326(12) -0.0047(10) 0.0137(11) 0.0017(11)
C12 0.0472(14) 0.0664(18) 0.0376(13) -0.0019(13) 0.0091(11) 0.0032(13)
C13 0.0687(19) 0.0713(19) 0.0332(13) 0.0033(13) 0.0080(12) -0.0034(15)
C14 0.0488(16) 0.0638(19) 0.0692(18) 0.0037(15) 0.0181(14) -0.0001(14)
C15 0.0377(14) 0.084(2) 0.0664(19) 0.0127(17) 0.0122(13) -0.0022(14)
C16 0.0409(14) 0.077(2) 0.0529(16) 0.0204(15) 0.0164(12) 0.0038(13)
C17 0.0602(19) 0.081(2) 0.076(2) -0.0005(18) 0.0194(16) -0.0128(17)
C7 0.060(2) 0.053(2) 0.0400(17) -0.0041(15) 0.0165(15) -0.009(2)
C18 0.070(3) 0.114(4) 0.049(2) -0.023(2) 0.0237(19) -0.041(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 S1 C14 89.58(13) . . y
C16 N1 C17 124.2(2) . . y
C16 N1 S1 115.2(2) . . y
C17 N1 S1 120.61(18) . . y
C2 C1 C6 117.4(2) . . ?
C2 C1 C7B 141.1(8) . . ?
C6 C1 C7B 100.3(7) . . ?
C2 C1 C7 118.1(3) . . ?
C6 C1 C7 124.5(3) . . ?
C7B C1 C7 25.4(6) . . ?
C1 C2 C3 122.1(3) . . ?
C4 C3 C2 119.9(2) . . ?
O2 C4 C3 122.4(2) . . ?
O2 C4 C5 118.0(2) . . ?
C3 C4 C5 119.6(2) . . ?
C4 C5 C6 119.4(3) . . ?
C5 C6 C1 121.5(2) . . ?
C13 C8 C9 117.3(2) . . ?
C13 C8 C7B 137.5(5) . . ?
C9 C8 C7B 104.1(6) . . ?
C13 C8 C7 116.0(3) . . ?
C9 C8 C7 126.7(3) . . ?
C7B C8 C7 25.3(6) . . ?
C8 C9 C10 121.5(3) . . ?
C11 C10 C9 119.9(3) . . ?
C10 C11 O1 118.4(2) . . ?
C10 C11 C12 119.5(2) . . ?
O1 C11 C12 122.0(2) . . ?
C13 C12 C11 119.5(3) . . ?
C12 C13 C8 122.4(3) . . ?
C15 C14 Cl1 127.4(2) . . y
C15 C14 S1 113.5(3) . . y
Cl1 C14 S1 119.11(17) . . y
C14 C15 C16 112.6(3) . . y
O3 C16 N1 122.0(3) . . y
O3 C16 C15 128.8(3) . . y
N1 C16 C15 109.2(2) . . y
C18 C7 C1 108.5(3) . . ?
C18 C7 C8 112.3(3) . . ?
C1 C7 C8 110.6(2) . . ?
C8 C7B C1 109.2(2) . . ?
C8 C7B C18B 103.6(12) . . ?
C1 C7B C18B 109.5(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C14 1.708(3) . y
S1 N1 1.687(2) . y
S1 C14 1.716(3) . y
O1 C11 1.375(3) . ?
O2 C4 1.373(3) . ?
O3 C16 1.236(3) . y
N1 C16 1.363(3) . y
N1 C17 1.465(4) . y
C1 C2 1.368(4) . ?
C1 C6 1.392(4) . ?
C1 C7B 1.5504(12) . ?
C1 C7 1.531(4) . ?
C2 C3 1.377(3) . ?
C3 C4 1.377(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.385(4) . ?
C8 C13 1.377(4) . ?
C8 C9 1.382(4) . ?
C8 C7B 1.5503(11) . ?
C8 C7 1.544(4) . ?
C9 C10 1.392(4) . ?
C10 C11 1.370(4) . ?
C11 C12 1.387(4) . ?
C12 C13 1.376(4) . ?
C14 C15 1.333(4) . y
C15 C16 1.438(4) . y
C7 C18 1.532(5) . ?
C7B C18B 1.520(17) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 S1 N1 C16 0.2(2) . . . . ?
C14 S1 N1 C17 177.7(2) . . . . ?
C6 C1 C2 C3 -0.3(4) . . . . ?
C7B C1 C2 C3 164.1(4) . . . . ?
C7 C1 C2 C3 178.1(2) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
C2 C3 C4 O2 -178.4(2) . . . . ?
C2 C3 C4 C5 2.2(4) . . . . ?
O2 C4 C5 C6 178.5(2) . . . . ?
C3 C4 C5 C6 -2.2(4) . . . . ?
C4 C5 C6 C1 0.9(4) . . . . ?
C2 C1 C6 C5 0.4(4) . . . . ?
C7B C1 C6 C5 -169.7(3) . . . . ?
C7 C1 C6 C5 -177.9(3) . . . . ?
C13 C8 C9 C10 -0.4(4) . . . . ?
C7B C8 C9 C10 -170.4(6) . . . . ?
C7 C8 C9 C10 176.9(3) . . . . ?
C8 C9 C10 C11 0.1(5) . . . . ?
C9 C10 C11 O1 -178.4(3) . . . . ?
C9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C13 -0.6(4) . . . . ?
O1 C11 C12 C13 178.1(2) . . . . ?
C11 C12 C13 C8 0.3(4) . . . . ?
C9 C8 C13 C12 0.2(4) . . . . ?
C7B C8 C13 C12 165.7(9) . . . . ?
C7 C8 C13 C12 -177.4(3) . . . . ?
N1 S1 C14 C15 -0.4(3) . . . . ?
N1 S1 C14 Cl1 179.4(2) . . . . ?
Cl1 C14 C15 C16 -179.3(2) . . . . ?
S1 C14 C15 C16 0.5(4) . . . . ?
C17 N1 C16 O3 2.2(5) . . . . ?
S1 N1 C16 O3 179.6(2) . . . . ?
C17 N1 C16 C15 -177.4(3) . . . . ?
S1 N1 C16 C15 0.0(3) . . . . ?
C14 C15 C16 O3 -179.8(3) . . . . ?
C14 C15 C16 N1 -0.3(4) . . . . ?
C2 C1 C7 C18 -108.0(4) . . . . ?
C6 C1 C7 C18 70.2(4) . . . . ?
C7B C1 C7 C18 51.1(8) . . . . ?
C2 C1 C7 C8 128.4(3) . . . . ?
C6 C1 C7 C8 -53.3(4) . . . . ?
C7B C1 C7 C8 -72.5(6) . . . . ?
C13 C8 C7 C18 159.1(4) . . . . ?
C9 C8 C7 C18 -18.3(5) . . . . ?
C7B C8 C7 C18 -48.3(8) . . . . ?
C13 C8 C7 C1 -79.5(4) . . . . ?
C9 C8 C7 C1 103.1(4) . . . . ?
C7B C8 C7 C1 73.1(6) . . . . ?
C13 C8 C7B C1 -31.8(17) . . . . ?
C9 C8 C7B C1 134.9(9) . . . . ?
C7 C8 C7B C1 -69.5(6) . . . . ?
C13 C8 C7B C18B 84.7(9) . . . . ?
C9 C8 C7B C18B -108.5(11) . . . . ?
C7 C8 C7B C18B 47.1(14) . . . . ?
C2 C1 C7B C8 100.2(9) . . . . ?
C6 C1 C7B C8 -93.9(10) . . . . ?
C7 C1 C7B C8 70.2(6) . . . . ?
C2 C1 C7B C18B -12.5(13) . . . . ?
C6 C1 C7B C18B 153.4(11) . . . . ?
C7 C1 C7B C18B -42.5(15) . . . . ?
|
1100673.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100673.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100673
loop_
_publ_author_name
'Sekine, Akiko'
'Mitsumori, Takahiro'
'Uekusa, Hidehiro'
'Ohashi, Yuji'
'Yagi, Minoru'
_publ_section_title
;
Crystal Structure of a Host-guest Complex of 4,4'-Ethylidenebisphenol
and 5-Chloro-2-methyl-4-isothiazoline-3-one
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x47
_journal_page_last x48
_journal_paper_doi 10.2116/analscix.19.x47
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C12 H12 Cl N O6 S'
_chemical_formula_weight 333.74
_chemical_name_common 'CMI gallate'
_chemical_name_systematic
;
5-chloro-2-methylisothiazol-3(2H)-one methyl 1,3,4,5-trihydroxybenzoate
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yab'
_symmetry_space_group_name_H-M 'P 1 21/a 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 96.856(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.402(2)
_cell_length_b 10.257(2)
_cell_length_c 11.295(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 30.0
_cell_measurement_theta_min 25.0
_cell_volume 1426.5(5)
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Rigaku AFC-5R'
_diffrn_measurement_method '\q-2\q scan'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'Rigaku rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0191
_diffrn_reflns_av_sigmaI/netI 0.0379
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 3758
_diffrn_reflns_theta_full 27.51
_diffrn_reflns_theta_max 27.51
_diffrn_reflns_theta_min 1.82
_diffrn_standards_decay_% -2.1
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.440
_exptl_absorpt_correction_T_max 1.0
_exptl_absorpt_correction_T_min 0.9675
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details North
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.554
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 688
_exptl_crystal_preparation
;
recrystallized from methanol solution
;
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.3
_refine_diff_density_max 0.246
_refine_diff_density_min -0.245
_refine_diff_density_rms 0.045
_refine_ls_extinction_coef 0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 0.913
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 206
_refine_ls_number_reflns 3278
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.913
_refine_ls_R_factor_all 0.0649
_refine_ls_R_factor_gt 0.0392
_refine_ls_shift/su_max 0.008
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.5981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1096
_refine_ls_wR_factor_ref 0.1251
_reflns_number_gt 2402
_reflns_number_total 3278
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'PSI-SCAN' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P21/a
_cod_database_code 1100673
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl -0.11931(7) -0.05025(8) 0.33676(9) 0.0855(3) Uani 1 1 d . . .
S1 S 0.03506(6) 0.16788(7) 0.34938(5) 0.0593(2) Uani 1 1 d . . .
N1 N 0.07713(15) 0.22845(19) 0.22407(15) 0.0457(4) Uani 1 1 d . . .
C9 C 0.03330(18) 0.1697(2) 0.12118(18) 0.0433(5) Uani 1 1 d . . .
C10 C -0.03972(19) 0.0678(2) 0.1487(2) 0.0513(5) Uani 1 1 d . . .
H10 H -0.0800 0.0057 0.0826 0.064(8) Uiso 1 1 d . . .
C11 C -0.04583(19) 0.0591(2) 0.2655(2) 0.0524(6) Uani 1 1 d . . .
C12 C 0.1450(2) 0.3448(3) 0.2261(2) 0.0627(7) Uani 1 1 d . . .
H12A H 0.2052 0.3362 0.2874 0.094 Uiso 1 1 calc R . .
H12B H 0.1028 0.4199 0.2420 0.094 Uiso 1 1 calc R . .
H12C H 0.1716 0.3550 0.1502 0.094 Uiso 1 1 calc R . .
O1 O 0.50119(13) 0.16372(17) 0.82071(14) 0.0509(4) Uani 1 1 d . . .
H1O H 0.517(2) 0.206(3) 0.887(3) 0.061(8) Uiso 1 1 d . . .
O2 O 0.45310(13) 0.09643(17) 0.58424(13) 0.0474(4) Uani 1 1 d . . .
H2O H 0.505(2) 0.066(3) 0.627(3) 0.063(8) Uiso 1 1 d . . .
O3 O 0.28995(14) 0.21621(19) 0.44537(13) 0.0523(4) Uani 1 1 d . . .
H3O H 0.331(3) 0.157(3) 0.426(3) 0.076(10) Uiso 1 1 d . . .
O4 O 0.13032(11) 0.54226(14) 0.71498(12) 0.0413(3) Uani 1 1 d . . .
O5 O 0.22955(13) 0.50300(16) 0.89011(13) 0.0491(4) Uani 1 1 d . . .
O21 O 0.05730(15) 0.20475(19) 0.02276(14) 0.0614(5) Uani 1 1 d . . .
C1 C 0.27029(15) 0.38081(19) 0.72718(16) 0.0322(4) Uani 1 1 d . . .
C2 C 0.35409(16) 0.32007(19) 0.80063(16) 0.0351(4) Uani 1 1 d . . .
H2 H 0.3674 0.3429 0.8807 0.042 Uiso 1 1 calc R . .
C3 C 0.41706(15) 0.2265(2) 0.75492(16) 0.0356(4) Uani 1 1 d . . .
C4 C 0.39577(15) 0.18978(19) 0.63543(17) 0.0352(4) Uani 1 1 d . . .
C5 C 0.31197(15) 0.2502(2) 0.56234(16) 0.0351(4) Uani 1 1 d . . .
C6 C 0.24978(15) 0.3460(2) 0.60725(16) 0.0355(4) Uani 1 1 d . . .
H6 H 0.1946 0.3869 0.5578 0.043 Uiso 1 1 calc R . .
C7 C 0.20303(15) 0.48236(19) 0.77388(16) 0.0335(4) Uani 1 1 d . . .
C8 C 0.1670(2) 0.5983(3) 0.9459(2) 0.0631(7) Uani 1 1 d . . .
H8A H 0.1955 0.6072 1.0283 0.095 Uiso 1 1 calc R . .
H8B H 0.0926 0.5706 0.9401 0.095 Uiso 1 1 calc R . .
H8C H 0.1711 0.6807 0.9063 0.095 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cl1 0.0722(5) 0.0722(5) 0.1173(7) 0.0342(5) 0.0334(5) -0.0002(4)
S1 0.0682(4) 0.0728(5) 0.0371(3) 0.0038(3) 0.0077(3) -0.0025(3)
N1 0.0510(11) 0.0500(11) 0.0347(9) 0.0041(8) -0.0017(7) -0.0029(8)
C9 0.0431(11) 0.0479(12) 0.0367(10) 0.0015(9) -0.0047(8) 0.0075(9)
C10 0.0488(12) 0.0459(13) 0.0569(14) -0.0002(10) -0.0037(10) 0.0008(10)
C11 0.0448(12) 0.0466(13) 0.0664(15) 0.0116(11) 0.0092(10) 0.0073(10)
C12 0.0682(17) 0.0592(16) 0.0574(15) 0.0044(12) -0.0066(12) -0.0153(13)
O1 0.0537(9) 0.0585(10) 0.0368(8) -0.0099(7) -0.0094(7) 0.0227(8)
O2 0.0483(9) 0.0575(10) 0.0349(7) -0.0095(7) -0.0012(6) 0.0173(8)
O3 0.0542(9) 0.0714(11) 0.0287(7) -0.0126(7) -0.0058(6) 0.0187(9)
O4 0.0414(8) 0.0410(8) 0.0416(8) 0.0071(6) 0.0052(6) 0.0062(6)
O5 0.0537(9) 0.0559(9) 0.0365(8) -0.0114(7) -0.0004(6) 0.0188(8)
O21 0.0711(11) 0.0762(12) 0.0346(8) 0.0111(8) -0.0035(7) 0.0018(10)
C1 0.0317(9) 0.0348(9) 0.0300(8) 0.0006(7) 0.0033(7) -0.0020(7)
C2 0.0388(10) 0.0383(10) 0.0275(9) -0.0034(7) 0.0014(7) 0.0016(8)
C3 0.0365(10) 0.0389(10) 0.0300(9) 0.0003(8) -0.0014(7) 0.0041(8)
C4 0.0350(10) 0.0384(10) 0.0324(9) -0.0034(7) 0.0044(7) 0.0021(8)
C5 0.0346(9) 0.0436(11) 0.0262(8) -0.0040(8) 0.0003(7) -0.0021(8)
C6 0.0323(9) 0.0421(10) 0.0312(9) 0.0016(8) 0.0006(7) 0.0027(8)
C7 0.0349(9) 0.0341(10) 0.0320(9) 0.0025(7) 0.0053(7) -0.0033(7)
C8 0.0729(17) 0.0670(17) 0.0503(13) -0.0161(12) 0.0107(12) 0.0234(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 S1 C11 89.73(11) . . ?
C9 N1 C12 123.08(19) . . ?
C9 N1 S1 114.91(16) . . ?
C12 N1 S1 121.62(16) . . ?
O21 C9 N1 121.5(2) . . ?
O21 C9 C10 129.0(2) . . ?
N1 C9 C10 109.52(19) . . ?
C11 C10 C9 111.9(2) . . ?
C10 C11 Cl1 127.4(2) . . ?
C10 C11 S1 113.95(19) . . ?
Cl1 C11 S1 118.62(16) . . ?
C7 O5 C8 117.17(17) . . ?
C6 C1 C2 119.94(17) . . ?
C6 C1 C7 118.96(17) . . ?
C2 C1 C7 121.09(16) . . ?
C3 C2 C1 120.24(17) . . ?
O1 C3 C2 123.71(17) . . ?
O1 C3 C4 116.24(17) . . ?
C2 C3 C4 120.05(17) . . ?
O2 C4 C5 116.83(17) . . ?
O2 C4 C3 123.52(18) . . ?
C5 C4 C3 119.65(17) . . ?
O3 C5 C6 118.78(17) . . ?
O3 C5 C4 120.68(18) . . ?
C6 C5 C4 120.53(17) . . ?
C5 C6 C1 119.57(17) . . ?
O4 C7 O5 122.46(18) . . ?
O4 C7 C1 125.07(17) . . ?
O5 C7 C1 112.47(16) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C11 1.706(3) . ?
S1 N1 1.6846(19) . ?
S1 C11 1.709(3) . ?
N1 C9 1.363(3) . ?
N1 C12 1.459(3) . ?
C9 O21 1.238(3) . ?
C9 C10 1.441(3) . ?
C10 C11 1.334(4) . ?
O1 C3 1.368(2) . ?
O2 C4 1.362(2) . ?
O3 C5 1.362(2) . ?
O4 C7 1.221(2) . ?
O5 C7 1.332(2) . ?
O5 C8 1.439(3) . ?
C1 C6 1.395(3) . ?
C1 C2 1.397(3) . ?
C1 C7 1.471(3) . ?
C2 C3 1.376(3) . ?
C3 C4 1.396(3) . ?
C4 C5 1.393(3) . ?
C5 C6 1.382(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 21122553 ChemSpider
|
1100674.cif | #------------------------------------------------------------------------------
#$Date: 2016-01-25 15:55:48 +0200 (Mon, 25 Jan 2016) $
#$Revision: 175028 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100674.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100674
loop_
_publ_author_name
'Shen, Xuan'
'Sakata, Kazunori'
'Hashimoto, Mamoru'
_publ_section_title
;
Crystal Structure of a Dinuclear 1,2-Bis(diphenylphosphinooxide)ethane-bridged
(6,8,15,17-Tetramethyldibenzo[b,i][1,4,8,11]-tetraazacyclotetradecinato)
zinc(II) Complex
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x49
_journal_page_last x50
_journal_paper_doi 10.2116/analscix.19.x49
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C74 H74 N10 O2 P2 Zn2'
_chemical_formula_weight 1328.17
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 103.23(1)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 15.456(3)
_cell_length_b 9.993(2)
_cell_length_c 21.691(2)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293.2
_cell_measurement_theta_max 14.7
_cell_measurement_theta_min 10.0
_cell_volume 3261(1)
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_device_type 'Rigaku AFC7R'
_diffrn_measurement_method \w-2\q
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.077
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 8611
_diffrn_reflns_theta_full 28.00
_diffrn_reflns_theta_max 28.00
_diffrn_standards_decay_% 0.78
_diffrn_standards_interval_count 150
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.840
_exptl_absorpt_correction_T_max 0.991
_exptl_absorpt_correction_T_min 0.853
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour red
_exptl_crystal_density_diffrn 1.352
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_size_max 0.400
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.100
_refine_diff_density_max 1.13
_refine_diff_density_min -2.26
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.022
_refine_ls_hydrogen_treatment noref
_refine_ls_number_parameters 406
_refine_ls_number_reflns 7865
_refine_ls_R_factor_gt 0.0480
_refine_ls_shift/su_max 0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1567
_reflns_number_gt 3324
_reflns_number_total 7865
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_database_code 1100674
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn(1) Zn 0.29265(3) 0.11853(5) 0.99928(2) 0.0313(1) Uani 1.00 d . . .
P(1) P 0.07771(8) 0.0349(1) 0.92816(6) 0.0352(3) Uani 1.00 d . . .
O(1) O 0.1573(2) 0.0923(3) 0.9702(2) 0.0442(10) Uani 1.00 d . . .
N(1) N 0.3491(2) -0.0027(3) 0.9450(2) 0.0307(10) Uani 1.00 d . . .
N(2) N 0.3196(3) -0.0107(4) 1.0739(2) 0.035(1) Uani 1.00 d . . .
N(3) N 0.2988(2) 0.2510(4) 1.0714(2) 0.033(1) Uani 1.00 d . . .
N(4) N 0.3248(2) 0.2601(4) 0.9402(2) 0.035(1) Uani 1.00 d . . .
N(5) N 0.1490(5) -0.4087(7) 1.0862(4) 0.117(3) Uani 1.00 d . . .
C(1) C 0.4666(3) -0.1632(5) 0.9301(2) 0.047(1) Uani 1.00 d . . .
C(2) C 0.4042(3) -0.1029(4) 0.9679(2) 0.036(1) Uani 1.00 d . . .
C(3) C 0.4137(3) -0.1524(4) 1.0291(2) 0.039(1) Uani 1.00 d . . .
C(4) C 0.3792(3) -0.1076(5) 1.0801(2) 0.037(1) Uani 1.00 d . . .
C(5) C 0.4209(4) -0.1679(6) 1.1441(3) 0.058(2) Uani 1.00 d . . .
C(6) C 0.2851(3) 0.0418(5) 1.1228(2) 0.037(1) Uani 1.00 d . . .
C(7) C 0.2505(3) -0.0321(6) 1.1654(2) 0.047(2) Uani 1.00 d . . .
C(8) C 0.2109(4) 0.0277(6) 1.2092(2) 0.056(2) Uani 1.00 d . . .
C(9) C 0.2025(4) 0.1645(7) 1.2097(2) 0.055(2) Uani 1.00 d . . .
C(10) C 0.2328(3) 0.2427(5) 1.1663(2) 0.045(1) Uani 1.00 d . . .
C(11) C 0.2749(3) 0.1828(5) 1.1223(2) 0.037(1) Uani 1.00 d . . .
C(12) C 0.3640(4) 0.4494(6) 1.1350(3) 0.057(2) Uani 1.00 d . . .
C(13) C 0.3362(3) 0.3713(5) 1.0737(2) 0.038(1) Uani 1.00 d . . .
C(14) C 0.3556(3) 0.4313(5) 1.0198(2) 0.043(1) Uani 1.00 d . . .
C(15) C 0.3544(3) 0.3793(5) 0.9589(2) 0.037(1) Uani 1.00 d . . .
C(16) C 0.3979(4) 0.4702(5) 0.9182(3) 0.054(2) Uani 1.00 d . . .
C(17) C 0.3277(3) 0.1979(5) 0.8826(2) 0.035(1) Uani 1.00 d . . .
C(18) C 0.3112(3) 0.2607(5) 0.8231(2) 0.047(2) Uani 1.00 d . . .
C(19) C 0.3110(4) 0.1901(7) 0.7690(3) 0.057(2) Uani 1.00 d . . .
C(20) C 0.3218(4) 0.0533(7) 0.7717(2) 0.055(2) Uani 1.00 d . . .
C(21) C 0.3352(3) -0.0122(5) 0.8285(2) 0.046(1) Uani 1.00 d . . .
C(22) C 0.3405(3) 0.0552(5) 0.8849(2) 0.034(1) Uani 1.00 d . . .
C(23) C 0.0431(3) 0.1276(5) 0.8556(2) 0.041(1) Uani 1.00 d . . .
C(24) C 0.0929(3) 0.1159(7) 0.8106(2) 0.060(2) Uani 1.00 d . . .
C(25) C 0.0717(4) 0.1946(8) 0.7563(3) 0.077(2) Uani 1.00 d . . .
C(26) C 0.0019(4) 0.2808(7) 0.7465(3) 0.069(2) Uani 1.00 d . . .
C(27) C -0.0474(4) 0.2934(6) 0.7908(3) 0.067(2) Uani 1.00 d . . .
C(28) C -0.0277(3) 0.2154(5) 0.8450(2) 0.048(2) Uani 1.00 d . . .
C(29) C 0.0935(3) -0.1359(5) 0.9078(2) 0.036(1) Uani 1.00 d . . .
C(30) C 0.0308(4) -0.1999(6) 0.8609(3) 0.060(2) Uani 1.00 d . . .
C(31) C 0.0420(5) -0.3333(7) 0.8480(3) 0.084(3) Uani 1.00 d . . .
C(32) C 0.1131(5) -0.4040(6) 0.8807(3) 0.073(2) Uani 1.00 d . . .
C(33) C 0.1746(5) -0.3405(6) 0.9267(3) 0.073(2) Uani 1.00 d . . .
C(34) C 0.1649(4) -0.2082(5) 0.9402(3) 0.051(2) Uani 1.00 d . . .
C(35) C -0.0146(3) 0.0349(5) 0.9674(2) 0.042(1) Uani 1.00 d . . .
C(36) C 0.0965(6) -0.6185(8) 1.0194(4) 0.105(3) Uani 1.00 d . . .
C(37) C 0.1243(5) -0.5019(8) 1.0564(4) 0.083(3) Uani 1.00 d . . .
H(1) H 0.4892 -0.1108 0.9043 0.1293 Uiso 1.00 calc . . .
H(2) H 0.4386 -0.2168 0.9030 0.1019 Uiso 1.00 calc . . .
H(3) H 0.5208 -0.1945 0.9556 0.0680 Uiso 1.00 calc . . .
H(4) H 0.4538 -0.2157 1.0409 0.0185 Uiso 1.00 calc . . .
H(5) H 0.4854 -0.2035 1.1443 0.1162 Uiso 1.00 calc . . .
H(6) H 0.3919 -0.2405 1.1460 0.1212 Uiso 1.00 calc . . .
H(7) H 0.4229 -0.1139 1.1726 0.0733 Uiso 1.00 calc . . .
H(8) H 0.2497 -0.1286 1.1635 0.0226 Uiso 1.00 calc . . .
H(9) H 0.1898 -0.0274 1.2394 0.0902 Uiso 1.00 calc . . .
H(10) H 0.1837 0.1958 1.2364 0.0488 Uiso 1.00 calc . . .
H(11) H 0.2104 0.3507 1.1619 0.0672 Uiso 1.00 calc . . .
H(12) H 0.3807 0.3940 1.1681 0.1013 Uiso 1.00 calc . . .
H(13) H 0.3214 0.5057 1.1346 0.1494 Uiso 1.00 calc . . .
H(14) H 0.4181 0.4918 1.1377 0.1018 Uiso 1.00 calc . . .
H(15) H 0.3796 0.5132 1.0264 0.0239 Uiso 1.00 calc . . .
H(16) H 0.4342 0.5172 0.9419 0.1283 Uiso 1.00 calc . . .
H(17) H 0.3481 0.5135 0.8939 0.0726 Uiso 1.00 calc . . .
H(18) H 0.4275 0.4228 0.8937 0.1033 Uiso 1.00 calc . . .
H(19) H 0.2949 0.3568 0.8255 0.0471 Uiso 1.00 calc . . .
H(20) H 0.3009 0.2326 0.7308 0.0591 Uiso 1.00 calc . . .
H(21) H 0.3260 -0.0011 0.7403 0.0434 Uiso 1.00 calc . . .
H(22) H 0.3426 -0.1101 0.8364 0.0433 Uiso 1.00 calc . . .
H(23) H 0.1429 0.0692 0.8157 0.0915 Uiso 1.00 calc . . .
H(24) H 0.1131 0.1947 0.7295 0.1164 Uiso 1.00 calc . . .
H(25) H -0.0123 0.3291 0.7099 0.0968 Uiso 1.00 calc . . .
H(26) H -0.0958 0.3344 0.7823 0.0921 Uiso 1.00 calc . . .
H(27) H -0.0569 0.2198 0.8743 0.0401 Uiso 1.00 calc . . .
H(28) H -0.0097 -0.1549 0.8403 0.0487 Uiso 1.00 calc . . .
H(29) H 0.0060 -0.3742 0.8215 0.0789 Uiso 1.00 calc . . .
H(30) H 0.1185 -0.4935 0.8732 0.1159 Uiso 1.00 calc . . .
H(31) H 0.2113 -0.3822 0.9475 0.1000 Uiso 1.00 calc . . .
H(32) H 0.2013 -0.1708 0.9765 0.0847 Uiso 1.00 calc . . .
H(33) H -0.0407 0.1228 0.9751 0.1355 Uiso 1.00 calc . . .
H(34) H -0.0315 0.0264 0.9434 0.2099 Uiso 1.00 calc . . .
H(35) H 0.1288 -0.6210 0.9901 0.1546 Uiso 1.00 calc . . .
H(36) H 0.0421 -0.6376 0.9935 0.2055 Uiso 1.00 calc . . .
H(37) H 0.1095 -0.6764 1.0468 0.2190 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Zn Zn 0.284 1.430
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100675.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100675.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100675
loop_
_publ_author_name
'Doi, Mitsunobu'
'Ijiri, Yoshio'
'Akagi, Masao'
'Uenishi, Miharu'
'Urata, Hidehito'
_publ_section_title
;
Crystal Structure of 5'-Hydroxythalidomide In Vivo Metabolite of
Thalidomide in Humans
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x51
_journal_page_last x52
_journal_paper_doi 10.2116/analscix.19.x51
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C13 H10 N2 O5'
_chemical_formula_sum 'C13 H10 N2 O5'
_chemical_formula_weight 274.23
_chemical_name_common 5hthalid
_chemical_name_systematic 5'-Hydroxythalidomide
_space_group_IT_number 15
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 95.9240(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 21.7240(17)
_cell_length_b 7.9633(6)
_cell_length_c 13.6074(11)
_cell_measurement_reflns_used 4272
_cell_measurement_temperature 90.0(2)
_cell_measurement_theta_max 28.0
_cell_measurement_theta_min 2.7
_cell_volume 2341.4(3)
_diffrn_ambient_temperature 90.0(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measurement_device_type 'Bruker AXS, SMART APEX area detector'
_diffrn_measurement_method \w-scan
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'MacScience, M18XCE rotating anode'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0234
_diffrn_reflns_av_sigmaI/netI 0.0226
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 9927
_diffrn_reflns_theta_max 28.28
_diffrn_reflns_theta_min 2.73
_diffrn_standards_decay_% 0.08
_diffrn_standards_interval_count 9927
_diffrn_standards_interval_time 360
_diffrn_standards_number 135
_exptl_absorpt_coefficient_mu 0.122
_exptl_absorpt_correction_T_max 1.0
_exptl_absorpt_correction_T_min 0.8821
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.556
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1136
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.10
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.248
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 185
_refine_ls_number_reflns 2770
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.248
_refine_ls_R_factor_all 0.0662
_refine_ls_R_factor_gt 0.0639
_refine_ls_shift/su_max <0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+5.7973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1432
_refine_ls_wR_factor_ref 0.1445
_reflns_number_gt 2661
_reflns_number_total 2770
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100675
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.02939(10) 0.6082(2) 0.63039(14) 0.0153(4) Uani 1 1 d . . .
O1 O 0.01652(7) 0.46223(19) 0.61661(12) 0.0213(4) Uani 1 1 d . . .
N2 N 0.08850(8) 0.6692(2) 0.66432(13) 0.0150(4) Uani 1 1 d . . .
C3 C 0.09019(10) 0.8447(3) 0.66399(14) 0.0151(4) Uani 1 1 d . . .
O3 O 0.13670(7) 0.92752(19) 0.68384(12) 0.0213(4) Uani 1 1 d . . .
C3A C 0.02551(9) 0.9003(3) 0.63583(14) 0.0141(4) Uani 1 1 d . . .
C4 C 0.00125(10) 1.0609(3) 0.62712(15) 0.0171(4) Uani 1 1 d . . .
H1 H 0.0266 1.1572 0.6400 0.021 Uiso 1 1 calc R . .
C5 C -0.06220(11) 1.0753(3) 0.59859(16) 0.0206(5) Uani 1 1 d . . .
H2 H -0.0805 1.1835 0.5916 0.025 Uiso 1 1 calc R . .
C6 C -0.09901(11) 0.9330(3) 0.58023(16) 0.0224(5) Uani 1 1 d . . .
H3 H -0.1421 0.9462 0.5615 0.027 Uiso 1 1 calc R . .
C7 C -0.07405(10) 0.7719(3) 0.58881(15) 0.0188(4) Uani 1 1 d . . .
H4 H -0.0991 0.6749 0.5761 0.023 Uiso 1 1 calc R . .
C7A C -0.01107(10) 0.7595(2) 0.61679(14) 0.0145(4) Uani 1 1 d . . .
N1' N 0.20422(8) 0.3992(2) 0.56697(12) 0.0151(4) Uani 1 1 d . . .
H5 H 0.2181 0.3819 0.5093 0.018 Uiso 1 1 calc R . .
C2' C 0.16300(9) 0.5297(3) 0.57195(15) 0.0156(4) Uani 1 1 d . . .
O2' O 0.14389(8) 0.6066(2) 0.49844(11) 0.0225(4) Uani 1 1 d . . .
C3' C 0.14497(9) 0.5700(3) 0.67457(14) 0.0138(4) Uani 1 1 d . . .
H6 H 0.1784 0.6430 0.7077 0.017 Uiso 1 1 calc R . .
C4' C 0.14231(9) 0.4122(3) 0.73765(14) 0.0154(4) Uani 1 1 d . . .
H7 H 0.1323 0.4429 0.8047 0.018 Uiso 1 1 calc R . .
H8 H 0.1095 0.3361 0.7076 0.018 Uiso 1 1 calc R . .
C5' C 0.20469(9) 0.3238(3) 0.74428(14) 0.0141(4) Uani 1 1 d . . .
H9 H 0.2355 0.4013 0.7801 0.017 Uiso 1 1 calc R . .
O5' O 0.20621(7) 0.17306(19) 0.79890(11) 0.0175(3) Uani 1 1 d . . .
H10 H 0.1799(13) 0.101(4) 0.765(2) 0.025(7) Uiso 1 1 d . . .
C6' C 0.22604(9) 0.2929(3) 0.64228(15) 0.0142(4) Uani 1 1 d . . .
O6' O 0.26113(7) 0.1789(2) 0.62674(11) 0.0225(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0228(10) 0.0115(9) 0.0118(9) 0.0002(7) 0.0030(7) 0.0018(8)
O1 0.0234(8) 0.0115(7) 0.0275(8) -0.0004(6) -0.0039(6) -0.0004(6)
N2 0.0186(9) 0.0111(8) 0.0157(8) 0.0004(6) 0.0033(6) 0.0036(6)
C3 0.0216(10) 0.0128(9) 0.0114(9) -0.0013(7) 0.0052(7) 0.0019(8)
O3 0.0213(8) 0.0171(7) 0.0254(8) -0.0024(6) 0.0018(6) -0.0029(6)
C3A 0.0189(10) 0.0133(9) 0.0112(8) 0.0000(7) 0.0057(7) 0.0022(7)
C4 0.0263(11) 0.0120(9) 0.0137(9) 0.0001(7) 0.0051(8) 0.0036(8)
C5 0.0289(11) 0.0168(10) 0.0172(10) 0.0038(8) 0.0083(8) 0.0091(9)
C6 0.0199(10) 0.0304(12) 0.0177(10) 0.0043(9) 0.0054(8) 0.0077(9)
C7 0.0211(11) 0.0199(10) 0.0159(10) 0.0028(8) 0.0035(8) -0.0022(8)
C7A 0.0206(10) 0.0115(9) 0.0122(9) 0.0006(7) 0.0053(7) 0.0020(8)
N1' 0.0202(9) 0.0156(8) 0.0100(7) 0.0015(6) 0.0040(6) 0.0053(7)
C2' 0.0171(10) 0.0134(9) 0.0163(9) -0.0002(8) 0.0021(7) 0.0015(7)
O2' 0.0299(9) 0.0228(8) 0.0151(7) 0.0058(6) 0.0040(6) 0.0116(7)
C3' 0.0139(9) 0.0135(9) 0.0139(9) -0.0016(7) 0.0006(7) 0.0012(7)
C4' 0.0160(9) 0.0176(10) 0.0128(9) 0.0007(8) 0.0027(7) 0.0018(8)
C5' 0.0180(9) 0.0134(9) 0.0111(9) 0.0007(7) 0.0024(7) 0.0013(7)
O5' 0.0212(8) 0.0151(7) 0.0162(7) 0.0039(6) 0.0016(6) 0.0018(6)
C6' 0.0133(9) 0.0141(9) 0.0150(9) 0.0014(7) 0.0013(7) 0.0007(7)
O6' 0.0261(8) 0.0254(8) 0.0167(7) 0.0054(6) 0.0059(6) 0.0140(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100676.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100676.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100676
loop_
_publ_author_name
'Kobayashi, Kimiko'
'Sassa, Masashi'
'Yajima, Keiji'
'Tsuboyama, Sei'
'Enomoto, Kouichiro'
'Miyamae, Hiroshi'
_publ_section_title
;
Molecular Structure and Absolute Configuration of
1-Benzyl-(+)-2- methylazetidine Hydrobromide
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x53
_journal_page_last x54
_journal_paper_doi 10.2116/analscix.19.x53
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C11 H16 N,Br '
_chemical_formula_sum 'C11 H16 Br N'
_chemical_formula_weight 242.16
_chemical_melting_point ?
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_cell_angle_alpha 90
_cell_angle_beta 103.665(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.1468(5)
_cell_length_b 10.7412(5)
_cell_length_c 9.0572(6)
_cell_measurement_reflns_used 5540
_cell_measurement_temperature 296.1
_cell_measurement_theta_max 29.5
_cell_measurement_theta_min 3.0
_cell_volume 581.07(7)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9948
_diffrn_measured_fraction_theta_max 0.9948
_diffrn_measurement_device_type 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method oscillation
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.076
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 5758
_diffrn_reflns_theta_full 29.57
_diffrn_reflns_theta_max 29.57
_exptl_absorpt_coefficient_mu 3.506
_exptl_absorpt_correction_T_max 0.755
_exptl_absorpt_correction_T_min 0.155
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.384
_exptl_crystal_density_meas 1.38
_exptl_crystal_density_method 'floating method with CCl4-benzene'
_exptl_crystal_description needle
_exptl_crystal_F_000 248.00
_exptl_crystal_size_max 0.48
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.87
_refine_diff_density_min -0.74
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 221 Friedel Pairs'
_refine_ls_abs_structure_Flack 0.07(2)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.081
_refine_ls_hydrogen_treatment riding-model
_refine_ls_number_parameters 135
_refine_ls_number_reflns 1930
_refine_ls_R_factor_gt 0.0470
_refine_ls_shift/su_max 0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
2.3284 -0.1647 1.8562
;
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.0520
_reflns_number_gt 1930
_reflns_number_total 2790
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C11 H16 Br N '
_cod_database_code 1100676
#BEGIN Tags that were not found in dictionaries:
_refine_ls_inverse_abs_structure_flack 0.93(2)
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.09112(7) 0.3493(1) -0.11035(6) 0.0534(1) Uani 1.00 1 d . . .
N1 N 0.4172(7) 0.1118(4) 0.0021(5) 0.041(1) Uani 1.00 1 d . . .
C2 C 0.3865(9) 0.0251(5) -0.1332(6) 0.046(1) Uani 1.00 1 d . . .
C3 C 0.546(1) 0.1074(8) -0.194(1) 0.061(2) Uani 1.00 1 d . . .
C4 C 0.628(1) 0.1599(6) -0.0360(8) 0.055(2) Uani 1.00 1 d . . .
C5 C 0.153(1) 0.0057(6) -0.2185(8) 0.064(2) Uani 1.00 1 d . . .
C6 C 0.424(1) 0.0565(6) 0.1541(9) 0.048(2) Uani 1.00 1 d . . .
C7 C 0.492(1) 0.1511(6) 0.2803(7) 0.049(1) Uani 1.00 1 d . . .
C8 C 0.708(1) 0.1539(7) 0.3659(7) 0.062(2) Uani 1.00 1 d . . .
C9 C 0.769(1) 0.2418(9) 0.4803(8) 0.081(2) Uani 1.00 1 d . . .
C10 C 0.619(2) 0.3249(8) 0.5109(8) 0.080(3) Uani 1.00 1 d . . .
C11 C 0.405(1) 0.3234(9) 0.4272(8) 0.082(3) Uani 1.00 1 d . . .
C12 C 0.342(1) 0.2361(8) 0.3119(8) 0.069(2) Uani 1.00 1 d . . .
H1 H 0.3051 0.1745 -0.0193 0.049 Uiso 1.00 1 c . . .
H2 H 0.4552 -0.0528 -0.1019 0.057 Uiso 1.00 1 c . . .
H3 H 0.473 0.1664 -0.267 0.076 Uiso 1.00 1 c . . .
H4 H 0.656 0.0638 -0.231 0.076 Uiso 1.00 1 c . . .
H5 H 0.643 0.2479 -0.0320 0.067 Uiso 1.00 1 c . . .
H6 H 0.761 0.1225 0.0211 0.067 Uiso 1.00 1 c . . .
H7 H 0.071 -0.0349 -0.1557 0.076 Uiso 1.00 1 c . . .
H8 H 0.087 0.0843 -0.2493 0.076 Uiso 1.00 1 c . . .
H9 H 0.151 -0.0439 -0.3056 0.076 Uiso 1.00 1 c . . .
H10 H 0.530 -0.0095 0.1716 0.059 Uiso 1.00 1 c . . .
H11 H 0.281 0.0249 0.1555 0.059 Uiso 1.00 1 c . . .
H12 H 0.815 0.0964 0.3459 0.072 Uiso 1.00 1 c . . .
H13 H 0.919 0.2444 0.5386 0.093 Uiso 1.00 1 c . . .
H14 H 0.664 0.3832 0.5913 0.096 Uiso 1.00 1 c . . .
H15 H 0.299 0.3815 0.4472 0.099 Uiso 1.00 1 c . . .
H16 H 0.192 0.2341 0.2532 0.082 Uiso 1.00 1 c . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Br Br -0.557 2.708
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100677.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100677.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100677
loop_
_publ_author_name
'Mahendra, M.'
'Doreswamy, B. H.'
'Adlakha, Priti'
'Raval, Kena'
'Varu, Bharat'
'Shah, Anamik'
'Sridhar, M. A.'
'Prasad, J. S.'
_publ_section_title
;
Synthesis and Crystal Structure of
3,5-dicyano-2,6-dimethyl-4-phenyl-1,4-dihydropyridine
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x55
_journal_page_last x56
_journal_paper_doi 10.2116/analscix.19.x55
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C15 H13 N3'
_chemical_formula_sum 'C15 H13 N3'
_chemical_formula_weight 235.28
_chemical_name_systematic
;
3,5-dicyano-2,6-dimethyl-4-phenyl-1,4-dihydropyridine
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90
_cell_angle_beta 104.101(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.7220(7)
_cell_length_b 11.4200(11)
_cell_length_c 13.3070(12)
_cell_measurement_temperature 293
_cell_volume 1285.5(2)
_diffrn_ambient_temperature 293
_diffrn_measured_fraction_theta_full 0.866
_diffrn_measured_fraction_theta_max 0.866
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_av_sigmaI/netI 0.0321
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 7541
_diffrn_reflns_theta_full 32.40
_diffrn_reflns_theta_max 32.40
_diffrn_reflns_theta_min 2.38
_exptl_absorpt_coefficient_mu 0.074
_exptl_crystal_density_diffrn 1.216
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 496
_refine_diff_density_max 0.373
_refine_diff_density_min -0.330
_refine_diff_density_rms 0.119
_refine_ls_abs_structure_Flack none
_refine_ls_extinction_coef 0.087(10)
_refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^
_refine_ls_extinction_method shelxl
_refine_ls_goodness_of_fit_ref 0.908
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_constraints ?
_refine_ls_number_parameters 164
_refine_ls_number_reflns 4001
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.908
_refine_ls_R_factor_all 0.1096
_refine_ls_R_factor_gt 0.0625
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1190P)^2^+0.2704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1755
_refine_ls_wR_factor_ref 0.2265
_reflns_number_gt 2190
_reflns_number_total 4001
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100677
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
N10 N Uani 0.6271(3) 1.16323(18) 0.02184(17) 1.000 0.0923(8) . .
N13 N Uani 0.86547(19) 0.78752(14) 0.02215(12) 1.000 0.0678(5) . .
N18 N Uani 1.0157(2) 0.8649(2) -0.29337(16) 1.000 0.0929(8) . .
C1 C Uani 0.6409(3) 1.08230(16) -0.28316(16) 1.000 0.0689(7) . .
C2 C Uani 0.5119(3) 1.08631(19) -0.36767(16) 1.000 0.0795(8) . .
C3 C Uani 0.4045(3) 0.9969(2) -0.38603(17) 1.000 0.0790(7) . .
C4 C Uani 0.4248(2) 0.90351(19) -0.31988(17) 1.000 0.0766(7) . .
C5 C Uani 0.5531(2) 0.89846(16) -0.23507(15) 1.000 0.0658(6) . .
C6 C Uani 0.6639(2) 0.98761(14) -0.21567(13) 1.000 0.0561(5) . .
C7 C Uani 0.8071(2) 0.97909(15) -0.12403(14) 1.000 0.0598(5) . .
C8 C Uani 0.7615(2) 0.97578(15) -0.02075(14) 1.000 0.0604(5) . .
C9 C Uani 0.6853(2) 1.07891(18) 0.00436(15) 1.000 0.0692(6) . .
C11 C Uani 0.7856(2) 0.88537(16) 0.04464(14) 1.000 0.0617(6) . .
C12 C Uani 0.7358(3) 0.8798(2) 0.14394(16) 1.000 0.0783(8) . .
C14 C Uani 0.9281(2) 0.78180(16) -0.06265(14) 1.000 0.0620(6) . .
C15 C Uani 1.0193(3) 0.67317(19) -0.07043(17) 1.000 0.0774(8) . .
C16 C Uani 0.9061(2) 0.87090(16) -0.13110(15) 1.000 0.0612(6) . .
C17 C Uani 0.9700(2) 0.86490(18) -0.21969(16) 1.000 0.0700(7) . .
H1 H Uiso 0.71500 1.14600 -0.27100 1.000 0.0830 . R
H2 H Uiso 0.49630 1.15220 -0.41380 1.000 0.0950 . R
H3 H Uiso 0.31670 0.99970 -0.44570 1.000 0.0950 . R
H4 H Uiso 0.34850 0.84130 -0.33150 1.000 0.0920 . R
H5 H Uiso 0.56590 0.83150 -0.19010 1.000 0.0790 . R
H7 H Uiso 0.87310 1.04840 -0.12460 1.000 0.0720 calc R
H12A H Uiso 0.68250 0.95110 0.15300 1.000 0.0940 . R
H12B H Uiso 0.82730 0.87030 0.20040 1.000 0.0940 . R
H12C H Uiso 0.66550 0.81470 0.14250 1.000 0.0940 . R
H13 H Uiso 0.87520 0.72170 0.06820 1.000 0.0810 . R
H15A H Uiso 1.05840 0.67740 -0.13180 1.000 0.0930 . R
H15B H Uiso 0.95290 0.60550 -0.07400 1.000 0.0930 . R
H15C H Uiso 1.10670 0.66740 -0.01070 1.000 0.0930 . R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
|
1100678.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100678.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100678
_chemical_formula_sum 'C20 H21 Cl4 Cu2 N5 S2'
_chemical_formula_weight 664.42
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 107.664(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 14.363(5)
_cell_length_b 11.881(3)
_cell_length_c 15.710(5)
_cell_measurement_reflns_used 3305
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.36
_cell_measurement_theta_min 2.19
_cell_volume 2554.4(14)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.634
_diffrn_measured_fraction_theta_max 0.634
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0958
_diffrn_reflns_av_sigmaI/netI 0.1598
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -2
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 4243
_diffrn_reflns_theta_full 26.36
_diffrn_reflns_theta_max 26.36
_diffrn_reflns_theta_min 2.19
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.267
_exptl_absorpt_correction_T_max 0.956
_exptl_absorpt_correction_T_min 0.379
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (sheldrick 1996)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.728
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'thin plate'
_exptl_crystal_F_000 1336
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.02
_refine_diff_density_max 0.535
_refine_diff_density_min -0.627
_refine_diff_density_rms 0.119
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.979
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 299
_refine_ls_number_reflns 3305
_refine_ls_number_restraints 63
_refine_ls_restrained_S_all 0.974
_refine_ls_R_factor_all 0.1540
_refine_ls_R_factor_gt 0.0596
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1073
_refine_ls_wR_factor_ref 0.1382
_reflns_number_gt 1676
_reflns_number_total 3305
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100678
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.41807(10) 0.28110(8) 0.16092(9) 0.0218(4) Uani 1 1 d . . .
Cu2 Cu 0.83926(11) 0.41065(10) 0.53986(10) 0.0369(5) Uani 1 1 d . . .
Cl1 Cl 0.3844(2) 0.13065(18) 0.23892(18) 0.0307(8) Uani 1 1 d . . .
Cl2 Cl 0.4884(2) 0.17712(19) 0.07846(18) 0.0335(8) Uani 1 1 d . . .
Cl4 Cl 0.7690(2) 0.3828(2) 0.6487(2) 0.0456(9) Uani 1 1 d . . .
Cl3 Cl 0.9078(3) 0.2379(2) 0.5521(3) 0.0665(12) Uani 1 1 d . . .
S1 S 0.3389(2) 0.38870(18) 0.24259(18) 0.0224(7) Uani 1 1 d . . .
S2 S 0.9086(2) 0.4392(2) 0.4240(2) 0.0392(10) Uani 1 1 d . . .
N1 N 0.3926(6) 0.4195(5) 0.0785(6) 0.020(2) Uani 1 1 d U . .
N2 N 0.5495(6) 0.3388(6) 0.2722(6) 0.018(2) Uani 1 1 d U . .
N3 N 0.7041(7) 0.3930(6) 0.4192(6) 0.023(2) Uani 1 1 d U . .
N4 N 0.8322(6) 0.5832(7) 0.5392(6) 0.028(3) Uani 1 1 d . . .
C1 C 0.3956(8) 0.4162(8) -0.0062(8) 0.027(3) Uani 1 1 d U . .
H1 H 0.4201 0.3518 -0.0253 0.032 Uiso 1 1 calc R . .
C2 C 0.3647(8) 0.5021(7) -0.0656(7) 0.033(3) Uani 1 1 d . . .
H2 H 0.3687 0.4962 -0.1234 0.039 Uiso 1 1 calc R . .
C3 C 0.3270(8) 0.5989(8) -0.0381(9) 0.038(3) Uani 1 1 d U . .
H3 H 0.3034 0.6581 -0.0775 0.045 Uiso 1 1 calc R . .
C4 C 0.3258(9) 0.6044(8) 0.0489(8) 0.037(3) Uani 1 1 d . . .
H4 H 0.3025 0.6690 0.0691 0.044 Uiso 1 1 calc R . .
C5 C 0.3586(8) 0.5160(7) 0.1065(7) 0.020(3) Uani 1 1 d . . .
C6 C 0.3635(8) 0.5251(7) 0.2023(7) 0.026(3) Uani 1 1 d U . .
H6A H 0.3158 0.5794 0.2090 0.031 Uiso 1 1 calc R . .
H6B H 0.4279 0.5508 0.2372 0.031 Uiso 1 1 calc R . .
C7 C 0.4299(8) 0.3847(8) 0.3499(7) 0.033(3) Uani 1 1 d U . .
H7A H 0.4246 0.4527 0.3822 0.040 Uiso 1 1 calc R . .
H7B H 0.4163 0.3214 0.3832 0.040 Uiso 1 1 calc R . .
C8 C 0.5341(8) 0.3745(7) 0.3463(7) 0.019(3) Uani 1 1 d . . .
C9 C 0.6116(8) 0.4014(7) 0.4198(7) 0.020(3) Uani 1 1 d . . .
H9 H 0.5992 0.4262 0.4714 0.024 Uiso 1 1 calc R . .
C10 C 0.6403(8) 0.3302(7) 0.2684(7) 0.016(2) Uani 1 1 d U . .
H10 H 0.6516 0.3041 0.2166 0.020 Uiso 1 1 calc R . .
C11 C 0.7192(9) 0.3604(7) 0.3422(8) 0.026(3) Uani 1 1 d . . .
C12 C 0.8221(8) 0.3529(9) 0.3383(7) 0.037(3) Uani 1 1 d . . .
H12A H 0.8235 0.3771 0.2797 0.044 Uiso 1 1 calc R . .
H12B H 0.8431 0.2750 0.3459 0.044 Uiso 1 1 calc R . .
C13 C 0.8608(8) 0.5784(8) 0.3952(7) 0.034(3) Uani 1 1 d U . .
H13A H 0.9054 0.6201 0.3715 0.041 Uiso 1 1 calc R . .
H13B H 0.7988 0.5728 0.3483 0.041 Uiso 1 1 calc R . .
C14 C 0.8457(8) 0.6426(8) 0.4715(8) 0.032(3) Uani 1 1 d U . .
C15 C 0.8456(8) 0.7605(9) 0.4700(8) 0.037(3) Uani 1 1 d . . .
H15 H 0.8571 0.7999 0.4230 0.044 Uiso 1 1 calc R . .
C16 C 0.8279(9) 0.8158(9) 0.5401(10) 0.052(4) Uani 1 1 d . . .
H16 H 0.8242 0.8940 0.5397 0.063 Uiso 1 1 calc R . .
C17 C 0.8157(9) 0.7566(9) 0.6107(10) 0.051(4) Uani 1 1 d . . .
H17 H 0.8060 0.7936 0.6595 0.062 Uiso 1 1 calc R . .
C18 C 0.8182(8) 0.6394(10) 0.6078(9) 0.042(4) Uani 1 1 d . . .
H18 H 0.8097 0.5988 0.6555 0.051 Uiso 1 1 calc R . .
C19 C 1.0070(15) 0.9794(17) 0.6785(16) 0.40(4) Uani 1 1 d D . .
C20 C 1.075(2) 0.975(3) 0.620(2) 0.213(17) Uani 1 1 d D . .
H201 H 1.1087 0.9043 0.6276 0.319 Uiso 1 1 calc R . .
H202 H 1.1224 1.0351 0.6367 0.319 Uiso 1 1 calc R . .
H203 H 1.0377 0.9842 0.5581 0.319 Uiso 1 1 calc R . .
N5 N 0.952(3) 0.989(3) 0.719(2) 0.246(14) Uani 1 1 d D . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0272(9) 0.0171(5) 0.0209(9) 0.0000(5) 0.0072(7) 0.0011(6)
Cu2 0.0318(11) 0.0352(7) 0.0426(12) -0.0060(6) 0.0097(9) -0.0019(6)
Cl1 0.036(2) 0.0215(11) 0.036(2) 0.0047(11) 0.0128(16) -0.0033(11)
Cl2 0.048(2) 0.0285(12) 0.025(2) 0.0015(11) 0.0129(17) 0.0137(12)
Cl4 0.052(2) 0.0478(16) 0.039(2) -0.0060(14) 0.0158(19) -0.0087(15)
Cl3 0.055(3) 0.0456(18) 0.104(3) 0.0103(17) 0.033(2) 0.0139(16)
S1 0.026(2) 0.0242(12) 0.0179(19) 0.0008(11) 0.0074(15) -0.0008(11)
S2 0.028(2) 0.0421(16) 0.044(2) -0.0115(14) 0.0050(19) -0.0054(13)
N1 0.022(4) 0.014(3) 0.021(4) -0.003(3) 0.003(3) 0.006(3)
N2 0.017(4) 0.018(3) 0.021(4) -0.001(3) 0.008(4) -0.003(3)
N3 0.019(4) 0.028(3) 0.019(4) -0.003(3) 0.001(4) -0.001(3)
N4 0.022(7) 0.047(5) 0.015(7) -0.004(5) 0.007(5) -0.005(4)
C1 0.030(5) 0.030(4) 0.027(5) -0.003(4) 0.017(4) 0.005(3)
C2 0.053(9) 0.033(6) 0.015(8) 0.003(5) 0.014(7) 0.007(5)
C3 0.045(5) 0.036(4) 0.035(5) 0.006(4) 0.016(4) 0.003(4)
C4 0.064(10) 0.025(5) 0.030(9) -0.002(5) 0.026(7) 0.001(6)
C5 0.024(8) 0.021(5) 0.017(8) -0.002(4) 0.011(6) 0.000(4)
C6 0.029(5) 0.028(4) 0.022(5) 0.003(3) 0.008(4) 0.001(3)
C7 0.035(5) 0.038(4) 0.032(5) -0.001(4) 0.018(4) 0.001(4)
C8 0.022(8) 0.017(4) 0.017(8) 0.001(4) 0.006(6) 0.001(4)
C9 0.020(8) 0.025(5) 0.015(8) 0.000(4) 0.003(6) 0.000(5)
C10 0.019(5) 0.018(3) 0.015(5) 0.001(3) 0.008(4) 0.003(3)
C11 0.022(9) 0.023(5) 0.037(9) 0.004(5) 0.015(7) -0.001(4)
C12 0.034(10) 0.054(7) 0.024(9) -0.018(5) 0.010(7) -0.007(6)
C13 0.027(5) 0.039(4) 0.038(5) -0.004(4) 0.010(4) -0.006(4)
C14 0.027(5) 0.036(4) 0.031(5) -0.003(4) 0.006(4) 0.001(4)
C15 0.025(9) 0.047(7) 0.038(10) 0.000(6) 0.010(7) -0.001(5)
C16 0.051(11) 0.032(6) 0.065(12) 0.008(7) 0.006(9) 0.006(6)
C17 0.055(11) 0.033(6) 0.061(11) -0.017(6) 0.011(9) -0.001(6)
C18 0.028(9) 0.061(8) 0.031(10) -0.003(6) -0.001(8) -0.015(6)
C19 0.55(9) 0.028(11) 0.29(6) 0.01(2) -0.34(5) -0.02(3)
C20 0.17(3) 0.14(2) 0.23(4) 0.05(2) -0.08(2) -0.028(19)
N5 0.38(4) 0.19(3) 0.14(2) -0.072(17) 0.05(3) -0.08(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 Cl2 95.9(2) . . ?
N1 Cu1 N2 101.1(3) . . ?
Cl2 Cu1 N2 101.4(2) . . ?
N1 Cu1 Cl1 158.6(2) . . ?
Cl2 Cu1 Cl1 94.82(10) . . ?
N2 Cu1 Cl1 94.9(2) . . ?
N1 Cu1 S1 83.4(2) . . ?
Cl2 Cu1 S1 177.76(12) . . ?
N2 Cu1 S1 80.8(2) . . ?
Cl1 Cu1 S1 85.22(10) . . ?
N4 Cu2 Cl4 96.8(3) . . ?
N4 Cu2 Cl3 158.0(3) . . ?
Cl4 Cu2 Cl3 94.93(13) . . ?
N4 Cu2 N3 93.4(3) . . ?
Cl4 Cu2 N3 98.8(3) . . ?
Cl3 Cu2 N3 103.1(2) . . ?
N4 Cu2 S2 83.3(3) . . ?
Cl4 Cu2 S2 178.59(13) . . ?
Cl3 Cu2 S2 85.44(13) . . ?
N3 Cu2 S2 79.8(3) . . ?
C7 S1 C6 100.8(5) . . ?
C7 S1 Cu1 99.5(4) . . ?
C6 S1 Cu1 96.8(4) . . ?
C13 S2 C12 102.0(5) . . ?
C13 S2 Cu2 96.2(4) . . ?
C12 S2 Cu2 97.8(4) . . ?
C1 N1 C5 117.7(8) . . ?
C1 N1 Cu1 123.2(6) . . ?
C5 N1 Cu1 118.6(7) . . ?
C8 N2 C10 119.6(9) . . ?
C8 N2 Cu1 117.2(7) . . ?
C10 N2 Cu1 123.0(7) . . ?
C9 N3 C11 117.3(9) . . ?
C9 N3 Cu2 125.9(8) . . ?
C11 N3 Cu2 116.4(8) . . ?
C18 N4 C14 118.1(10) . . ?
C18 N4 Cu2 121.0(8) . . ?
C14 N4 Cu2 120.8(7) . . ?
N1 C1 C2 123.7(9) . . ?
C1 C2 C3 118.8(11) . . ?
C4 C3 C2 118.1(10) . . ?
C5 C4 C3 120.9(10) . . ?
N1 C5 C4 120.8(10) . . ?
N1 C5 C6 118.3(8) . . ?
C4 C5 C6 120.8(9) . . ?
C5 C6 S1 109.5(6) . . ?
C8 C7 S1 114.3(8) . . ?
N2 C8 C9 120.4(10) . . ?
N2 C8 C7 119.3(10) . . ?
C9 C8 C7 120.4(10) . . ?
N3 C9 C8 122.0(10) . . ?
N2 C10 C11 120.3(10) . . ?
N3 C11 C10 120.4(11) . . ?
N3 C11 C12 118.8(10) . . ?
C10 C11 C12 120.8(10) . . ?
C11 C12 S2 113.0(8) . . ?
C14 C13 S2 114.0(8) . . ?
N4 C14 C15 122.7(11) . . ?
N4 C14 C13 117.4(9) . . ?
C15 C14 C13 119.9(11) . . ?
C16 C15 C14 117.8(12) . . ?
C17 C16 C15 120.3(11) . . ?
C16 C17 C18 118.4(13) . . ?
N4 C18 C17 122.6(13) . . ?
N5 C19 C20 175(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.056(8) . ?
Cu1 Cl2 2.240(3) . ?
Cu1 N2 2.255(8) . ?
Cu1 Cl1 2.300(3) . ?
Cu1 S1 2.336(3) . ?
Cu2 N4 2.052(8) . ?
Cu2 Cl4 2.258(4) . ?
Cu2 Cl3 2.260(3) . ?
Cu2 N3 2.274(9) . ?
Cu2 S2 2.349(4) . ?
S1 C7 1.793(11) . ?
S1 C6 1.813(9) . ?
S2 C13 1.795(10) . ?
S2 C12 1.842(10) . ?
N1 C1 1.345(12) . ?
N1 C5 1.370(11) . ?
N2 C8 1.319(11) . ?
N2 C10 1.328(11) . ?
N3 C9 1.335(12) . ?
N3 C11 1.349(12) . ?
N4 C18 1.334(13) . ?
N4 C14 1.339(13) . ?
C1 C2 1.363(13) . ?
C2 C3 1.395(14) . ?
C3 C4 1.374(14) . ?
C4 C5 1.374(13) . ?
C5 C6 1.489(14) . ?
C7 C8 1.520(14) . ?
C8 C9 1.377(13) . ?
C10 C11 1.399(13) . ?
C11 C12 1.500(15) . ?
C13 C14 1.491(14) . ?
C14 C15 1.400(14) . ?
C15 C16 1.371(15) . ?
C16 C17 1.369(16) . ?
C17 C18 1.393(14) . ?
C19 N5 1.1604(11) . ?
C19 C20 1.5405(11) . ?
|
1100679.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-24 01:57:32 +0200 (Wed, 24 Feb 2016) $
#$Revision: 176833 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100679.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100679
loop_
_publ_author_name
'Aksoy, Ilhan'
'\,Cukurovali, Alaaddin'
'G\"uven, Kutalms'
'Yilmaz, Ibrahim'
'Sari, Ugur'
_publ_section_title
;
Structure of 4-(1-phenyl-1-methylcyclobutyl-3-yl)-2-aminothiazole
;
_journal_coden_ASTM XSAOAF
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x59
_journal_page_last x60
_journal_paper_doi 10.2116/analscix.19.x59
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C14 H16 N2 S'
_chemical_formula_weight 244.35
_space_group_IT_number 2
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 102.365(16)
_cell_angle_beta 92.120(16)
_cell_angle_gamma 65.302(15)
_cell_formula_units_Z 2
_cell_length_a 10.4686(16)
_cell_length_b 11.9543(16)
_cell_length_c 5.9271(16)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 657.1(2)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type ?
_diffrn_measurement_method ?
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0101
_diffrn_reflns_av_sigmaI/netI 0.0222
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 4029
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 2.14
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.226
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.235
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 260
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.224
_refine_diff_density_min -0.262
_refine_diff_density_rms 0.037
_refine_ls_extinction_coef 0.027(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 156
_refine_ls_number_reflns 3836
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.050
_refine_ls_R_factor_all 0.0727
_refine_ls_R_factor_gt 0.0419
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.1601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1149
_refine_ls_wR_factor_ref 0.1333
_reflns_number_gt 2561
_reflns_number_total 3836
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.1601P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.1601P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100679
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.29613(5) 0.29883(4) 1.02974(10) 0.06480(18) Uani 1 d . . .
N1 N 0.51156(16) 0.36496(15) 1.1237(3) 0.0718(5) Uani 1 d . . .
H1A H 0.5563 0.4107 1.1190 0.086 Uiso 1 calc R . .
H1B H 0.5459 0.3029 1.1922 0.086 Uiso 1 calc R . .
N2 N 0.32819(13) 0.48227(12) 0.9170(2) 0.0460(3) Uani 1 d . . ..
C1 C 0.38836(16) 0.39043(14) 1.0244(3) 0.0498(4) Uani 1 d . . .
C2 C 0.16829(19) 0.39381(16) 0.8776(4) 0.0584(4) Uani 1 d . . .
H2 H 0.0873 0.3835 0.8317 0.070 Uiso 1 calc R . .
C3 C 0.20124(16) 0.48482(15) 0.8341(3) 0.0462(3) Uani 1 d . . ..
C4 C 0.11132(16) 0.58942(15) 0.7207(3) 0.0473(4) Uani 1 d . . .
H4 H 0.0238 0.5820 0.6749 0.057 Uiso 1 calc R . .
C5 C 0.07999(17) 0.72492(14) 0.8578(3) 0.0462(3) Uani 1 d . . .
H5A H -0.0166 0.7727 0.9204 0.055 Uiso 1 calc R . ..
H5B H 0.1455 0.7280 0.9765 0.055 Uiso 1 calc R . .
C6 C 0.17879(18) 0.61554(15) 0.5214(3) 0.0504(4) Uani 1 d . . .
H6A H 0.1446 0.5944 0.3711 0.061 Uiso 1 calc R . .
H6B H 0.2809 0.5781 0.5152 0.061 Uiso 1 calc R . .
C7 C 0.11056(16) 0.75928(15) 0.6341(3) 0.0453(3) Uani 1 d . . ..
C8 C -0.0263(2) 0.83151(19) 0.5245(3) 0.0617(5) Uani 1 d . . .
H8A H -0.0732 0.9155 0.6170 0.093 Uiso 1 calc R . .
H8B H -0.0867 0.7887 0.5168 0.093 Uiso 1 calc R . .
H8C H -0.0046 0.8355 0.3712 0.093 Uiso 1 calc R . .
C9 C 0.20555(17) 0.82621(14) 0.6526(3) 0.0470(3) Uani 1 d . . ..
C10 C 0.3009(2) 0.80162(19) 0.4722(3) 0.0643(5) Uani 1 d . . .
H10 H 0.3048 0.7441 0.3363 0.077 Uiso 1 calc R . .
C11 C 0.3900(3) 0.8611(2) 0.4910(4) 0.0805(6) Uani 1 d . . .
H11 H 0.4528 0.8438 0.3678 0.097 Uiso 1 calc R . .
C12 C 0.3867(2) 0.9463(2) 0.6915(5) 0.0784(6) Uani 1 d .. . .
H12 H 0.4481 0.9851 0.7049 0.094 Uiso 1 calc R . .
C13 C 0.2918(2) 0.97311(18) 0.8709(4) 0.0672(5) Uani 1 d . . .
H13 H 0.2877 1.0316 1.0054 0.081 Uiso 1 calc R . .
C14 C 0.20254(18) 0.91343(15) 0.8520(3) 0.0539(4) Uani 1 d . . ..
H14 H 0.1392 0.9320 0.9751 0.065 Uiso 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0585(3) 0.0459(2) 0.1010(4) 0.0248(2) -0.0051(2) -0.0283(2)
N1 0.0525(9) 0.0640(9) 0.1174(15) 0.0512(10) -0.0285(9) -0.0291(7)
N2 0.0397(6) 0.0429(6) 0.0606(8) 0.0152(6) -0.0074(6) -0.0209(5)
C1 0.0429(8) 0.0412(7) 0.0676(10) 0.0149(7) -0.0023(7) -0.0185(6)
C2 0.0502(9) 0.0502(9) 0.0815(13) 0.0107(8) -0.0076(8) -0.0296(8)
C3 0.0423(7) 0.0431(7) 0.0548(9) 0.0067(6) -0.0043(6) -0.0215(6)
C4 0.0423(8) 0.0507(8) 0.0497(9) 0.0086(7) -0.0097(6) -0.0220(7)
C5 0.0449(8) 0.0473(8) 0.0420(8) 0.0077(6) -0.0048(6) -0.0163(6)
C6 0.0534(9) 0.0509(8) 0.0407(8) 0.0029(6) -0.0057(7) -0.0195(7)
C7 0.0461(8) 0.0463(8) 0.0380(7) 0.0086(6) -0.0086(6) -0.0147(6)
C8 0.0560(10) 0.0656(11) 0.0540(10) 0.0158(8) -0.0183(8) -0.0163(8)
C9 0.0474(8) 0.0437(8) 0.0474(8) 0.0158(6) -0.0076(6) -0.0143(6)
C10 0.0747(13) 0.0712(12) 0.0520(10) 0.0165(9) 0.0029(9) -0.0334(10)
C11 0.0866(16) 0.0885(15) 0.0811(15) 0.0281(13) 0.0114(12) -0.0449(13)
C12 0.0787(14) 0.0713(13) 0.1046(18) 0.0322(13) -0.0070(13) -0.0441(12)
C13 0.0719(12) 0.0494(9) 0.0827(14) 0.0125(9) -0.0090(10) -0.0290(9)
C14 0.0534(9) 0.0448(8) 0.0586(10) 0.0079(7) -0.0033(8) -0.0174(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 S1 C1 88.57(8) . . ?
C1 N2 C3 110.78(13) . . ?
N2 C1 N1 124.35(15) . . ?
N2 C1 S1 114.67(12) . . ?
N1 C1 S1 120.98(12) . . ?
C3 C2 S1 111.04(13) . . ?
C2 C3 N2 114.94(15) . . ?
C2 C3 C4 126.19(15) . . ?
N2 C3 C4 118.76(13) . . ?
C3 C4 C6 118.51(14) . . ?
C3 C4 C5 116.02(13) . . ?
C6 C4 C5 88.33(12) . . ?
C7 C5 C4 90.16(12) . . ?
C4 C6 C7 89.95(12) . . ?
C9 C7 C8 110.40(14) .. . ?
C9 C7 C5 116.61(12) . . ?
C8 C7 C5 111.35(14) . . ?
C9 C7 C6 116.26(13) . . ?
C8 C7 C6 112.63(13) . . ?
C5 C7 C6 87.99(12) . . ?
C10 C9 C14 117.64(17) . . ?
C10 C9 C7 121.08(16) . . ?
C14 C9 C7 121.27(15) . . ?
C11 C10 C9 121.1(2) . . ?
C10 C11 C12 120.5(2) . . ?
C13 C12 C11 119.3(2) . . ?
C12 C13 C14 120.2(2) . . ?
C13 C14 C9 121.29(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C2 1.724(2) . ?
S1 C1 1.7415(16) . ?
N1 C1 1.340(2) . ?
N2 C1 1.304(2) . ?
N2 C3 1.3903(19) . ?
C2 C3 1.345(2) . ?
C3 C4 1.493(2) . ?
C4 C6 1.548(2) . ?
C4 C5 1.550(2) . ?
C5 C7 1.550(2) . ?
C6 C7 1.558(2) . ?
C7 C9 1.503(2) . ?
C7 C8 1.536(2) . ?
C9 C10 1.388(2) . ?
C9 C14 1.390(2) . ?
C10 C11 1.379(3) . ?
C11 C12 1.380(3) . ?
C12 C13 1.373(3) . ?
C13 C14 1.382(3) . ?
|
1100680.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100680.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100680
loop_
_publ_author_name
'Sari, Ugur'
'Bati, H\"umeyra'
'G\"uven, Kutalms'
'Tas, Murat'
'Aksoy, Ilhan'
_publ_section_title
;
Structure of 1-(4-Methylphenylamino)-2-phenyl-1,2-ethandione-1-oxime
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x61
_journal_page_last x62
_journal_paper_doi 10.2116/analscix.19.x61
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C15 H14 N2 O2'
_chemical_formula_weight 254.28
_space_group_IT_number 33
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2c -2n'
_symmetry_space_group_name_H-M 'P n a 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 8
_cell_length_a 23.516(3)
_cell_length_b 5.364(3)
_cell_length_c 21.872(3)
_cell_measurement_temperature 293(2)
_cell_volume 2758.7(17)
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71069
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0423
_diffrn_reflns_limit_h_max 33
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4128
_diffrn_reflns_theta_max 29.99
_diffrn_reflns_theta_min 2.54
_exptl_absorpt_coefficient_mu 0.083
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.224
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1072
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.35
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.5(19)
_refine_ls_extinction_coef 0.0054(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 362
_refine_ls_number_reflns 4128
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.059
_refine_ls_R_factor_all 0.1098
_refine_ls_R_factor_gt 0.0410
_refine_ls_shift/su_max 0.041
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1284
_refine_ls_wR_factor_ref 0.1759
_reflns_number_gt 2204
_reflns_number_total 4128
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M P
_cod_database_code 1100680
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.25055(11) 0.5564(6) 0.01283(12) 0.0592(7) Uani 1 d . . .
C24 C 0.21688(13) 0.4511(6) 0.04509(15) 0.0414(7) Uani 1 d . . .
O2 O 0.50733(12) 0.0098(6) 0.34315(13) 0.0603(7) Uani 1 d . . .
C6 C 0.42786(13) -0.2205(7) 0.24837(16) 0.0460(8) Uani 1 d . . .
N3 N 0.27948(13) 0.4394(7) 0.13684(16) 0.0511(7) Uani 1 d . . .
C21 C 0.32428(13) 0.3004(6) 0.11052(15) 0.0416(7) Uani 1 d . . .
O1 O 0.56201(13) -0.0232(8) 0.15092(15) 0.0818(12) Uani 1 d . . .
C10 C 0.58322(15) -0.2791(7) 0.33679(15) 0.0453(7) Uani 1 d . . .
N4 N 0.18075(12) 0.5129(7) 0.14344(15) 0.0567(8) Uani 1 d . . .
C16 C 0.38025(14) 0.3795(7) 0.11828(17) 0.0462(8) Uani 1 d . . .
H16 H 0.3880 0.5251 0.1398 0.055 Uiso 1 calc R . .
N2 N 0.57461(13) -0.0659(7) 0.21313(15) 0.0599(9) Uani 1 d . . .
N1 N 0.47571(13) -0.1125(8) 0.21945(16) 0.0587(9) Uani 1 d . .. .
C17 C 0.42380(13) 0.2419(7) 0.09408(18) 0.0484(8) Uani 1 d . . .
H17 H 0.4610 0.2946 0.1006 0.058 Uiso 1 calc R . .
C19 C 0.35813(16) -0.0477(7) 0.05268(19) 0.0514(8) Uani 1 d . .. .
H19 H 0.3503 -0.1896 0.0297 0.062 Uiso 1 calc R . .
C9 C 0.53751(13) -0.1204(7) 0.31181(15) 0.0446(7) Uani 1 d . . .
C25 C 0.16478(14) 0.3293(6) 0.02095(15) 0.0437(7) Uani 1 d . . .
C20 C 0.31410(15) 0.0837(6) 0.07842(18) 0.0479(8) Uani 1 d . . .
H20 H 0.2770 0.0259 0.0742 0.057 Uiso 1 calc R . .
C8 C 0.52884(14) -0.1097(7) 0.24253(16) 0.0480(8) Uani 1 d . . .
C4 C 0.32818(17) -0.2143(9) 0.2703(2) 0.0638(11) Uani 1 d . . ..
H4 H 0.2927 -0.1404 0.2651 0.077 Uiso 1 calc R . .
O3 O 0.19397(13) 0.5545(8) 0.20609(13) 0.0777(10) Uani 1 d . . .
C5 C 0.37508(15) -0.1122(8) 0.24145(19) 0.0540(9) Uani 1 d . . .
H5 H 0.3710 0.0295 0.2174 0.065 Uiso 1 calc R . .
C2 C 0.3863(2) -0.5344(8) 0.3109(2) 0.0665(11) Uani 1 d . . .
H2 H 0.3902 -0.6792 0.3339 0.080 Uiso 1 calc R . .
C18 C 0.41475(15) 0.0289(7) 0.06052(17) 0.0491(8) Uani 1 d . . .
C22 C 0.46256(18) -0.1215(9) 0.0330(2) 0.0674(11) Uani 1 d . . ..
H22A H 0.4912 -0.0108 0.0175 0.101 Uiso 1 calc R . .
H22B H 0.4481 -0.2219 0.0002 0.101 Uiso 1 calc R . .
H22C H 0.4788 -0.2275 0.0638 0.101 Uiso 1 calc R . .
C23 C 0.22621(13) 0.4562(7) 0.11378(15) 0.0435(7) Uani 1 d . . .
C1 C 0.43308(17) -0.4363(7) 0.28210(19) 0.0556(9) Uani 1 d . . .
H1 H 0.4682 -0.5151 0.2854 0.067 Uiso 1 calc R . .
C26 C 0.14249(18) 0.4162(9) -0.0337(2) 0.0611(10) Uani 1 d . . .
H26 H 0.1596 0.5489 -0.0539 0.073 Uiso 1 calc R . .
C30 C 0.13919(17) 0.1279(8) 0.0501(2) 0.0592(9) Uani 1 d .. . .
H30 H 0.1540 0.0685 0.0867 0.071 Uiso 1 calc R . .
C15 C 0.60634(16) -0.4774(8) 0.30472(19) 0.0563(9) Uani 1 d . . .
H15 H 0.5941 -0.5112 0.2651 0.068 Uiso 1 calc R . .
C11 C 0.60155(17) -0.2383(8) 0.39641(17) 0.0601(10) Uani 1 d . . .
H11 H 0.5856 -0.1095 0.4191 0.072 Uiso 1 calc R . .
C12 C 0.64256(19) -0.3848(9) 0.4219(2) 0.0711(12) Uani 1 d . . .
H12 H 0.6547 -0.3526 0.4616 0.085 Uiso 1 calc R . .
C28 C 0.0694(2) 0.1057(12) -0.0281(3) 0.0904(17) Uani 1 d . . .
H28 H 0.0369 0.0321 -0.0443 0.109 Uiso 1 calc R . .
C14 C 0.6473(2) -0.6241(10) 0.3314(2) 0.0740(13) Uani 1 d . . .
H14 H 0.6626 -0.7568 0.3095 0.089 Uiso 1 calc R . .
C3 C 0.33297(19) -0.4223(9) 0.3064(2) 0.0689(11) Uani 1 d . . .
C13 C 0.6660(2) -0.5776(9) 0.3902(2) 0.0733(12) Uani 1 d . . .
H13 H 0.6942 -0.6761 0.4077 0.088 Uiso 1 calc R . .
C29 C 0.0923(2) 0.0171(10) 0.0251(3) 0.0822(15) Uani 1 d . . .
H29 H 0.0759 -0.1195 0.0444 0.099 Uiso 1 calc R . ..
C27 C 0.0945(2) 0.3040(11) -0.0578(2) 0.0823(15) Uani 1 d . . .
H27 H 0.0791 0.3627 -0.0942 0.099 Uiso 1 calc R . .
C7 C 0.2828(3) -0.5272(14) 0.3416(3) 0.111(2) Uani 1 d . . .
H7A H 0.2502 -0.4222 0.3356 0.166 Uiso 1 calc R . ..
H7B H 0.2920 -0.5336 0.3844 0.166 Uiso 1 calc R . .
H7C H 0.2745 -0.6923 0.3272 0.166 Uiso 1 calc R . .
H2B H 0.286(2) 0.493(8) 0.172(3) 0.065(13) Uiso 1 d . . .
H2A H 0.4732(17) -0.055(7) 0.187(2) 0.044(11) Uiso 1 d . . .
H1A* H 0.591(2) -0.018(9) 0.135(2) 0.064(14) Uiso 1 d . . ..
H1B* H 0.158(2) 0.607(9) 0.222(2) 0.076(14) Uiso 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O4 0.0477(14) 0.0807(18) 0.0492(14) 0.0050(13) 0.0079(12) -0.0122(13)
C24 0.0333(14) 0.0512(17) 0.0398(17) -0.0011(14) 0.0043(12) 0.0052(13)
O2 0.0488(14) 0.0803(18) 0.0519(15) -0.0038(13) 0.0059(12) 0.0134(13)
C6 0.0388(16) 0.060(2) 0.0396(17) -0.0026(15) -0.0018(14) -0.0040(15)
N3 0.0409(15) 0.0693(19) 0.0432(17) -0.0095(15) -0.0048(12) 0.0057(13)
C21 0.0383(16) 0.0487(18) 0.0379(17) 0.0054(14) -0.0014(13) 0.0034(13)
O1 0.0427(15) 0.157(3) 0.0455(15) 0.0259(19) 0.0045(12) -0.0116(18)
C10 0.0438(16) 0.0544(19) 0.0376(16) -0.0018(15) 0.0036(14) 0.0003(14)
N4 0.0425(15) 0.089(2) 0.0385(15) -0.0057(16) 0.0027(13) 0.0008(16)
C16 0.0406(16) 0.0475(18) 0.0506(19) 0.0009(16) -0.0102(14) -0.0015(14)
N2 0.0431(16) 0.098(3) 0.0385(15) 0.0077(16) 0.0042(12) -0.0054(16)
N1 0.0403(15) 0.094(3) 0.0417(16) 0.0207(18) -0.0015(13) -0.0023(15)
C17 0.0325(15) 0.0542(19) 0.058(2) 0.0145(17) -0.0058(14) 0.0001(14)
C19 0.0490(18) 0.0463(17) 0.059(2) -0.0015(17) -0.0055(16) 0.0027(15)
C9 0.0374(15) 0.0587(19) 0.0376(16) 0.0006(16) 0.0022(13) -0.0046(15)
C25 0.0363(15) 0.0523(18) 0.0424(17) -0.0053(15) 0.0021(13) 0.0025(14)
C20 0.0399(16) 0.0493(19) 0.054(2) 0.0048(16) -0.0052(15) -0.0039(14)
C8 0.0383(16) 0.064(2) 0.0418(17) 0.0066(16) 0.0024(13) 0.0007(15)
C4 0.0401(18) 0.080(3) 0.072(3) -0.009(2) 0.0007(17) -0.0003(18)
O3 0.0505(15) 0.140(3) 0.0424(15) -0.0148(17) -0.0003(12) 0.0141(18)
C5 0.045(2) 0.061(2) 0.057(2) 0.0052(18) -0.0036(16) 0.0007(16)
C2 0.071(3) 0.060(2) 0.068(3) 0.009(2) -0.005(2) -0.022(2)
C18 0.0419(17) 0.0527(19) 0.0525(19) 0.0132(16) 0.0014(14) 0.0082(15)
C22 0.052(2) 0.073(3) 0.077(3) 0.008(2) 0.006(2) 0.022(2)
C23 0.0351(15) 0.0574(18) 0.0379(16) 0.0016(14) 0.0001(12) 0.0006(14)
C1 0.052(2) 0.055(2) 0.060(2) 0.0014(18) -0.0066(17) -0.0012(16)
C26 0.058(2) 0.075(3) 0.051(2) -0.0027(19) -0.0092(17) 0.0025(19)
C30 0.0498(19) 0.063(2) 0.065(2) 0.004(2) -0.0027(17) -0.0041(18)
C15 0.054(2) 0.068(2) 0.047(2) -0.0116(18) -0.0057(16) 0.0070(18)
C11 0.064(2) 0.072(2) 0.0451(19) -0.0100(19) -0.0057(17) 0.017(2)
C12 0.075(3) 0.090(3) 0.048(2) -0.010(2) -0.022(2) 0.023(2)
C28 0.059(3) 0.108(4) 0.104(4) -0.037(4) -0.019(3) -0.015(3)
C14 0.077(3) 0.075(3) 0.071(3) -0.019(2) -0.011(2) 0.027(2)
C3 0.060(2) 0.085(3) 0.062(2) -0.001(2) 0.000(2) -0.028(2)
C13 0.077(3) 0.081(3) 0.062(2) -0.006(2) -0.018(2) 0.028(2)
C29 0.060(3) 0.076(3) 0.110(4) -0.010(3) -0.002(3) -0.020(2)
C27 0.071(3) 0.106(4) 0.069(3) -0.017(3) -0.027(2) 0.009(3)
C7 0.074(3) 0.159(6) 0.099(4) 0.015(4) 0.016(3) -0.053(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100681.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100681.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100681
loop_
_publ_author_name
'Imai, Tokiko'
'Yoshihiro, Yokoyama'
'Sekine, Akiko'
'Uekusa, Hidediro'
'Ohashi, Yuji'
_publ_section_title
;
The Structure of 2-Amino-2-deoxyascorbic acid and
2-Amino-2-deoxyerythorbic acid
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x65
_journal_page_last x66
_journal_paper_doi 10.2116/analscix.19.x65
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C6 H9 N O5'
_chemical_formula_weight 175.14
_chemical_name_common 'Scorbamic acid'
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.8162(6)
_cell_length_b 16.9420(15)
_cell_length_c 4.8651(3)
_cell_measurement_reflns_used 3092
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 27.51
_cell_measurement_theta_min 2.40
_cell_volume 726.67(9)
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measurement_device_type 'Rigaku R-AXIS CS Imaging Plate'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71070
_diffrn_reflns_av_R_equivalents 0.0569
_diffrn_reflns_av_sigmaI/netI 0.0400
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 4
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_number 3092
_diffrn_reflns_theta_max 27.51
_diffrn_reflns_theta_min 2.40
_exptl_absorpt_coefficient_mu 0.141
_exptl_absorpt_correction_type none
_exptl_crystal_colour 'clear yellow'
_exptl_crystal_density_diffrn 1.601
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 368
_exptl_crystal_size_max 0.80
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 1.6(16)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.116
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 112
_refine_ls_number_reflns 1543
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.116
_refine_ls_R_factor_all 0.0444
_refine_ls_R_factor_gt 0.0421
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.2257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1233
_refine_ls_wR_factor_ref 0.1280
_reflns_number_gt 1459
_reflns_number_total 1543
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P212121
_cod_database_code 1100681
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.88499(16) 0.44673(8) 0.7717(4) 0.0316(4) Uani 1 1 d . . .
O2 O 1.12075(18) 0.47637(10) 0.6256(4) 0.0396(4) Uani 1 1 d . . .
O3 O 0.93622(19) 0.31463(9) 1.3340(4) 0.0371(4) Uani 1 1 d . . .
O4 O 0.75352(17) 0.28253(8) 0.7412(4) 0.0346(4) Uani 1 1 d . . .
H4 H 0.8159 0.2985 0.6291 0.052 Uiso 1 1 calc R . .
O5 O 0.44540(17) 0.34613(9) 0.6640(5) 0.0434(5) Uani 1 1 d . . .
H5 H 0.4670 0.2991 0.6672 0.065 Uiso 1 1 calc R . .
N1 N 1.2319(2) 0.37311(11) 1.0878(5) 0.0339(5) Uani 1 1 d . . .
H1A H 1.2351 0.3279 1.1811 0.051 Uiso 1 1 calc R . .
H1B H 1.2659 0.4121 1.1936 0.051 Uiso 1 1 calc R . .
H1C H 1.2899 0.3692 0.9387 0.051 Uiso 1 1 calc R . .
C1 C 1.0407(2) 0.44040(11) 0.7866(5) 0.0288(5) Uani 1 1 d . . .
C2 C 1.0774(2) 0.38943(12) 1.0067(5) 0.0282(4) Uani 1 1 d . . .
C3 C 0.9500(2) 0.36199(11) 1.1371(5) 0.0287(4) Uani 1 1 d . . .
C4 C 0.8174(2) 0.40243(12) 0.9953(5) 0.0298(5) Uani 1 1 d . . .
H4A H 0.7715 0.4398 1.1247 0.036 Uiso 1 1 calc R . .
C5 C 0.6939(2) 0.34731(12) 0.8899(5) 0.0296(5) Uani 1 1 d . . .
H5A H 0.6405 0.3260 1.0504 0.035 Uiso 1 1 calc R . .
C6 C 0.5782(2) 0.39172(12) 0.7168(6) 0.0333(5) Uani 1 1 d . . .
H6A H 0.5495 0.4399 0.8115 0.040 Uiso 1 1 calc R . .
H6B H 0.6244 0.4065 0.5433 0.040 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0268(7) 0.0240(6) 0.0440(10) 0.0068(6) -0.0006(7) -0.0014(5)
O2 0.0336(8) 0.0380(9) 0.0471(10) 0.0153(8) -0.0032(8) -0.0102(6)
O3 0.0405(8) 0.0313(7) 0.0395(10) 0.0083(6) 0.0128(7) 0.0058(6)
O4 0.0325(7) 0.0209(6) 0.0503(10) -0.0020(6) 0.0143(8) -0.0019(6)
O5 0.0279(7) 0.0314(7) 0.0708(14) -0.0016(8) -0.0051(9) -0.0013(6)
N1 0.0274(8) 0.0266(8) 0.0478(13) 0.0046(7) -0.0052(9) -0.0032(6)
C1 0.0262(9) 0.0221(8) 0.0380(13) 0.0010(7) -0.0019(9) -0.0036(7)
C2 0.0256(9) 0.0248(8) 0.0343(12) 0.0047(8) -0.0006(8) -0.0003(8)
C3 0.0294(9) 0.0198(8) 0.0368(12) -0.0016(7) 0.0029(9) 0.0013(7)
C4 0.0269(9) 0.0220(9) 0.0405(13) 0.0001(9) 0.0044(9) 0.0018(7)
C5 0.0234(8) 0.0246(9) 0.0407(13) 0.0005(8) 0.0078(9) -0.0004(7)
C6 0.0263(9) 0.0267(9) 0.0470(14) 0.0007(9) 0.0038(9) -0.0003(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100682.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100682.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100682
loop_
_publ_author_name
'Imai, Tokiko'
'Yoshihiro, Yokoyama'
'Sekine, Akiko'
'Uekusa, Hidediro'
'Ohashi, Yuji'
_publ_section_title
;
The Structure of 2-Amino-2-deoxyascorbic acid and
2-Amino-2-deoxyerythorbic acid
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x65
_journal_page_last x66
_journal_paper_doi 10.2116/analscix.19.x65
_journal_volume 19
_journal_year 2003
_chemical_absolute_configuration syn
_chemical_formula_sum 'C6 H9 N O5'
_chemical_formula_weight 175.14
_chemical_name_common 'Erythroscorbamic acid'
_space_group_IT_number 19
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.3338(13)
_cell_length_b 10.294(2)
_cell_length_c 8.029(2)
_cell_measurement_reflns_used 2689
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 27.52
_cell_measurement_theta_min 3.14
_cell_volume 688.8(2)
_diffrn_ambient_temperature 296(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID Imaging Plate'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71070
_diffrn_reflns_av_R_equivalents 0.0442
_diffrn_reflns_av_sigmaI/netI 0.0347
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 2689
_diffrn_reflns_theta_full 27.52
_diffrn_reflns_theta_max 27.52
_diffrn_reflns_theta_min 3.14
_exptl_absorpt_coefficient_mu 0.149
_exptl_absorpt_correction_type none
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.689
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'transparent prism'
_exptl_crystal_F_000 368
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.40
_refine_diff_density_max 0.248
_refine_diff_density_min -0.297
_refine_diff_density_rms 0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.1(17)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.113
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 112
_refine_ls_number_reflns 1431
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.113
_refine_ls_R_factor_all 0.0455
_refine_ls_R_factor_gt 0.0439
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+0.4232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1249
_refine_ls_wR_factor_ref 0.1262
_reflns_number_gt 1386
_reflns_number_total 1431
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M P212121
_cod_database_code 1100682
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5698(3) 0.29433(16) 0.8493(2) 0.0270(4) Uani 1 1 d . . .
O2 O 0.4829(3) 0.35523(16) 1.1042(2) 0.0308(4) Uani 1 1 d . . .
O3 O 0.6725(2) -0.04222(16) 0.8904(2) 0.0261(4) Uani 1 1 d . . .
O4 O 0.4888(3) 0.23578(16) 0.5117(2) 0.0264(4) Uani 1 1 d . . .
H4 H 0.4369 0.2979 0.5461 0.040 Uiso 1 1 calc R . .
O5 O 0.2168(3) 0.0738(2) 0.5883(3) 0.0364(5) Uani 1 1 d . . .
H5 H 0.1712 0.1383 0.5513 0.055 Uiso 1 1 calc R . .
N1 N 0.5466(3) 0.08533(19) 1.2149(2) 0.0226(4) Uani 1 1 d . . .
H1A H 0.4788 0.0187 1.2088 0.034 Uiso 1 1 calc R . .
H1B H 0.5056 0.1464 1.2807 0.034 Uiso 1 1 calc R . .
H1C H 0.6398 0.0583 1.2565 0.034 Uiso 1 1 calc R . .
C1 C 0.5350(3) 0.2701(2) 1.0140(3) 0.0232(5) Uani 1 1 d . . .
C2 C 0.5721(3) 0.1383(2) 1.0502(3) 0.0229(5) Uani 1 1 d . . .
C3 C 0.6269(3) 0.0741(2) 0.9122(3) 0.0202(5) Uani 1 1 d . . .
C4 C 0.6179(3) 0.1731(2) 0.7715(3) 0.0217(5) Uani 1 1 d . . .
H4A H 0.7239 0.1832 0.7203 0.026 Uiso 1 1 calc R . .
C5 C 0.4946(3) 0.1366(2) 0.6384(3) 0.0219(5) Uani 1 1 d . . .
H5A H 0.5305 0.0559 0.5855 0.026 Uiso 1 1 calc R . .
C6 C 0.3298(4) 0.1124(3) 0.7116(3) 0.0282(6) Uani 1 1 d . . .
H6A H 0.3375 0.0451 0.7958 0.034 Uiso 1 1 calc R . .
H6B H 0.2922 0.1910 0.7654 0.034 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0469(12) 0.0159(7) 0.0181(7) 0.0005(6) -0.0016(7) -0.0004(7)
O2 0.0428(12) 0.0223(8) 0.0272(9) -0.0054(7) 0.0002(8) 0.0054(8)
O3 0.0338(11) 0.0190(8) 0.0257(8) -0.0022(6) 0.0033(7) 0.0033(6)
O4 0.0403(11) 0.0230(8) 0.0158(7) 0.0022(6) 0.0017(7) 0.0044(7)
O5 0.0356(12) 0.0374(10) 0.0361(10) -0.0003(9) -0.0126(9) -0.0042(8)
N1 0.0307(12) 0.0207(9) 0.0164(8) 0.0020(7) -0.0001(8) -0.0003(8)
C1 0.0318(15) 0.0199(11) 0.0180(10) -0.0004(8) -0.0050(9) -0.0022(9)
C2 0.0336(14) 0.0208(11) 0.0143(9) 0.0010(8) -0.0016(9) -0.0003(9)
C3 0.0251(13) 0.0186(10) 0.0168(9) 0.0006(8) -0.0023(8) -0.0015(8)
C4 0.0276(13) 0.0204(10) 0.0171(9) 0.0007(8) 0.0021(9) -0.0005(9)
C5 0.0312(13) 0.0190(10) 0.0153(9) 0.0000(8) 0.0013(9) 0.0023(9)
C6 0.0288(15) 0.0320(13) 0.0239(11) 0.0004(10) -0.0049(10) -0.0050(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C4 108.39(17) . . ?
C5 O4 H4 109.5 . . ?
C6 O5 H5 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
O2 C1 O1 121.1(2) . . ?
O2 C1 C2 130.0(2) . . ?
O1 C1 C2 108.88(19) . . ?
C3 C2 C1 111.56(19) . . ?
C3 C2 N1 127.4(2) . . ?
C1 C2 N1 121.0(2) . . ?
O3 C3 C2 131.8(2) . . ?
O3 C3 C4 123.0(2) . . ?
C2 C3 C4 105.16(19) . . ?
O1 C4 C3 105.64(18) . . ?
O1 C4 C5 109.04(19) . . ?
C3 C4 C5 112.78(19) . . ?
O1 C4 H4A 109.8 . . ?
C3 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
O4 C5 C6 111.1(2) . . ?
O4 C5 C4 109.97(19) . . ?
C6 C5 C4 112.21(18) . . ?
O4 C5 H5A 107.8 . . ?
C6 C5 H5A 107.8 . . ?
C4 C5 H5A 107.8 . . ?
O5 C6 C5 112.1(2) . . ?
O5 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
O5 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.377(3) . ?
O1 C4 1.452(3) . ?
O2 C1 1.217(3) . ?
O3 C3 1.269(3) . ?
O4 C5 1.441(2) . ?
O4 H4 0.8200 . ?
O5 C6 1.423(3) . ?
O5 H5 0.8200 . ?
N1 C2 1.446(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C2 1.422(3) . ?
C2 C3 1.368(3) . ?
C3 C4 1.522(3) . ?
C4 C5 1.530(3) . ?
C4 H4A 0.9800 . ?
C5 C6 1.514(4) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O3 0.82 1.95 2.765(3) 173.4 4_656
O5 H5 O4 0.82 2.06 2.845(3) 159.9 3_456
N1 H1A O5 0.89 2.12 2.922(3) 149.2 2
N1 H1A O2 0.89 2.28 2.789(3) 116.4 4_647
N1 H1B O4 0.89 2.08 2.883(3) 150.5 1_556
N1 H1C O3 0.89 1.91 2.768(3) 162.8 2_655
|
1100683.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-28 23:09:42 +0300 (Mon, 28 Mar 2016) $
#$Revision: 180569 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100683.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100683
loop_
_publ_author_name
'Caradoc-Davies, Paula L.'
'Gregory, Duncan H.'
'Hanton, Lyall R.'
'Turnbull, Julia M.'
_publ_section_title
;
Probing copper halide supramolecular arrays of a ditopic ligand with
complexes of a monotopic analogue
;
_journal_coden_ASTM JCSDAA
_journal_issue 8
_journal_name_full
;
Journal of the Chemical Society, Dalton Transactions
;
_journal_page_first 1574
_journal_page_last 1580
_journal_paper_doi 10.1039/b111176k
_journal_year 2002
_chemical_formula_sum 'C22 H24 Cl4 Cu2 N6 S2'
_chemical_formula_weight 705.47
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 86.02(3)
_cell_angle_beta 77.61(3)
_cell_angle_gamma 71.18(3)
_cell_formula_units_Z 1
_cell_length_a 7.735(2)
_cell_length_b 7.989(2)
_cell_length_c 11.949(2)
_cell_measurement_reflns_used 1381
_cell_measurement_temperature 153(2)
_cell_measurement_theta_max 25.96
_cell_measurement_theta_min 2.84
_cell_volume 682.6(3)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SHELXTL'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'Bruker SHELXTL'
_diffrn_ambient_temperature 153(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.515
_diffrn_measured_fraction_theta_max 0.515
_diffrn_measurement_device_type ?
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0533
_diffrn_reflns_av_sigmaI/netI 0.1115
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -2
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 1768
_diffrn_reflns_theta_full 25.96
_diffrn_reflns_theta_max 25.96
_diffrn_reflns_theta_min 2.84
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.127
_exptl_absorpt_correction_T_max 0.9184
_exptl_absorpt_correction_T_min 0.07081
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (sheldrick 1996)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.716
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description plate
_exptl_crystal_F_000 356
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.04
_refine_diff_density_max 2.162
_refine_diff_density_min -1.109
_refine_diff_density_rms 0.290
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.892
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 155
_refine_ls_number_reflns 1381
_refine_ls_number_restraints 36
_refine_ls_restrained_S_all 1.868
_refine_ls_R_factor_all 0.1950
_refine_ls_R_factor_gt 0.1773
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.4681
_refine_ls_wR_factor_ref 0.4752
_reflns_number_gt 1138
_reflns_number_total 1381
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file b111176k.txt
_cod_data_source_block anti-Cu2Cl4L
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M P-1
_cod_database_code 1100683
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.4629(5) 0.8744(4) 0.8577(3) 0.0378(16) Uani 1 1 d . . .
Cl1 Cl 0.7619(10) 0.8407(10) 0.7708(7) 0.046(3) Uani 1 1 d . . .
Cl2 Cl 0.5298(10) 0.7443(9) 1.0246(7) 0.044(3) Uani 1 1 d . . .
S1 S 0.3665(10) 0.6300(9) 0.7826(6) 0.038(3) Uani 1 1 d . . .
N1 N 0.380(3) 1.002(3) 0.724(2) 0.045(8) Uani 1 1 d . . .
N2 N 0.183(3) 0.953(3) 0.939(2) 0.037(8) Uani 1 1 d . . .
C1 C 0.407(4) 1.164(3) 0.693(2) 0.036(6) Uani 1 1 d U . .
H1 H 0.4679 1.2107 0.7363 0.043 Uiso 1 1 calc R . .
C2 C 0.344(4) 1.259(4) 0.598(3) 0.042(7) Uani 1 1 d U . .
H2 H 0.3576 1.3701 0.5834 0.051 Uiso 1 1 calc R . .
C3 C 0.267(4) 1.198(4) 0.528(3) 0.045(10) Uani 1 1 d . . .
H3 H 0.2318 1.2628 0.4638 0.054 Uiso 1 1 calc R . .
C4 C 0.239(4) 1.034(4) 0.553(3) 0.046(11) Uani 1 1 d . . .
H4 H 0.1853 0.9864 0.5065 0.056 Uiso 1 1 calc R . .
C5 C 0.295(4) 0.944(4) 0.650(3) 0.036(6) Uani 1 1 d U . .
C6 C 0.264(4) 0.769(4) 0.673(3) 0.043(7) Uani 1 1 d U . .
H6A H 0.3101 0.7025 0.6024 0.051 Uiso 1 1 calc R . .
H6B H 0.1307 0.7899 0.6936 0.051 Uiso 1 1 calc R . .
C7 C 0.182(5) 0.652(4) 0.900(2) 0.066(14) Uani 1 1 d . . .
H7A H 0.0875 0.6138 0.8766 0.079 Uiso 1 1 calc R . .
H7B H 0.2272 0.5721 0.9596 0.079 Uiso 1 1 calc R . .
C8 C 0.088(3) 0.838(3) 0.951(2) 0.017(5) Uani 1 1 d U . .
C9 C 0.104(2) 1.108(2) 0.9960(18) 0.036(9) Uani 1 1 d . . .
H9 H 0.1760 1.1800 1.0004 0.043 Uiso 1 1 calc R . .
N3 N 0.245(2) 0.608(2) 0.4165(18) 0.086(17) Uani 1 1 d R . .
C11 C 0.200(2) 0.637(2) 0.3389(18) 0.08(2) Uani 1 1 d R . .
C10 C 0.143(2) 0.662(2) 0.2295(18) 0.072(11) Uani 1 1 d RU . .
H10A H 0.1997 0.5545 0.1861 0.108 Uiso 1 1 calc R . .
H10B H 0.1824 0.7554 0.1880 0.108 Uiso 1 1 calc R . .
H10C H 0.0100 0.6930 0.2418 0.108 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.039(2) 0.024(2) 0.041(3) 0.0053(18) -0.001(2) -0.0019(15)
Cl1 0.040(4) 0.055(5) 0.036(6) 0.009(4) -0.008(4) -0.005(3)
Cl2 0.047(4) 0.037(4) 0.042(5) 0.011(4) -0.007(4) -0.009(3)
S1 0.044(4) 0.029(4) 0.032(5) -0.004(4) -0.003(4) -0.002(3)
N1 0.054(14) 0.027(13) 0.036(18) 0.013(13) -0.001(15) 0.003(11)
N2 0.022(11) 0.031(13) 0.048(17) 0.007(13) 0.002(13) -0.004(10)
C1 0.037(7) 0.034(7) 0.034(8) 0.001(5) -0.008(5) -0.009(5)
C2 0.043(8) 0.042(8) 0.043(9) 0.000(5) -0.011(5) -0.012(5)
C3 0.043(16) 0.041(19) 0.04(2) 0.015(16) -0.009(18) -0.001(14)
C4 0.06(2) 0.038(17) 0.04(2) -0.007(17) 0.000(19) -0.017(16)
C5 0.038(7) 0.035(7) 0.035(8) 0.001(5) -0.008(5) -0.010(5)
C6 0.044(8) 0.043(8) 0.043(8) 0.001(5) -0.009(5) -0.014(5)
C7 0.09(2) 0.06(2) 0.05(2) -0.028(18) 0.05(2) -0.047(19)
C8 0.017(6) 0.014(6) 0.018(7) 0.000(4) -0.005(4) -0.002(5)
C9 0.049(16) 0.035(17) 0.025(18) -0.005(15) -0.007(16) -0.015(14)
N3 0.09(3) 0.06(2) 0.11(4) -0.01(2) -0.02(3) -0.03(2)
C11 0.06(2) 0.04(2) 0.13(5) -0.02(3) 0.04(3) -0.015(18)
C10 0.071(13) 0.073(13) 0.067(14) 0.011(9) -0.009(9) -0.021(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N2 86.6(9) . . ?
N1 Cu1 Cl1 89.7(7) . . ?
N2 Cu1 Cl1 169.7(6) . . ?
N1 Cu1 Cl2 173.7(6) . . ?
N2 Cu1 Cl2 87.6(7) . . ?
Cl1 Cu1 Cl2 95.6(3) . . ?
N1 Cu1 S1 83.1(7) . . ?
N2 Cu1 S1 81.3(6) . . ?
Cl1 Cu1 S1 107.8(3) . . ?
Cl2 Cu1 S1 98.3(3) . . ?
C7 S1 C6 104.8(17) . . ?
C7 S1 Cu1 92.3(9) . . ?
C6 S1 Cu1 93.6(8) . . ?
C1 N1 C5 114(3) . . ?
C1 N1 Cu1 121(2) . . ?
C5 N1 Cu1 125(2) . . ?
C8 N2 C9 119.0(16) . . ?
C8 N2 Cu1 119.2(15) . . ?
C9 N2 Cu1 121.0(12) . . ?
N1 C1 C2 121(3) . . ?
C3 C2 C1 124(3) . . ?
C2 C3 C4 117(3) . . ?
C3 C4 C5 119(3) . . ?
N1 C5 C4 125(2) . . ?
N1 C5 C6 118(3) . . ?
C4 C5 C6 117(2) . . ?
C5 C6 S1 119(2) . . ?
C8 C7 S1 115.8(15) . . ?
N2 C8 C9 119.5(17) . 2_577 ?
N2 C8 C7 120.6(18) . . ?
C9 C8 C7 119.8(16) 2_577 . ?
N2 C9 C8 120.5(14) . 2_577 ?
N3 C11 C10 175.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.94(3) . ?
Cu1 N2 2.082(17) . ?
Cu1 Cl1 2.260(7) . ?
Cu1 Cl2 2.266(10) . ?
Cu1 S1 2.577(7) . ?
S1 C7 1.75(2) . ?
S1 C6 1.80(4) . ?
N1 C1 1.39(3) . ?
N1 C5 1.39(4) . ?
N2 C8 1.34(2) . ?
N2 C9 1.35(2) . ?
C1 C2 1.41(4) . ?
C2 C3 1.32(4) . ?
C3 C4 1.40(3) . ?
C4 C5 1.40(5) . ?
C5 C6 1.49(3) . ?
C7 C8 1.53(3) . ?
C8 C9 1.42(2) 2_577 ?
C9 C8 1.42(2) 2_577 ?
N3 C11 1.0435 . ?
C11 C10 1.4487 . ?
|
1100684.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100684.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100684
loop_
_publ_author_name
'Kitamura, Chitoshi'
'Fujimoto, Jun'
'Ouchi, Mikio'
'Yoneda, Akio'
_publ_section_title
;
Crystal Structure of 1,4-Dimethoxyanthracene
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x69
_journal_page_last x70
_journal_paper_doi 10.2116/analscix.19.x69
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C16 H14 O2'
_chemical_formula_sum 'C16 H14 O2'
_chemical_formula_weight 238.29
_chemical_melting_point 407
_space_group_IT_number 61
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2ac 2ab'
_symmetry_space_group_name_H-M 'P b c a'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 6.3805(5)
_cell_length_b 15.624(1)
_cell_length_c 24.778(2)
_cell_measurement_reflns_used 5975
_cell_measurement_temperature 296.2
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.1
_cell_volume 2470.0(4)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9816
_diffrn_measured_fraction_theta_max 0.9816
_diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.7107
_diffrn_reflns_av_R_equivalents 0.101
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 19675
_diffrn_reflns_theta_full 27.48
_diffrn_reflns_theta_max 27.48
_exptl_absorpt_coefficient_mu 0.083
_exptl_absorpt_correction_type none
_exptl_crystal_colour Yellow
_exptl_crystal_density_diffrn 1.281
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Needle
_exptl_crystal_preparation chloroform-methanol
_exptl_crystal_size_max 1.000
_exptl_crystal_size_mid 0.250
_exptl_crystal_size_min 0.150
_refine_diff_density_max 0.17
_refine_diff_density_min -0.18
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.772
_refine_ls_hydrogen_treatment refall
_refine_ls_number_parameters 219
_refine_ls_number_reflns 2779
_refine_ls_R_factor_gt 0.0711
_refine_ls_shift/su_max 0.0600
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_ref 0.1573
_reflns_number_gt 2184
_reflns_number_total 2779
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_sg_symbol_H-M 'P 21/b 21/c 21/a'
_cod_original_formula_sum 'C16 H14 O2 '
_cod_database_code 1100684
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,-z
-x,1/2+y,1/2-z
1/2-x,-y,1/2+z
-x,-y,-z
1/2-x,1/2+y,z
x,1/2-y,1/2+z
1/2+x,y,1/2-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O(1) O 0.2775(2) 0.33282(9) 0.69050(5) 0.0605(4) Uani 1.00 d . . .
O(2) O 0.3990(2) 0.11646(9) 0.51563(5) 0.0545(4) Uani 1.00 d . . .
C(1) C 0.3171(3) 0.2849(1) 0.64496(7) 0.0462(5) Uani 1.00 d . . .
C(2) C 0.4815(3) 0.2964(1) 0.61099(8) 0.0518(5) Uani 1.00 d . . .
C(3) C 0.5119(3) 0.2410(1) 0.56605(8) 0.0501(5) Uani 1.00 d . . .
C(4) C 0.3796(2) 0.1749(1) 0.55665(7) 0.0438(5) Uani 1.00 d . . .
C(5) C 0.2012(2) 0.1610(1) 0.59091(7) 0.0392(4) Uani 1.00 d . . .
C(6) C 0.0590(3) 0.0950(1) 0.58218(7) 0.0423(5) Uani 1.00 d . . .
C(7) C -0.1138(2) 0.0817(1) 0.61602(7) 0.0409(4) Uani 1.00 d . . .
C(8) C -0.2599(3) 0.0140(1) 0.60752(8) 0.0481(5) Uani 1.00 d . . .
C(9) C -0.4256(3) 0.0029(1) 0.64155(8) 0.0554(6) Uani 1.00 d . . .
C(10) C -0.4567(3) 0.0590(1) 0.68557(8) 0.0563(6) Uani 1.00 d . . .
C(11) C -0.3219(3) 0.1244(1) 0.69510(8) 0.0507(5) Uani 1.00 d . . .
C(12) C -0.1454(2) 0.1382(1) 0.66076(7) 0.0414(4) Uani 1.00 d . . .
C(13) C -0.0044(3) 0.2053(1) 0.66940(7) 0.0441(5) Uani 1.00 d . . .
C(14) C 0.1686(2) 0.2177(1) 0.63580(7) 0.0401(4) Uani 1.00 d . . .
C(15) C 0.4282(4) 0.3951(2) 0.7050(1) 0.0732(8) Uani 1.00 d . . .
C(16) C 0.5813(3) 0.1226(2) 0.48236(9) 0.0595(6) Uani 1.00 d . . .
H(1) H 0.584(3) 0.343(1) 0.6176(8) 0.057(5) Uiso 1.00 calc . . .
H(2) H 0.634(3) 0.252(1) 0.5430(8) 0.062(6) Uiso 1.00 calc . . .
H(3) H 0.082(2) 0.056(1) 0.5515(7) 0.045(5) Uiso 1.00 calc . . .
H(4) H -0.236(3) -0.024(1) 0.5763(9) 0.061(5) Uiso 1.00 calc . . .
H(5) H -0.532(3) -0.044(1) 0.6365(7) 0.059(5) Uiso 1.00 calc . . .
H(6) H -0.579(3) 0.050(1) 0.7096(8) 0.068(6) Uiso 1.00 calc . . .
H(7) H -0.342(3) 0.163(1) 0.7262(9) 0.070(6) Uiso 1.00 calc . . .
H(8) H -0.031(3) 0.242(1) 0.7003(8) 0.057(6) Uiso 1.00 calc . . .
H(9) H 0.570(4) 0.369(2) 0.710(1) 0.091(8) Uiso 1.00 calc . . .
H(10) H 0.380(3) 0.418(2) 0.739(1) 0.085(8) Uiso 1.00 calc . . .
H(11) H 0.433(4) 0.440(2) 0.678(1) 0.086(8) Uiso 1.00 calc . . .
H(12) H 0.713(3) 0.123(1) 0.5043(8) 0.066(6) Uiso 1.00 calc . . .
H(13) H 0.560(3) 0.173(2) 0.460(1) 0.077(7) Uiso 1.00 calc . . .
H(14) H 0.584(4) 0.065(2) 0.460(1) 0.101(8) Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
|
1100685.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100685.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100685
loop_
_publ_author_name
'Ranjbar, Maryam'
'Aghabozorg, Hossein'
'Moghimi, Abolghasem'
_publ_section_title
;
Crystal Structure of a Binuclear Seven-Coordinate Tin(IV) Complex
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x71
_journal_page_last x72
_journal_paper_doi 10.2116/analscix.19.x71
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C7 H7 N1 O7 Sn1 2(H2 O)'
_chemical_formula_sum 'C7 H11 N O9 Sn'
_chemical_formula_weight 371.86
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 85.42(3)
_cell_angle_beta 82.92(3)
_cell_angle_gamma 74.83(3)
_cell_formula_units_Z 2
_cell_length_a 6.5534(13)
_cell_length_b 7.4907(15)
_cell_length_c 12.030(2)
_cell_measurement_reflns_used 24
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 15.0
_cell_measurement_theta_min 10.0
_cell_volume 564.9(2)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Siemens P3/PC'
_diffrn_measurement_method '\q/2\q scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0288
_diffrn_reflns_av_sigmaI/netI 0.0337
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 3258
_diffrn_reflns_theta_full 29.06
_diffrn_reflns_theta_max 29.06
_diffrn_reflns_theta_min 2.82
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 2.305
_exptl_absorpt_correction_T_max 0.49
_exptl_absorpt_correction_T_min 0.25
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'North et al. (1968)'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 2.186
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 364
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.05
_exptl_crystal_size_min 0.03
_refine_diff_density_max 3.248
_refine_diff_density_min -2.550
_refine_diff_density_rms 0.292
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 163
_refine_ls_number_reflns 3008
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.026
_refine_ls_R_factor_all 0.0608
_refine_ls_R_factor_gt 0.0528
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1371
_refine_ls_wR_factor_ref 0.1400
_reflns_number_gt 2641
_reflns_number_total 3008
_reflns_threshold_expression I>2\s(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_atom_sites_solution_hydrogens' value 'difmap and geom' was changed
to 'mixed'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_database_code 1100685
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 1.00563(4) 0.43188(4) -0.13313(2) 0.02346(14) Uani 1 1 d . . .
O1 O 1.3169(6) 0.2358(6) -0.1831(3) 0.0313(8) Uani 1 1 d . . .
O2 O 1.5301(6) 0.0669(7) -0.3163(4) 0.0444(11) Uani 1 1 d . . .
O3 O 0.6890(6) 0.5563(6) -0.1965(3) 0.0351(9) Uani 1 1 d . . .
O4 O 0.4794(6) 0.5761(7) -0.3322(4) 0.0402(10) Uani 1 1 d . . .
O5 O 0.9080(7) 0.2016(6) -0.0751(4) 0.0381(9) Uani 1 1 d . . .
H5 H 0.7893 0.1923 -0.0323 0.050 Uiso 1 1 d . . .
O6 O 0.8198(6) 0.5851(5) -0.0029(3) 0.0312(8) Uani 1 1 d . . .
H6 H 0.7020 0.6615 -0.0183 0.050 Uiso 1 1 d . . .
C1 C 1.3602(8) 0.1711(7) -0.2810(4) 0.0275(9) Uani 1 1 d . . .
C2 C 1.1844(7) 0.2289(7) -0.3549(4) 0.0245(9) Uani 1 1 d . . .
C3 C 1.1918(9) 0.1709(8) -0.4627(5) 0.0343(11) Uani 1 1 d . . .
H3A H 1.3156 0.0951 -0.4970 0.041 Uiso 1 1 calc R . .
C4 C 1.0109(10) 0.2287(9) -0.5178(5) 0.0378(12) Uani 1 1 d . . .
H4A H 1.0124 0.1911 -0.5898 0.045 Uiso 1 1 calc R . .
C5 C 0.8278(9) 0.3420(8) -0.4665(4) 0.0303(10) Uani 1 1 d . . .
H5A H 0.7051 0.3810 -0.5027 0.036 Uiso 1 1 calc R . .
C6 C 0.8329(7) 0.3958(7) -0.3591(4) 0.0237(8) Uani 1 1 d . . .
C7 C 0.6492(7) 0.5198(7) -0.2923(4) 0.0272(9) Uani 1 1 d . . .
N1 N 1.0062(6) 0.3394(5) -0.3073(3) 0.0213(7) Uani 1 1 d . . .
O1W O 1.1001(7) 0.6501(5) -0.2047(4) 0.0353(8) Uani 1 1 d . . .
H1WA H 1.2276 0.6718 -0.2270 0.050 Uiso 1 1 d . . .
H1WB H 1.0520 0.7746 -0.2121 0.050 Uiso 1 1 d . . .
O2W O 0.4300(9) 0.8390(7) -0.0643(5) 0.0543(12) Uani 1 1 d . . .
H2WB H 0.3995 0.9564 -0.0923 0.050 Uiso 1 1 d . . .
H2WA H 0.5149 0.7475 -0.1074 0.050 Uiso 1 1 d . . .
O3W O 0.1141(8) 0.0184(6) 0.2124(5) 0.0509(12) Uani 1 1 d . . .
H3WA H 0.2351 0.0103 0.2422 0.050 Uiso 1 1 d . . .
H3WB H 0.1060 -0.0621 0.1629 0.050 Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.02317(19) 0.0306(2) 0.01369(19) -0.01007(12) -0.00131(11) 0.00067(12)
O1 0.0271(17) 0.042(2) 0.0190(17) -0.0121(15) -0.0036(13) 0.0046(14)
O2 0.031(2) 0.056(3) 0.036(2) -0.021(2) -0.0045(17) 0.0141(18)
O3 0.0254(16) 0.054(2) 0.0197(17) -0.0167(16) -0.0028(13) 0.0053(15)
O4 0.0256(18) 0.064(3) 0.025(2) -0.0120(18) -0.0056(14) 0.0028(17)
O5 0.044(2) 0.040(2) 0.029(2) -0.0098(16) 0.0011(17) -0.0087(17)
O6 0.0246(16) 0.044(2) 0.0175(17) -0.0185(15) -0.0037(13) 0.0099(14)
C1 0.027(2) 0.032(2) 0.018(2) -0.0101(17) -0.0003(17) 0.0042(18)
C2 0.025(2) 0.028(2) 0.016(2) -0.0088(17) -0.0003(16) 0.0018(17)
C3 0.036(3) 0.043(3) 0.020(2) -0.014(2) -0.001(2) 0.000(2)
C4 0.046(3) 0.053(3) 0.013(2) -0.014(2) -0.005(2) -0.006(3)
C5 0.033(2) 0.043(3) 0.015(2) -0.0071(19) -0.0059(18) -0.005(2)
C6 0.025(2) 0.031(2) 0.0124(19) -0.0065(16) -0.0007(16) -0.0022(17)
C7 0.021(2) 0.040(3) 0.018(2) -0.0066(19) -0.0024(16) -0.0028(18)
N1 0.0217(17) 0.0237(17) 0.0156(18) -0.0052(14) 0.0006(14) -0.0006(14)
O1W 0.0337(19) 0.0306(18) 0.038(2) -0.0060(16) 0.0051(16) -0.0038(15)
O2W 0.058(3) 0.048(3) 0.045(3) -0.005(2) 0.009(2) 0.002(2)
O3W 0.052(3) 0.039(2) 0.061(3) -0.012(2) -0.021(2) 0.000(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Sn1 O5 174.52(16) . . ?
O1W Sn1 O6 92.57(17) . . ?
O5 Sn1 O6 91.75(17) . . ?
O1W Sn1 O6 92.94(18) . 2_765 ?
O5 Sn1 O6 91.72(18) . 2_765 ?
O6 Sn1 O6 69.56(16) . 2_765 ?
O1W Sn1 O1 92.91(16) . . ?
O5 Sn1 O1 85.48(17) . . ?
O6 Sn1 O1 144.74(14) . . ?
O6 Sn1 O1 75.39(14) 2_765 . ?
O1W Sn1 O3 87.99(18) . . ?
O5 Sn1 O3 89.93(18) . . ?
O6 Sn1 O3 74.57(14) . . ?
O6 Sn1 O3 144.13(14) 2_765 . ?
O1 Sn1 O3 140.42(14) . . ?
O1W Sn1 N1 87.76(16) . . ?
O5 Sn1 N1 86.76(16) . . ?
O6 Sn1 N1 144.39(14) . . ?
O6 Sn1 N1 146.01(14) 2_765 . ?
O1 Sn1 N1 70.65(14) . . ?
O3 Sn1 N1 69.85(14) . . ?
C1 O1 Sn1 121.2(3) . . ?
C7 O3 Sn1 121.6(3) . . ?
Sn1 O6 Sn1 110.44(16) . 2_765 ?
O2 C1 O1 125.2(5) . . ?
O2 C1 C2 119.4(5) . . ?
O1 C1 C2 115.3(4) . . ?
N1 C2 C3 120.1(5) . . ?
N1 C2 C1 114.2(4) . . ?
C3 C2 C1 125.6(4) . . ?
C4 C3 C2 118.5(5) . . ?
C3 C4 C5 120.4(5) . . ?
C4 C5 C6 117.9(5) . . ?
N1 C6 C5 121.2(5) . . ?
N1 C6 C7 114.1(4) . . ?
C5 C6 C7 124.7(4) . . ?
O4 C7 O3 126.2(5) . . ?
O4 C7 C6 119.1(5) . . ?
O3 C7 C6 114.7(4) . . ?
C6 N1 C2 121.9(4) . . ?
C6 N1 Sn1 119.6(3) . . ?
C2 N1 Sn1 118.4(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O1W 1.992(4) . ?
Sn1 O5 2.036(4) . ?
Sn1 O6 2.084(3) . ?
Sn1 O6 2.086(4) 2_765 ?
Sn1 O1 2.225(4) . ?
Sn1 O3 2.241(4) . ?
Sn1 N1 2.258(4) . ?
O1 C1 1.281(6) . ?
O2 C1 1.229(6) . ?
O3 C7 1.277(6) . ?
O4 C7 1.226(6) . ?
O6 Sn1 2.086(4) 2_765 ?
C1 C2 1.495(7) . ?
C2 N1 1.335(6) . ?
C2 C3 1.391(7) . ?
C3 C4 1.382(8) . ?
C4 C5 1.381(8) . ?
C5 C6 1.391(6) . ?
C6 N1 1.319(6) . ?
C6 C7 1.501(6) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1W Sn1 O1 C1 -83.0(4) . . . . ?
O5 Sn1 O1 C1 91.8(4) . . . . ?
O6 Sn1 O1 C1 178.4(4) . . . . ?
O6 Sn1 O1 C1 -175.3(5) 2_765 . . . ?
O3 Sn1 O1 C1 7.4(6) . . . . ?
N1 Sn1 O1 C1 3.6(4) . . . . ?
O1W Sn1 O3 C7 90.3(5) . . . . ?
O5 Sn1 O3 C7 -84.6(5) . . . . ?
O6 Sn1 O3 C7 -176.5(5) . . . . ?
O6 Sn1 O3 C7 -177.5(4) 2_765 . . . ?
O1 Sn1 O3 C7 -1.8(6) . . . . ?
N1 Sn1 O3 C7 2.0(4) . . . . ?
O1W Sn1 O6 Sn1 -92.2(2) . . . 2_765 ?
O5 Sn1 O6 Sn1 91.2(2) . . . 2_765 ?
O6 Sn1 O6 Sn1 0.0 2_765 . . 2_765 ?
O1 Sn1 O6 Sn1 6.5(4) . . . 2_765 ?
O3 Sn1 O6 Sn1 -179.4(2) . . . 2_765 ?
N1 Sn1 O6 Sn1 178.07(17) . . . 2_765 ?
Sn1 O1 C1 O2 177.7(5) . . . . ?
Sn1 O1 C1 C2 -3.0(7) . . . . ?
O2 C1 C2 N1 178.8(5) . . . . ?
O1 C1 C2 N1 -0.4(7) . . . . ?
O2 C1 C2 C3 1.8(9) . . . . ?
O1 C1 C2 C3 -177.5(5) . . . . ?
N1 C2 C3 C4 -0.7(9) . . . . ?
C1 C2 C3 C4 176.2(5) . . . . ?
C2 C3 C4 C5 0.3(9) . . . . ?
C3 C4 C5 C6 0.4(9) . . . . ?
C4 C5 C6 N1 -0.5(8) . . . . ?
C4 C5 C6 C7 179.3(5) . . . . ?
Sn1 O3 C7 O4 177.4(5) . . . . ?
Sn1 O3 C7 C6 -2.6(7) . . . . ?
N1 C6 C7 O4 -178.3(5) . . . . ?
C5 C6 C7 O4 1.8(8) . . . . ?
N1 C6 C7 O3 1.7(7) . . . . ?
C5 C6 C7 O3 -178.2(5) . . . . ?
C5 C6 N1 C2 0.1(7) . . . . ?
C7 C6 N1 C2 -179.7(4) . . . . ?
C5 C6 N1 Sn1 179.8(4) . . . . ?
C7 C6 N1 Sn1 0.0(6) . . . . ?
C3 C2 N1 C6 0.5(8) . . . . ?
C1 C2 N1 C6 -176.7(4) . . . . ?
C3 C2 N1 Sn1 -179.2(4) . . . . ?
C1 C2 N1 Sn1 3.6(6) . . . . ?
O1W Sn1 N1 C6 -89.6(4) . . . . ?
O5 Sn1 N1 C6 90.2(4) . . . . ?
O6 Sn1 N1 C6 1.7(5) . . . . ?
O6 Sn1 N1 C6 178.5(3) 2_765 . . . ?
O1 Sn1 N1 C6 176.6(4) . . . . ?
O3 Sn1 N1 C6 -0.9(3) . . . . ?
O1W Sn1 N1 C2 90.1(4) . . . . ?
O5 Sn1 N1 C2 -90.1(4) . . . . ?
O6 Sn1 N1 C2 -178.6(3) . . . . ?
O6 Sn1 N1 C2 -1.8(5) 2_765 . . . ?
O1 Sn1 N1 C2 -3.7(3) . . . . ?
O3 Sn1 N1 C2 178.8(4) . . . . ?
|
1100686.cif | #------------------------------------------------------------------------------
#$Date: 2024-09-10 15:03:03 +0300 (Tue, 10 Sep 2024) $
#$Revision: 294696 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100686.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100686
loop_
_publ_author_name
'Hwang, Long-Chih'
'Wu, Rang-Rong'
'Jane, Shin-Yi'
'Lee, Gene-Hsiang'
_publ_section_title
;
Crystal Structure of 3-Amino-1,2,4-triazine
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x73
_journal_page_last x74
_journal_paper_doi 10.2116/analscix.19.x73
_journal_volume 19
_journal_year 2003
_chemical_formula_sum 'C3 H4 N4'
_chemical_formula_weight 96.10
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 101.545(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 5.20950(10)
_cell_length_b 14.1845(5)
_cell_length_c 6.0638(2)
_cell_measurement_reflns_used 1716
_cell_measurement_temperature 295(2)
_cell_volume 439.01(2)
_diffrn_ambient_temperature 295(2)
_diffrn_measurement_device 'Siemens SMART CCD'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0484
_diffrn_reflns_av_sigmaI/netI 0.0353
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 5927
_diffrn_reflns_theta_max 29.51
_diffrn_reflns_theta_min 2.87
_exptl_absorpt_coefficient_mu 0.105
_exptl_absorpt_correction_T_max 0.4804
_exptl_absorpt_correction_T_min 0.4445
_exptl_absorpt_correction_type sadabs
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.454
_exptl_crystal_description plate
_exptl_crystal_F_000 200
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.224
_refine_diff_density_min -0.179
_refine_diff_density_rms 0.038
_refine_ls_extinction_coef 0.0561(139)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_all 1.010
_refine_ls_goodness_of_fit_obs 1.096
_refine_ls_matrix_type full
_refine_ls_number_parameters 65
_refine_ls_number_reflns 1172
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.010
_refine_ls_restrained_S_obs 1.096
_refine_ls_R_factor_all 0.0716
_refine_ls_R_factor_obs 0.0477
_refine_ls_shift/esd_max 0.000
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.0508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.1228
_refine_ls_wR_factor_obs 0.1124
_reflns_number_observed 850
_reflns_number_total 1172
_reflns_observed_criterion >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.0508P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+0.0508P] where P=(Fo^2^+2Fc^2^)/3'.
Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100686
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0373(6) 0.0486(7) 0.0290(6) 0.0000(5) 0.0089(5) -0.0059(5)
N2 0.0461(7) 0.0528(8) 0.0289(7) -0.0022(5) 0.0078(5) -0.0051(6)
N3 0.0375(6) 0.0373(6) 0.0355(6) 0.0026(5) 0.0105(5) -0.0031(5)
N4 0.0446(7) 0.0599(9) 0.0270(6) 0.0001(5) 0.0077(5) -0.0168(6)
C1 0.0316(7) 0.0343(7) 0.0295(7) 0.0034(5) 0.0079(5) 0.0012(5)
C2 0.0455(8) 0.0501(9) 0.0329(7) -0.0061(6) 0.0033(6) -0.0063(7)
C3 0.0357(8) 0.0392(8) 0.0435(8) -0.0018(6) 0.0075(6) -0.0053(6)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.2475(2) 0.57512(8) 0.6820(2) 0.0380(3) Uani 1 d . .
N2 N 0.3881(2) 0.60521(9) 0.8778(2) 0.0425(4) Uani 1 d . .
N3 N 0.5427(2) 0.65253(8) 0.4825(2) 0.0363(3) Uani 1 d . .
N4 N 0.1886(2) 0.56679(9) 0.2986(2) 0.0437(4) Uani 1 d . .
H4A H 0.0511(2) 0.53328(9) 0.2989(2) 0.052 Uiso 1 calc R .
H4B H 0.2345(2) 0.57994(9) 0.1736(2) 0.052 Uiso 1 calc R .
C1 C 0.3303(3) 0.59827(9) 0.4917(2) 0.0316(3) Uani 1 d . .
C2 C 0.6013(3) 0.65556(10) 0.8796(3) 0.0435(4) Uani 1 d . .
H2B H 0.7023(3) 0.67519(10) 1.0161(3) 0.052 Uiso 1 calc R .
C3 C 0.6765(3) 0.67962(10) 0.6789(2) 0.0395(4) Uani 1 d . .
H3B H 0.8262(3) 0.71598(10) 0.6845(2) 0.047 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 C1 118.06(12) . . ?
C2 N2 N1 119.48(12) . . ?
C3 N3 C1 114.73(12) . . ?
N4 C1 N1 117.04(12) . . ?
N4 C1 N3 117.87(12) . . ?
N1 C1 N3 125.08(12) . . ?
N2 C2 C3 120.59(14) . . ?
N3 C3 C2 122.00(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N2 1.334(2) . ?
N1 C1 1.351(2) . ?
N2 C2 1.319(2) . ?
N3 C3 1.312(2) . ?
N3 C1 1.358(2) . ?
N4 C1 1.330(2) . ?
C2 C3 1.394(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 63880
|
1100687.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100687.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100687
_chemical_formula_moiety 'C22 H22 O2 P, I3'
_chemical_formula_sum 'C22 H22 I3 O2 P'
_chemical_formula_weight 730.07
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 89.795(9)
_cell_angle_beta 78.487(9)
_cell_angle_gamma 89.933(9)
_cell_formula_units_Z 4
_cell_length_a 10.935(3)
_cell_length_b 13.921(3)
_cell_length_c 17.152(5)
_cell_measurement_reflns_used 536
_cell_measurement_temperature 273(2)
_cell_measurement_theta_max 23.54
_cell_measurement_theta_min 1.37
_cell_volume 2558.4(11)
_computing_data_collection 'SMART (Bruker, 2000)'
_diffrn_ambient_temperature 273(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'bruker smart apex CCD area detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0201
_diffrn_reflns_av_sigmaI/netI 0.0284
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 19190
_diffrn_reflns_theta_full 25.10
_diffrn_reflns_theta_max 25.10
_diffrn_reflns_theta_min 1.21
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 3.742
_exptl_absorpt_correction_T_max 0.378
_exptl_absorpt_correction_T_min 0.247
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS; Bruker, 2000)'
_exptl_crystal_colour corlorless
_exptl_crystal_density_diffrn 1.895
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 1376
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.26
_refine_diff_density_max 2.130
_refine_diff_density_min -0.976
_refine_diff_density_rms 0.136
_refine_ls_extinction_coef 0.00
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.141
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 506
_refine_ls_number_reflns 9019
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.144
_refine_ls_R_factor_all 0.0772
_refine_ls_R_factor_gt 0.0592
_refine_ls_shift/su_max 0.040
_refine_ls_shift/su_mean 0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+2.4824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1849
_refine_ls_wR_factor_ref 0.1969
_reflns_number_gt 6461
_reflns_number_total 9019
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_Hall -p1
_cod_original_sg_symbol_H-M p-1
_cod_database_code 1100687
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I5 I 0.60686(6) 0.69100(5) 0.21778(4) 0.0854(2) Uani 1 1 d . . .
I2 I 0.89302(5) 0.19091(5) 0.28219(4) 0.0859(3) Uani 1 1 d . . .
I1 I 0.75138(7) 0.27489(6) 0.42948(5) 0.1026(3) Uani 1 1 d . . .
I6 I 0.74846(7) 0.77496(6) 0.07054(5) 0.1025(3) Uani 1 1 d . . .
I3 I 1.02964(7) 0.11514(6) 0.12997(5) 0.1025(3) Uani 1 1 d . . .
I4 I 0.47024(7) 0.61516(6) 0.37013(5) 0.1021(3) Uani 1 1 d . . .
P1 P 0.45501(15) 0.32677(12) 0.22794(9) 0.0420(4) Uani 1 1 d . . .
P2 P 0.95516(15) 0.17316(12) 0.72790(9) 0.0420(4) Uani 1 1 d . . .
O1 O 0.6841(5) 0.3694(5) 0.1070(3) 0.0763(16) Uani 1 1 d . . .
O2 O 0.7937(5) 0.4357(5) 0.1902(4) 0.089(2) Uani 1 1 d . . .
O3 O 1.1845(5) 0.1316(5) 0.6073(3) 0.0779(16) Uani 1 1 d . . .
O4 O 1.2944(5) 0.0646(5) 0.6906(4) 0.091(2) Uani 1 1 d . . .
C1 C 0.995(2) 0.414(2) 0.126(2) 0.39(3) Uani 1 1 d D . .
H1A H 1.0632 0.4315 0.0843 0.590 Uiso 1 1 calc R . .
H1B H 0.9754 0.3471 0.1210 0.590 Uiso 1 1 calc R . .
H1C H 1.0190 0.4232 0.1768 0.590 Uiso 1 1 calc R . .
C2 C 0.8926(12) 0.4692(14) 0.1225(9) 0.170(8) Uani 1 1 d D . .
H2A H 0.8667 0.4600 0.0722 0.204 Uiso 1 1 calc R . .
H2B H 0.9108 0.5367 0.1281 0.204 Uiso 1 1 calc R . .
C3 C 0.6956(7) 0.3923(5) 0.1719(4) 0.0572(17) Uani 1 1 d . . .
C4 C 0.5986(6) 0.3778(5) 0.2460(4) 0.0510(15) Uani 1 1 d . . .
H4A H 0.5803 0.4392 0.2723 0.061 Uiso 1 1 calc R . .
H4B H 0.6321 0.3358 0.2819 0.061 Uiso 1 1 calc R . .
C5 C 0.4808(6) 0.2098(5) 0.1838(4) 0.0477(15) Uani 1 1 d . . .
C6 C 0.5862(8) 0.1564(6) 0.1903(5) 0.067(2) Uani 1 1 d . . .
H6A H 0.6454 0.1825 0.2161 0.080 Uiso 1 1 calc R . .
C7 C 0.6036(9) 0.0663(6) 0.1591(6) 0.079(2) Uani 1 1 d . . .
H7A H 0.6742 0.0314 0.1640 0.095 Uiso 1 1 calc R . .
C8 C 0.5181(9) 0.0272(6) 0.1209(6) 0.077(2) Uani 1 1 d . . .
H8A H 0.5321 -0.0335 0.0983 0.092 Uiso 1 1 calc R . .
C9 C 0.4110(8) 0.0765(6) 0.1153(5) 0.067(2) Uani 1 1 d . . .
H9A H 0.3515 0.0484 0.0907 0.081 Uiso 1 1 calc R . .
C10 C 0.3921(7) 0.1688(5) 0.1469(4) 0.0558(17) Uani 1 1 d . . .
H10A H 0.3202 0.2027 0.1432 0.067 Uiso 1 1 calc R . .
C11 C 0.3511(6) 0.3171(4) 0.3229(4) 0.0447(14) Uani 1 1 d . . .
C12 C 0.3925(7) 0.3240(7) 0.3940(4) 0.071(2) Uani 1 1 d . . .
H12A H 0.4769 0.3333 0.3932 0.085 Uiso 1 1 calc R . .
C13 C 0.3101(9) 0.3172(8) 0.4653(5) 0.082(3) Uani 1 1 d . . .
H13A H 0.3382 0.3240 0.5127 0.099 Uiso 1 1 calc R . .
C14 C 0.1864(8) 0.3006(6) 0.4666(5) 0.0646(19) Uani 1 1 d . . .
H14A H 0.1311 0.2929 0.5150 0.078 Uiso 1 1 calc R . .
C15 C 0.1450(7) 0.2954(6) 0.3985(5) 0.0619(19) Uani 1 1 d . . .
H15A H 0.0601 0.2865 0.4005 0.074 Uiso 1 1 calc R . .
C16 C 0.2249(6) 0.3029(5) 0.3247(4) 0.0543(16) Uani 1 1 d . . .
H16A H 0.1947 0.2985 0.2779 0.065 Uiso 1 1 calc R . .
C17 C 0.3852(6) 0.4052(4) 0.1663(4) 0.0457(14) Uani 1 1 d . . .
C18 C 0.3191(9) 0.4821(5) 0.2010(5) 0.067(2) Uani 1 1 d . . .
H18A H 0.3073 0.4908 0.2557 0.081 Uiso 1 1 calc R . .
C19 C 0.2693(11) 0.5478(6) 0.1541(6) 0.085(3) Uani 1 1 d . . .
H19A H 0.2245 0.6006 0.1776 0.102 Uiso 1 1 calc R . .
C20 C 0.2863(9) 0.5345(6) 0.0744(6) 0.076(2) Uani 1 1 d . . .
H20A H 0.2510 0.5775 0.0437 0.091 Uiso 1 1 calc R . .
C21 C 0.3552(8) 0.4578(6) 0.0382(5) 0.065(2) Uani 1 1 d . . .
H21A H 0.3688 0.4508 -0.0167 0.078 Uiso 1 1 calc R . .
C22 C 0.4036(7) 0.3920(5) 0.0839(4) 0.0545(16) Uani 1 1 d . . .
H22A H 0.4482 0.3392 0.0602 0.065 Uiso 1 1 calc R . .
C23 C 1.476(3) 0.106(2) 0.599(2) 0.52(5) Uani 1 1 d D . .
H23A H 1.5416 0.0852 0.5564 0.774 Uiso 1 1 calc R . .
H23B H 1.5110 0.1284 0.6424 0.774 Uiso 1 1 calc R . .
H23C H 1.4305 0.1575 0.5800 0.774 Uiso 1 1 calc R . .
C24 C 1.3951(12) 0.0296(14) 0.6240(9) 0.155(7) Uani 1 1 d D . .
H24A H 1.4404 -0.0230 0.6423 0.186 Uiso 1 1 calc R . .
H24B H 1.3588 0.0068 0.5803 0.186 Uiso 1 1 calc R . .
C25 C 1.1957(7) 0.1073(5) 0.6725(4) 0.0571(17) Uani 1 1 d . . .
C26 C 1.0978(6) 0.1226(5) 0.7465(4) 0.0493(15) Uani 1 1 d . . .
H26A H 1.1312 0.1649 0.7819 0.059 Uiso 1 1 calc R . .
H26B H 1.0794 0.0614 0.7735 0.059 Uiso 1 1 calc R . .
C27 C 0.8512(6) 0.1827(4) 0.8228(3) 0.0433(13) Uani 1 1 d . . .
C28 C 0.8938(7) 0.1760(7) 0.8935(4) 0.071(2) Uani 1 1 d . . .
H28A H 0.9781 0.1654 0.8924 0.085 Uiso 1 1 calc R . .
C29 C 0.8117(9) 0.1850(8) 0.9655(5) 0.085(3) Uani 1 1 d . . .
H29A H 0.8405 0.1811 1.0129 0.101 Uiso 1 1 calc R . .
C30 C 0.6863(8) 0.1999(6) 0.9668(5) 0.066(2) Uani 1 1 d . . .
H30A H 0.6309 0.2064 1.0152 0.079 Uiso 1 1 calc R . .
C31 C 0.6435(7) 0.2052(6) 0.8983(5) 0.0608(18) Uani 1 1 d . . .
H31A H 0.5586 0.2141 0.9002 0.073 Uiso 1 1 calc R . .
C32 C 0.7246(6) 0.1974(5) 0.8247(4) 0.0534(16) Uani 1 1 d . . .
H32A H 0.6948 0.2020 0.7777 0.064 Uiso 1 1 calc R . .
C33 C 0.9810(6) 0.2903(5) 0.6836(4) 0.0465(14) Uani 1 1 d . . .
C34 C 1.0869(8) 0.3430(6) 0.6902(5) 0.066(2) Uani 1 1 d . . .
H34A H 1.1462 0.3163 0.7159 0.080 Uiso 1 1 calc R . .
C35 C 1.1038(9) 0.4348(6) 0.6587(6) 0.081(3) Uani 1 1 d . . .
H35A H 1.1742 0.4699 0.6635 0.097 Uiso 1 1 calc R . .
C36 C 1.0182(9) 0.4735(6) 0.6210(6) 0.075(2) Uani 1 1 d . . .
H36A H 1.0313 0.5345 0.5986 0.090 Uiso 1 1 calc R . .
C37 C 0.9106(8) 0.4230(6) 0.6154(5) 0.068(2) Uani 1 1 d . . .
H37A H 0.8513 0.4510 0.5904 0.082 Uiso 1 1 calc R . .
C38 C 0.8916(6) 0.3314(5) 0.6467(4) 0.0536(16) Uani 1 1 d . . .
H38A H 0.8196 0.2977 0.6432 0.064 Uiso 1 1 calc R . .
C39 C 0.8856(6) 0.0952(5) 0.6663(4) 0.0464(14) Uani 1 1 d . . .
C40 C 0.9041(7) 0.1082(5) 0.5839(4) 0.0551(17) Uani 1 1 d . . .
H40A H 0.9491 0.1606 0.5597 0.066 Uiso 1 1 calc R . .
C41 C 0.8539(8) 0.0412(6) 0.5382(5) 0.067(2) Uani 1 1 d . . .
H41A H 0.8660 0.0488 0.4833 0.080 Uiso 1 1 calc R . .
C42 C 0.7876(9) -0.0347(6) 0.5743(5) 0.073(2) Uani 1 1 d . . .
H42A H 0.7548 -0.0790 0.5436 0.088 Uiso 1 1 calc R . .
C43 C 0.7683(11) -0.0471(6) 0.6545(6) 0.087(3) Uani 1 1 d . . .
H43A H 0.7223 -0.0994 0.6782 0.104 Uiso 1 1 calc R . .
C44 C 0.8168(9) 0.0172(5) 0.7006(5) 0.068(2) Uani 1 1 d . . .
H44A H 0.8031 0.0084 0.7554 0.082 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I5 0.0652(4) 0.0970(5) 0.1056(5) -0.0268(4) -0.0445(3) 0.0084(3)
I2 0.0655(4) 0.0967(5) 0.1067(5) 0.0264(4) -0.0447(3) -0.0083(3)
I1 0.0809(5) 0.1309(6) 0.1022(6) 0.0194(4) -0.0333(4) 0.0098(4)
I6 0.0810(5) 0.1307(6) 0.1022(6) -0.0196(4) -0.0329(4) -0.0100(4)
I3 0.0929(5) 0.1237(6) 0.0951(5) 0.0277(4) -0.0297(4) 0.0077(4)
I4 0.0921(5) 0.1236(6) 0.0951(5) -0.0282(4) -0.0290(4) -0.0073(4)
P1 0.0412(8) 0.0541(9) 0.0314(8) 0.0031(6) -0.0090(6) -0.0037(7)
P2 0.0407(8) 0.0540(9) 0.0320(8) -0.0039(6) -0.0093(6) 0.0042(7)
O1 0.070(4) 0.111(4) 0.044(3) -0.002(3) -0.002(3) -0.017(3)
O2 0.058(3) 0.136(5) 0.068(4) -0.005(4) 0.001(3) -0.039(4)
O3 0.070(4) 0.116(5) 0.043(3) 0.004(3) 0.001(3) 0.018(3)
O4 0.055(3) 0.142(6) 0.069(4) 0.001(4) 0.002(3) 0.042(3)
C1 0.141(19) 0.35(4) 0.60(7) 0.25(4) 0.15(3) 0.09(2)
C2 0.091(10) 0.28(2) 0.119(11) -0.038(12) 0.025(8) -0.083(13)
C3 0.053(4) 0.068(4) 0.049(4) 0.005(3) -0.005(3) -0.003(3)
C4 0.044(3) 0.068(4) 0.041(4) -0.002(3) -0.009(3) -0.013(3)
C5 0.054(4) 0.055(4) 0.033(3) 0.004(3) -0.007(3) -0.004(3)
C6 0.067(5) 0.070(5) 0.070(5) 0.005(4) -0.030(4) 0.004(4)
C7 0.084(6) 0.063(5) 0.094(7) 0.007(4) -0.027(5) 0.019(4)
C8 0.085(6) 0.055(4) 0.085(6) -0.001(4) -0.006(5) -0.004(4)
C9 0.067(5) 0.067(5) 0.069(5) -0.013(4) -0.012(4) -0.011(4)
C10 0.047(4) 0.068(4) 0.053(4) -0.004(3) -0.009(3) -0.001(3)
C11 0.043(3) 0.052(3) 0.036(3) 0.005(3) -0.002(3) -0.003(3)
C12 0.053(4) 0.117(7) 0.043(4) 0.010(4) -0.013(3) -0.024(4)
C13 0.079(6) 0.135(8) 0.036(4) 0.008(4) -0.017(4) -0.026(5)
C14 0.065(5) 0.077(5) 0.046(4) -0.001(3) 0.002(4) -0.010(4)
C15 0.044(4) 0.075(5) 0.062(5) -0.004(4) 0.000(3) -0.004(3)
C16 0.045(4) 0.072(4) 0.047(4) -0.001(3) -0.012(3) 0.000(3)
C17 0.051(4) 0.050(3) 0.038(3) 0.006(3) -0.014(3) -0.007(3)
C18 0.102(6) 0.057(4) 0.045(4) -0.007(3) -0.019(4) 0.013(4)
C19 0.133(9) 0.054(4) 0.072(6) -0.005(4) -0.032(6) 0.022(5)
C20 0.096(6) 0.062(5) 0.073(6) 0.017(4) -0.029(5) -0.002(4)
C21 0.071(5) 0.082(5) 0.046(4) 0.014(4) -0.019(4) -0.011(4)
C22 0.062(4) 0.060(4) 0.041(4) 0.003(3) -0.008(3) 0.007(3)
C23 0.17(2) 0.43(5) 0.84(10) -0.44(6) 0.19(4) -0.14(3)
C24 0.083(8) 0.26(2) 0.103(10) 0.038(11) 0.013(7) 0.046(11)
C25 0.057(4) 0.063(4) 0.050(4) -0.005(3) -0.006(3) 0.004(3)
C26 0.043(3) 0.068(4) 0.039(3) -0.001(3) -0.010(3) 0.012(3)
C27 0.044(3) 0.056(4) 0.029(3) -0.007(2) -0.005(3) 0.005(3)
C28 0.052(4) 0.117(7) 0.044(4) -0.005(4) -0.012(3) 0.021(4)
C29 0.078(6) 0.140(8) 0.035(4) -0.004(4) -0.010(4) 0.026(5)
C30 0.067(5) 0.074(5) 0.048(4) -0.002(3) 0.007(4) 0.012(4)
C31 0.043(4) 0.076(5) 0.058(5) 0.004(4) 0.002(3) 0.007(3)
C32 0.045(4) 0.069(4) 0.047(4) 0.002(3) -0.009(3) 0.003(3)
C33 0.051(4) 0.053(3) 0.035(3) -0.004(3) -0.006(3) 0.002(3)
C34 0.069(5) 0.071(5) 0.065(5) -0.005(4) -0.027(4) -0.007(4)
C35 0.084(6) 0.065(5) 0.095(7) -0.009(5) -0.023(5) -0.018(4)
C36 0.084(6) 0.057(4) 0.081(6) 0.000(4) -0.009(5) 0.002(4)
C37 0.068(5) 0.069(5) 0.066(5) 0.013(4) -0.012(4) 0.013(4)
C38 0.047(4) 0.061(4) 0.052(4) 0.004(3) -0.009(3) 0.005(3)
C39 0.051(4) 0.051(3) 0.039(3) -0.004(3) -0.014(3) 0.007(3)
C40 0.066(4) 0.062(4) 0.036(3) -0.004(3) -0.008(3) -0.006(3)
C41 0.074(5) 0.085(5) 0.047(4) -0.016(4) -0.024(4) 0.006(4)
C42 0.093(6) 0.060(4) 0.073(6) -0.021(4) -0.034(5) -0.004(4)
C43 0.139(9) 0.052(4) 0.071(6) 0.002(4) -0.028(6) -0.025(5)
C44 0.102(6) 0.056(4) 0.050(4) 0.004(3) -0.019(4) -0.014(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I6 I5 I4 176.88(3) . . ?
I1 I2 I3 176.91(3) . . ?
C17 P1 C11 108.2(3) . . ?
C17 P1 C5 110.6(3) . . ?
C11 P1 C5 109.5(3) . . ?
C17 P1 C4 110.5(3) . . ?
C11 P1 C4 106.7(3) . . ?
C5 P1 C4 111.2(3) . . ?
C39 P2 C33 110.6(3) . . ?
C39 P2 C27 108.4(3) . . ?
C33 P2 C27 109.4(3) . . ?
C39 P2 C26 110.7(3) . . ?
C33 P2 C26 111.1(3) . . ?
C27 P2 C26 106.5(3) . . ?
C3 O2 C2 116.9(8) . . ?
C25 O4 C24 118.5(8) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 O2 105.0(16) . . ?
C1 C2 H2A 110.8 . . ?
O2 C2 H2A 110.7 . . ?
C1 C2 H2B 110.7 . . ?
O2 C2 H2B 110.8 . . ?
H2A C2 H2B 108.8 . . ?
O1 C3 O2 126.1(7) . . ?
O1 C3 C4 124.7(7) . . ?
O2 C3 C4 109.2(6) . . ?
C3 C4 P1 113.5(5) . . ?
C3 C4 H4A 108.9 . . ?
P1 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
P1 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C10 C5 C6 118.8(7) . . ?
C10 C5 P1 120.2(5) . . ?
C6 C5 P1 120.8(6) . . ?
C7 C6 C5 120.8(8) . . ?
C7 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C8 C7 C6 120.3(8) . . ?
C8 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C7 C8 C9 120.7(8) . . ?
C7 C8 H8A 119.7 . . ?
C9 C8 H8A 119.7 . . ?
C8 C9 C10 119.5(8) . . ?
C8 C9 H9A 120.2 . . ?
C10 C9 H9A 120.2 . . ?
C5 C10 C9 119.8(7) . . ?
C5 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C12 C11 C16 119.2(6) . . ?
C12 C11 P1 122.2(5) . . ?
C16 C11 P1 118.5(5) . . ?
C13 C12 C11 120.6(7) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C14 C13 C12 119.9(8) . . ?
C14 C13 H13A 120.1 . . ?
C12 C13 H13A 120.1 . . ?
C15 C14 C13 120.1(7) . . ?
C15 C14 H14A 119.9 . . ?
C13 C14 H14A 119.9 . . ?
C14 C15 C16 122.0(7) . . ?
C14 C15 H15A 119.0 . . ?
C16 C15 H15A 119.0 . . ?
C11 C16 C15 118.2(7) . . ?
C11 C16 H16A 120.9 . . ?
C15 C16 H16A 120.9 . . ?
C18 C17 C22 120.3(6) . . ?
C18 C17 P1 118.1(5) . . ?
C22 C17 P1 121.4(5) . . ?
C17 C18 C19 119.8(7) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 119.8(8) . . ?
C20 C19 H19A 120.1 . . ?
C18 C19 H19A 120.1 . . ?
C19 C20 C21 121.0(8) . . ?
C19 C20 H20A 119.5 . . ?
C21 C20 H20A 119.5 . . ?
C22 C21 C20 119.7(7) . . ?
C22 C21 H21A 120.1 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C17 119.4(7) . . ?
C21 C22 H22A 120.3 . . ?
C17 C22 H22A 120.3 . . ?
C24 C23 H23A 109.4 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.1 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C23 C24 O4 108.0(18) . . ?
C23 C24 H24A 109.8 . . ?
O4 C24 H24A 110.1 . . ?
C23 C24 H24B 110.4 . . ?
O4 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
O3 C25 O4 125.8(7) . . ?
O3 C25 C26 124.0(7) . . ?
O4 C25 C26 110.2(6) . . ?
C25 C26 P2 113.8(5) . . ?
C25 C26 H26A 108.8 . . ?
P2 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
P2 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 C32 119.7(6) . . ?
C28 C27 P2 121.7(5) . . ?
C32 C27 P2 118.5(5) . . ?
C29 C28 C27 120.3(7) . . ?
C29 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?
C28 C29 C30 119.6(8) . . ?
C28 C29 H29A 120.2 . . ?
C30 C29 H29A 120.2 . . ?
C31 C30 C29 120.6(7) . . ?
C31 C30 H30A 119.7 . . ?
C29 C30 H30A 119.7 . . ?
C30 C31 C32 121.0(7) . . ?
C30 C31 H31A 119.5 . . ?
C32 C31 H31A 119.5 . . ?
C27 C32 C31 118.8(7) . . ?
C27 C32 H32A 120.6 . . ?
C31 C32 H32A 120.6 . . ?
C38 C33 C34 119.5(6) . . ?
C38 C33 P2 120.0(5) . . ?
C34 C33 P2 120.4(6) . . ?
C35 C34 C33 120.1(8) . . ?
C35 C34 H34A 119.9 . . ?
C33 C34 H34A 119.9 . . ?
C36 C35 C34 120.1(8) . . ?
C36 C35 H35A 119.9 . . ?
C34 C35 H35A 119.9 . . ?
C35 C36 C37 120.6(8) . . ?
C35 C36 H36A 119.7 . . ?
C37 C36 H36A 119.7 . . ?
C38 C37 C36 120.2(8) . . ?
C38 C37 H37A 119.9 . . ?
C36 C37 H37A 119.9 . . ?
C37 C38 C33 119.4(7) . . ?
C37 C38 H38A 120.3 . . ?
C33 C38 H38A 120.3 . . ?
C44 C39 C40 119.0(6) . . ?
C44 C39 P2 119.1(5) . . ?
C40 C39 P2 121.8(5) . . ?
C39 C40 C41 119.2(7) . . ?
C39 C40 H40A 120.4 . . ?
C41 C40 H40A 120.4 . . ?
C42 C41 C40 119.9(7) . . ?
C42 C41 H41A 120.1 . . ?
C40 C41 H41A 120.1 . . ?
C41 C42 C43 121.2(7) . . ?
C41 C42 H42A 119.4 . . ?
C43 C42 H42A 119.4 . . ?
C42 C43 C44 120.1(8) . . ?
C42 C43 H43A 119.9 . . ?
C44 C43 H43A 119.9 . . ?
C43 C44 C39 120.6(8) . . ?
C43 C44 H44A 119.7 . . ?
C39 C44 H44A 119.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I5 I6 2.9263(13) . ?
I5 I4 2.9327(13) . ?
I2 I1 2.9331(13) . ?
I2 I3 2.9360(13) . ?
P1 C17 1.790(6) . ?
P1 C11 1.795(6) . ?
P1 C5 1.796(7) . ?
P1 C4 1.807(6) . ?
P2 C39 1.790(7) . ?
P2 C33 1.795(6) . ?
P2 C27 1.795(6) . ?
P2 C26 1.796(6) . ?
O1 C3 1.189(9) . ?
O2 C3 1.324(9) . ?
O2 C2 1.494(13) . ?
O3 C25 1.196(9) . ?
O4 C25 1.321(9) . ?
O4 C24 1.502(15) . ?
C1 C2 1.376(17) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.498(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C10 1.384(10) . ?
C5 C6 1.393(10) . ?
C6 C7 1.364(12) . ?
C6 H6A 0.9300 . ?
C7 C8 1.359(13) . ?
C7 H7A 0.9300 . ?
C8 C9 1.376(13) . ?
C8 H8A 0.9300 . ?
C9 C10 1.396(11) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.387(10) . ?
C11 C16 1.388(9) . ?
C12 C13 1.370(11) . ?
C12 H12A 0.9300 . ?
C13 C14 1.368(12) . ?
C13 H13A 0.9300 . ?
C14 C15 1.337(11) . ?
C14 H14A 0.9300 . ?
C15 C16 1.391(10) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C18 1.361(10) . ?
C17 C22 1.400(9) . ?
C18 C19 1.396(11) . ?
C18 H18A 0.9300 . ?
C19 C20 1.356(13) . ?
C19 H19A 0.9300 . ?
C20 C21 1.381(13) . ?
C20 H20A 0.9300 . ?
C21 C22 1.376(10) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.396(18) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.503(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.385(10) . ?
C27 C32 1.393(9) . ?
C28 C29 1.380(11) . ?
C28 H28A 0.9300 . ?
C29 C30 1.383(12) . ?
C29 H29A 0.9300 . ?
C30 C31 1.350(11) . ?
C30 H30A 0.9300 . ?
C31 C32 1.395(10) . ?
C31 H31A 0.9300 . ?
C32 H32A 0.9300 . ?
C33 C38 1.388(9) . ?
C33 C34 1.396(10) . ?
C34 C35 1.384(12) . ?
C34 H34A 0.9300 . ?
C35 C36 1.350(13) . ?
C35 H35A 0.9300 . ?
C36 C37 1.390(12) . ?
C36 H36A 0.9300 . ?
C37 C38 1.382(10) . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9300 . ?
C39 C44 1.382(10) . ?
C39 C40 1.399(9) . ?
C40 C41 1.400(10) . ?
C40 H40A 0.9300 . ?
C41 C42 1.358(12) . ?
C41 H41A 0.9300 . ?
C42 C43 1.361(13) . ?
C42 H42A 0.9300 . ?
C43 C44 1.371(12) . ?
C43 H43A 0.9300 . ?
C44 H44A 0.9300 . ?
|
1100688.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-24 04:14:37 +0200 (Wed, 24 Feb 2016) $
#$Revision: 176838 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100688.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100688
loop_
_publ_author_name
'Zhao, Pu Su'
'Jian, Fang Fang'
'Xiao, Hai Lian'
'Hou, Yu Xia'
_publ_section_title
;
A Novel Synthesis and Crystal Structure of
2,3-Substituted-1,4-2H-tetrazolthione
;
_journal_coden_ASTM BKCSDE
_journal_issue 12
_journal_name_full 'Bulletin of the Korean Chemical Society'
_journal_page_first 1935
_journal_page_last 1936
_journal_paper_doi 10.5012/bkcs.2004.25.12.1935
_journal_volume 25
_journal_year 2004
_chemical_formula_sum 'C15 H16 N4 S'
_chemical_formula_weight 142.19
_chemical_name_systematic 2,3-bis(4-methylphenyl)tetrazolidine-5-thione
_space_group_IT_number 31
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2ac -2'
_symmetry_space_group_name_H-M 'P m n 21'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 18.381(4)
_cell_length_b 6.1799(12)
_cell_length_c 6.1865(12)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 702.7(2)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0731
_diffrn_reflns_av_sigmaI/netI 0.0808
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -7
_diffrn_reflns_number 2213
_diffrn_reflns_theta_full 27.44
_diffrn_reflns_theta_max 27.44
_diffrn_reflns_theta_min 3.30
_exptl_absorpt_coefficient_mu 0.226
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type ?
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.344
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 300
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_refine_diff_density_max 0.934
_refine_diff_density_min -0.454
_refine_diff_density_rms 0.138
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.4(4)
_refine_ls_extinction_coef 0.35(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.219
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 95
_refine_ls_number_reflns 1310
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.218
_refine_ls_R_factor_all 0.1207
_refine_ls_R_factor_gt 0.1089
_refine_ls_shift/su_max 0.082
_refine_ls_shift/su_mean 0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3064
_refine_ls_wR_factor_ref 0.3127
_reflns_number_gt 1036
_reflns_number_total 1310
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
Determined systematic IUPAC name of this compound from PubMed
entry
https://pubchem.ncbi.nlm.nih.gov/compound/73849486?from=summary#section=Identification
Saulius Gra\<zulis
2014-10-30
;
_cod_original_sg_symbol_H-M Pmn2(1)
_cod_original_formula_sum 'C7.50 H8 N2 S0.50'
_cod_database_code 1100688
#BEGIN Tags that were not found in dictionaries:
_chemical_name_iupac 2,3-bis(4-methylphenyl)tetrazolidine-5-thione
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.0000 1.1710(4) 0.2148(4) 0.0605(10) Uani 1 2 d S . .
N1 N 0.0363(3) 0.7481(8) 0.6423(9) 0.0418(13) Uani 1 1 d . . .
N2 N 0.0610(3) 0.8900(10) 0.5024(10) 0.0498(15) Uani 1 1 d . . .
H2A H 0.1057 0.9192 0.4737 0.060 Uiso 1 1 calc R . .
C1 C 0.0815(4) 0.6119(12) 0.7721(11) 0.0486(18) Uani 1 1 d . . .
C2 C 0.1045(4) 0.6897(11) 0.9709(13) 0.0504(19) Uani 1 1 d . . .
H2B H 0.0898 0.8254 1.0194 0.060 Uiso 1 1 calc R . .
C3 C 0.1504(4) 0.5586(12) 1.0976(13) 0.057(2) Uani 1 1 d . . .
H3A H 0.1657 0.6059 1.2329 0.068 Uiso 1 1 calc R . .
C4 C 0.1732(5) 0.3545(12) 1.0182(15) 0.059(2) Uani 1 1 d . . .
C5 C 0.1504(4) 0.2861(13) 0.8177(14) 0.056(2) Uani 1 1 d . . .
H5A H 0.1670 0.1545 0.7640 0.067 Uiso 1 1 calc R . .
C6 C 0.1030(4) 0.4097(11) 0.6939(15) 0.0556(18) Uani 1 1 d . . .
H6A H 0.0860 0.3590 0.5617 0.067 Uiso 1 1 calc R . .
C7 C 0.2212(5) 0.2136(15) 1.1530(17) 0.074(3) Uani 1 1 d . . .
H7A H 0.2321 0.2855 1.2866 0.111 Uiso 1 1 calc R . .
H7B H 0.2656 0.1851 1.0763 0.111 Uiso 1 1 calc R . .
H7C H 0.1968 0.0794 1.1825 0.111 Uiso 1 1 calc R . .
C8 C 0.0000 0.9821(19) 0.4114(17) 0.054(3) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.0667(18) 0.0672(16) 0.0477(16) 0.0175(13) 0.000 0.000
N1 0.038(2) 0.050(3) 0.037(3) 0.013(2) 0.001(2) 0.007(2)
N2 0.043(3) 0.059(3) 0.047(4) 0.018(3) 0.004(3) 0.002(3)
C1 0.042(4) 0.065(4) 0.039(4) 0.007(3) 0.007(3) 0.003(3)
C2 0.051(4) 0.064(4) 0.037(4) -0.002(3) -0.001(3) -0.001(3)
C3 0.061(5) 0.066(4) 0.043(4) -0.004(3) -0.004(4) 0.000(3)
C4 0.053(4) 0.067(4) 0.056(5) 0.005(4) -0.015(4) -0.001(3)
C5 0.053(5) 0.061(4) 0.053(4) -0.004(4) 0.002(4) 0.001(3)
C6 0.063(4) 0.057(3) 0.047(4) 0.004(4) -0.005(4) -0.001(3)
C7 0.074(6) 0.073(5) 0.075(7) 0.015(4) -0.010(5) 0.019(4)
C8 0.055(6) 0.077(7) 0.029(5) 0.014(5) 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 N1 110.2(3) . 3 ?
N2 N1 C1 124.2(5) . . ?
N1 N1 C1 125.6(3) 3 . ?
N1 N2 C8 105.3(6) . . ?
C2 C1 C6 122.1(7) . . ?
C2 C1 N1 118.1(6) . . ?
C6 C1 N1 119.7(7) . . ?
C1 C2 C3 118.5(7) . . ?
C2 C3 C4 119.7(7) . . ?
C5 C4 C3 119.7(7) . . ?
C5 C4 C7 120.3(8) . . ?
C3 C4 C7 120.0(8) . . ?
C6 C5 C4 121.3(7) . . ?
C5 C6 C1 118.6(8) . . ?
N2 C8 N2 108.9(8) 3 . ?
N2 C8 S1 125.5(4) 3 . ?
N2 C8 S1 125.5(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C8 1.686(10) . ?
N1 N2 1.313(8) . ?
N1 N1 1.333(11) 3 ?
N1 C1 1.430(8) . ?
N2 C8 1.377(8) . ?
C1 C2 1.386(11) . ?
C1 C6 1.397(10) . ?
C2 C3 1.409(10) . ?
C3 C4 1.417(11) . ?
C4 C5 1.376(12) . ?
C4 C7 1.495(11) . ?
C5 C6 1.389(11) . ?
C8 N2 1.377(8) 3 ?
|
1100689.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100689.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100689
loop_
_publ_author_name
'Soriano-Garc\'ia, Manuel'
'Valencia, Norma'
'Flores, Eugenio'
'Bratoeff, Eugene'
'Ram\'irez, Elena'
'Cabeza, Marisa'
_publ_section_title
'Crystal structure and Synthesis of \b-(p-Fluorobenzoyloxy)-4,16-pregnadiene-6,20-dione'
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x79
_journal_page_last x80
_journal_paper_doi 10.2116/analscix.19.x79
_journal_volume 19
_journal_year 2003
_chemical_formula_moiety 'C28 H31 F O4'
_chemical_formula_sum 'C28 H31 F O4'
_chemical_formula_weight 450.53
_chemical_name_systematic
'Crystal structure and Synthesis of \b-(p-Fluorobenzoyloxy)-4,16-pregnadiene-6,20-dione'
_space_group_IT_number 4
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall 'P 2yb'
_symmetry_space_group_name_H-M 'P 1 21 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 102.243(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 12.4629(10)
_cell_length_b 6.1705(5)
_cell_length_c 15.5815(13)
_cell_measurement_reflns_used 3041
_cell_measurement_temperature 291(2)
_cell_measurement_theta_max 30.91
_cell_measurement_theta_min 2.35
_cell_volume 1171.00(17)
_diffrn_ambient_temperature 291(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method 'omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0409
_diffrn_reflns_av_sigmaI/netI 0.0742
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 9645
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 2.35
_diffrn_standards_interval_time 90
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.089
_exptl_absorpt_correction_type none
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.278
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 480
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.328
_refine_diff_density_min -0.137
_refine_diff_density_rms 0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.0(12)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.911
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 301
_refine_ls_number_reflns 4105
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.911
_refine_ls_R_factor_all 0.0812
_refine_ls_R_factor_gt 0.0476
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0794
_refine_ls_wR_factor_ref 0.0868
_reflns_number_gt 2458
_reflns_number_total 4105
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'No' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_original_sg_symbol_H-M 'P2(1) '
_cod_database_code 1100689
_solved_by 'Simon Hernandez-Ortega'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
F1 F 0.89588(16) -0.2856(4) 0.93806(15) 0.1216(9) Uani 1 1 d . . .
O1 O 0.47275(15) 0.2761(4) 0.85507(13) 0.0760(7) Uani 1 1 d . . .
O2 O 0.11870(16) -0.0393(4) 0.86268(14) 0.0790(7) Uani 1 1 d . . .
O3 O 0.55700(17) 0.4447(4) 0.97741(16) 0.0895(8) Uani 1 1 d . . .
O4 O -0.35254(19) 0.8746(4) 0.51195(17) 0.0998(9) Uani 1 1 d . . .
C1 C 0.2393(2) 0.6067(5) 0.7320(2) 0.0658(10) Uani 1 1 d . .. .
H1A H 0.2260 0.7092 0.7758 0.079 Uiso 1 1 calc R . .
H1B H 0.2298 0.6829 0.6765 0.079 Uiso 1 1 calc R . .
C2 C 0.3579(2) 0.5249(6) 0.7583(2) 0.0707(10) Uani 1 1 d . . .
H2A H 0.3726 0.4247 0.7142 0.085 Uiso 1 1 calc R . .
H2B H 0.4083 0.6460 0.7617 0.085 Uiso 1 1 calc R . ..
C3 C 0.3753(2) 0.4127(6) 0.8462(2) 0.0676(10) Uani 1 1 d . . .
H3 H 0.3876 0.5217 0.8930 0.081 Uiso 1 1 calc R . .
C4 C 0.2824(2) 0.2735(6) 0.85550(19) 0.0665(10) Uani 1 1 d . . .
H4 H 0.2941 0.1744 0.9015 0.080 Uiso 1 1 calc R . .
C5 C 0.0962(3) 0.1368(5) 0.82529(19) 0.0538(8) Uani 1 1 d . . .
C6 C -0.0186(2) 0.2159(5) 0.80490(17) 0.0523(8) Uani 1 1 d . . .
H6A H -0.0301 0.3095 0.8522 0.063 Uiso 1 1 calc R . .
H6B H -0.0678 0.0930 0.8022 0.063 Uiso 1 1 calc R . .
C7 C -0.0479(2) 0.3402(5) 0.71859(17) 0.0438(7) Uani 1 1 d . . .
H7 H -0.0486 0.2387 0.6701 0.053 Uiso 1 1 calc R . .
C8 C 0.0368(2) 0.5170(5) 0.71485(18) 0.0441(7) Uani 1 1 d . . .
H8 H 0.0396 0.6057 0.7674 0.053 Uiso 1 1 calc R . .
C9 C 0.1549(2) 0.4247(5) 0.72332(18) 0.0454(7) Uani 1 1 d . . .
C10 C 0.1834(2) 0.2785(5) 0.80326(18) 0.0493(8) Uani 1 1 d . . .
C11 C 0.0019(2) 0.6724(5) 0.63654(19) 0.0582(9) Uani 1 1 d . . .
H11A H 0.0512 0.7960 0.6449 0.070 Uiso 1 1 calc R .. .
H11B H 0.0106 0.5986 0.5835 0.070 Uiso 1 1 calc R . .
C12 C -0.1164(2) 0.7555(5) 0.62308(19) 0.0585(9) Uani 1 1 d . . .
H12A H -0.1225 0.8535 0.6705 0.070 Uiso 1 1 calc R . .
H12B H -0.1349 0.8353 0.5683 0.070 Uiso 1 1 calc R . .
C13 C -0.1961(2) 0.5684(4) 0.62092(18) 0.0437(7) Uani 1 1 d . . .
C14 C -0.1607(2) 0.4427(5) 0.70715(17) 0.0443(7) Uani 1 1 d . . .
H14 H -0.1531 0.5527 0.7534 0.053 Uiso 1 1 calc R . .
C15 C -0.2640(2) 0.3117(6) 0.71456(19) 0.0609(9) Uani 1 1 d . . .
H15A H -0.2693 0.1778 0.6813 0.073 Uiso 1 1 calc R . .
H15B H -0.2656 0.2795 0.7752 0.073 Uiso 1 1 calc R . .
C16 C -0.3518(2) 0.4684(6) 0.67502(19) 0.0614(9) Uani 1 1 d . .. .
H16 H -0.4232 0.4641 0.6840 0.074 Uiso 1 1 calc R . .
C17 C -0.3151(2) 0.6164(5) 0.6249(2) 0.0532(8) Uani 1 1 d . . .
C18 C -0.1999(2) 0.4263(5) 0.53894(17) 0.0619(9) Uani 1 1 d . . .
H18A H -0.1265 0.3863 0.5353 0.074 Uiso 1 1 calc R .. .
H18B H -0.2334 0.5062 0.4873 0.074 Uiso 1 1 calc R . .
H18C H -0.2420 0.2980 0.5431 0.074 Uiso 1 1 calc R . .
C19 C 0.1606(2) 0.2852(5) 0.64282(17) 0.0636(9) Uani 1 1 d . . .
H19A H 0.2320 0.2204 0.6505 0.076 Uiso 1 1 calc R .. .
H19B H 0.1474 0.3745 0.5912 0.076 Uiso 1 1 calc R . .
H19C H 0.1059 0.1735 0.6364 0.076 Uiso 1 1 calc R . .
C20 C -0.3827(3) 0.7843(6) 0.5708(2) 0.0640(9) Uani 1 1 d . . .
C21 C -0.4921(2) 0.8383(6) 0.5906(2) 0.0954(13) Uani 1 1 d . .. .
H21A H -0.4826 0.8788 0.6513 0.114 Uiso 1 1 calc R . .
H21B H -0.5393 0.7141 0.5792 0.114 Uiso 1 1 calc R . .
H21C H -0.5244 0.9566 0.5541 0.114 Uiso 1 1 calc R . .
C22 C 0.5541(2) 0.3037(6) 0.9236(2) 0.0584(9) Uani 1 1 d . .. .
C23 C 0.6445(2) 0.1450(6) 0.92648(19) 0.0504(8) Uani 1 1 d . . .
C24 C 0.7465(3) 0.1907(6) 0.97516(19) 0.0632(9) Uani 1 1 d . . .
H24 H 0.7585 0.3203 1.0062 0.076 Uiso 1 1 calc R . .
C25 C 0.8323(3) 0.0457(8) 0.9787(2) 0.0800(12) Uani 1 1 d . . .
H25 H 0.9020 0.0772 1.0114 0.096 Uiso 1 1 calc R . .
C26 C 0.8122(3) -0.1426(7) 0.9337(3) 0.0745(11) Uani 1 1 d . . .
C27 C 0.7130(3) -0.1965(6) 0.8856(2) 0.0775(10) Uani 1 1 d . .. .
H27 H 0.7019 -0.3284 0.8562 0.093 Uiso 1 1 calc R . .
C28 C 0.6279(3) -0.0495(7) 0.8811(2) 0.0687(10) Uani 1 1 d . . .
H28 H 0.5588 -0.0817 0.8473 0.082 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
F1 0.0798(14) 0.134(2) 0.157(2) 0.0349(18) 0.0392(14) 0.0445(15)
O1 0.0461(13) 0.109(2) 0.0678(14) -0.0186(16) 0.0010(11) 0.0104(14)
O2 0.0752(16) 0.0749(19) 0.0853(17) 0.0228(16) 0.0131(13) 0.0091(15)
O3 0.0664(15) 0.094(2) 0.1009(19) -0.0428(18) 0.0023(13) 0.0030(15)
O4 0.0761(18) 0.103(2) 0.115(2) 0.0533(19) 0.0072(15) 0.0122(15)
C1 0.051(2) 0.065(2) 0.081(2) 0.001(2) 0.0134(18) -0.0033(19)
C2 0.0449(19) 0.080(3) 0.086(3) 0.002(2) 0.0124(18) -0.0040(19)
C3 0.0417(19) 0.093(3) 0.068(2) -0.012(2) 0.0111(17) 0.009(2)
C4 0.059(2) 0.089(3) 0.0527(19) 0.003(2) 0.0143(17) 0.014(2)
C5 0.065(2) 0.052(2) 0.0433(19) 0.0079(17) 0.0086(16) 0.0125(19)
C6 0.0519(19) 0.057(2) 0.0513(19) 0.0072(17) 0.0176(15) 0.0043(16)
C7 0.0467(17) 0.0461(19) 0.0390(16) 0.0022(14) 0.0101(13) 0.0042(15)
C8 0.0419(17) 0.0380(18) 0.0516(19) -0.0026(15) 0.0081(14) -0.0034(15)
C9 0.0494(18) 0.0437(18) 0.0454(18) -0.0038(17) 0.0149(14) -0.0029(16)
C10 0.0467(18) 0.058(2) 0.0438(18) -0.0010(17) 0.0105(15) 0.0136(18)
C11 0.0505(19) 0.050(2) 0.070(2) 0.0157(18) 0.0033(16) -0.0105(16)
C12 0.055(2) 0.047(2) 0.068(2) 0.0087(18) -0.0003(16) -0.0049(18)
C13 0.0463(18) 0.0371(17) 0.0438(18) 0.0022(15) 0.0011(14) -0.0029(15)
C14 0.0467(17) 0.0429(19) 0.0426(17) -0.0007(16) 0.0085(14) -0.0013(16)
C15 0.061(2) 0.061(2) 0.062(2) 0.015(2) 0.0172(16) 0.0004(19)
C16 0.0388(17) 0.078(3) 0.069(2) 0.019(2) 0.0146(16) 0.0002(19)
C17 0.0439(19) 0.052(2) 0.058(2) -0.0025(18) -0.0012(16) 0.0029(17)
C18 0.062(2) 0.067(2) 0.0538(19) 0.0060(19) 0.0057(15) -0.0115(19)
C19 0.065(2) 0.074(2) 0.0530(18) 0.002(2) 0.0153(15) 0.001(2)
C20 0.056(2) 0.056(2) 0.076(2) 0.007(2) 0.0035(19) 0.002(2)
C21 0.064(2) 0.089(3) 0.127(3) 0.024(3) 0.006(2) 0.020(2)
C22 0.051(2) 0.069(2) 0.056(2) -0.011(2) 0.0124(17) -0.012(2)
C23 0.0388(18) 0.059(2) 0.054(2) 0.0023(18) 0.0116(15) -0.0058(17)
C24 0.050(2) 0.079(3) 0.059(2) 0.002(2) 0.0089(17) -0.013(2)
C25 0.049(2) 0.118(4) 0.071(3) 0.017(3) 0.0058(19) -0.010(3)
C26 0.050(2) 0.091(3) 0.088(3) 0.021(3) 0.028(2) 0.015(2)
C27 0.069(2) 0.067(3) 0.098(3) -0.011(2) 0.022(2) 0.008(2)
C28 0.053(2) 0.087(3) 0.064(2) -0.003(2) 0.0084(17) -0.014(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 O1 C3 118.9(3) . . y
C9 C1 C2 112.9(2) . . y
C3 C2 C1 109.8(2) .. . y
O1 C3 C4 108.0(3) . . y
O1 C3 C2 107.9(2) . . y
C4 C3 C2 113.1(3) . . y
C10 C4 C3 125.0(3) . . y
O2 C5 C6 120.2(3) .. . y
O2 C5 C10 121.4(3) . . y
C6 C5 C10 118.4(3) . . y
C5 C6 C7 113.3(2) . . y
C14 C7 C6 110.9(2) . . y
C14 C7 C8 109.2(2) . . y
C6 C7 C8 110.8(2) . . y
C7 C8 C11 113.2(2) . . y
C7 C8 C9 112.6(2) . .. y
C11 C8 C9 113.4(2) . . y
C10 C9 C1 109.1(2) . . y
C10 C9 C19 107.1(2) . . y
C1 C9 C19 109.6(2) . . y
C10 C9 C8 109.8(2) .. . y
C1 C9 C8 111.1(2) . . y
C19 C9 C8 110.0(2) . . y
C4 C10 C5 118.3(3) . . y
C4 C10 C9 122.9(3) . . y
C5 C10 C9 118.9(2) . . y
C12 C11 C8 114.7(2) . . y
C13 C12 C11 110.8(2) . . y
C12 C13 C17 119.2(2) . . y
C12 C13 C14 107.4(2) . . y
C17 C13 C14 99.5(2) . . y
C12 C13 C18 110.8(2) . . y
C17 C13 C18 106.5(2) . . y
C14 C13 C18 113.0(2) . . y
C7 C14 C13 113.7(2) . . y
C7 C14 C15 122.6(2) . . y
C13 C14 C15 103.9(2) . . y
C16 C15 C14 100.3(2) . . y
C17 C16 C15 111.7(3) . . y
C16 C17 C20 125.7(3) . . y
C16 C17 C13 110.2(3) . . y
C20 C17 C13 123.6(3) . . y
O4 C20 C17 121.8(3) . . y
O4 C20 C21 120.1(3) . . y
C17 C20 C21 118.1(3) . . y
O3 C22 O1 124.2(3) . . y
O3 C22 C23 123.0(3) . . y
O1 C22 C23 112.8(3) . . y
C24 C23 C28 119.0(3) . . y
C24 C23 C22 119.4(3) . . y
C28 C23 C22 121.6(3) . . y
C23 C24 C25 120.6(4) . . y
C26 C25 C24 118.5(3) . . y
C27 C26 C25 123.3(4) . . y
C27 C26 F1 118.2(4) . . y
C25 C26 F1 118.5(4) . . y
C26 C27 C28 118.0(4) . . y
C23 C28 C27 120.7(3) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C26 1.356(4) . y
O1 C22 1.318(3) . y
O1 C3 1.460(3) . y
O2 C5 1.236(3) . y
O3 C22 1.203(3) . y
O4 C20 1.199(3) . y
C1 C9 1.525(4) . y
C1 C2 1.533(3) . y
C2 C3 1.509(4) . y
C3 C4 1.473(4) . y
C4 C10 1.327(3) . y
C5 C6 1.482(3) . y
C5 C10 1.490(4) . y
C6 C7 1.524(3) . y
C7 C14 1.516(3) . y
C7 C8 1.528(3) . y
C8 C11 1.541(4) . y
C8 C9 1.558(3) . y
C9 C10 1.518(4) . y
C9 C19 1.535(4) . y
C11 C12 1.532(3) . y
C12 C13 1.519(4) . y
C13 C17 1.526(4) . y
C13 C14 1.533(3) . y
C13 C18 1.542(4) . y
C14 C15 1.545(4) . y
C15 C16 1.492(4) . y
C16 C17 1.344(4) . y
C17 C20 1.481(4) . y
C20 C21 1.497(4) . y
C22 C23 1.487(4) . y
C23 C24 1.364(4) . y
C23 C28 1.386(4) . y
C24 C25 1.386(5) . y
C25 C26 1.353(5) . y
C26 C27 1.345(4) . y
C27 C28 1.387(4) . y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 9503364
|
1100690.cif | #------------------------------------------------------------------------------
#$Date: 2015-03-19 18:12:06 +0200 (Thu, 19 Mar 2015) $
#$Revision: 134161 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100690.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100690
loop_
_publ_author_name
'Hemissi, Han\`ene'
'Abid, Sonia'
'Rzaigui, Mohamed'
_publ_section_title
;
Structural Characterization of a New Organic Cyclotetraphosphate,
[C~4~H~8~N~2~H~4~]~2~P~4~O~12~·4H~2~O
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x1
_journal_page_last x2
_journal_paper_doi 10.2116/analscix.20.x1
_journal_volume 20
_journal_year 2004
_chemical_formula_moiety 'C4 H16 N2 O8 P2'
_chemical_formula_sum 'C8 H32 N4 O16 P4'
_chemical_formula_weight 564.25
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 98.17(2)
_cell_angle_beta 109.89(2)
_cell_angle_gamma 82.79(2)
_cell_formula_units_Z 1
_cell_length_a 7.733(3)
_cell_length_b 10.511(2)
_cell_length_c 7.715(2)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 296.2
_cell_measurement_theta_max 10.0
_cell_measurement_theta_min 8.0
_cell_volume 581.7(3)
_diffrn_ambient_temperature 296
_diffrn_measurement_device MACH3
_diffrn_measurement_method \w-2\q
_diffrn_orient_matrix_UB_11 -0.09465
_diffrn_orient_matrix_UB_12 0.06406
_diffrn_orient_matrix_UB_13 -0.03452
_diffrn_orient_matrix_UB_21 -0.09901
_diffrn_orient_matrix_UB_22 0.07207
_diffrn_orient_matrix_UB_23 -0.00769
_diffrn_orient_matrix_UB_31 -0.01678
_diffrn_orient_matrix_UB_32 0.00174
_diffrn_orient_matrix_UB_33 0.13405
_diffrn_radiation_detector 'scintillation counter'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type 'Ag K\a'
_diffrn_radiation_wavelength 0.5608
_diffrn_reflns_av_R_equivalents 0.01750
_diffrn_reflns_av_sigmaI/netI 0.048
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 0
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 4351
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max 24.96
_diffrn_reflns_theta_min 2.22
_diffrn_standards_decay_% 0.16
_diffrn_standards_interval_count 0
_diffrn_standards_number 2
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.611
_exptl_crystal_description parallelipedic
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.09
_reflns_number_gt 3006
_reflns_number_total 4154
_reflns_threshold_expression I>3.00\s(I)
_cod_depositor_comments
;
Changed the order of tags in '_atom_site' loop after consulting the original
paper. Also, added Hall spacegroup symbol.
Antanas Vaitkus,
2015-03-19
;
_cod_database_code 1100690
loop_
_symmetry_equiv_pos_as_xyz
' +x, +y, +z'
' -x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_calc_attached_atom
P1 0.93565(4) 0.89152(3) 0.64530(4) 0.01933(7) 1.000 Uani d ? ?
P2 0.90377(4) 1.17329(3) 0.65185(4) 0.02008(7) 1.000 Uani d ? ?
O1 0.4189(1) 0.33846(10) 0.6247(2) 0.0478(3) 1.000 Uani d ? ?
O2 0.7023(2) 0.41156(11) 1.2787(2) 0.0669(4) 1.000 Uani d ? ?
O3 0.80308(13) 0.81769(8) 0.68154(12) 0.0287(2) 1.000 Uani d ? ?
O4 1.12406(12) 0.90031(8) 0.77608(12) 0.0295(2) 1.000 Uani d ? ?
O5 0.93907(12) 0.83641(8) 0.44183(11) 0.0258(2) 1.000 Uani d ? ?
O6 0.83309(12) 1.03229(8) 0.60463(12) 0.0264(2) 1.000 Uani d ? ?
O7 0.99873(13) 1.20006(9) 0.85367(12) 0.0309(2) 1.000 Uani d ? ?
O8 0.74636(13) 1.26155(8) 0.55865(13) 0.0331(3) 1.000 Uani d ? ?
N1 0.9250(2) 0.40893(10) 1.0720(2) 0.0372(3) 1.000 Uani d ? ?
N2 0.6554(1) 0.94668(10) 0.9462(1) 0.0281(3) 1.000 Uani d ? ?
C1 0.8036(2) 0.5007(1) 0.9447(2) 0.0445(4) 1.000 Uani d ? ?
C2 0.8955(3) 0.53745(13) 0.8201(2) 0.0460(4) 1.000 Uani d ? ?
C3 0.5631(2) 0.86698(12) 1.0270(2) 0.0317(3) 1.000 Uani d ? ?
C4 0.4766(2) 0.9517(1) 1.1558(2) 0.0328(4) 1.000 Uani d ? ?
H1 0.5364 0.3117 0.6209 0.020 1.000 Uiso c ? ?
H2 0.3321 0.2845 0.5416 0.020 1.000 Uiso c ? ?
H3 0.7151 0.3516 1.3708 0.056 1.000 Uiso c ? ?
H4 0.6671 0.4912 1.3237 0.052 1.000 Uiso c ? ?
H5 0.8610 0.3954 1.1602 0.040 1.000 Uiso c ? ?
H6 0.9549 0.3325 1.0013 0.037 1.000 Uiso c ? ?
H7 0.7531 0.5746 1.0113 0.039 1.000 Uiso c ? ?
H8 0.6938 0.4544 0.8746 0.041 1.000 Uiso c ? ?
H9 0.8273 0.5995 0.7481 0.040 1.000 Uiso c ? ?
H10 0.9186 0.4668 0.7433 0.038 1.000 Uiso c ? ?
H11 0.7178 0.8959 0.8614 0.038 1.000 Uiso c ? ?
H12 0.7479 0.9847 1.0439 0.029 1.000 Uiso c ? ?
H13 0.4646 0.8256 0.9215 0.035 1.000 Uiso c ? ?
H14 0.6578 0.8099 1.0983 0.033 1.000 Uiso c ? ?
H15 0.4103 0.8983 1.2099 0.039 1.000 Uiso c ? ?
H16 0.5769 1.0051 1.2543 0.036 1.000 Uiso c ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 8 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N 0 4 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
P 0 4 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O 0 16 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
H 0 32 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-5 2 -4
-4 2 -6
|
1100691.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/06/1100691.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100691
loop_
_publ_author_name
'Cherni, Saoussen Namouchi'
'Samba, Mohamadou'
'Dachraoui, Mohamed'
_publ_section_title
;
Crystal Structure of Tetrakis(N,N-dimethyl, N'-phenylthiourea-S) cadmium(II)
diperchlorate [Cd((CH~3~)~2~NCSNHPh)~4~](ClO~4~)~2~
;
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x3
_journal_page_last x4
_journal_paper_doi 10.2116/analscix.20.x3
_journal_volume 20
_journal_year 2004
_chemical_formula_moiety 'C36 H48 Cd Cl2 N8 O8 S4'
_chemical_formula_structural 'Cd S4 Cl2 N8 O8 C36 H48'
_chemical_formula_sum 'C36 H48 Cd Cl2 N8 O8 S4'
_chemical_formula_weight 1032.36
_chemical_name_systematic
;
Tetrakis(N,N-dimethyl,N'-phenylthiourea-S)cadmium(II)diperchlorate
;
_space_group_IT_number 14
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary 'heavy method'
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 106.04(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 11.082(3)
_cell_length_b 35.856(8)
_cell_length_c 12.135(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 14.89
_cell_measurement_theta_min 9.39
_cell_volume 4634(2)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0312
_diffrn_reflns_av_sigmaI/netI 0.0728
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 37
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 5963
_diffrn_reflns_theta_full 21.98
_diffrn_reflns_theta_max 21.98
_diffrn_reflns_theta_min 1.14
_diffrn_standards_decay_% 1.0800
_diffrn_standards_interval_time 120
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 0.822
_exptl_absorpt_correction_T_max 0.8474
_exptl_absorpt_correction_T_min 0.7869
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details '(North, Phillips & Mathews,1968)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.480
_exptl_crystal_description rod
_exptl_crystal_F_000 2120
_exptl_crystal_size_max 0.63
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.525
_refine_diff_density_min -0.829
_refine_diff_density_rms 0.099
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 661
_refine_ls_number_reflns 5620
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.024
_refine_ls_R_factor_all 0.0981
_refine_ls_R_factor_gt 0.0496
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+5.1739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1180
_refine_ls_wR_factor_ref 0.1515
_reflns_number_gt 3717
_reflns_number_total 5620
_reflns_threshold_expression I>2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_original_formula_sum 'C36 H48 Cd1 Cl2 N8 O8 S4'
_cod_database_code 1100691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.11159(5) 0.10965(2) 0.25499(5) 0.0436(2) Uani 1 1 d . . .
S1 S 0.0680(2) 0.10686(7) 0.4491(2) 0.0576(6) Uani 1 1 d . . .
S2 S 0.0550(2) 0.05152(7) 0.1332(2) 0.0603(6) Uani 1 1 d . . .
S3 S 0.0596(2) 0.17560(6) 0.1771(2) 0.0505(5) Uani 1 1 d . . .
S4 S 0.3475(2) 0.10313(8) 0.2846(2) 0.0640(7) Uani 1 1 d . . .
Cl1 Cl 0.1599(2) 0.25090(7) 0.8363(2) 0.0614(6) Uani 1 1 d . . .
Cl2 Cl 0.4394(2) 0.08432(8) 0.8367(2) 0.0669(7) Uani 1 1 d . . .
N1 N 0.2594(5) 0.1732(2) 0.0888(5) 0.042(2) Uani 1 1 d . . .
N2 N 0.4891(6) 0.1273(2) 0.4860(6) 0.055(2) Uani 1 1 d . . .
N3 N 0.2606(7) 0.2205(2) 0.2165(6) 0.050(2) Uani 1 1 d . . .
N4 N -0.1590(8) 0.0667(2) -0.0295(6) 0.053(2) Uani 1 1 d . . .
N5 N 0.8881(6) 0.1591(2) 0.3907(6) 0.051(2) Uani 1 1 d D . .
N6 N -0.1754(6) 0.0240(2) 0.1057(6) 0.057(2) Uani 1 1 d . . .
N7 N 0.3889(7) 0.0716(2) 0.4948(6) 0.053(2) Uani 1 1 d . . .
N8 N 0.0759(7) 0.1788(2) 0.5099(6) 0.060(2) Uani 1 1 d . . .
O1 O 0.1604(14) 0.2539(4) 0.9572(13) 0.088(4) Uiso 0.53 1 d P . .
O11 O 0.2145(17) 0.2681(5) 0.9471(14) 0.097(5) Uiso 0.47 1 d P . .
O2 O 0.0342(7) 0.2559(3) 0.7774(8) 0.156(4) Uani 1 1 d . . .
O3 O 0.2142(13) 0.2165(4) 0.8218(11) 0.097(4) Uiso 0.70 1 d P . .
O31 O 0.157(2) 0.2119(7) 0.829(2) 0.075(7) Uiso 0.30 1 d P . .
O4 O 0.223(4) 0.2717(11) 0.751(5) 0.086(19) Uiso 0.28 1 d P . .
O41 O 0.195(3) 0.2836(9) 0.797(3) 0.093(13) Uiso 0.39 1 d P . .
O42 O 0.270(5) 0.2666(10) 0.807(5) 0.106(17) Uiso 0.33 1 d P . .
O5 O 0.449(3) 0.1277(7) 0.857(2) 0.074(7) Uiso 0.21 1 d P . .
O51 O 0.3864(19) 0.1249(6) 0.8123(19) 0.061(5) Uiso 0.22 1 d P . .
O52 O 0.366(4) 0.1042(13) 0.745(4) 0.107(13) Uiso 0.29 1 d P . .
O53 O 0.348(2) 0.0857(14) 0.725(2) 0.047(8) Uiso 0.28 1 d P . .
O6 O 0.373(3) 0.0684(9) 0.7393(18) 0.060(6) Uiso 0.32 1 d P . .
O61 O 0.419(4) 0.0543(12) 0.757(3) 0.100(12) Uiso 0.32 1 d P . .
O62 O 0.447(4) 0.0362(12) 0.801(4) 0.095(12) Uiso 0.36 1 d P . .
O7 O 0.4022(7) 0.0730(2) 0.9318(6) 0.092(2) Uani 1 1 d . . .
O8 O 0.5715(12) 0.0919(4) 0.8623(11) 0.064(4) Uiso 0.54 1 d P . .
O81 O 0.5673(15) 0.0744(5) 0.8459(14) 0.075(5) Uiso 0.46 1 d P . .
C1 C 0.3822(8) 0.1847(3) 0.0782(8) 0.059(2) Uani 1 1 d . . .
H1 H 0.3811 0.2109 0.0623 0.07(3) Uiso 1 1 calc R . .
H2 H 0.4011 0.1711 0.0168 0.085 Uiso 1 1 calc R . .
H3 H 0.4452 0.1795 0.1487 0.07(3) Uiso 1 1 calc R . .
C2 C -0.1052(7) 0.0476(2) 0.0656(7) 0.046(2) Uani 1 1 d . . .
C3 C 0.5084(9) 0.1627(3) 0.4304(9) 0.077(3) Uani 1 1 d . . .
H4 H 0.5543 0.1579 0.3754 0.054 Uiso 1 1 calc R . .
H5 H 0.5550 0.1798 0.4875 0.050 Uiso 1 1 calc R . .
H6 H 0.4284 0.1735 0.3923 0.057 Uiso 1 1 calc R . .
C4 C 0.3280(7) 0.0374(2) 0.4521(7) 0.049(2) Uani 1 1 d . . .
C5 C 0.8003(7) 0.1326(2) 0.3279(7) 0.051(2) Uani 1 1 d . . .
C6 C 0.2477(11) 0.2840(3) 0.4519(10) 0.087(3) Uani 1 1 d . . .
H7 H 0.2990 0.2912 0.5231 0.020 Uiso 1 1 calc R . .
C7 C -0.1527(9) 0.1226(3) -0.1365(9) 0.064(3) Uani 1 1 d . . .
C8 C 0.2118(8) 0.2470(2) 0.2820(8) 0.052(2) Uani 1 1 d . . .
C9 C 0.6193(10) 0.0841(4) 0.2104(13) 0.081(4) Uani 1 1 d . . .
C10 C 0.2015(10) 0.1427(3) 0.0137(9) 0.056(2) Uani 1 1 d . . .
C11 C 0.6594(10) 0.1129(4) 0.1517(10) 0.075(3) Uani 1 1 d . . .
C12 C 0.2335(9) 0.0240(3) 0.4967(9) 0.058(2) Uani 1 1 d . . .
C13 C 0.3674(10) 0.0160(3) 0.3721(8) 0.068(3) Uani 1 1 d . . .
C14 C 0.3093(14) -0.0174(3) 0.3383(10) 0.087(4) Uani 1 1 d . . .
C15 C -0.2986(9) 0.0119(3) 0.0340(9) 0.084(3) Uani 1 1 d . . .
H8 H -0.3603 0.0305 0.0358 0.055 Uiso 1 1 calc R . .
H9 H -0.3211 -0.0112 0.0629 0.056 Uiso 1 1 calc R . .
H10 H -0.2949 0.0085 -0.0434 0.054 Uiso 1 1 calc R . .
C16 C -0.0061(9) 0.0745(3) -0.1416(8) 0.064(3) Uani 1 1 d . . .
C17 C 0.7487(9) 0.1375(3) 0.2116(8) 0.065(3) Uani 1 1 d . . .
C18 C -0.1033(7) 0.0885(2) -0.1003(6) 0.046(2) Uani 1 1 d . . .
C19 C 0.2141(12) -0.0309(3) 0.3824(9) 0.081(3) Uani 1 1 d . . .
C20 C 0.7609(9) 0.1034(3) 0.3842(9) 0.060(2) Uani 1 1 d . . .
C21 C 0.0077(8) 0.1517(2) 0.4486(6) 0.049(2) Uani 1 1 d . . .
C22 C 0.1307(13) 0.3001(3) 0.4098(14) 0.091(4) Uani 1 1 d . . .
C23 C 0.6700(10) 0.0787(3) 0.3234(12) 0.074(3) Uani 1 1 d . . .
C24 C 0.0209(13) 0.2157(4) 0.5147(12) 0.087(3) Uani 1 1 d . . .
C25 C 0.4123(7) 0.1005(3) 0.4317(7) 0.051(2) Uani 1 1 d . . .
C26 C 0.5641(10) 0.1234(3) 0.6047(8) 0.079(3) Uani 1 1 d . . .
H11 H 0.5140 0.1298 0.6551 0.051 Uiso 1 1 calc R . .
H12 H 0.6353 0.1398 0.6188 0.051 Uiso 1 1 calc R . .
H13 H 0.5925 0.0981 0.6185 0.058 Uiso 1 1 calc R . .
C27 C 0.0377(10) 0.0966(4) -0.2168(9) 0.079(3) Uani 1 1 d . . .
H14 H 0.1029 0.0879 -0.2443 0.020 Uiso 1 1 calc R . .
C28 C 0.0961(10) 0.2631(3) 0.2400(11) 0.066(3) Uani 1 1 d . . .
C29 C 0.2029(7) 0.1903(2) 0.1578(6) 0.041(2) Uani 1 1 d . . .
C30 C 0.1784(9) -0.0098(3) 0.4615(8) 0.069(3) Uani 1 1 d . . .
H15 H 0.1155 -0.0184 0.4921 0.020 Uiso 1 1 calc R . .
C31 C 0.2101(9) 0.1749(3) 0.5683(9) 0.089(3) Uani 1 1 d . . .
H16 H 0.2202 0.1635 0.6419 0.051 Uiso 1 1 calc R . .
H17 H 0.2489 0.1990 0.5784 0.051 Uiso 1 1 calc R . .
H18 H 0.2489 0.1595 0.5230 0.058 Uiso 1 1 calc R . .
C32 C -0.0127(12) 0.1305(4) -0.2506(9) 0.087(4) Uani 1 1 d . . .
C33 C -0.1089(12) 0.1437(4) -0.2119(10) 0.086(4) Uani 1 1 d . . .
C34 C 0.2885(9) 0.2573(3) 0.3891(9) 0.066(3) Uani 1 1 d . . .
C35 C -0.1363(11) 0.0093(3) 0.2219(8) 0.086(3) Uani 1 1 d . . .
H19 H -0.0616 -0.0054 0.2317 0.057 Uiso 1 1 calc R . .
H20 H -0.2020 -0.0060 0.2351 0.051 Uiso 1 1 calc R . .
H21 H -0.1197 0.0296 0.2757 0.057 Uiso 1 1 calc R . .
C36 C 0.0556(12) 0.2896(3) 0.3065(14) 0.088(4) Uani 1 1 d . . .
H22 H -0.066(10) 0.209(3) 0.540(8) 0.10(3) Uiso 1 1 d . . .
H23 H 0.241(6) 0.118(2) 0.035(5) 0.03(2) Uiso 1 1 d . . .
H24 H 0.005(8) 0.230(3) 0.450(8) 0.06(3) Uiso 1 1 d . . .
H25 H 0.575(7) 0.069(2) 0.168(7) 0.04(3) Uiso 1 1 d . . .
H26 H 0.337(7) -0.033(2) 0.288(7) 0.06(3) Uiso 1 1 d . . .
H27 H 0.785(9) 0.163(3) 0.184(9) 0.10(3) Uiso 1 1 d . . .
H28 H 0.226(7) 0.038(2) 0.545(6) 0.03(2) Uiso 1 1 d . . .
H29 H 0.027(8) 0.147(2) -0.297(7) 0.06(3) Uiso 1 1 d . . .
H30 H 0.370(9) 0.242(2) 0.431(7) 0.08(3) Uiso 1 1 d . . .
H31 H 0.791(9) 0.102(2) 0.463(8) 0.07(3) Uiso 1 1 d . . .
H32 H 0.076(8) 0.234(2) 0.561(7) 0.06(3) Uiso 1 1 d . . .
H33 H 0.214(11) 0.148(3) -0.050(11) 0.12(5) Uiso 1 1 d . . .
H34 H 0.115(9) 0.315(3) 0.457(9) 0.08(4) Uiso 1 1 d . . .
H35 H 0.043(8) 0.054(2) -0.101(7) 0.07(3) Uiso 1 1 d . . .
H36 H -0.214(7) 0.132(2) -0.116(6) 0.04(2) Uiso 1 1 d . . .
H37 H -0.009(9) 0.297(2) 0.272(7) 0.05(3) Uiso 1 1 d . . .
H38 H 0.065(8) 0.258(2) 0.177(7) 0.05(3) Uiso 1 1 d . . .
H39 H 0.166(9) -0.056(3) 0.339(8) 0.10(3) Uiso 1 1 d . . .
H40 H 0.113(9) 0.136(2) 0.019(7) 0.08(3) Uiso 1 1 d . . .
H41 H 0.647(6) 0.059(2) 0.364(6) 0.03(2) Uiso 1 1 d . . .
H42 H 0.604(12) 0.118(3) 0.074(11) 0.13(5) Uiso 1 1 d . . .
H43 H -0.146(9) 0.163(3) -0.236(8) 0.07(3) Uiso 1 1 d . . .
H44 H 0.439(8) 0.025(2) 0.345(7) 0.06(3) Uiso 1 1 d . . .
H45 H 0.332(8) 0.226(2) 0.215(7) 0.05(3) Uiso 1 1 d . . .
H46 H 0.407(8) 0.073(2) 0.568(8) 0.07(3) Uiso 1 1 d . . .
H47 H -0.226(6) 0.0669(17) -0.043(5) 0.009(19) Uiso 1 1 d . . .
H48 H 0.862(8) 0.1821(15) 0.378(7) 0.07(3) Uiso 1 1 d D . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd 0.0404(3) 0.0488(4) 0.0425(3) -0.0026(3) 0.0130(2) 0.0001(3)
S1 0.0618(14) 0.0703(16) 0.0458(12) 0.0127(11) 0.0235(10) 0.0255(12)
S2 0.0502(13) 0.0585(15) 0.0640(14) -0.0161(12) 0.0018(11) 0.0097(11)
S3 0.0363(11) 0.0489(13) 0.0686(14) 0.0076(11) 0.0184(10) 0.0031(9)
S4 0.0396(12) 0.105(2) 0.0480(13) 0.0210(13) 0.0132(10) 0.0181(12)
Cl1 0.0556(14) 0.0529(15) 0.0689(15) 0.0020(11) 0.0059(11) 0.0087(11)
Cl2 0.0457(13) 0.101(2) 0.0501(13) 0.0098(13) 0.0069(11) -0.0148(13)
N1 0.038(4) 0.048(4) 0.042(4) 0.000(3) 0.014(3) -0.002(3)
N2 0.051(4) 0.051(5) 0.063(5) 0.006(4) 0.015(4) 0.005(4)
N3 0.035(4) 0.054(5) 0.066(5) -0.006(4) 0.022(4) 0.002(4)
N4 0.029(5) 0.067(5) 0.061(5) 0.009(4) 0.010(4) -0.005(4)
N5 0.046(5) 0.047(5) 0.059(4) 0.002(4) 0.013(4) 0.011(4)
N6 0.056(5) 0.054(5) 0.064(5) 0.012(4) 0.022(4) -0.003(4)
N7 0.058(5) 0.062(5) 0.039(4) 0.006(4) 0.010(4) -0.008(4)
N8 0.051(5) 0.072(6) 0.059(5) 0.000(4) 0.018(4) 0.003(4)
O2 0.058(5) 0.275(13) 0.117(7) 0.013(8) -0.005(5) 0.063(7)
O7 0.107(6) 0.110(6) 0.071(5) 0.004(4) 0.044(4) -0.022(5)
C1 0.056(6) 0.066(7) 0.061(6) -0.009(5) 0.026(5) -0.007(5)
C2 0.048(5) 0.044(5) 0.045(5) -0.006(4) 0.013(4) 0.004(4)
C3 0.072(7) 0.070(7) 0.094(8) 0.016(6) 0.030(6) 0.002(5)
C4 0.044(5) 0.043(5) 0.048(5) 0.008(4) -0.003(4) 0.001(4)
C5 0.044(5) 0.059(6) 0.050(5) 0.006(5) 0.013(4) 0.019(4)
C6 0.082(8) 0.081(8) 0.094(8) -0.049(7) 0.017(6) -0.007(6)
C7 0.051(6) 0.071(7) 0.073(7) 0.020(6) 0.019(5) 0.006(5)
C8 0.050(5) 0.041(5) 0.071(6) 0.001(4) 0.026(5) -0.002(4)
C9 0.046(6) 0.067(8) 0.126(12) -0.030(9) 0.015(7) -0.001(6)
C10 0.063(7) 0.058(7) 0.052(6) -0.005(5) 0.021(5) -0.005(5)
C11 0.056(6) 0.087(9) 0.074(7) -0.019(7) 0.004(6) 0.020(6)
C12 0.061(6) 0.049(7) 0.060(6) 0.009(5) 0.010(5) 0.002(5)
C13 0.066(7) 0.075(8) 0.059(6) -0.010(5) 0.013(5) 0.005(6)
C14 0.130(11) 0.061(8) 0.064(7) -0.012(6) 0.016(7) 0.006(8)
C15 0.073(7) 0.077(8) 0.108(9) 0.019(6) 0.036(6) -0.018(6)
C16 0.059(6) 0.072(7) 0.062(6) -0.023(6) 0.017(5) -0.012(6)
C17 0.069(7) 0.076(8) 0.051(6) 0.006(5) 0.019(5) 0.021(6)
C18 0.045(5) 0.050(6) 0.042(5) 0.001(4) 0.009(4) -0.010(4)
C19 0.108(9) 0.059(7) 0.056(6) 0.002(6) -0.009(6) -0.011(7)
C20 0.057(6) 0.059(7) 0.066(7) 0.009(5) 0.021(5) 0.010(5)
C21 0.057(6) 0.062(6) 0.034(4) 0.005(4) 0.021(4) 0.005(5)
C22 0.089(10) 0.072(8) 0.128(12) -0.041(8) 0.054(9) -0.021(7)
C23 0.061(7) 0.065(8) 0.101(9) 0.015(7) 0.032(7) 0.013(6)
C24 0.097(10) 0.066(8) 0.089(9) -0.006(7) 0.011(8) -0.010(7)
C25 0.036(5) 0.068(7) 0.048(5) 0.006(5) 0.014(4) 0.018(4)
C26 0.092(7) 0.075(7) 0.067(7) -0.011(5) 0.015(6) -0.031(6)
C27 0.080(7) 0.105(9) 0.067(7) -0.029(7) 0.046(6) -0.028(7)
C28 0.073(8) 0.054(6) 0.071(8) 0.001(6) 0.022(6) 0.003(6)
C29 0.032(4) 0.048(5) 0.039(4) 0.011(4) 0.001(4) -0.005(4)
C30 0.061(6) 0.069(7) 0.069(7) 0.020(6) 0.004(5) -0.015(5)
C31 0.072(7) 0.110(9) 0.086(8) -0.003(7) 0.024(6) -0.009(6)
C32 0.084(9) 0.117(11) 0.055(6) 0.016(7) 0.010(6) -0.039(8)
C33 0.075(8) 0.078(9) 0.095(9) 0.044(7) 0.010(7) 0.007(7)
C34 0.060(6) 0.061(7) 0.075(7) -0.021(5) 0.018(5) -0.016(5)
C35 0.122(9) 0.066(7) 0.083(7) 0.032(6) 0.051(7) 0.039(6)
C36 0.054(8) 0.064(8) 0.143(13) 0.009(8) 0.022(8) 0.008(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Cd S1 115.46(8) . . y
S2 Cd S4 94.92(8) . . y
S1 Cd S4 108.49(7) . . y
S2 Cd S3 123.52(8) . . y
S1 Cd S3 107.41(7) . . y
S4 Cd S3 104.77(8) . . y
C21 S1 Cd 97.6(3) . . y
C2 S2 Cd 113.4(3) . . y
C29 S3 Cd 102.0(3) . . y
C25 S4 Cd 105.5(3) . . y
O41 Cl1 O2 93.0(13) . . y
O2 Cl1 O31 95.5(12) . . y
O41 Cl1 O3 122.6(19) . . y
O2 Cl1 O3 116.9(7) . . y
O31 Cl1 O3 28.0(10) . . y
O41 Cl1 O11 82.5(15) . . y
O2 Cl1 O11 121.5(8) . . y
O31 Cl1 O11 118.8(12) . . y
O3 Cl1 O11 114.0(9) . . y
O41 Cl1 O42 42(2) . . y
O2 Cl1 O42 127(3) . . y
O31 Cl1 O42 111.7(18) . . y
O3 Cl1 O42 83.9(16) . . y
O11 Cl1 O42 84(2) . . y
O41 Cl1 O1 111.3(17) . . y
O2 Cl1 O1 103.3(7) . . y
O31 Cl1 O1 97.7(12) . . y
O3 Cl1 O1 107.7(8) . . y
O11 Cl1 O1 32.7(7) . . y
O42 Cl1 O1 116(2) . . y
O41 Cl1 O4 31.5(12) . . y
O2 Cl1 O4 99(2) . . y
O31 Cl1 O4 116(2) . . y
O3 Cl1 O4 92.9(18) . . y
O11 Cl1 O4 105(2) . . y
O42 Cl1 O4 28.6(14) . . y
O6 Cl2 O7 112.9(9) . . y
O52 Cl2 O7 125.4(15) . . y
O6 Cl2 O61 29.6(16) . . y
O52 Cl2 O61 84(2) . . y
O7 Cl2 O61 108.3(15) . . y
O6 Cl2 O81 104.9(15) . . y
O52 Cl2 O81 122.5(16) . . y
O7 Cl2 O81 112.1(7) . . y
O61 Cl2 O81 80.5(18) . . y
O6 Cl2 O8 123.7(12) . . y
O52 Cl2 O8 114.4(17) . . y
O7 Cl2 O8 113.2(6) . . y
O61 Cl2 O8 104.7(16) . . y
O81 Cl2 O8 26.5(7) . . y
O52 Cl2 O53 29.0(17) . . y
O7 Cl2 O53 119.5(12) . . y
O81 Cl2 O53 120.3(13) . . y
O8 Cl2 O53 127.2(12) . . y
O6 Cl2 O51 98.2(16) . . y
O52 Cl2 O51 42.6(18) . . y
O7 Cl2 O51 104.3(8) . . y
O61 Cl2 O51 126(2) . . y
O81 Cl2 O51 123.7(10) . . y
O8 Cl2 O51 99.8(10) . . y
O6 Cl2 O5 124.0(17) . . y
O7 Cl2 O5 100.5(9) . . y
O81 Cl2 O5 102.0(12) . . y
O51 Cl2 O5 28.1(9) . . y
O6 Cl2 O62 54.8(19) . . y
O52 Cl2 O62 111(2) . . y
O7 Cl2 O62 87.9(14) . . y
O61 Cl2 O62 27.5(18) . . y
O81 Cl2 O62 70.7(14) . . y
O8 Cl2 O62 97.2(13) . . y
O53 Cl2 O62 83(2) . . y
C29 N1 C10 122.7(7) . . y
C29 N1 C1 122.6(7) . . y
C10 N1 C1 114.7(7) . . y
C25 N2 C26 122.1(7) . . y
C25 N2 C3 123.1(8) . . y
C26 N2 C3 114.7(8) . . y
C29 N3 C8 128.6(7) . . y
C29 N3 H45 119(6) . . y
C8 N3 H45 112(6) . . y
C2 N4 C18 129.9(8) . . y
C2 N4 H47 113(5) . . y
C18 N4 H47 117(5) . . y
C21 N5 C5 125.5(7) 1_655 . y
C21 N5 H48 120(6) 1_655 . y
C5 N5 H48 113(6) . . y
C2 N6 C35 122.6(8) . . y
C2 N6 C15 121.0(7) . . y
C35 N6 C15 116.4(8) . . y
C25 N7 C4 126.7(7) . . y
C25 N7 H46 120(6) . . y
C4 N7 H46 113(6) . . y
C21 N8 C24 120.4(8) . . y
C21 N8 C31 123.0(8) . . y
C24 N8 C31 116.4(9) . . y
O11 O1 Cl1 72.4(18) . . y
O1 O11 Cl1 74.9(18) . . y
O31 O3 Cl1 76(3) . . n
O3 O31 Cl1 76(3) . . n
O42 O4 O41 79(6) . . n
O42 O4 Cl1 67(4) . . n
O41 O4 Cl1 59(3) . . n
O4 O41 O42 48(3) . . n
O4 O41 Cl1 89(4) . . n
O42 O41 Cl1 75(3) . . n
O4 O42 O41 54(4) . . n
O4 O42 Cl1 84(5) . . n
O41 O42 Cl1 64(2) . . n
O51 O5 Cl2 75(3) . . n
O51 O5 O52 32(2) . . n
Cl2 O5 O52 50.7(15) . . n
O5 O51 Cl2 76(3) . . n
O52 O51 Cl2 60(2) . . n
O52 O51 O53 12(2) . . n
Cl2 O51 O53 51.7(12) . . n
O53 O52 Cl2 81(4) . . n
O51 O52 Cl2 78(3) . . n
O6 O52 Cl2 59.9(18) . . n
O51 O52 O5 22.0(17) . . n
O6 O52 O5 122(3) . . n
Cl2 O52 O5 61.7(19) . . n
O52 O53 O61 126(5) . . n
O6 O53 Cl2 67(3) . . n
O52 O53 Cl2 70(4) . . n
O61 O53 Cl2 60.5(18) . . n
O6 O53 O51 125(4) . . n
O52 O53 O51 18(4) . . n
O61 O53 O51 118(2) . . n
Cl2 O53 O51 58.0(13) . . n
O61 O6 O52 138(5) . . n
O61 O6 Cl2 82(4) . . n
O61 O6 O62 17(4) . . n
O52 O6 O62 141(3) . . n
Cl2 O6 O62 78(2) . . n
O62 O61 O53 154(5) . . n
O6 O61 Cl2 69(4) . . n
O62 O61 Cl2 101(5) . . n
O53 O61 Cl2 63(2) . . n
O61 O62 O6 15(3) . . n
O61 O62 Cl2 51(4) . . n
O6 O62 Cl2 47.1(14) . . n
O81 O8 Cl2 77(2) . . n
O8 O81 Cl2 77(2) . . n
N1 C1 H1 109.5 . . y
N1 C1 H2 109.5 . . y
H1 C1 H2 109.5 . . y
N1 C1 H3 109.5 . . y
H1 C1 H3 109.5 . . y
H2 C1 H3 109.5 . . y
N6 C2 N4 118.5(7) . . y
N6 C2 S2 120.2(6) . . y
N4 C2 S2 121.2(7) . . y
N2 C3 H4 109.5 . . y
N2 C3 H5 109.5 . . y
H4 C3 H5 109.5 . . y
N2 C3 H6 109.5 . . y
H4 C3 H6 109.5 . . y
H5 C3 H6 109.5 . . y
C12 C4 C13 119.6(9) . . y
C12 C4 N7 119.2(8) . . y
C13 C4 N7 121.0(8) . . y
C17 C5 C20 120.2(10) . . y
C17 C5 N5 119.4(9) . . y
C20 C5 N5 120.2(8) . . y
C34 C6 C22 120.3(11) . . y
C34 C6 H7 119.8 . . y
C22 C6 H7 119.8 . . y
C18 C7 C33 121.6(11) . . y
C18 C7 H36 124(5) . . y
C33 C7 H36 115(5) . . y
C28 C8 C34 120.2(9) . . y
C28 C8 N3 122.0(9) . . y
C34 C8 N3 117.7(8) . . y
C23 C9 C11 121.6(11) . . y
C23 C9 H25 125(6) . . y
C11 C9 H25 112(6) . . y
N1 C10 H23 115(4) . . y
N1 C10 H33 105(8) . . y
H23 C10 H33 105(9) . . y
N1 C10 H40 114(5) . . y
H23 C10 H40 97(6) . . y
H33 C10 H40 121(10) . . y
C17 C11 C9 119.3(11) . . y
C17 C11 H42 124(7) . . y
C9 C11 H42 114(7) . . y
C30 C12 C4 120.2(10) . . y
C30 C12 H28 132(6) . . y
C4 C12 H28 108(5) . . y
C14 C13 C4 118.5(11) . . y
C14 C13 H44 122(5) . . y
C4 C13 H44 120(5) . . y
C13 C14 C19 122.2(12) . . y
C13 C14 H26 121(5) . . y
C19 C14 H26 117(5) . . y
N6 C15 H8 109.5 . . y
N6 C15 H9 109.5 . . y
H8 C15 H9 109.5 . . y
N6 C15 H10 109.5 . . y
H8 C15 H10 109.5 . . y
H9 C15 H10 109.5 . . y
C27 C16 C18 118.2(10) . . y
C27 C16 H35 121(5) . . y
C18 C16 H35 118(5) . . y
C11 C17 C5 119.6(11) . . y
C11 C17 H27 130(5) . . y
C5 C17 H27 110(5) . . y
C7 C18 C16 119.2(9) . . y
C7 C18 N4 119.0(8) . . y
C16 C18 N4 121.6(8) . . y
C30 C19 C14 118.2(11) . . y
C30 C19 H39 127(5) . . y
C14 C19 H39 115(5) . . y
C5 C20 C23 120.0(10) . . y
C5 C20 H31 118(6) . . y
C23 C20 H31 121(6) . . y
N8 C21 N5 118.5(8) . 1_455 y
N8 C21 S1 121.1(7) . . y
N5 C21 S1 120.3(7) 1_455 . y
C36 C22 C6 120.0(12) . . y
C36 C22 H34 129(7) . . y
C6 C22 H34 111(7) . . y
C9 C23 C20 119.2(11) . . y
C9 C23 H41 123(4) . . y
C20 C23 H41 118(4) . . y
N8 C24 H22 102(5) . . y
N8 C24 H24 117(6) . . y
H22 C24 H24 113(8) . . y
N8 C24 H32 115(5) . . y
H22 C24 H32 116(7) . . y
H24 C24 H32 94(7) . . y
N2 C25 N7 117.9(7) . . y
N2 C25 S4 119.8(7) . . y
N7 C25 S4 122.3(7) . . y
N2 C26 H11 109.5 . . y
N2 C26 H12 109.5 . . y
H11 C26 H12 109.5 . . y
N2 C26 H13 109.5 . . y
H11 C26 H13 109.5 . . y
H12 C26 H13 109.5 . . y
C32 C27 C16 121.3(11) . . y
C32 C27 H14 119.3 . . y
C16 C27 H14 119.3 . . y
C8 C28 C36 119.3(12) . . y
C8 C28 H38 113(7) . . y
C36 C28 H38 127(7) . . y
N1 C29 N3 117.7(7) . . y
N1 C29 S3 123.3(6) . . y
N3 C29 S3 118.9(6) . . y
C19 C30 C12 121.3(10) . . y
C19 C30 H15 119.3 . . y
C12 C30 H15 119.3 . . y
N8 C31 H16 109.5 . . y
N8 C31 H17 109.5 . . y
H16 C31 H17 109.5 . . y
N8 C31 H18 109.5 . . y
H16 C31 H18 109.5 . . y
H17 C31 H18 109.5 . . y
C27 C32 C33 120.3(11) . . y
C27 C32 H29 119(5) . . y
C33 C32 H29 120(5) . . y
C32 C33 C7 119.4(12) . . y
C32 C33 H43 122(7) . . y
C7 C33 H43 118(7) . . y
C6 C34 C8 119.5(10) . . y
C6 C34 H30 117(5) . . y
C8 C34 H30 122(5) . . y
N6 C35 H19 109.5 . . y
N6 C35 H20 109.5 . . y
H19 C35 H20 109.5 . . y
N6 C35 H21 109.5 . . y
H19 C35 H21 109.5 . . y
H20 C35 H21 109.5 . . y
C22 C36 C28 120.7(12) . . y
C22 C36 H37 131(7) . . y
C28 C36 H37 109(7) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd S2 2.532(2) . y
Cd S1 2.534(2) . y
Cd S4 2.550(2) . y
Cd S3 2.553(2) . y
S1 C21 1.741(9) . y
S2 C2 1.743(8) . y
S3 C29 1.750(7) . y
S4 C25 1.733(8) . y
Cl1 O41 1.36(2) . y
Cl1 O2 1.390(7) . y
Cl1 O31 1.40(2) . y
Cl1 O3 1.40(1) . y
Cl1 O11 1.45(2) . y
Cl1 O42 1.47(3) . y
Cl1 O1 1.47(1) . y
Cl1 O4 1.58(4) . y
Cl2 O6 1.34(2) . y
Cl2 O52 1.38(4) . y
Cl2 O7 1.390(7) . y
Cl2 O61 1.42(4) . y
Cl2 O81 1.43(2) . y
Cl2 O8 1.44(1) . y
Cl2 O53 1.45(3) . y
Cl2 O51 1.57(2) . y
Cl2 O5 1.57(2) . y
Cl2 O62 1.79(4) . y
N1 C29 1.326(9) . y
N1 C10 1.45(1) . y
N1 C1 1.46(1) . y
N2 C25 1.33(1) . y
N2 C26 1.46(1) . y
N2 C3 1.48(1) . y
N3 C29 1.35(1) . y
N3 C8 1.44(1) . y
N3 H45 0.82(8) . y
N4 C2 1.33(1) . y
N4 C18 1.42(1) . y
N4 H47 0.72(6) . y
N5 C21 1.34(1) 1_655 y
N5 C5 1.42(1) . y
N5 H48 0.87(5) . y
N6 C2 1.33(1) . y
N6 C35 1.46(1) . y
N6 C15 1.47(1) . y
N7 C25 1.36(1) . y
N7 C4 1.42(1) . y
N7 H46 0.86(9) . y
N8 C21 1.32(1) . y
N8 C24 1.46(1) . y
N8 C31 1.47(1) . y
O1 O11 0.82(2) . y
O3 O31 0.68(3) . y
O4 O42 0.76(4) . y
O4 O41 0.83(3) . y
O41 O42 1.01(5) . y
O5 O51 0.76(2) . y
O51 O52 1.08(4) . y
O52 O53 0.71(4) . y
O6 O61 0.71(4) . y
O61 O62 0.84(5) . y
O8 O81 0.66(2) . y
C1 H1 0.9600 . y
C1 H2 0.9600 . y
C1 H3 0.9600 . y
C3 H4 0.9600 . y
C3 H5 0.9600 . y
C3 H6 0.9600 . y
C4 C12 1.39(1) . y
C4 C13 1.40(1) . y
C5 C17 1.38(1) . y
C5 C20 1.38(1) . y
C6 C34 1.37(1) . y
C6 C22 1.38(2) . y
C6 H7 0.9300 . y
C7 C18 1.36(1) . y
C7 C33 1.38(1) . y
C7 H36 0.85(8) . y
C8 C28 1.37(1) . y
C8 C34 1.39(1) . y
C9 C23 1.34(2) . y
C9 C11 1.40(2) . y
C9 H25 0.81(8) . y
C10 H23 0.98(7) . y
C10 H33 0.85(13) . y
C10 H40 1.03(10) . y
C11 C17 1.37(1) . y
C11 H42 0.99(13) . y
C12 C30 1.37(1) . y
C12 H28 0.80(7) . y
C13 C14 1.37(1) . y
C13 H44 0.99(8) . y
C14 C19 1.39(2) . y
C14 H26 0.95(8) . y
C15 H8 0.9600 . y
C15 H9 0.9600 . y
C15 H10 0.9600 . y
C16 C27 1.39(1) . y
C16 C18 1.40(1) . y
C16 H35 0.97(9) . y
C17 H27 1.09(10) . y
C19 C30 1.36(1) . y
C19 H39 1.11(10) . y
C20 C23 1.39(1) . y
C20 H31 0.93(9) . y
C21 N5 1.34(1) 1_455 y
C22 C36 1.35(2) . y
C22 H34 0.83(10) . y
C23 H41 0.94(7) . y
C24 H22 1.12(10) . y
C24 H24 0.92(9) . y
C24 H32 0.96(9) . y
C26 H11 0.9600 . y
C26 H12 0.9600 . y
C26 H13 0.9600 . y
C27 C32 1.35(2) . y
C27 H14 0.9300 . y
C28 C36 1.40(2) . y
C28 H38 0.77(8) . y
C30 H15 0.9300 . y
C31 H16 0.9600 . y
C31 H17 0.9600 . y
C31 H18 0.9600 . y
C32 C33 1.36(2) . y
C32 H29 0.99(9) . y
C33 H43 0.81(9) . y
C34 H30 1.06(9) . y
C35 H19 0.9600 . y
C35 H20 0.9600 . y
C35 H21 0.9600 . y
C36 H37 0.77(8) . y
|
1100692.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/06/1100692.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1100692
loop_
_publ_author_name
'Falah, Chiraz'
'Boughzala, Habib'
'Jouini, Tahar'
_publ_section_title
;
Preparation and the Crystal Structure of Non-centrosymmetric
K~6~Bi~2~(P~2~O~7~)~3~
;
_journal_coden_ASTM XSAOAF
_journal_name_full
;
Analytical Sciences: X-ray Structure Analysis Online
;
_journal_page_first x17
_journal_page_last x18
_journal_paper_doi 10.2116/analscix.20.x17
_journal_volume 20
_journal_year 2004
_chemical_formula_moiety 'Bi2 K6 O21 P6'
_chemical_formula_sum 'Bi2 K6 O21 P6'
_chemical_formula_weight 1174.38
_chemical_name_systematic
;
hexapotassium dibismuth diphosphate
;
_space_group_IT_number 1
_space_group_name_Hall 'P 1'
_space_group_name_H-M_alt 'P 1'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall 'P 1'
_symmetry_space_group_name_H-M 'P 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 111.87(2)
_cell_angle_beta 104.25(2)
_cell_angle_gamma 102.00(2)
_cell_formula_units_Z 1
_cell_length_a 6.985(2)
_cell_length_b 9.045(2)
_cell_length_c 10.256(3)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 14
_cell_measurement_theta_min 10
_cell_volume 549.5(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type 'diffractometer CAD4'
_diffrn_measurement_method \w/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0447
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 2754
_diffrn_reflns_theta_max 27.98
_diffrn_reflns_theta_min 2.57
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 120
_diffrn_standards_number 2
_exptl_absorpt_coefficient_mu 17.659
_exptl_absorpt_correction_T_max 0.2866
_exptl_absorpt_correction_T_min 0.1871
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 3.549
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description parallelipipedic
_exptl_crystal_F_000 538
_exptl_crystal_size_max 0.12
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.07
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.00
_refine_ls_extinction_coef 0.0087(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 158
_refine_ls_number_reflns 2754
_refine_ls_number_restraints 4
_refine_ls_restrained_S_all 1.052
_refine_ls_R_factor_all 0.0770
_refine_ls_R_factor_gt 0.0732
_refine_ls_shift/su_max 0.040
_refine_ls_shift/su_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+71.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1715
_refine_ls_wR_factor_ref 0.1753
_reflns_number_gt 2651
_reflns_number_total 2754
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (77 times).
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
The following automatic conversions were performed:
'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.
Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas
;
_cod_database_code 1100692
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.67687(13) 0.66883(12) 0.85113(12) 0.0042(4) Uiso 1 1 d . . .
Bi2 Bi 0.3217(3) 0.3305(2) 0.1483(2) 0.0271(6) Uiso 1 1 d . . .
P1 P 0.8382(17) 0.0825(14) 0.8579(12) 0.016(2) Uiso 1 1 d . . .
P2 P 0.574(2) 0.3016(19) 0.8679(17) 0.027(3) Uiso 1 1 d . . .
P3 P 0.434(2) 0.7029(16) 0.1198(16) 0.025(3) Uiso 1 1 d . . .
P4 P 0.170(2) 0.9106(16) 0.1153(15) 0.028(3) Uiso 1 1 d . . .
P5 P 0.2671(16) 0.4239(13) 0.4921(11) 0.0228(19) Uiso 1 1 d . . .
P6 P 0.6830(15) 0.3908(12) 0.4949(11) 0.0204(18) Uiso 1 1 d . . .
K1 K 0.943(2) 0.5979(18) 0.2386(18) 0.044(3) Uiso 1 1 d . . .
K2 K 0.2609(19) 0.8894(14) 0.8138(14) 0.035(2) Uiso 1 1 d . . .
K3 K 0.070(2) 0.4206(15) 0.7785(15) 0.035(3) Uiso 1 1 d . . .
K4 K 0.768(2) 0.1270(16) 0.2183(15) 0.040(3) Uiso 1 1 d . . .
K5 K 0.628(2) 0.7536(17) 0.5102(16) 0.054(3) Uiso 1 1 d . . .
K6' K 0.251(7) 0.040(3) 0.498(3) 0.045(10) Uiso 0.47(9) 1 d P . .
K6'' K 0.163(7) 0.031(3) 0.501(3) 0.051(9) Uiso 0.53(9) 1 d P . .
O1 O 0.932(7) 0.018(6) 0.745(6) 0.060(11) Uiso 1 1 d . . .
O2 O 0.969(5) 0.214(4) 0.009(4) 0.031(7) Uiso 1 1 d . . .
O3 O 0.686(4) 0.928(4) 0.844(3) 0.020(6) Uiso 1 1 d . . .
O4 O 0.698(5) 0.180(4) 0.794(3) 0.025(6) Uiso 1 1 d . . .
O5 O 0.754(5) 0.479(4) 0.950(3) 0.026(6) Uiso 1 1 d . . .
O6 O 0.551(5) 0.288(4) 0.015(4) 0.032(7) Uiso 1 1 d . . .
O7 O 0.395(4) 0.295(3) 0.759(3) 0.024(5) Uiso 1 1 d . . .
O8 O 0.652(6) 0.764(5) 0.210(4) 0.044(8) Uiso 1 1 d . . .
O9 O 0.484(5) 0.761(4) 0.016(4) 0.025(6) Uiso 1 1 d . . .
O10 O 0.316(7) 0.551(6) 0.109(5) 0.057(11) Uiso 1 1 d . . .
O11 O 0.348(4) 0.852(4) 0.203(3) 0.026(7) Uiso 1 1 d . . .
O12 O 0.295(6) 0.059(5) 0.116(4) 0.040(9) Uiso 1 1 d . . .
O13 O 0.005(6) 0.928(5) 0.200(5) 0.043(9) Uiso 1 1 d . . .
O14 O 0.038(5) 0.777(4) 0.953(4) 0.030(7) Uiso 1 1 d . . .
O15 O 0.209(6) 0.442(4) 0.361(4) 0.033(8) Uiso 1 1 d . . .
O16 O 0.448(4) 0.335(4) 0.491(3) 0.026(6) Uiso 1 1 d . . .
O17 O 0.336(5) 0.584(4) 0.648(3) 0.019(6) Uiso 1 1 d . . .
O18 O 0.084(7) 0.313(6) 0.486(5) 0.060(11) Uiso 1 1 d . . .
O19 O 0.634(5) 0.413(4) 0.364(4) 0.024(7) Uiso 1 1 d . . .
O20 O 0.762(4) 0.538(3) 0.645(3) 0.015(5) Uiso 1 1 d . . .
O21 O 0.779(4) 0.253(3) 0.494(3) 0.025(5) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi1 O14 2.31(3) 1_655 y
Bi1 O20 2.30(3) . y
Bi1 O5 2.38(3) . y
Bi1 O3 2.36(3) . y
Bi1 O9 2.43(3) 1_556 y
Bi1 O17 2.49(3) . y
Bi1 K5 3.801(14) . ?
Bi1 K2 3.873(11) . ?
Bi1 K3 3.933(12) 1_655 ?
Bi1 K3 4.099(14) . ?
Bi1 K4 4.226(13) 1_566 ?
Bi1 K1 4.293(16) 1_556 ?
Bi2 O10 2.18(4) . y
Bi2 O2 2.30(3) 1_455 y
Bi2 O12 2.32(4) . y
Bi2 O6 2.35(3) . y
Bi2 O15 2.44(4) . y
Bi2 O19 2.43(3) . y
Bi2 K5 3.885(14) . ?
Bi2 K1 3.986(15) 1_455 ?
Bi2 K4 3.983(13) . ?
Bi2 K2 4.031(12) 1_544 ?
Bi2 K1 4.188(16) . ?
Bi2 K3 4.216(13) 1_554 ?
P1 O2 1.46(4) 1_556 y
P1 O1 1.47(5) . y
P1 O3 1.50(3) 1_545 y
P1 O4 1.62(3) . y
P1 K5 3.381(18) 1_545 ?
P1 K3 3.618(17) 1_655 ?
P1 K4 3.733(17) 1_556 ?
P1 K2 3.767(15) 1_645 ?
P2 O7 1.43(3) . y
P2 O5 1.58(3) . y
P2 O6 1.60(4) 1_556 y
P2 O4 1.63(3) . y
P2 K6' 3.46(3) . ?
P2 K1 3.61(2) 1_556 ?
P2 K2 3.67(2) 1_545 ?
P2 K6'' 3.65(3) . ?
P2 K3 3.84(2) 1_655 ?
P3 O10 1.40(5) . y
P3 O8 1.43(4) . y
P3 O9 1.43(3) . y
P3 O11 1.63(3) . y
P3 K3 3.39(2) 1_554 ?
P3 K4 3.661(18) 1_565 ?
P3 K5 3.71(2) . ?
P4 O12 1.44(4) 1_565 y
P4 O14 1.53(4) 1_554 y
P4 O13 1.60(4) . y
P4 O11 1.64(3) . y
P4 K2 3.252(18) 1_554 ?
P4 K6' 3.50(3) 1_565 ?
P4 K1 3.728(19) 1_455 ?
P4 K6'' 3.71(3) 1_565 ?
P5 O15 1.39(4) . y
P5 O18 1.42(5) . y
P5 O17 1.57(3) . y
P5 O16 1.64(3) . y
P5 K5 3.394(17) . ?
P5 K6' 3.47(3) . ?
P5 K3 3.543(17) . ?
P5 K6'' 3.51(3) . ?
P5 K4 3.596(17) 1_455 ?
P6 O19 1.41(3) . y
P6 O20 1.48(3) . y
P6 O21 1.53(3) . y
P6 O16 1.60(3) . y
P6 K4 3.234(16) . ?
P6 K3 3.330(16) 1_655 ?
P6 K5 3.333(17) . ?
K1 O5 2.60(3) 1_554 y
K1 O8 2.79(4) . y
K1 O15 2.87(4) 1_655 y
K1 O13 3.12(4) 1_655 y
K1 O6 3.09(4) . y
K1 O10 3.24(5) 1_655 y
K1 O19 3.25(4) . y
K1 O11 3.44(3) 1_655 y
K1 K6'' 3.55(3) 1_665 ?
K1 P2 3.61(2) 1_554 ?
K1 K6' 3.66(3) 1_665 ?
K1 P4 3.728(19) 1_655 ?
K2 O14 2.65(4) . y
K2 O3 2.84(3) . y
K2 O1 2.84(5) 1_465 y
K2 O12 2.82(4) 1_566 y
K2 O17 2.89(3) . y
K2 O9 3.01(3) 1_556 y
K2 O6 3.28(4) 1_566 y
K2 P4 3.252(18) 1_556 ?
K2 P2 3.67(2) 1_565 ?
K2 P1 3.767(15) 1_465 ?
K2 K6'' 3.84(3) 1_565 ?
K3 O21 2.73(3) 1_455 y
K3 O7 2.76(3) . y
K3 O18 2.82(5) . y
K3 O20 2.87(3) 1_455 y
K3 O17 3.00(3) . y
K3 O10 3.02(5) 1_556 y
K3 O4 3.10(3) 1_455 y
K3 O14 3.14(3) . y
K3 O5 3.16(3) 1_455 y
K3 P6 3.330(16) 1_455 ?
K3 O9 3.32(3) 1_556 y
K3 P3 3.39(2) 1_556 ?
K4 O21 2.60(3) . y
K4 O18 2.69(5) 1_655 y
K4 O13 2.68(4) 1_645 y
K4 O19 2.94(3) . y
K4 O9 3.05(3) 1_545 y
K4 O12 3.06(4) . y
K4 O2 3.08(4) . y
K4 O8 3.18(4) 1_545 y
K4 O6 3.22(4) . y
K4 O15 3.28(4) 1_655 y
K4 O11 3.36(3) 1_545 y
K5 O1 2.67(5) 1_565 y
K5 O19 2.89(3) . y
K5 O20 2.95(3) . y
K5 O3 3.07(3) . y
K5 O17 3.20(3) . y
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