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1100093.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/00/1100093.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_1100093
loop_
_publ_author_name
'Coing-Boyat, J'
_journal_name_full
;
Bulletin de la Societe Chimique de France (Vol=Year)
;
_journal_page_first 3863
_journal_page_last 3865
_journal_volume 1971
_journal_year 1971
_chemical_formula_structural 'Mg S O4 (H2 O)7'
_chemical_name_mineral Kieserite
_chemical_name_systematic 'Magnesium sulfate hydrate'
_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 116.25
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.891
_cell_length_b 7.624
_cell_length_c 7.549
_cell_volume 355.7
_exptl_crystal_density_meas 2.57
_refine_ls_R_factor_all 0.058
_cod_database_code 1100093
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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 4 c 0.25 0.25 0. 1. 0 d
S1 S6+ 4 e 0. 0.0952(5) 0.25 1. 0 d
O1 O2- 4 e 0. 0.6134(7) 0.25 1. 2 d
O2 O2- 8 f 0.0313(9) 0.2055(5) 0.1058(6) 1. 0 d
O3 O2- 8 f 0.1910(9) -0.0167(5) 0.3515(6) 1. 0 d
H1 H1+ 8 f 0.077(4) 0.542(4) 0.202(3) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
|
1100094.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/00/1100094.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_1100094
loop_
_publ_author_name
'Hawthorne, F C'
'Groat, L A'
'Raudsepp, M'
'Ercit, T S'
_journal_name_full
;
Neues Jahrbuch fuer Mineralogie. Abhandlungen (Band-Nr) (1950-)
;
_journal_page_first 121
_journal_page_last 132
_journal_volume 157
_journal_year 1987
_chemical_formula_structural 'Mg S O4 (H2 O)7'
_chemical_name_mineral Kieserite
_chemical_name_systematic 'Magnesium sulfate hydrate'
_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 117.70(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.891(2)
_cell_length_b 7.624(2)
_cell_length_c 7.645(2)
_cell_volume 355.6
_exptl_crystal_density_meas 2.57
_cod_database_code 1100094
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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 4 b 0. 0.5 0. 1. 0 d
S1 S6+ 4 e 0. 0.15490(8) 0.25 1. 0 d
O1 O2- 8 f 0.1761(2) 0.0447(2) 0.3943(2) 1. 0 d
O2 O2- 8 f 0.0916(2) 0.2676(2) 0.1491(2) 1. 0 d
O3 O2- 4 e 0. 0.6353(3) 0.25 1. 2 d
H1 H1+ 8 f 0.120(3) 0.693(3) 0.296(3) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
|
1100095.cif | #------------------------------------------------------------------------------
#$Date: 2016-11-14 04:19:24 +0200 (Mon, 14 Nov 2016) $
#$Revision: 188422 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/00/1100095.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_1100095
loop_
_publ_author_name
'Hamada, E.'
'Ishizawa, N.'
'Marumo, F.'
'Ohsumi, K.'
'Shimizugawa, Y.'
'Reizen, K.'
'Matsunami, T.'
_publ_section_title
;
Structure of Mg~6~SO~2~(OH)~14~ determined by micro single-crystal X-ray
diffraction
;
_journal_issue 2
_journal_name_full 'Acta Crystallographica B (39,1983-)'
_journal_page_first 266
_journal_page_last 269
_journal_paper_doi 10.1107/S0108768195014443
_journal_volume 52
_journal_year 1996
_chemical_formula_structural 'Mg6 (S O2) (O H)14'
_chemical_formula_sum 'H14 Mg6 O16 S'
_chemical_name_systematic 'Hexamagnesium dihydrogensulfate hydroxide'
_space_group_IT_number 63
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 63
_symmetry_space_group_name_Hall '-C 2c 2c'
_symmetry_space_group_name_H-M 'C c m m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 15.895(1)
_cell_length_b 3.105(1)
_cell_length_c 13.367(1)
_cell_volume 659.7
_exptl_crystal_density_meas 2.3
_refine_ls_R_factor_all 0.073
_cod_database_code 1100095
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y,-z
x,y,1/2-z
-x,y,1/2+z
-x,-y,-z
x,-y,z
-x,-y,1/2+z
x,-y,1/2-z
1/2+x,1/2+y,z
1/2-x,1/2+y,-z
1/2+x,1/2+y,1/2-z
1/2-x,1/2+y,1/2+z
1/2-x,1/2-y,-z
1/2+x,1/2-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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 4 a 0. 0. 0. 1. 0 d
Mg2 Mg2+ 8 f 0.3748(5) 0. 0.1322(6) 1. 0 d
S1 S6+ 4 c 0.1929(12) 0. 0.25 0.5 0 d
O1 O2- 4 c 0.3887(13) 0.5 0.25 1. 1 d
O2 O2- 8 g 0.1404(16) 0.370(16) 0.25 0.5 0 d
O3 O2- 8 f 0.0028(10) 0.5 0.1066(10) 1. 1 d
O4 O2- 8 f 0.1290(9) 0. -0.034(1) 1. 1 d
O5 O2- 8 f 0.2441(10) 0. 0.1511(11) 1. 1 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
|
1100096.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-26 01:39:39 +0300 (Mon, 26 Sep 2022) $
#$Revision: 278162 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/00/1100096.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_1100096
loop_
_publ_author_name
'Baur, W. H.'
'Rolin, J. L.'
_publ_section_title
;
Salt hydrates. IX. The comparison of the crystal structure of magnesium
sulfate pentahydrate with copper sulfate pentahydrate and magnesium chromate
pentahydrate
;
_journal_coden_ASTM ACBCAR
_journal_issue 5
_journal_name_full
;
Acta Crystallographica, Section B: Structural Crystallography
and Crystal Chemistry
;
_journal_page_first 1448
_journal_page_last 1455
_journal_paper_doi 10.1107/S0567740872004443
_journal_volume 28
_journal_year 1972
_chemical_formula_structural 'Mg S O4 (H2 O)5'
_chemical_formula_sum 'H10 Mg O9 S'
_chemical_name_mineral Pentahydrite
_chemical_name_systematic 'Magnesium sulfate(VI) pentahydrate'
_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 81.12(20)
_cell_angle_beta 109.82(20)
_cell_angle_gamma 105.08(5)
_cell_formula_units_Z 2
_cell_length_a 6.314(5)
_cell_length_b 10.565(18)
_cell_length_c 6.030(6)
_cell_volume 364.4
_exptl_crystal_density_meas 1.9
_refine_ls_R_factor_all 0.057
_cod_database_code 1100096
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 1 a 0. 0. 0. 1. 0 d
Mg2 Mg2+ 1 e 0.5 0.5 0. 1. 0 d
S1 S6+ 2 i 0.0371(1) 0.2897(1) 0.6624(1) 1. 0 d
O1 O2- 2 i 0.9464(4) 0.1509(2) 0.7309(3) 1. 0 d
O2 O2- 2 i 0.2680(4) 0.3344(2) 0.8331(3) 1. 0 d
O3 O2- 2 i 0.8808(4) 0.3711(2) 0.6610(3) 1. 0 d
O4 O2- 2 i 0.0590(4) 0.2686(2) 0.4256(3) 1. 0 d
O5 O2- 2 i 0.8279(4) 0.0768(3) 0.1639(4) 1. 0 d
O6 O2- 2 i 0.3086(4) 0.1139(3) 0.1848(4) 1. 0 d
O7 O2- 2 i 0.4745(4) 0.4042(3) 0.3153(4) 1. 0 d
O8 O2- 2 i 0.7567(4) 0.4077(3) 0.0318(4) 1. 0 d
O9 O2- 2 i 0.4589(4) 0.1324(3) 0.6699(4) 1. 0 d
H1 H1+ 2 i 0.908(15) 0.146(8) 0.260(13) 1. 0 d
H2 H1+ 2 i 0.724(14) 0.023(8) 0.230(13) 1. 0 d
H3 H1+ 2 i 0.331(13) 0.192(7) 0.117(12) 1. 0 d
H4 H1+ 2 i 0.336(12) 0.148(8) 0.321(11) 1. 0 d
H5 H1+ 2 i 0.562(13) 0.402(8) 0.411(11) 1. 0 d
H6 H1+ 2 i 0.350(15) 0.392(8) 0.349(10) 1. 0 d
H7 H1+ 2 i 0.786(13) 0.385(9) 0.919(14) 1. 0 d
H8 H1+ 2 i 0.842(13) 0.374(8) 0.179(12) 1. 0 d
H9 H1+ 2 i 0.585(13) 0.115(8) 0.733(11) 1. 0 d
H10 H1+ 2 i 0.433(13) 0.201(9) 0.706(10) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2022-09-26T01:35:00+03:00
;
Corrected multiple values of the '_atom_site_attached_hydrogens' data item
by changing them from '2' to '0' since all hydrogen atoms are represented
using explicit coordinates. Added the summary chemical formula.
;
|
1100097.cif | #------------------------------------------------------------------------------
#$Date: 2023-03-26 11:09:57 +0300 (Sun, 26 Mar 2023) $
#$Revision: 282068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/00/1100097.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_1100097
loop_
_publ_author_name
'Baur, W. H.'
_publ_section_title
;
Zur Kristallchemie der Salzhydrate. Die Kristallstrukturen von
MgSO~4~.4H~2~O (leonhardtit) und FeSO~4~.4H~2~O (rozenit)
;
_journal_coden_ASTM ACCRA9
_journal_issue 9
_journal_name_full 'Acta Crystallographica'
_journal_page_first 815
_journal_page_last 826
_journal_paper_doi 10.1107/S0365110X62002200
_journal_volume 15
_journal_year 1962
_chemical_compound_source Synthetic
_chemical_formula_moiety 'Mg S O4, 4(H2 O)'
_chemical_formula_sum 'H8 Mg O8 S'
_chemical_name_mineral Starkeyite
_chemical_name_systematic 'Magnesium sulfate(VI) tetrahydrate'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_cell_angle_alpha 90
_cell_angle_beta 90.85(17)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 5.922(6)
_cell_length_b 13.604(4)
_cell_length_c 7.905(5)
_cell_volume 636.8
_database_code_amcsd 0009275
_exptl_crystal_density_diffrn 2.007
_exptl_crystal_density_meas 2.01
_refine_ls_R_factor_all 0.078
_cod_depositor_comments
;
Adding the _chemical_formula_moiety and _chemical_formula_sum data items.
Antanas Vaitkus,
2017-09-09
;
_cod_database_code 1100097
loop_
_space_group_symop_id
_space_group_symop_operation_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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_U_iso_or_equiv
Mg1 Mg2+ 4 e 0.0694(6) 0.1028(3) 0.2213(4) 1 d 0.01393
S1 S6+ 4 e 0.1957(3) 0.1068(1) 0.8259(2) 1 d 0.01013
O1 O2- 4 e 0.0058(8) 0.0461(4) 0.7595(6) 1 d 0.01646
O2 O2- 4 e 0.2485(8) 0.0772(4) 0.0024(6) 1 d 0.01646
O3 O2- 4 e 0.3983(8) 0.0911(4) 0.7227(6) 1 d 0.01646
O4 O2- 4 e 0.1290(8) 0.2112(4) 0.8145(6) 1 d 0.01646
O5 O2- 4 e 0.3555(11) 0.0748(5) 0.3591(8) 1 d 0.02280
O6 O2- 4 e 0.7718(11) 0.1394(5) 0.0910(8) 1 d 0.02280
O7 O2- 4 e 0.8907(11) 0.1273(5) 0.4405(8) 1 d 0.02280
O8 O2- 4 e 0.1778(11) 0.2491(5) 0.2195(8) 1 d 0.02280
H1 H1+ 4 e 0.36(1) 0.070(4) 0.485(7) 1 d 0.03040
H2 H1+ 4 e 0.444(10) 0.017(4) 0.323(7) 1 d 0.03040
H3 H1+ 4 e 0.682(10) 0.198(4) 0.092(7) 1 d 0.03040
H4 H1+ 4 e 0.684(10) 0.098(4) 0.017(7) 1 d 0.03040
H5 H1+ 4 e 0.766(10) 0.171(4) 0.463(7) 1 d 0.03040
H6 H1+ 4 e 0.935(10) 0.096(4) 0.547(7) 1 d 0.03040
H7 H1+ 4 e 0.322(10) 0.242(4) 0.275(7) 1 d 0.03040
H8 H1+ 4 e 0.62(1) 0.190(4) 0.759(7) 1 d 0.03040
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0009275
|
1100098.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/00/1100098.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_1100098
loop_
_publ_author_name
'Yamnova, N A'
'Pushcharovskii, D Y'
'Apollonov, V N'
_journal_name_full 'Vestnik Moskovskogo Universiteta, Geologiya'
_journal_page_first 73
_journal_page_last 75
_journal_volume 5
_journal_year 1989
_chemical_name_mineral Caminite
_chemical_name_systematic 'Magnesium bis(sulfate(VI)) dihydroxide'
_space_group_IT_number 141
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall '-I 4bd 2'
_symmetry_space_group_name_H-M 'I 41/a m d :2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 5.254(2)
_cell_length_b 5.254(2)
_cell_length_c 12.971(7)
_cell_volume 358.1
_exptl_crystal_density_meas 2.8
_refine_ls_R_factor_all 0.12
_cod_original_sg_symbol_H-M 'I 41/a m d Z'
_cod_database_code 1100098
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,1/2-y,z
1/4+y,1/4+x,3/4+z
1/4+y,1/4-x,3/4+z
-x,y,z
-x,1/2-y,z
3/4-y,1/4+x,3/4+z
3/4-y,1/4-x,3/4+z
-x,-y,-z
-x,1/2+y,-z
3/4-y,3/4-x,1/4-z
3/4-y,3/4+x,1/4-z
x,-y,-z
x,1/2+y,-z
1/4+y,3/4-x,1/4-z
1/4+y,3/4+x,1/4-z
1/2+x,1/2+y,1/2+z
1/2+x,-y,1/2+z
3/4+y,3/4+x,1/4+z
3/4+y,3/4-x,1/4+z
1/2-x,1/2+y,1/2+z
1/2-x,-y,1/2+z
1/4-y,3/4+x,1/4+z
1/4-y,3/4-x,1/4+z
1/2-x,1/2-y,1/2-z
1/2-x,y,1/2-z
1/4-y,1/4-x,3/4-z
1/4-y,1/4+x,3/4-z
1/2+x,1/2-y,1/2-z
1/2+x,y,1/2-z
3/4+y,1/4-x,3/4-z
3/4+y,1/4+x,3/4-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
S1 S6+ 4 a 0. 0.75 0.125 1. 0 d
Mg1 Mg2+ 8 d 0. 0. 0.5 0.75 0 d
O1 O2- 16 h 0. 0.5200(5) 0.1888(2) 1. 0 d
O2 O2- 4 b 0. 0.25 0.375 1. 1 d
H1 H1+ 16 h 0. 0.475 0.388 0.25 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
S6+ 6.000
Mg2+ 2.000
O2- -2.000
H1+ 1.000
|
1100099.cif | #------------------------------------------------------------------------------
#$Date: 2016-11-14 06:39:14 +0200 (Mon, 14 Nov 2016) $
#$Revision: 188424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/00/1100099.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_1100099
loop_
_publ_author_name
'Fleet, M. E.'
'Knipe, S. W.'
_publ_section_title
;
Structure of magnesium hydroxide sulfate (2(Mg S O4) . (Mg (O H)2)) and
solid solution in magnesium hydroxide sulfate hydrate and caminite
;
_journal_issue 3
_journal_name_full 'Acta Crystallographica B (39,1983-)'
_journal_page_first 358
_journal_page_last 363
_journal_paper_doi 10.1107/S0108768197000104
_journal_volume 53
_journal_year 1997
_chemical_formula_structural '(Mg (S O4))2 (Mg (O H)2)'
_chemical_formula_sum 'H2 Mg3 O10 S2'
_chemical_name_systematic 'Trimagnesium bis(sulfate(VI)) dihydroxide'
_space_group_IT_number 96
_symmetry_cell_setting tetragonal
_symmetry_Int_Tables_number 96
_symmetry_space_group_name_Hall 'P 4nw 2abw'
_symmetry_space_group_name_H-M 'P 43 21 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.454(1)
_cell_length_b 7.454(1)
_cell_length_c 12.885(2)
_cell_volume 715.9
_cod_database_code 1100099
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,1/2+z
1/2-y,1/2+x,3/4+z
1/2+y,1/2-x,1/4+z
y,x,-z
-y,-x,1/2-z
1/2-x,1/2+y,3/4-z
1/2+x,1/2-y,1/4-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 4 a 0.1239(4) 0.1239(4) 0.5 1. 0 d
Mg2 Mg2+ 8 b 0.1007(2) 0.3555(2) 0.25618(6) 1. 0 d
S1 S6+ 8 b 0.2506(1) 0.99719(9) 0.12740(5) 1. 0 d
O1 O2- 8 b 0.1416(6) 0.1099(6) 0.1943(1) 1. 0 d
O2 O2- 8 b 0.3696(6) 0.8796(6) 0.1897(1) 1. 0 d
O3 O2- 8 b 0.2417(3) 0.4884(3) 0.1378(1) 1. 1 d
O4 O2- 8 b 0.1351(6) 0.8737(6) 0.0669(1) 1. 0 d
O5 O2- 8 b 0.3555(6) 0.1109(7) 0.0586(1) 1. 0 d
H1 H1+ 8 b -1. -1. -1. 1. 0 dum
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
|
1100100.cif | #------------------------------------------------------------------------------
#$Date: 2016-12-27 15:11:05 +0200 (Tue, 27 Dec 2016) $
#$Revision: 189442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100100.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_1100100
loop_
_publ_author_name
'Zalkin, A.'
'Ruben, H.'
'Templeton, D. H.'
_publ_section_title
;
The crystal structure and hydrogen bonding of magnesium sulfate hexahydrate
;
_journal_issue 3
_journal_name_full 'Acta Crystallographica (1,1948-23,1967)'
_journal_page_first 235
_journal_page_last 240
_journal_paper_doi 10.1107/S0365110X64000603
_journal_volume 17
_journal_year 1964
_chemical_formula_structural 'Mg S O4 (H2 O)6'
_chemical_name_mineral Hexahydrite
_chemical_name_systematic 'Magnesium sulfate hexahydrate'
_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 98.30(5)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 10.110(5)
_cell_length_b 7.212(4)
_cell_length_c 24.40999(1000)
_cell_volume 1761.2
_exptl_crystal_density_meas 1.76
_refine_ls_R_factor_all 0.115
_cod_database_code 1100100
_cod_depositor_comments
;
Reducing the number of attached hydrogen atoms from 2 to 0 for
water molecules since explicit coordinates of theese hydrogen
atoms are provided.
Antanas Vaitkus,
2016-12-27
Changing the x coordinate of atom 'H12' from '0.647' to '0.847'
after consulting the original publication.
Antanas Vaitkus,
2016-12-27
;
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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 4 a 0. 0. 0. 1. 0 d
Mg2 Mg2+ 4 e 0. 0.9425(2) 0.25 1. 0 d
S1 S6+ 8 f 0.8659(1) 0.4490(1) 0.1241 1. 0 d
O1 O2- 8 f 0.7747(2) 0.5986(3) 0.1361(1) 1. 0 d
O2 O2- 8 f 0.9834(2) 0.4442(3) 0.1665(1) 1. 0 d
O3 O2- 8 f 0.9096(2) 0.4854(3) 0.0692(1) 1. 0 d
O4 O2- 8 f 0.7961(2) 0.2688(3) 0.1211(1) 1. 0 d
O5 O2- 8 f 0.5852(2) 0.7125(3) 0.0483(1) 1. 0 d
O6 O2- 8 f 0.5393(2) 0.3162(3) 0.0640(1) 1. 0 d
O7 O2- 8 f 0.3126(2) 0.5464(3) 0.0231(1) 1. 0 d
O8 O2- 8 f 0.8887(2) 0.1486(3) 0.2820(1) 1. 0 d
O9 O2- 8 f 0.8884(2) 0.7405(3) 0.2811(1) 1. 0 d
O10 O2- 8 f 0.8598(2) 0.9435(3) 0.1799(1) 1. 0 d
H1 H1+ 8 f 0.643 0.698 0.076 1. 0 d
H2 H1+ 8 f 0.539 0.806 0.045 1. 0 d
H3 H1+ 8 f 0.495 0.232 0.06 1. 0 d
H4 H1+ 8 f 0.614 0.34 0.093 1. 0 d
H5 H1+ 8 f 0.304 0.65 0.055 1. 0 d
H6 H1+ 8 f 0.271 0.544 0.014 1. 0 d
H7 H1+ 8 f 0.84 0.092 0.312 1. 0 d
H8 H1+ 8 f 0.937 0.235 0.296 1. 0 d
H9 H1+ 8 f 0.94 0.651 0.291 1. 0 d
H10 H1+ 8 f 0.82 0.733 0.275 1. 0 d
H11 H1+ 8 f 0.849 0.831 0.164 1. 0 d
H12 H1+ 8 f 0.847 0.033 0.164 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
|
1100101.cif | #------------------------------------------------------------------------------
#$Date: 2023-03-26 11:09:57 +0300 (Sun, 26 Mar 2023) $
#$Revision: 282068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100101.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_1100101
loop_
_publ_author_name
'Calleri, M.'
'Gavetti, A.'
'Ivaldi, G.'
'Rubbo, M.'
_publ_section_title
;
Synthetic epsomite, MgSO~4~ . 7H~2~O: absolute configuration and surface
features of the complementary {111} forms
;
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section B'
_journal_page_first 218
_journal_page_last 222
_journal_paper_doi 10.1107/S0108768184002019
_journal_volume 40
_journal_year 1984
_chemical_compound_source Synthetic
_chemical_formula_moiety 'Mg S O4, 7(H2 O)'
_chemical_formula_sum 'H14 Mg O11 S'
_chemical_name_mineral Epsomite
_chemical_name_systematic 'Magnesium sulfate heptahydrate'
_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 11.887(2)
_cell_length_b 12.013(2)
_cell_length_c 6.861(1)
_cell_volume 979.7
_database_code_amcsd 0021005
_exptl_crystal_density_diffrn 1.671
_exptl_crystal_density_meas 1.68
_cod_depositor_comments
;
Adding the _chemical_formula_moiety and _chemical_formula_sum data items.
Antanas Vaitkus,
2017-09-10
;
_cod_database_code 1100101
loop_
_space_group_symop_operation_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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 4 a 0.42279(3) 0.10616(3) 0.04023(6) 1. 0 d
S1 S6+ 4 a 0.72658(2) 0.18391(2) 0.49046(3) 1. 0 d
O1 O2- 4 a 0.68483(12) 0.07519(8) 0.42752(18) 1. 0 d
O2 O2- 4 a 0.85049(7) 0.18643(9) 0.48316(15) 1. 0 d
O3 O2- 4 a 0.68864(8) 0.20604(10) 0.69088(14) 1. 0 d
O4 O2- 4 a 0.68056(8) 0.27242(8) 0.36211(15) 1. 0 d
O5 O2- 4 a 0.26513(7) 0.17375(9) 0.00335(14) 1. 0 d
O6 O2- 4 a 0.47188(7) 0.24819(7) 0.19796(14) 1. 0 d
O7 O2- 4 a 0.46916(8) 0.17613(9) 0.77947(14) 1. 0 d
O8 O2- 4 a 0.58271(8) 0.04587(9) 0.07720(16) 1. 0 d
O9 O2- 4 a 0.37616(9) 0.96138(7) 0.88932(14) 1. 0 d
O10 O2- 4 a 0.36233(9) 0.03435(9) 0.29140(15) 1. 0 d
O11 O2- 4 a 0.49164(10) 0.43790(8) 0.93903(19) 1. 0 d
H1 H1+ 4 a 0.2343(18) 0.2274(16) 0.075(3) 1. 0 d
H2 H1+ 4 a 0.2395(19) 0.1864(17) -0.1179(28) 1. 0 d
H3 H1+ 4 a 0.4263(15) 0.2639(17) 0.2947(30) 1. 0 d
H4 H1+ 4 a 0.5407(14) 0.2442(17) 0.2528(28) 1. 0 d
H5 H1+ 4 a 0.4397(18) 0.2367(17) 0.7072(34) 1. 0 d
H6 H1+ 4 a 0.5416(15) 0.1857(16) 0.7393(33) 1. 0 d
H7 H1+ 4 a 0.6257(19) 0.0665(19) 0.1858(33) 1. 0 d
H8 H1+ 4 a 0.6100(21) -0.0223(16) 0.0401(34) 1. 0 d
H9 H1+ 4 a 0.3613(18) 0.8905(15) 0.9316(32) 1. 0 d
H10 H1+ 4 a 0.4117(18) 0.9540(18) 0.7849(29) 1. 0 d
H11 H1+ 4 a 0.2896(15) 0.0333(19) 0.3358(35) 1. 0 d
H12 H1+ 4 a 0.4045(18) -0.0009(18) 0.3946(33) 1. 0 d
H13 H1+ 4 a 0.4241(18) 0.4791(17) 0.9345(37) 1. 0 d
H14 H1+ 4 a 0.4746(17) 0.3777(14) 0.9894(33) 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S6+ 6.000
O2- -2.000
H1+ 1.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0021005
|
1100102.cif | #------------------------------------------------------------------------------
#$Date: 2023-04-06 15:31:51 +0300 (Thu, 06 Apr 2023) $
#$Revision: 282478 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100102.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_1100102
loop_
_publ_author_name
'Buchmeier, W.'
'Engelen, B.'
'M\"uller, H.'
_publ_section_title
;
Kristallstruktur von MgSO~3~ * H~2~O
;
_journal_issue 2
_journal_name_full 'Zeitschrift f\"ur Naturforschung B'
_journal_page_first 131
_journal_page_last 134
_journal_paper_doi 10.1515/znb-1998-0201
_journal_volume 53
_journal_year 1998
_chemical_formula_structural 'Mg (S O3) (H2 O)'
_chemical_formula_sum 'H2 Mg O4 S'
_chemical_name_systematic 'Magnesium sulfate(IV) hydrate'
_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 90.49(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.699(1)
_cell_length_b 12.751(3)
_cell_length_c 5.618(1)
_cell_volume 336.6
_database_code_amcsd 0018266
_cod_database_code 1100102
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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
S1 S4+ 4 e 0.4243(2) 0.38783(9) 0.6777(2) 1. 0 d
Mg1 Mg2+ 4 e 0.3476(3) 0.26920(13) 0.1767(3) 1. 0 d
O1 O2- 4 e 0.5594(6) 0.3262(3) 0.4700(6) 1. 0 d
O2 O2- 4 e 0.0600(6) 0.1735(3) 0.3865(6) 1. 0 d
O3 O2- 4 e 0.6163(7) 0.1408(3) 0.1759(6) 1. 0 d
O4 O2- 4 e 0.0644(7) 0.3956(3) 0.1731(6) 1. 0 d
H1 H1+ 4 ? -1. -1. -1. 2. 0 dum
loop_
_atom_type_symbol
_atom_type_oxidation_number
S4+ 4.000
Mg2+ 2.000
O2- -2.000
H1+ 1.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0018266
|
1100103.cif | #------------------------------------------------------------------------------
#$Date: 2016-09-18 22:09:47 +0300 (Sun, 18 Sep 2016) $
#$Revision: 186639 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100103.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_1100103
loop_
_publ_author_name
'Flack, H'
_publ_section_title
;
Etude de la structure cristalline du sulfite de magnesium hexahydrate,
Mg S O3 (H2 O)6
;
_journal_name_full 'Acta Crystallographica B (24,1968-38,1982)'
_journal_page_first 656
_journal_page_last 658
_journal_paper_doi 10.1107/S0567740873003110
_journal_volume 29
_journal_year 1973
_chemical_formula_structural 'Mg (S O3) (H2 O)6'
_chemical_formula_sum 'H12 Mg O9 S'
_chemical_name_systematic 'Magnesium sulfate(IV) hexahydrate'
_space_group_IT_number 146
_symmetry_cell_setting trigonal
_symmetry_space_group_name_Hall 'R 3'
_symmetry_space_group_name_H-M 'R 3 :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 3
_cell_length_a 8.830(1)
_cell_length_b 8.830(1)
_cell_length_c 9.075(1)
_cell_volume 612.8
_exptl_crystal_density_meas 1.73
_refine_ls_R_factor_all 0.059
_cod_original_sg_symbol_H-M 'R 3 H'
_cod_database_code 1100103
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,z
y-x,-x,z
1/3+x,2/3+y,2/3+z
2/3+x,1/3+y,1/3+z
1/3-y,2/3+x-y,2/3+z
2/3-y,1/3+x-y,1/3+z
1/3-x+y,2/3-x,2/3+z
2/3-x+y,1/3-x,1/3+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Mg1 Mg2+ 3 a 0. 0. 0. 1. 0 d
S1 S4+ 3 a 0. 0. 0.5001(6) 1. 0 d
O1 O2- 9 b 0.1271(5) 0.1775(5) 0.4303(6) 1. 0 d
O2 O2- 9 b -0.1951(6) -0.1975(6) -0.1249(5) 1. 2 d
O3 O2- 9 b 0.1845(4) 0.1931(4) 0.1392(4) 1. 2 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Mg2+ 2.000
S4+ 4.000
O2- -2.000
|
1100104.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100104.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_1100104
loop_
_publ_author_name
'J. Androulakis'
'N. Katsarakis'
'J. Giapintzakis'
'N. Vouroutzis'
'E. Pavlidou'
'K. Chrissafis'
'E. K. Polychroniadis'
'V. Perdikatsis'
_publ_section_title
;
LaSrMnCoO6: A new cubic double perovskite oxide
;
_journal_name_full 'Journal of Solid State Chemistry'
_journal_page_first 350
_journal_page_last 354
_journal_paper_doi 10.1016/S0022-4596(03)00109-9
_journal_volume 173
_journal_year 2003
_chemical_formula_sum 'Co La Mn O6 Sr'
_symmetry_space_group_name_H-M 'F m -3 m'
_cell_angle_alpha 90.000
_cell_angle_beta 90.000
_cell_angle_gamma 90.000
_cell_length_a 7.6891
_cell_length_b 7.6891
_cell_length_c 7.6891
_cell_volume 454.60
_cod_original_formula_sum LaSrMnCoO6
_cod_database_code 1100104
loop_
_atom_site_label
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_uiso_or_biso
La 8 c 0.25 0.25 0.25 0.485 0.30
Sr 8 c 0.25 0.25 0.25 0.514 0.28
Mn 4 b 0.5 0 0 1 0.36
Co 4 b 0 0 0 1 0.05
O 24 e 0.2492 0 0 1 1.48
|
1100105.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100105.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_1100105
_chemical_formula_moiety ?
_chemical_formula_sum 'As3 Fe2 Na3 O12'
_chemical_formula_weight 597.43
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_space_group_IT_number 230
_symmetry_cell_setting ?
_symmetry_space_group_name_Hall '-I 4bd 2c 3'
_symmetry_space_group_name_H-M 'I a -3 d'
_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 12.250(2)
_cell_length_b 12.250(2)
_cell_length_c 12.250(2)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1838.3(5)
_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 0.71073
_diffrn_reflns_av_R_equivalents 0.0337
_diffrn_reflns_av_sigmaI/netI 0.0175
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 1241
_diffrn_reflns_theta_full 29.94
_diffrn_reflns_theta_max 29.94
_diffrn_reflns_theta_min 4.07
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 14.091
_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 4.317
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 2240
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.482
_refine_diff_density_min -0.665
_refine_diff_density_rms 0.138
_refine_ls_extinction_coef 0.0076(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 1.368
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 18
_refine_ls_number_reflns 231
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.368
_refine_ls_R_factor_all 0.0225
_refine_ls_R_factor_gt 0.0197
_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^)+(0.0201P)^2^+4.0229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0504
_refine_ls_wR_factor_ref 0.0512
_reflns_number_gt 213
_reflns_number_total 231
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M Ia3d
_cod_database_code 1100105
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'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, x+3/4, -z+3/4'
'y+1/4, -x+1/4, z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y, z, x'
'-y+1/2, -z, x+1/2'
'y, -z, -x+1/2'
'-y+1/2, z, -x'
'-z+1/4, y+3/4, x+1/4'
'-z+1/4, -y+1/4, -x+1/4'
'z+1/4, -y+1/4, x+3/4'
'z+1/4, y+3/4, -x+3/4'
'z, x, y'
'-z, x+1/2, -y+1/2'
'-z, -x+1/2, y'
'z, -x, -y+1/2'
'-x+1/4, -z+1/4, -y+1/4'
'-x+1/4, z+3/4, y+1/4'
'x+3/4, -z+3/4, y+1/4'
'x+1/4, z+3/4, -y+3/4'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, -y+1/2, z+1'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, x+5/4, -z+5/4'
'y+3/4, -x+3/4, z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'y+1/2, z+1/2, x+1/2'
'-y+1, -z+1/2, x+1'
'y+1/2, -z+1/2, -x+1'
'-y+1, z+1/2, -x+1/2'
'-z+3/4, y+5/4, x+3/4'
'-z+3/4, -y+3/4, -x+3/4'
'z+3/4, -y+3/4, x+5/4'
'z+3/4, y+5/4, -x+5/4'
'z+1/2, x+1/2, y+1/2'
'-z+1/2, x+1, -y+1'
'-z+1/2, -x+1, y+1/2'
'z+1/2, -x+1/2, -y+1'
'-x+3/4, -z+3/4, -y+3/4'
'-x+3/4, z+5/4, y+3/4'
'x+5/4, -z+5/4, y+3/4'
'x+3/4, z+5/4, -y+5/4'
'-x, -y, -z'
'-x, y, z-1/2'
'x-1/2, y, -z-1/2'
'x-1/2, -y, z'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, -x-3/4, z-3/4'
'-y-1/4, x-1/4, -z-3/4'
'y-1/4, x-1/4, z-1/4'
'-y, -z, -x'
'y-1/2, z, -x-1/2'
'-y, z, x-1/2'
'y-1/2, -z, x'
'z-1/4, -y-3/4, -x-1/4'
'z-1/4, y-1/4, x-1/4'
'-z-1/4, y-1/4, -x-3/4'
'-z-1/4, -y-3/4, x-3/4'
'-z, -x, -y'
'z, -x-1/2, y-1/2'
'z, x-1/2, -y'
'-z, x, y-1/2'
'x-1/4, z-1/4, y-1/4'
'x-1/4, -z-3/4, -y-1/4'
'-x-3/4, z-3/4, -y-1/4'
'-x-1/4, -z-3/4, y-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x, y+1/2, -z'
'x, -y+1/2, z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, -x-1/4, z-1/4'
'-y+1/4, x+1/4, -z-1/4'
'y+1/4, x+1/4, z+1/4'
'-y+1/2, -z+1/2, -x+1/2'
'y, z+1/2, -x'
'-y+1/2, z+1/2, x'
'y, -z+1/2, x+1/2'
'z+1/4, -y-1/4, -x+1/4'
'z+1/4, y+1/4, x+1/4'
'-z+1/4, y+1/4, -x-1/4'
'-z+1/4, -y-1/4, x-1/4'
'-z+1/2, -x+1/2, -y+1/2'
'z+1/2, -x, y'
'z+1/2, x, -y+1/2'
'-z+1/2, x+1/2, y'
'x+1/4, z+1/4, y+1/4'
'x+1/4, -z-1/4, -y+1/4'
'-x-1/4, z-1/4, -y+1/4'
'-x+1/4, -z-1/4, y-1/4'
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
As As 0.5000 0.2500 0.1250 0.0010(2) Uani 1 4 d S . .
Fe Fe 0.5000 0.5000 0.0000 0.0019(2) Uani 1 6 d S . .
Na Na 0.5000 0.2500 0.3750 0.0075(5) Uani 1 4 d S . .
O1 O 0.54790(13) 0.34738(13) 0.03894(13) 0.0040(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
As 0.0010(2) 0.0010(2) 0.0009(3) 0.000 0.000 0.000
Fe 0.0019(2) 0.0019(2) 0.0019(2) 0.00026(14) -0.00026(14) -0.00026(14)
Na 0.0103(7) 0.0103(7) 0.0020(9) 0.000 0.000 0.0014(7)
O1 0.0056(8) 0.0021(7) 0.0041(7) 0.0015(6) 0.0007(6) -0.0005(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
Na Na 0.0362 0.0249 '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
O1 As O1 112.71(6) 27_554 77_565 ?
O1 As O1 103.17(11) 27_554 . ?
O1 As O1 112.71(6) 77_565 . ?
O1 As O1 112.71(6) 27_554 55_656 ?
O1 As O1 103.17(11) 77_565 55_656 ?
O1 As O1 112.71(6) . 55_656 ?
O1 As Na 51.59(6) 27_554 50_655 ?
O1 As Na 128.41(6) 77_565 50_655 ?
O1 As Na 51.59(6) . 50_655 ?
O1 As Na 128.41(6) 55_656 50_655 ?
O1 As Na 128.41(6) 27_554 . ?
O1 As Na 51.59(6) 77_565 . ?
O1 As Na 128.41(6) . . ?
O1 As Na 51.59(6) 55_656 . ?
Na As Na 180.0 50_655 . ?
O1 Fe O1 180.00(3) 43_554 91 ?
O1 Fe O1 88.95(7) 43_554 84_554 ?
O1 Fe O1 91.05(7) 91 84_554 ?
O1 Fe O1 91.05(7) 43_554 36 ?
O1 Fe O1 88.95(7) 91 36 ?
O1 Fe O1 180.00(9) 84_554 36 ?
O1 Fe O1 88.95(7) 43_554 49_665 ?
O1 Fe O1 91.05(7) 91 49_665 ?
O1 Fe O1 91.05(7) 84_554 49_665 ?
O1 Fe O1 88.95(7) 36 49_665 ?
O1 Fe O1 91.05(7) 43_554 . ?
O1 Fe O1 88.95(7) 91 . ?
O1 Fe O1 88.95(7) 84_554 . ?
O1 Fe O1 91.05(7) 36 . ?
O1 Fe O1 180.00(9) 49_665 . ?
O1 Fe Na 47.56(4) 43_554 50_655 ?
O1 Fe Na 132.44(4) 91 50_655 ?
O1 Fe Na 85.33(5) 84_554 50_655 ?
O1 Fe Na 94.67(5) 36 50_655 ?
O1 Fe Na 136.33(5) 49_665 50_655 ?
O1 Fe Na 43.67(5) . 50_655 ?
O1 Fe Na 132.44(4) 43_554 2_565 ?
O1 Fe Na 47.56(4) 91 2_565 ?
O1 Fe Na 94.67(5) 84_554 2_565 ?
O1 Fe Na 85.33(5) 36 2_565 ?
O1 Fe Na 43.67(5) 49_665 2_565 ?
O1 Fe Na 136.33(5) . 2_565 ?
Na Fe Na 180.0 50_655 2_565 ?
O1 Fe Na 43.67(5) 43_554 85_565 ?
O1 Fe Na 136.33(5) 91 85_565 ?
O1 Fe Na 132.44(4) 84_554 85_565 ?
O1 Fe Na 47.56(4) 36 85_565 ?
O1 Fe Na 85.33(5) 49_665 85_565 ?
O1 Fe Na 94.67(5) . 85_565 ?
Na Fe Na 66.4 50_655 85_565 ?
Na Fe Na 113.6 2_565 85_565 ?
O1 Fe Na 85.33(5) 43_554 10_564 ?
O1 Fe Na 94.67(5) 91 10_564 ?
O1 Fe Na 43.67(5) 84_554 10_564 ?
O1 Fe Na 136.33(5) 36 10_564 ?
O1 Fe Na 47.56(4) 49_665 10_564 ?
O1 Fe Na 132.44(4) . 10_564 ?
Na Fe Na 113.6 50_655 10_564 ?
Na Fe Na 66.4 2_565 10_564 ?
Na Fe Na 113.6 85_565 10_564 ?
O1 Fe Na 94.67(5) 43_554 58_656 ?
O1 Fe Na 85.33(5) 91 58_656 ?
O1 Fe Na 136.33(5) 84_554 58_656 ?
O1 Fe Na 43.67(5) 36 58_656 ?
O1 Fe Na 132.44(4) 49_665 58_656 ?
O1 Fe Na 47.56(4) . 58_656 ?
Na Fe Na 66.4 50_655 58_656 ?
Na Fe Na 113.6 2_565 58_656 ?
Na Fe Na 66.4 85_565 58_656 ?
Na Fe Na 180.0 10_564 58_656 ?
O1 Fe Na 136.33(5) 43_554 37_544 ?
O1 Fe Na 43.67(5) 91 37_544 ?
O1 Fe Na 47.56(4) 84_554 37_544 ?
O1 Fe Na 132.44(4) 36 37_544 ?
O1 Fe Na 94.67(5) 49_665 37_544 ?
O1 Fe Na 85.33(5) . 37_544 ?
Na Fe Na 113.6 50_655 37_544 ?
Na Fe Na 66.4 2_565 37_544 ?
Na Fe Na 180.0 85_565 37_544 ?
Na Fe Na 66.4 10_564 37_544 ?
Na Fe Na 113.6 58_656 37_544 ?
O1 Na O1 67.01(7) 50_656 76 ?
O1 Na O1 117.00(7) 50_656 55_656 ?
O1 Na O1 159.50(8) 76 55_656 ?
O1 Na O1 159.50(8) 50_656 77_565 ?
O1 Na O1 117.00(7) 76 77_565 ?
O1 Na O1 67.01(7) 55_656 77_565 ?
O1 Na O1 91.91(4) 50_656 71_766 ?
O1 Na O1 75.22(6) 76 71_766 ?
O1 Na O1 123.18(3) 55_656 71_766 ?
O1 Na O1 71.00(7) 77_565 71_766 ?
O1 Na O1 123.18(3) 50_656 92_545 ?
O1 Na O1 71.00(7) 76 92_545 ?
O1 Na O1 91.91(4) 55_656 92_545 ?
O1 Na O1 75.22(6) 77_565 92_545 ?
O1 Na O1 112.50(7) 71_766 92_545 ?
O1 Na O1 75.22(6) 50_656 70_566 ?
O1 Na O1 91.91(4) 76 70_566 ?
O1 Na O1 71.00(7) 55_656 70_566 ?
O1 Na O1 123.18(3) 77_565 70_566 ?
O1 Na O1 164.72(7) 71_766 70_566 ?
O1 Na O1 69.68(8) 92_545 70_566 ?
O1 Na O1 71.00(7) 50_656 90_565 ?
O1 Na O1 123.18(3) 76 90_565 ?
O1 Na O1 75.22(6) 55_656 90_565 ?
O1 Na O1 91.91(4) 77_565 90_565 ?
O1 Na O1 69.68(8) 71_766 90_565 ?
O1 Na O1 164.72(7) 92_545 90_565 ?
O1 Na O1 112.50(7) 70_566 90_565 ?
O1 Na As 33.50(4) 50_656 50_656 ?
O1 Na As 33.50(4) 76 50_656 ?
O1 Na As 146.50(4) 55_656 50_656 ?
O1 Na As 146.50(4) 77_565 50_656 ?
O1 Na As 82.36(4) 71_766 50_656 ?
O1 Na As 97.64(4) 92_545 50_656 ?
O1 Na As 82.36(4) 70_566 50_656 ?
O1 Na As 97.64(4) 90_565 50_656 ?
O1 Na As 146.50(4) 50_656 . ?
O1 Na As 146.50(4) 76 . ?
O1 Na As 33.50(4) 55_656 . ?
O1 Na As 33.50(4) 77_565 . ?
O1 Na As 97.64(4) 71_766 . ?
O1 Na As 82.36(4) 92_545 . ?
O1 Na As 97.64(4) 70_566 . ?
O1 Na As 82.36(4) 90_565 . ?
As Na As 180.0 50_656 . ?
O1 Na Fe 35.32(4) 50_656 2_565 ?
O1 Na Fe 94.02(4) 76 2_565 ?
O1 Na Fe 98.92(4) 55_656 2_565 ?
O1 Na Fe 126.21(4) 77_565 2_565 ?
O1 Na Fe 76.87(4) 71_766 2_565 ?
O1 Na Fe 158.43(4) 92_545 2_565 ?
O1 Na Fe 96.21(4) 70_566 2_565 ?
O1 Na Fe 35.81(4) 90_565 2_565 ?
As Na Fe 63.4 50_656 2_565 ?
As Na Fe 116.6 . 2_565 ?
O1 Na Fe 98.92(4) 50_656 31_454 ?
O1 Na Fe 126.21(4) 76 31_454 ?
O1 Na Fe 35.32(4) 55_656 31_454 ?
O1 Na Fe 94.02(4) 77_565 31_454 ?
O1 Na Fe 158.43(4) 71_766 31_454 ?
O1 Na Fe 76.87(4) 92_545 31_454 ?
O1 Na Fe 35.81(4) 70_566 31_454 ?
O1 Na Fe 96.21(4) 90_565 31_454 ?
As Na Fe 116.6 50_656 31_454 ?
As Na Fe 63.4 . 31_454 ?
Fe Na Fe 101.5 2_565 31_454 ?
As O1 Fe 134.28(9) . . ?
As O1 Na 94.91(7) . 50_655 ?
Fe O1 Na 101.01(6) . 50_655 ?
As O1 Na 123.13(8) . 58_656 ?
Fe O1 Na 96.63(6) . 58_656 ?
Na O1 Na 98.43(6) 50_655 58_656 ?
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
As O1 1.6967(15) 27_554 ?
As O1 1.6967(16) 77_565 ?
As O1 1.6967(16) . ?
As O1 1.6967(15) 55_656 ?
As Na 3.0625(5) 50_655 ?
As Na 3.0625(5) . ?
Fe O1 2.0167(16) 43_554 ?
Fe O1 2.0167(16) 91 ?
Fe O1 2.0167(16) 84_554 ?
Fe O1 2.0167(16) 36 ?
Fe O1 2.0167(16) 49_665 ?
Fe O1 2.0167(16) . ?
Fe Na 3.4240(6) 50_655 ?
Fe Na 3.4240(6) 2_565 ?
Fe Na 3.4240(6) 85_565 ?
Fe Na 3.4240(6) 10_564 ?
Fe Na 3.4240(6) 58_656 ?
Fe Na 3.4240(6) 37_544 ?
Na O1 2.4084(17) 50_656 ?
Na O1 2.4084(17) 76 ?
Na O1 2.4084(17) 55_656 ?
Na O1 2.4084(17) 77_565 ?
Na O1 2.5439(16) 71_766 ?
Na O1 2.5439(16) 92_545 ?
Na O1 2.5439(16) 70_566 ?
Na O1 2.5439(16) 90_565 ?
Na As 3.0625(5) 50_656 ?
Na Fe 3.4240(6) 2_565 ?
Na Fe 3.4240(6) 31_454 ?
O1 Na 2.4084(17) 50_655 ?
O1 Na 2.5439(16) 58_656 ?
|
1100106.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100106.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_1100106
_publ_section_title 'Clay Montmorillonite'
_chemical_name_common Montmorillonite
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M C2:b1
_audit_update_record 'Last update Thu Dec 18 14:12:16 CET 2003'
_cell_angle_alpha 90
_cell_angle_beta 100.3(1)
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 5.411(4)
_cell_length_b 9.0(5)
_cell_length_c 10.25(2)
_refine_ls_goodness_of_fit_all 1.1109964
_refine_ls_R_factor_all 0.04240644
_refine_ls_wR_factor_all 0.06303699
_cod_database_code 1100106
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
Al1 Al3+ 1.00000 0 0 0 0.5
Al2 Al3+ 1.00000 0 0.321 0 0.5
Mg1 Mg2+ 1.00000 0 0.654 0 0.5
Si1 Si4+ 1.00000 0.432 0.333 0.27 0.5
Si2 Si4+ 1.00000 0.432 0.662 0.27 0.5
K1 K1+ 1.00000 0.5 0 0.5 0.5
O1 O2- 1.00000 0.489 0.496 0.335 0.8
O2 O2- 1.00000 0.173 0.725 0.335 0.8
O3 O2- 1.00000 0.17 0.268 0.32 0.8
O4 O2- 1.00000 0.334 -0.024 0.105 0.8
O5 O2- 1.00000 0.417 0.656 0.109 0.8
O6 O2- 1.00000 0.343 0.347 0.109 0.8
|
1100107.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-11 17:58:40 +0300 (Wed, 11 Oct 2017) $
#$Revision: 201917 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100107.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1100107
loop_
_publ_author_name
'Aubert, Emmanuel'
'Porcher, Florence'
'Souhassou, Mohamed'
'Lecomte, Claude'
_publ_section_title
;
Characterization of intra-framework and guest/host interactions
in the AlPO~4~-15 molecular sieve by charge-density analysis
;
_journal_coden_ASTM ASBSDK
_journal_issue 6
_journal_name_full
;
Acta Crystallographica, Section B: Structural Science
;
_journal_page_first 687
_journal_page_last 700
_journal_paper_doi 10.1107/S0108768103017075
_journal_volume 59
_journal_year 2003
_chemical_formula_moiety 'H3 Al2 O10 P2, H4 N, H2 O'
_chemical_formula_structural NH4AL2(OH)(H2O)(PO4)2,H20
_chemical_formula_sum 'Al2 H9 N O11 P2'
_chemical_formula_weight 314.98
_chemical_name_common AlPO~4~-15
_chemical_name_mineral AlPO4-15
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method in-house
_cell_angle_alpha 90.00
_cell_angle_beta 103.580(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.5560(10)
_cell_length_b 9.5630(10)
_cell_length_c 9.6150(10)
_cell_measurement_temperature 115.0(10)
_cell_volume 854.1(2)
_computing_cell_refinement 'HKL2000 (Otwinowski et al.,2000)'
_computing_data_collection 'Nonius Kappa'
_computing_data_reduction 'DREAD (Blessing,1989)'
_computing_structure_refinement 'MoPro (Guillot et al., 2001)'
_computing_structure_solution 'Nrcvax (Gabe et al., 1989)'
_diffrn_ambient_temperature 115
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measurement_device_type 'Nonius KappaCCD diffractometer'
_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 0.7107
_diffrn_reflns_av_R_equivalents 0.029
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 145662
_diffrn_reflns_theta_full 46
_diffrn_reflns_theta_max 49
_diffrn_reflns_theta_min 3
_exptl_absorpt_coefficient_mu 0.76
_exptl_absorpt_correction_T_max 0.93
_exptl_absorpt_correction_T_min 0.89
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details 'Absorb, (DeTitta, 1985)'
_exptl_crystal_colour Colourless
_exptl_crystal_density_diffrn 2.450
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description '12-faced polyhedron'
_exptl_crystal_F_000 640
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.14
_refine_diff_density_max 0.20
_refine_diff_density_min -0.20
_refine_ls_extinction_coef 870
_refine_ls_extinction_expression 'Becker & Coppens 1974'
_refine_ls_extinction_method Becker-Coppens
_refine_ls_goodness_of_fit_all 1.652
_refine_ls_goodness_of_fit_ref 1.652
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 510
_refine_ls_number_reflns 4725
_refine_ls_R_factor_all 0.0102
_refine_ls_R_factor_gt 0.0102
_refine_ls_shift/su_max 0.09
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_all 0.0066
_refine_ls_wR_factor_ref 0.0066
_reflns_number_gt 8561
_reflns_number_total 8561
_reflns_threshold_expression 'I > 0 u(I)'
_cod_duplicate_entry 2104014
_cod_database_code 1100107
loop_
_space_group_symop_id
_space_group_symop_operation_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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
P1 0.00269(2) 0.00301(2) 0.00288(2) -0.00020(2) 0.00065(2) 0.00016(2)
P2 0.00267(2) 0.00285(2) 0.00263(2) -0.00014(2) 0.00011(2) 0.00001(2)
Al1 0.00293(3) 0.00345(3) 0.00288(3) -0.00011(2) 0.00044(2) -0.00014(2)
Al2 0.00298(3) 0.00359(3) 0.00296(3) -0.00019(2) 0.00015(2) -0.00008(2)
O1 0.00301(6) 0.00517(6) 0.00459(6) -0.00106(5) 0.00085(5) -0.00055(5)
O2 0.00466(6) 0.00528(6) 0.00497(6) -0.00086(5) 0.00184(5) 0.00185(5)
O3 0.00417(6) 0.00584(6) 0.00276(5) -0.00048(4) 0.00078(5) 0.00070(5)
O4 0.00487(6) 0.00320(5) 0.00516(6) 0.00068(5) 0.00190(5) 0.00029(5)
O5 0.00297(6) 0.00675(6) 0.00437(6) -0.00015(5) -0.00006(5) 0.00136(5)
O6 0.00481(6) 0.00359(6) 0.00418(6) -0.00141(4) -0.00003(5) 0.00027(4)
O7 0.00580(6) 0.00403(6) 0.00469(6) -0.00013(5) 0.00129(5) -0.00189(5)
O8 0.00518(6) 0.00585(6) 0.00250(5) 0.00006(5) -0.00058(5) -0.00055(5)
O9 0.00413(6) 0.00453(6) 0.00448(6) -0.00044(5) 0.00098(5) 0.00059(5)
O10 0.00491(7) 0.00631(6) 0.00889(6) -0.00198(5) 0.00084(5) 0.00096(5)
O11 0.01051(7) 0.00863(7) 0.00823(7) 0.00091(5) 0.00336(6) -0.00036(5)
N 0.00693(8) 0.00947(7) 0.00683(7) 0.00152(6) 0.00134(6) 0.00044(6)
loop_
_atom_site_label
_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_calc_flag
_atom_site_occupancy
_atom_site_type_symbol
P1 0.301122(5) 0.532947(5) 0.151339(5) 0.002860(10) Uani d 1 P
P2 0.794553(5) 0.808911(5) 0.136246(5) 0.002800(10) Uani d 1 P
Al1 0.613765(7) 0.537615(6) 0.127745(6) 0.00313(2) Uani d 1 Al
Al2 0.393032(7) 0.229762(6) 0.184785(6) 0.00327(2) Uani d 1 Al
O1 0.456755(15) 0.586563(15) 0.203054(15) 0.00426(3) Uani d 1 O
O2 0.192884(15) 0.629269(14) 0.193560(15) 0.00485(3) Uani d 1 O
O3 0.262779(16) 0.520503(15) -0.013996(14) 0.00426(3) Uani d 1 O
O4 0.289272(15) 0.386617(14) 0.215291(14) 0.00429(3) Uani d 1 O
O5 0.954219(15) 0.769346(15) 0.165480(15) 0.00485(3) Uani d 1 O
O6 0.779190(15) 0.950289(14) 0.209248(14) 0.00437(3) Uani d 1 O
O7 0.708209(16) 0.699363(14) 0.196520(15) 0.00483(3) Uani d 1 O
O8 0.739606(16) 0.824787(15) -0.024687(14) 0.00476(3) Uani d 1 O
O9 0.496655(16) 0.364433(15) 0.054527(14) 0.00439(3) Uani d 1 O
O10 0.500178(16) 0.067277(16) 0.146993(16) 0.00683(4) Uani d 1 O
O11 0.318871(17) 0.856812(16) 0.038092(16) 0.00893(4) Uani d 1 O
N 0.987422(19) 0.308528(19) 0.102664(19) 0.00779(4) Uani d 1 N
H1 0.5608(4) 0.2984(6) 0.0206(3) 0.0084(8) Uiso d 1 H
H2 0.4449(5) -0.0098(5) 0.0992(4) 0.0132(10) Uiso d 1 H
H3 0.5961(4) 0.0363(4) 0.1889(4) 0.0131(10) Uiso d 1 H
H4 0.2668(4) 0.8587(5) 0.1118(4) 0.0154(10) Uiso d 1 H
H5 0.2650(4) 0.9090(4) -0.0409(4) 0.0145(9) Uiso d 1 H
H6 0.9988(4) 0.2780(5) 0.0066(4) 0.0132(10) Uiso d 1 H
H7 0.8975(4) 0.3652(4) 0.0898(4) 0.0144(9) Uiso d 1 H
H8 0.9910(4) 0.2261(5) 0.1671(4) 0.0134(10) Uiso d 1 H
H9 1.0756(4) 0.3634(4) 0.1466(4) 0.0134(10) Uiso d 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0657 0.0525 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0114 0.0062 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1039 0.0959 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 P1 O2 1.555 1.555 112.360(10) y
O1 P1 O3 1.555 1.555 109.530(10) y
O1 P1 O4 1.555 1.555 109.190(10) y
O2 P1 O3 1.555 1.555 108.100(10) y
O2 P1 O4 1.555 1.555 109.090(10) y
O3 P1 O4 1.555 1.555 108.500(10) y
O5 P2 O6 1.555 1.555 109.220(10) y
O5 P2 O7 1.555 1.555 111.340(10) y
O5 P2 O8 1.555 1.555 107.600(10) y
O6 P2 O7 1.555 1.555 108.050(10) y
O6 P2 O8 1.555 1.555 109.140(10) y
O7 P2 O8 1.555 1.555 111.470(10) y
O1 Al1 O7 1.555 1.555 91.200(10) y
O1 Al1 O9 1.555 1.555 84.920(10) y
O1 Al1 O3 1.555 3.665 166.580(10) y
O1 Al1 O9 1.555 3.665 85.290(10) y
O7 Al1 O9 1.555 1.555 176.020(10) y
O7 Al1 O3 1.555 3.665 97.860(10) y
O7 Al1 O9 1.555 3.665 91.940(10) y
O9 Al1 O3 1.555 3.665 85.810(10) y
O9 Al1 O9 1.555 3.665 86.850(10) y
O3 Al1 O9 3.665 3.665 84.520(10) y
O7 Al1 O6 1.555 2.645 87.020(10) y
O6 Al1 O3 2.645 3.665 93.540(10) y
O6 Al1 O1 2.645 1.555 96.820(10) y
O6 Al1 O9 2.645 1.555 94.320(10) y
O6 Al1 O9 2.645 3.665 177.660(10) y
O4 Al2 O9 1.555 1.555 86.860(10) y
O4 Al2 O10 1.555 1.555 178.320(10) y
O4 Al2 O2 1.555 2.545 89.260(10) y
O4 Al2 O8 1.555 3.665 94.200(10) y
O9 Al2 O10 1.555 1.555 91.980(10) y
O9 Al2 O2 1.555 2.545 174.810(10) y
O9 Al2 O8 1.555 3.665 90.200(10) y
O10 Al2 O2 1.555 2.545 91.970(10) y
O2 Al2 O8 2.545 3.665 93.520(10) y
O5 Al2 O2 2.645 2.545 90.030(10) y
O5 Al2 O4 2.645 1.555 93.740(10) y
O5 Al2 O10 2.645 1.555 87.400(10) y
O8 Al2 O5 3.665 2.645 171.340(10) y
O5 Al2 O9 2.645 1.555 86.790(10) y
O10 Al2 O8 1.555 3.665 84.590(10) y
P1 O1 Al1 1.555 1.555 126.330(10) y
P1 O3 Al1 1.555 3.665 126.340(10) y
P2 O5 Al2 1.555 2.655 140.350(10) y
P2 O7 Al1 1.555 1.555 134.800(10) y
P1 O2 Al2 1.555 2.555 157.120(10) y
P1 O4 Al2 1.555 1.555 125.240(10) y
P2 O6 Al1 1.555 2.655 133.180(10) y
P2 O8 Al2 1.555 3.665 146.640(10) y
Al1 O9 Al1 1.555 3.665 93.150(10) y
Al1 O9 Al2 1.555 1.555 124.630(10) y
Al2 O9 Al1 1.555 3.665 123.190(10) y
Al1 O9 H1 1.555 1.555 107.6(3) y
Al2 O9 H1 1.555 1.555 102.2(3) y
H1 O9 Al1 1.555 3.665 104.2(2) y
Al2 O10 H2 1.555 1.555 116.7(3) y
Al2 O10 H3 1.555 1.555 131.6(2) y
H2 O10 H3 1.555 1.555 109.2(4) y
H4 O11 H5 1.555 1.555 107.6(3) y
H6 N H7 1.555 1.555 108.7(3) y
H6 N H8 1.555 1.555 110.4(4) y
H6 N H9 1.555 1.555 106.3(3) y
H7 N H8 1.555 1.555 114.1(3) y
H7 N H9 1.555 1.555 112.5(3) y
H8 N H9 1.555 1.555 104.5(3) y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
P1 O1 1.555 1.5410(2) y
P1 O2 1.555 1.5101(2) y
P1 O3 1.555 1.5498(2) y
P1 O4 1.555 1.5433(2) y
P2 O5 1.555 1.5326(2) y
P2 O6 1.555 1.5461(2) y
P2 O7 1.555 1.5293(2) y
P2 O8 1.555 1.5204(2) y
Al1 O1 1.555 1.8721(3) y
Al1 O3 3.665 1.8716(3) y
Al1 O6 2.645 1.8567(2) y
Al1 O7 1.555 1.8342(2) y
Al1 O9 1.555 2.0300(3) y
Al1 O9 3.665 2.0479(3) y
Al2 O2 2.545 1.8485(2) y
Al2 O4 1.555 1.8590(2) y
Al2 O5 2.645 1.8330(2) y
Al2 O8 3.665 1.8254(2) y
Al2 O9 1.555 2.1886(3) y
Al2 O10 1.555 1.9415(3) y
O9 H1 1.555 0.987(5) y
O10 H2 1.555 0.959(5) y
O10 H3 1.555 0.958(4) y
O11 H4 1.555 0.957(4) y
O11 H5 1.555 0.953(4) y
N H6 1.555 0.999(4) y
N H7 1.555 0.999(4) y
N H8 1.555 0.998(4) y
N H9 1.555 0.998(4) y
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0009930
|
1100108.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100108.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_1100108
_publ_section_title Fe-5Al-20Ni(5to)0.1
_chemical_formula_sum Fe
_chemical_name_common alfa-Fe
_symmetry_cell_setting cubic
_symmetry_space_group_name_H-M Im-3m
_audit_update_record 'Last update Sat Feb 14 17:27:25 MSK 2004'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 2.8680182
_cell_length_b 2.8680182
_cell_length_c 2.8680182
_refine_ls_goodness_of_fit_all 1.1737101
_refine_ls_R_factor_all 0.04816144
_refine_ls_wR_factor_all 0.06062723
_cod_database_code 1100108
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
Fe1 Fe 1 0 0 0 -0.21(3)
loop_
_cod_related_entry_id
_cod_related_entry_code
_cod_related_entry_database
1 22368 ChemSpider
|
1100109.cif | #------------------------------------------------------------------------------
#$Date: 2018-07-21 16:12:36 +0300 (Sat, 21 Jul 2018) $
#$Revision: 209172 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100109.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_1100109
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_cell_angle_alpha 90.000003
_cell_angle_beta 90.144305
_cell_angle_gamma 90.000003
_cell_length_a 8.213380
_cell_length_b 8.268060
_cell_length_c 8.328060
_cod_depositor_comments
;
Updating space group information and correcting the symmetry operation list
by adding the '-x,-y,-z', 'x+1/2,-y+1/2,z+1/2' operations.
Antanas Vaitkus,
2018-07-22
;
_cod_original_sg_symbol_H-M 'P 21/N'
_cod_database_code 1100109
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2
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_type_symbol
B1 -0.1737 0.9988 0.3877 0.034 1.000 B
B2 -0.0076 1.1286 0.3355 0.034 1.000 B
B3 0.1784 1.0295 0.4016 0.034 1.000 B
B4 0.1281 0.8389 0.4768 0.034 1.000 B
B5 -0.0932 0.8102 0.4778 0.034 1.000 B
B6 0.0127 0.9140 0.3142 0.034 1.000 B
O1 -0.3247 1.0008 0.2934 0.043 1.000 O
O2 -0.0178 1.2442 0.2089 0.043 1.000 O
O3 0.3249 1.0450 0.3081 0.043 1.000 O
O4 0.2408 0.7034 0.4692 0.043 1.000 O
O5 -0.1670 0.6587 0.4574 0.043 1.000 O
O6 0.0293 0.8421 0.1558 0.043 1.000 O
H1 -0.3952 0.9101 0.3196 0.070 1.000 H
H2 0.1402 1.2423 0.1859 0.070 1.000 H
H3 0.3593 1.1399 0.4385 0.070 1.000 H
H4 0.2001 0.5895 0.3575 0.070 1.000 H
H5 -0.3013 0.6140 0.5720 0.070 1.000 H
H6 -0.0477 0.8929 0.0882 0.070 1.000 H
|
1100110.cif | #------------------------------------------------------------------------------
#$Date: 2016-06-30 19:44:13 +0300 (Thu, 30 Jun 2016) $
#$Revision: 184082 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100110.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1100110
_cod_duplicate_entry 2203515
loop_
_publ_author_name
'Chen, X.-L.'
'He, M.'
'Xu, Y.-P.'
'Li H.-Q.'
'Tu Q.-Y,'
_publ_section_title
;
KCaFCO~3~, from X-ray Powder Data
;
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first i50
_journal_page_last i51
_journal_paper_doi 10.1107/S1600536804005069
_journal_volume 60
_journal_year 2004
_chemical_formula_iupac 'K Ca F (C O3)'
_chemical_formula_moiety 'C Ca F K O3'
_chemical_formula_structural 'Ca F K (CO3)'
_chemical_formula_sum 'C Ca F K O3'
_chemical_formula_weight 158.17
_chemical_melting_point 774.0
_chemical_name_systematic
;
Potassium calcium flurine-carbonate
;
_space_group_IT_number 187
_symmetry_cell_setting hexagonal
_symmetry_Int_Tables_number 187
_symmetry_space_group_name_Hall 'P -6 2'
_symmetry_space_group_name_H-M 'P -6 m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 1
_cell_length_a 5.10093(7)
_cell_length_b 5.10093(7)
_cell_length_c 4.45510(7)
_cell_measurement_temperature 295
_cell_volume 100.389(5)
_computing_cell_refinement 'Highscore1.0b (Philips Electronics, 2002)'
_computing_data_collection 'Rint2400 (Rigaku Corporation, 1993)'
_computing_data_reduction 'Highscore1.0b (Philips Electronics, 2002)'
_computing_molecular_graphics 'Balls & Sticks (Kang & Ozawa, 2003)'
_computing_structure_refinement 'FULLPROF (Rodriguez-Carvajal, 2003)'
_computing_structure_solution 'SHEXLS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 295
_diffrn_measurement_device_type Rint2400
_diffrn_radiation_monochromator 'curved graphite'
_exptl_crystal_density_diffrn 2.615
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 78
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 2.26
_refine_ls_matrix_type fullcycle
_refine_ls_number_parameters 26
_refine_ls_R_factor_all 0.08
_refine_ls_shift/su_max .01
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme 1/Y~i~
_cod_data_source_URL
http://scripts.iucr.org/cgi-bin/sendcif?wn6225sup1
_cod_data_source_block I
_cod_depositor_comments
;
Data in this entry were merged with the data items from the IUCr Web site:
svn cat 1100110.cif \
| cif_merge - <(curl -sSL http://scripts.iucr.org/cgi-bin/sendcif?wn6225sup1 \
| cif_filter --renumber --start-data 1100110) \
| cif_filter --exclude-empty-tags --add-cif-header $(codid2file 2105696) \
| sponge 1100110.cif
Saulius Gra\<zulis
2016.06.30
===================================================================
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
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_formula_sum 'C Ca F K (CO3)'
_cod_database_code 1100110
loop_
_symmetry_equiv_pos_as_xyz
_symmetry_equiv_pos_site_id
x,y,z 1
-y,x-y,z 2
-x+y,-x,z 3
x,y,-z 4
-y,x-y,-z 5
-x+y,-x,-z 6
-y,-x,z 7
-x+y,y,z 8
x,x-y,z 9
-y,-x,-z 10
-x+y,y,-z 11
x,x-y,-z 12
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
K K1+ 1 a 0 0 0 1 0 d .0126(6) Uiso
C C4+ 1 f .66667 .33333 .5 1 0 d .018(2) Uiso
Ca Ca2+ 1 d .33333 .66667 .5 1 0 d .0100(6) Uiso
O O2- 3 k .8120(3) .1880(3) .5 1 0 d .0129 Uiso
F F1- 1 c .33333 .66667 0 1 0 d .01960(10) Uiso
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C4+ 4.000 Ca 0.341 1.286 'International Tables for Crystallography (Vol. IV)'
Ca2+ 2.000 K 0.365 1.066 'International Tables for Crystallography (Vol. IV)'
K1+ 1.000 F 0.069 0.053 'International Tables for Crystallography (Vol. IV)'
F1- -1.000 O .047 .032 'International Tables for Crystallography (Vol. IV)'
O2- -2.000 C .017 .009 'International Tables for Crystallography (Vol. IV)'
loop_
_diffrn_radiation_type
_diffrn_radiation_wavelength
CuK\a~1~ 1.54056
CuK\a~2~ 1.54439
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O C O . 2_655 120 yes
O C O . 3_665 120 yes
O C O 2_655 3_665 120 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K O 1_454 2.7790(10) yes
K O 1_455 2.7790(10) yes
K O 2_544 2.7790(10) yes
K O 2_545 2.7790(10) yes
K O 3_664 2.7790(10) yes
K O 3_665 2.7790(10) yes
K F 1_445 2.94500(10) yes
K F 1_545 2.94500(10) yes
K F . 2.94500(10) yes
C O . 1.2840(10) yes
C O 2_655 1.2840(10) yes
C O 3_665 1.2840(10) yes
Ca O 1_455 2.5570(10) yes
Ca O 1_565 2.5570(10) yes
Ca O 2_555 2.5570(10) yes
Ca O 2_655 2.5570(10) yes
Ca O 3_665 2.5570(10) yes
Ca O 3_675 2.5570(10) yes
Ca F . 2.22750(10) yes
Ca F 1_556 2.22750(10) yes
|
1100111.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-25 22:10:12 +0300 (Sun, 25 Sep 2022) $
#$Revision: 278158 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100111.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_1100111
loop_
_publ_author_name
'Daniel J. Stasko'
'Kevin J. Perzynski'
'Mark A. Wasil'
'Julia K. Brodbeck'
'Kristin Kirschbaum'
'Yong Wah Kim'
'Cora Lind'
_publ_contact_author
;
Daniel J. Stasko
;
_publ_contact_author_email daniel.stasko@utoledo.edu
_publ_contact_author_fax 419-530-4033
_publ_contact_author_phone 419-530-4087
_publ_section_title
;
An Addition to the Oxoacid Family: H2B12(OH)12
;
_journal_name_full 'Inorganic Chemistry'
_journal_page_first 3786
_journal_page_last 3788
_journal_paper_doi 10.1021/ic049564k
_journal_volume 43
_journal_year 2004
_chemical_formula_sum 'B12 H12 N2 O12'
_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'
_cell_angle_alpha 90.000003
_cell_angle_beta 92.990499
_cell_angle_gamma 90.000003
_cell_formula_units_Z 2
_cell_length_a 7.135660
_cell_length_b 10.392400
_cell_length_c 9.247710
_cod_original_sg_symbol_H-M 'P 21/n '
_cod_original_formula_sum 'H12 B12 N2 O12'
_cod_database_code 1100111
loop_
_symmetry_equiv_pos_as_xyz
X,Y,Z
1/2-X,1/2+Y,1/2-Z
-X,-Y,-Z
X+1/2,-Y+1/2,Z+1/2
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_type_symbol
N1 0.7780 0.5475 0.5155 0.006 1.000 N
B1 0.6971 0.5239 0.1129 0.005 1.000 B
O1 0.8592 0.5408 0.2093 0.041 1.000 O
B2 0.4567 0.5581 0.1667 0.005 1.000 B
O2 0.4241 0.6063 0.3188 0.041 1.000 O
B3 0.5592 0.6542 0.0362 0.005 1.000 B
O3 0.5974 0.7970 0.0602 0.041 1.000 O
B4 0.6930 0.5596 -0.0863 0.005 1.000 B
O4 0.8586 0.6068 -0.1444 0.041 1.000 O
B5 0.6741 0.3853 -0.0184 0.005 1.000 B
O5 0.8444 0.3208 -0.0246 0.041 1.000 O
B6 0.5377 0.3922 0.1396 0.005 1.000 B
O6 0.5748 0.3063 0.2708 0.041 1.000 O
H1 0.9691 0.5345 0.1966 0.041 1.000 H
H2 0.2980 0.6179 0.3171 0.041 1.000 H
H3 0.7117 0.7996 0.0683 0.041 1.000 H
H4 0.9715 0.5991 -0.1424 0.041 1.000 H
H5 0.9567 0.3219 -0.0257 0.041 1.000 H
H6 0.4627 0.2918 0.2479 0.041 1.000 H
|
1100112.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100112.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_1100112
_chemical_formula_sum 'Fe2 Ni0.5 O4 Zn0.5'
_chemical_name_common Ni0,5Zn0,5Fe2O4
_symmetry_cell_setting cubic
_symmetry_space_group_name_H-M Fd-3m:1
_audit_update_record 'Last update Tue May 04 16:52:08 CEST 2004'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 8.4171(1)
_cell_length_b 8.417067
_cell_length_c 8.417067
_refine_ls_goodness_of_fit_all 1.163656
_refine_ls_R_factor_all 0.04240644
_refine_ls_wR_factor_all 0.06303699
_cod_original_formula_sum 'Ni0.5 Zn0.5 Fe2 O4'
_cod_database_code 1100112
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
Fe1 Fe3+ 0.5 0.0 0.0 0.0 0.0
Fe2 Fe3+ 0.75 0.625 0.625 0.625 0.0
Ni Ni2+ 0.25 0.625 0.625 0.625 0.0
Zn Zn2+ 0.5 0.0 0.0 0.0 0.0
O O2- 1.0 0.38 0.38 0.38 0.
|
1100113.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-04 14:24:42 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177548 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100113.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_1100113
loop_
_publ_author_name
'Touret, J.'
'Bourdon, X.'
'Leblanc, M.'
'Retoux, R.'
'Renaudin, J.'
'Maisonneuve, V.'
_publ_section_title
;
Crystal structure of new hydroxide fluorides with isolated F- anions:
[H~3~N(CH~2~)~6~NH~3~]~2~M(F, OH)~6~(F,OH)·H~2~O (M = Al, In)
;
_journal_coden_ASTM JFLCAR
_journal_issue 2
_journal_name_full 'Journal of Fluorine Chemistry'
_journal_page_first 133
_journal_page_last 138
_journal_paper_doi 10.1016/s0022-1139(01)00420-1
_journal_volume 110
_journal_year 2001
_chemical_formula_moiety
;
2(C6 H18 N2 2+),Al1 F6 3-,F1 1-,H2 O1
;
_chemical_formula_sum 'C12 H38 Al F7 N4 O'
_chemical_name_systematic
;
bis(Hexane-1,6-diammonium) hexa-fluoro-aluminium(iii) fluoride monohydrate
;
_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 90.966(14)
_cell_angle_beta 90.515(12)
_cell_angle_gamma 94.351(19)
_cell_formula_units_Z 2
_cell_length_a 6.3004(18)
_cell_length_b 12.691(2)
_cell_length_c 12.7423(14)
_cell_volume 1015.719
_diffrn_ambient_temperature 293
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.355
_exptl_crystal_description lamellar
_refine_ls_R_factor_gt 0.0449
_refine_ls_wR_factor_gt 0.0449
_cod_original_formula_sum 'C12 H38 Al1 F7 N4 O1'
_cod_database_code 1100113
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
Al1 Al 0.00000 0.00000 0.00000
Al2 Al 0.00000 0.00000 -0.50000
F1 F 0.1496(2) 0.04113(11) -0.11338(11)
F2 F 0.1560(2) 0.01538(11) -0.61835(11)
F3 F 0.2334(2) -0.03521(11) -0.43155(11)
F4 F 0.2381(2) 0.02274(11) 0.08012(11)
F5 F 0.0674(2) 0.13899(11) -0.46368(12)
F6 F 0.0645(2) -0.13602(11) -0.02597(11)
F7 F -0.4343(3) 0.19686(13) -0.24728(13)
N1 N 0.4888(3) -0.15721(16) -0.54981(18)
H1 H 0.46810 -0.16600 -0.61870
H2 H 0.62670 -0.14190 -0.53650
H3 H 0.41530 -0.10450 -0.52660
C1 C 0.4164(4) -0.2556(2) -0.4960(2)
H4 H 0.26480 -0.27040 -0.50830
H5 H 0.43930 -0.24560 -0.42110
C2 C 0.5319(5) -0.3497(2) -0.5334(2)
H6 H 0.68250 -0.33700 -0.51710
H7 H 0.51640 -0.35730 -0.60910
C3 C 0.4460(5) -0.4514(2) -0.4824(3)
H8 H 0.46250 -0.44320 -0.40680
H9 H 0.29490 -0.46270 -0.49800
N2 N 0.4748(3) -0.15706(16) 0.04346(18)
H10 H 0.34340 -0.14720 0.02150
H11 H 0.56030 -0.09990 0.03010
H12 H 0.47400 -0.16830 0.11220
C4 C 0.5524(4) -0.24985(19) -0.0122(2)
H13 H 0.70560 -0.24910 -0.00340
H14 H 0.52130 -0.24530 -0.08660
C5 C 0.4501(5) -0.3521(2) 0.0285(2)
H15 H 0.29840 -0.35600 0.01360
H16 H 0.46950 -0.35380 0.10400
C6 C 0.5458(5) -0.4473(2) -0.0217(2)
H17 H 0.69870 -0.44090 -0.01000
H18 H 0.52020 -0.44710 -0.09690
N3 N 0.0701(4) -0.13454(16) -0.24741(18)
H19 H 0.04870 -0.13060 -0.17850
H20 H 0.00600 -0.08340 -0.27890
H21 H 0.20910 -0.12720 -0.25990
C7 C -0.0190(5) -0.2385(2) -0.2886(2)
H22 H 0.00590 -0.24270 -0.36350
H23 H -0.17170 -0.24470 -0.27790
C8 C 0.0784(5) -0.3286(2) -0.2359(2)
H24 H 0.05540 -0.32390 -0.16090
H25 H 0.23070 -0.32320 -0.24760
C9 C -0.0179(5) -0.4353(2) -0.2781(2)
H26 H -0.17020 -0.43990 -0.26620
H27 H 0.00390 -0.43890 -0.35330
C10 C 0.0758(5) -0.5292(2) -0.2281(2)
H28 H 0.05170 -0.52630 -0.15300
H29 H 0.22850 -0.52380 -0.23880
C11 C -0.0164(5) -0.6353(2) -0.2712(2)
H30 H -0.16990 -0.64010 -0.26370
H31 H 0.01500 -0.64070 -0.34540
C12 C 0.0742(4) -0.7258(2) -0.2143(2)
H32 H 0.22700 -0.72240 -0.22430
H33 H 0.04830 -0.71840 -0.13980
N4 N -0.0208(4) -0.83006(16) -0.25227(17)
H34 H 0.02610 -0.88070 -0.21260
H35 H 0.01650 -0.84060 -0.31860
H36 H -0.16190 -0.83150 -0.24840
O1 O 0.4700(3) 0.10848(17) -0.75122(16)
H37 H 0.414(4) 0.074(2) -0.6968(16)
H38 H 0.415(4) 0.079(2) -0.8094(14)
F1A F -0.1496(2) -0.04113(11) 0.11338(11)
F4A F -0.2381(2) -0.02274(11) -0.08012(11)
F6A F -0.0645(2) 0.13602(11) 0.02597(11)
F2A* F -0.1560(2) -0.01538(11) -0.38165(11)
F3A* F -0.2334(2) 0.03521(11) -0.56845(11)
F5A* F -0.0674(2) -0.13899(11) -0.53632(12)
C3A* C 0.5540(5) -0.5486(2) -0.5176(3)
C2A* C 0.4681(5) -0.6503(2) -0.4666(2)
C1A* C 0.5836(4) -0.7444(2) -0.5040(2)
N1A* N 0.5112(3) -0.84279(16) -0.45019(18)
H1A* H 0.53190 -0.83400 -0.38130
H2A* H 0.37330 -0.85810 -0.46350
H3A* H 0.58470 -0.89550 -0.47340
H4A* H 0.73520 -0.72960 -0.49170
H5A* H 0.56070 -0.75440 -0.57890
H6A* H 0.31750 -0.66300 -0.48290
H7A* H 0.48360 -0.64270 -0.39090
H8A* H 0.53750 -0.55680 -0.59320
H9A* H 0.70510 -0.53730 -0.50200
C6A* C 0.4542(5) -0.5527(2) 0.0217(2)
C5A* C 0.5499(5) -0.6479(2) -0.0285(2)
C4A* C 0.4476(4) -0.75015(19) 0.0122(2)
N2A* N 0.5252(3) -0.84294(16) -0.04346(18)
H10A* H 0.65660 -0.85280 -0.02150
H11A* H 0.43970 -0.90010 -0.03010
H12A* H 0.52600 -0.83170 -0.11220
H13A* H 0.29440 -0.75090 0.00340
H14A* H 0.47870 -0.75470 0.08660
H15A* H 0.70160 -0.64400 -0.01360
H16A* H 0.53050 -0.64620 -0.10400
H17A* H 0.30130 -0.55910 0.01000
H18A* H 0.47980 -0.55290 0.09690
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Al 1.35
F 0.64
N 0.68
O 0.68
|
1100114.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-04 14:24:42 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177548 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100114.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_1100114
loop_
_publ_author_name
'Touret, J.'
'Bourdon, X.'
'Leblanc, M.'
'Retoux, R.'
'Renaudin, J.'
'Maisonneuve, V.'
_publ_section_title
;
Crystal structure of new hydroxide fluorides with isolated F- anions:
[H~3~N(CH~2~)~6~NH~3~]~2~M(F, OH)~6~(F,OH)·H~2~O (M = Al, In)
;
_journal_coden_ASTM JFLCAR
_journal_issue 2
_journal_name_full 'Journal of Fluorine Chemistry'
_journal_page_first 133
_journal_page_last 138
_journal_paper_doi 10.1016/s0022-1139(01)00420-1
_journal_volume 110
_journal_year 2001
_chemical_formula_moiety
;
2(C6 H18 N2 2+),F6 In1 3-,F1 1-,H2 O1
;
_chemical_formula_sum 'C12 H38 F7 In N4 O'
_chemical_name_systematic
;
bis(Hexane-1,6-diammonium) hexa-fluoro-indium(iii) fluoride monohydrate
;
_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 90.160(6)
_cell_angle_beta 90.683(4)
_cell_angle_gamma 94.138(5)
_cell_formula_units_Z 2
_cell_length_a 6.4714(3)
_cell_length_b 12.9203(9)
_cell_length_c 13.0843(6)
_cell_volume 1091.073
_diffrn_ambient_temperature 293
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.529
_exptl_crystal_description lamellar
_refine_ls_R_factor_gt 0.0309
_refine_ls_wR_factor_gt 0.0309
_cod_original_formula_sum 'C12 H38 F7 In1 N4 O1'
_cod_database_code 1100114
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
In1 In 0.00000 0.00000 0.00000
In2 In 0.00000 0.00000 -0.50000
F1 F 0.1439(3) 0.05101(15) -0.13134(14)
F2 F 0.1461(3) 0.01486(16) -0.63895(15)
F3 F 0.2725(3) -0.04009(15) -0.43560(15)
F4 F 0.2799(3) 0.02765(15) 0.07551(15)
F5 F 0.0790(3) 0.15603(13) -0.46245(14)
F6 F 0.0801(3) -0.15061(13) -0.03247(14)
F7 F -0.4249(3) 0.20800(17) -0.24813(16)
N1 N 0.4949(4) -0.1645(2) -0.5563(2)
H1 H 0.46790 -0.17210 -0.62290
H2 H 0.63100 -0.15350 -0.54630
H3 H 0.43160 -0.11060 -0.53250
C1 C 0.4187(6) -0.2596(3) -0.5019(3)
H4 H 0.27100 -0.27240 -0.51430
H5 H 0.44060 -0.24960 -0.42890
C2 C 0.5291(6) -0.3533(3) -0.5367(3)
H6 H 0.67620 -0.34150 -0.52200
H7 H 0.51130 -0.36190 -0.61000
C3 C 0.4457(7) -0.4520(3) -0.4834(3)
H8 H 0.29850 -0.46340 -0.49820
H9 H 0.46280 -0.44280 -0.41010
N2 N 0.4729(4) -0.1647(2) 0.0509(2)
H10 H 0.34380 -0.15800 0.02920
H11 H 0.55090 -0.10690 0.03760
H12 H 0.47310 -0.17610 0.11800
C4 C 0.5574(5) -0.2531(2) -0.0021(3)
H13 H 0.70530 -0.25200 0.01120
H14 H 0.53630 -0.24610 -0.07520
C5 C 0.4548(6) -0.3561(2) 0.0328(3)
H15 H 0.30760 -0.35810 0.01740
H16 H 0.47160 -0.36190 0.10630
C6 C 0.5468(6) -0.4480(3) -0.0190(3)
H17 H 0.52400 -0.44370 -0.09220
H18 H 0.69530 -0.44380 -0.00650
N3 N 0.1008(5) -0.1357(2) -0.2455(2)
H19 H 0.09250 -0.13690 -0.17760
H20 H 0.03200 -0.08370 -0.26980
H21 H 0.23310 -0.12680 -0.26340
C7 C 0.0089(6) -0.2350(3) -0.2880(3)
H22 H 0.03170 -0.23640 -0.36110
H23 H -0.13940 -0.23960 -0.27700
C8 C 0.1000(6) -0.3268(3) -0.2398(3)
H24 H 0.08200 -0.32410 -0.16640
H25 H 0.24740 -0.32380 -0.25310
C9 C -0.0018(7) -0.4291(3) -0.2812(3)
H26 H -0.14980 -0.43100 -0.26950
H27 H 0.01880 -0.43210 -0.35450
C10 C 0.0839(7) -0.5233(3) -0.2321(3)
H28 H 0.05880 -0.52130 -0.15920
H29 H 0.23270 -0.51970 -0.24160
C11 C -0.0096(6) -0.6255(3) -0.2749(3)
H30 H -0.15910 -0.62830 -0.26840
H31 H 0.02170 -0.62970 -0.34710
C12 C 0.0728(6) -0.7171(2) -0.2201(3)
H32 H 0.22160 -0.71560 -0.22870
H33 H 0.04580 -0.71160 -0.14760
N4 N -0.0235(4) -0.8170(2) -0.2592(2)
H34 H 0.02370 -0.86890 -0.22320
H35 H 0.00820 -0.82440 -0.32470
H36 H -0.16050 -0.81790 -0.25310
O1 O 0.4571(5) 0.1170(2) -0.7529(2)
H37 H 0.398(6) 0.081(3) -0.702(2)
H38 H 0.404(6) 0.096(3) -0.8129(16)
F1A F -0.1439(3) -0.05101(15) 0.13134(14)
F4A F -0.2799(3) -0.02765(15) -0.07551(15)
F6A F -0.0801(3) 0.15061(13) 0.03247(14)
F2A* F -0.1461(3) -0.01486(16) -0.36105(15)
F3A* F -0.2725(3) 0.04009(15) -0.56440(15)
F5A* F -0.0790(3) -0.15603(13) -0.53755(14)
C3A* C 0.5543(7) -0.5480(3) -0.5166(3)
C2A* C 0.4709(6) -0.6467(3) -0.4633(3)
C1A* C 0.5813(6) -0.7404(3) -0.4981(3)
N1A* N 0.5051(4) -0.8355(2) -0.4437(2)
H1A* H 0.53210 -0.82790 -0.37710
H2A* H 0.36900 -0.84650 -0.45370
H3A* H 0.56840 -0.88940 -0.46750
H4A* H 0.72900 -0.72760 -0.48570
H5A* H 0.55940 -0.75040 -0.57110
H6A* H 0.32380 -0.65850 -0.47800
H7A* H 0.48870 -0.63810 -0.39000
H8A* H 0.70150 -0.53660 -0.50180
H9A* H 0.53720 -0.55720 -0.58990
C6A* C 0.4532(6) -0.5520(3) 0.0190(3)
C5A* C 0.5452(6) -0.6439(2) -0.0328(3)
C4A* C 0.4426(5) -0.7469(2) 0.0021(3)
N2A* N 0.5271(4) -0.8353(2) -0.0509(2)
H10A* H 0.65620 -0.84200 -0.02920
H11A* H 0.44910 -0.89310 -0.03760
H12A* H 0.52690 -0.82390 -0.11800
H13A* H 0.29470 -0.74800 -0.01120
H14A* H 0.46370 -0.75390 0.07520
H15A* H 0.69240 -0.64190 -0.01740
H16A* H 0.52840 -0.63810 -0.10630
H17A* H 0.47600 -0.55630 0.09220
H18A* H 0.30470 -0.55620 0.00650
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
F 0.64
In 1.63
N 0.68
O 0.68
|
1100115.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100115.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_1100115
loop_
_publ_author_name
E.Goreshnik
M.Leblanc
E.Gaudin
F.Taulelle
V.Maisonneuve
_publ_section_title
;
Structural and NMR studies of the series of related
[H_3_ N(CH_2_)_x_ NH_3_]·AlF_5_ (x = 6, 8, 10, 12) hybrid compounds
;
_journal_name_full 'Solid State Sciences'
_journal_page_first 1213
_journal_page_last 1219
_journal_paper_doi 10.1016/S1293-2558(02)01384-5
_journal_volume 4
_journal_year 2002
_chemical_formula_moiety
;
(C8 H22 N2 2+)n,n(Al1 F5 2-)
;
_chemical_formula_sum 'C8 H22 Al F5 N2'
_chemical_name_systematic
;
catena-(1,8-Octanediammonium (\m~2~-fluoro)-tetrafluoro-aluminium)
;
_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 112.03(4)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.887(6)
_cell_length_b 5.502(5)
_cell_length_c 15.812(3)
_cell_volume 636.053
_diffrn_ambient_temperature ?
_exptl_crystal_density_diffrn 1.403
_exptl_crystal_description platelets
_refine_ls_R_factor_gt 0.0755
_refine_ls_wR_factor_gt 0.0755
_cod_depositor_comments
;
The following fixes were made to the structure:
1. Tag _atom_site_attached_hydrogens with values N = 3, C = 2, else = 0
was added. As a result, calculated summary formula contains the correct
amount of hydrogens.
2. Two atoms were removed, as they seem to be symmetric equivalents of
Al1 and F3:
Al1A* Al 0.6749(2) 0.50000 0.0344(1)
F3A* F 0.5047(9) -0.245(1) -0.0049(4)
As a result, amount of Al and F in the calculated summary formula is now
correct. Moreover, symmetry reconstruction does not result in bumps
(distance between atoms = 0) any more.
Andrius Merkys
2015-09-15
;
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C8 H22 Al1 F5 N2'
_cod_database_code 1100115
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
_atom_site_attached_hydrogens
Al1 Al 0.3251(2) 0.00000 -0.0344(1) 0
F1 F 0.3408(5) -0.024(1) 0.0820(2) 0
F2 F 0.3409(5) 0.022(1) -0.1441(2) 0
F3 F 0.4953(9) 0.255(1) 0.0049(4) 0
F4 F 0.1532(7) 0.232(1) -0.0587(3) 0
F5 F 0.1524(6) -0.226(1) -0.0734(3) 0
N1 N 0.1914(7) 0.5268(13) 0.0883(3) 3
N2 N 0.2837(7) 0.5041(14) 0.8213(3) 3
C1 C 0.268(1) 0.418(2) 0.1814(5) 2
C2 C 0.210(1) 0.560(2) 0.2479(4) 2
C3 C 0.291(1) 0.452(2) 0.3437(4) 2
C4 C 0.2112(11) 0.575(2) 0.4082(5) 2
C5 C 0.2915(11) 0.462(2) 0.5046(5) 2
C6 C 0.211(1) 0.570(2) 0.5691(5) 2
C7 C 0.287(1) 0.468(2) 0.6650(4) 2
C8 C 0.197(1) 0.580(2) 0.7257(4) 2
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
Al 1.35
F 0.64
N 0.68
|
1100116.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100116.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_1100116
loop_
_publ_author_name
E.Goreshnik
M.Leblanc
E.Gaudin
F.Taulelle
V.Maisonneuve
_publ_section_title
;
Structural and NMR studies of the series of related
[H_3_ N(CH_2_)_x_ NH_3_]·AlF_5_ (x = 6, 8, 10, 12) hybrid compounds
;
_journal_name_full 'Solid State Sciences'
_journal_page_first 1213
_journal_page_last 1219
_journal_paper_doi 10.1016/S1293-2558(02)01384-5
_journal_volume 4
_journal_year 2002
_chemical_formula_moiety
;
(C10 H26 N2 2+)n,n(Al1 F5 2-)
;
_chemical_formula_sum 'C10 H26 Al F5 N2'
_chemical_name_systematic
;
catena-(1,10-Decanediammonium (\m~2~-fluoro)-tetrafluoro-aluminium)
;
_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 112.21(6)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.881(5)
_cell_length_b 5.489(2)
_cell_length_c 18.36(1)
_cell_volume 735.303
_diffrn_ambient_temperature ?
_exptl_crystal_density_diffrn 1.331
_refine_ls_R_factor_gt 0.0892
_refine_ls_wR_factor_gt 0.0892
_cod_depositor_comments
;
The following fixes were made to the structure:
1. Tag _atom_site_attached_hydrogens with values N = 3, C = 2, else = 0
was added. As a result, calculated summary formula contains the correct
amount of hydrogens.
2. Two atoms were removed, as they seem to be symmetric equivalents of
Al1 and F3:
Al1A* Al 0.6750(4) 0.50000 0.0295(2)
F3A* F 0.490(2) -0.256(2) 0.004(6)
As a result, amount of Al and F in the calculated summary formula is now
correct. Moreover, symmetry reconstruction does not result in bumps
(distance between atoms = 0) any more.
Andrius Merkys
2015-09-15
;
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C10 H26 Al1 F5 N2'
_cod_database_code 1100116
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
_atom_site_attached_hydrogens
Al1 Al 0.3250(4) 0.00000 -0.0295(2) 0
F1 F 0.3416(7) -0.002(3) 0.0713(3) 0
F2 F 0.3391(8) -0.013(2) -0.1235(3) 0
F3 F 0.510(2) 0.244(2) -0.004(6) 0
F4 F 0.1549(7) 0.232(2) -0.0598(3) 0
F5 F 0.150(1) -0.230(1) -0.0546(4) 0
N1 N 0.189(1) 0.526(2) 0.0771(4) 3
N2 N 0.283(1) 0.505(3) 0.8459(5) 3
C1 C 0.266(2) 0.418(3) 0.1580(6) 2
C2 C 0.214(2) 0.562(3) 0.2139(6) 2
C3 C 0.292(2) 0.449(3) 0.2962(6) 2
C4 C 0.218(2) 0.573(3) 0.3539(8) 2
C5 C 0.292(2) 0.455(3) 0.4357(7) 2
C6 C 0.216(2) 0.564(3) 0.4926(7) 2
C7 C 0.289(2) 0.458(3) 0.5740(7) 2
C8 C 0.205(2) 0.563(3) 0.6294(7) 2
C9 C 0.285(2) 0.475(4) 0.7127(6) 2
C10 C 0.189(2) 0.573(3) 0.7627(6) 2
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
Al 1.35
F 0.64
N 0.68
|
1100117.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100117.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_1100117
loop_
_publ_author_name
E.Goreshnik
M.Leblanc
E.Gaudin
F.Taulelle
V.Maisonneuve
_publ_section_title
;
Structural and NMR studies of the series of related
[H_3_ N(CH_2_)_x_ NH_3_]·AlF_5_ (x = 6, 8, 10, 12) hybrid compounds
;
_journal_name_full 'Solid State Sciences'
_journal_page_first 1213
_journal_page_last 1219
_journal_paper_doi 10.1016/S1293-2558(02)01384-5
_journal_volume 4
_journal_year 2002
_chemical_formula_moiety
;
(C12 H30 N2 2+)n,n(Al1 F5 2-)
;
_chemical_formula_sum 'C12 H30 Al F5 N2'
_chemical_name_systematic
;
catena-(1,12-Dodecanediammonium (\m~2~-fluoro)-tetrafluoro-aluminium)
;
_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 112.422(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.8713(3)
_cell_length_b 5.4739(4)
_cell_length_c 20.898(2)
_cell_volume 832.354
_diffrn_ambient_temperature ?
_exptl_crystal_density_diffrn 1.29
_pd_proc_ls_prof_R_factor 0.13
_pd_proc_ls_prof_wR_expected 0.025
_pd_proc_ls_prof_wR_factor 0.17
_cod_depositor_comments
;
The following fixes were made to the structure:
1. Tag _atom_site_attached_hydrogens with values N = 3, C = 2, else = 0
was added. As a result, calculated summary formula contains the correct
amount of hydrogens.
2. Two atoms were removed, as they seem to be symmetric equivalents of
Al1 and F3:
Al1A* Al 0.6756(9) 0.50000 0.0223(5) 0
F3A* F 0.500(4) -0.249(8) 0.001(1) 0
As a result, amount of Al and F in the calculated summary formula is now
correct. Moreover, symmetry reconstruction does not result in bumps
(distance between atoms = 0) any more.
3. Tag _refine_ls_R_factor_gt was replaced by more relevant tag from
powder diffraction CIF dictionary. Tags _pd_proc_ls_prof_wR_factor and
_pd_proc_ls_prof_wR_expected were added with data from original
publication.
Andrius Merkys
2015-09-15
;
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C12 H30 Al1 F5 N2'
_cod_database_code 1100117
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
_atom_site_attached_hydrogens
Al1 Al 0.3244(9) 0.00000 -0.0223(5) 0
F1 F 0.340(1) -0.002(5) 0.0647(4) 0
F2 F 0.340(1) 0.003(5) -0.1057(5) 0
F3 F 0.500(4) 0.251(8) -0.001(1) 0
F4 F 0.150(2) 0.236(2) -0.0492(6) 0
F5 F 0.155(2) -0.225(2) -0.0377(6) 0
N1 N 0.199(2) 0.556(5) 0.0751(6) 3
N2 N 0.282(2) 0.450(4) 0.8649(7) 3
C1 C 0.276(2) 0.452(5) 0.1494(9) 2
C2 C 0.191(2) 0.552(6) 0.1994(9) 2
C3 C 0.283(2) 0.451(5) 0.2732(9) 2
C4 C 0.216(2) 0.556(6) 0.3256(8) 2
C5 C 0.306(2) 0.451(5) 0.3961(7) 2
C6 C 0.216(2) 0.538(8) 0.4439(8) 2
C7 C 0.295(2) 0.446(7) 0.516(1) 2
C8 C 0.194(2) 0.530(9) 0.5593(8) 2
C9 C 0.290(2) 0.448(5) 0.6325(8) 2
C10 C 0.194(2) 0.549(7) 0.6752(8) 2
C11 C 0.294(2) 0.452(5) 0.7461(9) 2
C12 C 0.202(2) 0.545(7) 0.7935(9) 2
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
Al 1.35
F 0.64
N 0.68
|
1100118.cif | #------------------------------------------------------------------------------
#$Date: 2025-01-29 09:25:17 +0200 (Wed, 29 Jan 2025) $
#$Revision: 297521 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100118.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_1100118
loop_
_publ_author_name
'Goreshnik, E.'
'Leblanc, M.'
'Maisonneuve, V.'
_publ_section_title
;
1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium
bis(aquapentafluoroaluminate) dihydrate
;
_journal_coden_ASTM ACSEBH
_journal_issue 11
_journal_name_full
;
Acta Crystallographica, Section E: Structure Reports Online
;
_journal_page_first 1059
_journal_page_last 1061
_journal_paper_doi 10.1107/S1600536803023699
_journal_volume 59
_journal_year 2003
_chemical_formula_iupac '(C10 H28 N4) [Al F5 (H2 O)]2, 2H2 O'
_chemical_formula_moiety 'C10 H28 N4 1+, 2Al F5 H2 O 2-, 2H2 O'
_chemical_formula_sum 'C10 H36 Al2 F10 N4 O4'
_chemical_formula_weight 520.3675
_chemical_name_systematic
;
1,4,8,11-Tetraazacyclodecane-1,4,8,11-tetraium
bis(aquapentafluoroaluminate) dihydrate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 97.141(8)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 8.4930(8)
_cell_length_b 8.9320(10)
_cell_length_c 13.434(2)
_cell_measurement_reflns_used 32
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 10
_cell_measurement_theta_min 2.5
_cell_volume 1011.2(2)
_computing_cell_refinement 'STADI4 (Stoe & Cie, 1998)'
_computing_data_collection 'STADI4 (Stoe & Cie, 1998)'
_computing_data_reduction 'X-RED (Stoe & Cie, 1998)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2001), ORTEPIII (Burnett & Johnson, 1996)
and ORTEP-3 Farrugia, 1997)
;
_computing_publication_material 'enCIFer (CCDC, 2003)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1985)'
_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 'Siemens AED2'
_diffrn_measurement_method 2\q/\w
_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 0.0919
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 2955
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 2.69
_diffrn_standards_decay_% 15
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.261
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.709
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description parallelepiped
_exptl_crystal_F_000 544
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.06
_exptl_crystal_size_min 0.04
_exptl_special_details
;
?
;
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.453
_refine_diff_density_min -0.468
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.094
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 148
_refine_ls_number_reflns 2955
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.094
_refine_ls_R_factor_all 0.1639
_refine_ls_R_factor_gt 0.0632
_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^)+(0.0473P)^2^+0.517P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1198
_refine_ls_wR_factor_ref 0.1508
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_reflns_number_gt 1591
_reflns_number_total 2955
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1100118
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Al 0.34962(11) 0.21382(12) 0.06661(8) 0.0178(2) Uani d . 1 . . Al
F1 0.3863(2) 0.3257(3) 0.17890(16) 0.0324(5) Uani d . 1 . . F
F2 0.4504(2) 0.3417(3) -0.00278(17) 0.0329(5) Uani d . 1 . . F
F3 0.2390(2) 0.0843(3) 0.13107(16) 0.0335(5) Uani d . 1 . . F
F4 0.5146(2) 0.1058(2) 0.09959(16) 0.0319(5) Uani d . 1 . . F
F5 0.1823(2) 0.3229(2) 0.03060(15) 0.0232(5) Uani d . 1 . . F
O1 0.3038(3) 0.0969(3) -0.0546(2) 0.0302(6) Uani d D 1 . . O
H1WA 0.357(4) 0.027(3) -0.073(3) 0.036 Uiso d D 1 . . H
H1WB 0.212(2) 0.088(4) -0.081(3) 0.036 Uiso d D 1 . . H
O2 0.0375(3) 0.0195(4) 0.8369(3) 0.0479(9) Uani d D 1 . . O
H2WA -0.031(4) 0.000(6) 0.873(3) 0.058 Uiso d D 1 . . H
H2WB 0.007(5) 0.068(5) 0.787(2) 0.058 Uiso d D 1 . . H
N1 0.2341(3) 0.0972(3) 0.5466(2) 0.0219(6) Uani d . 1 . . N
H1A 0.2650 0.0067 0.5270 0.026 Uiso calc R 1 . . H
H1B 0.1275 0.1003 0.5344 0.026 Uiso calc R 1 . . H
N2 0.3241(3) 0.0578(3) 0.3272(2) 0.0219(6) Uani d . 1 . . N
H2A 0.2853 -0.0263 0.3520 0.026 Uiso calc R 1 . . H
H2B 0.2937 0.0588 0.2606 0.026 Uiso calc R 1 . . H
C1 0.2989(4) 0.2118(4) 0.4837(3) 0.0246(7) Uani d . 1 . . C
H1C 0.4138 0.2108 0.4974 0.029 Uiso calc R 1 . . H
H1D 0.2626 0.3096 0.5023 0.029 Uiso calc R 1 . . H
C2 0.5509(4) -0.0952(4) 0.3105(3) 0.0253(8) Uani d . 1 . . C
H2C 0.4945 -0.1761 0.3387 0.030 Uiso calc R 1 . . H
H2D 0.5308 -0.1022 0.2380 0.030 Uiso calc R 1 . . H
C3 0.2799(4) 0.1101(5) 0.6576(3) 0.0290(8) Uani d . 1 . . C
H3A 0.2450 0.2067 0.6796 0.035 Uiso calc R 1 . . H
H3B 0.2243 0.0335 0.6907 0.035 Uiso calc R 1 . . H
C4 0.2521(4) 0.1894(4) 0.3728(3) 0.0273(8) Uani d . 1 . . C
H4A 0.1376 0.1796 0.3607 0.033 Uiso calc R 1 . . H
H4B 0.2806 0.2789 0.3382 0.033 Uiso calc R 1 . . H
C5 0.4908(4) 0.0525(4) 0.3441(3) 0.0266(8) Uani d . 1 . . C
H5A 0.5259 0.0665 0.4150 0.032 Uiso calc R 1 . . H
H5B 0.5345 0.1330 0.3076 0.032 Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Al 0.0138(4) 0.0195(5) 0.0198(5) 0.0021(4) 0.0013(3) 0.0001(4)
F1 0.0273(11) 0.0366(14) 0.0310(12) 0.0051(9) -0.0049(9) -0.0142(10)
F2 0.0170(10) 0.0407(13) 0.0409(13) -0.0052(9) 0.0037(9) 0.0106(11)
F3 0.0255(10) 0.0455(14) 0.0289(11) -0.0104(10) 0.0015(9) 0.0126(10)
F4 0.0223(10) 0.0353(13) 0.0357(12) 0.0139(9) -0.0058(9) -0.0045(10)
F5 0.0142(9) 0.0267(11) 0.0283(11) 0.0042(8) 0.0011(7) 0.0015(9)
O1 0.0199(12) 0.0372(17) 0.0317(14) 0.0080(11) -0.0040(11) -0.0127(12)
O2 0.0246(15) 0.070(2) 0.0464(19) -0.0048(15) -0.0067(13) 0.0148(18)
N1 0.0132(12) 0.0292(17) 0.0235(14) 0.0025(11) 0.0028(11) -0.0016(13)
N2 0.0187(13) 0.0255(16) 0.0209(14) -0.0051(12) 0.0001(11) -0.0006(12)
C1 0.0233(16) 0.0219(18) 0.0287(18) -0.0017(15) 0.0040(14) -0.0006(16)
C2 0.0234(16) 0.029(2) 0.0237(17) 0.0001(15) 0.0022(13) -0.0027(15)
C3 0.0238(17) 0.037(2) 0.0271(18) 0.0045(16) 0.0072(14) -0.0025(17)
C4 0.0204(16) 0.031(2) 0.0304(19) 0.0053(15) 0.0028(14) 0.0061(16)
C5 0.0179(16) 0.029(2) 0.0316(19) -0.0007(14) -0.0042(14) -0.0005(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0560 0.0520 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0140 0.0100 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F4 Al F5 . . 178.87(12) ?
F4 Al F2 . . 93.80(11) ?
F5 Al F2 . . 85.63(11) ?
F4 Al F3 . . 88.40(12) ?
F5 Al F3 . . 92.12(11) ?
F2 Al F3 . . 176.81(12) ?
F4 Al F1 . . 92.57(11) ?
F5 Al F1 . . 88.43(11) ?
F2 Al F1 . . 92.20(12) ?
F3 Al F1 . . 90.00(12) ?
F4 Al O1 . . 89.21(11) ?
F5 Al O1 . . 89.79(11) ?
F2 Al O1 . . 87.99(13) ?
F3 Al O1 . . 89.74(12) ?
F1 Al O1 . . 178.19(12) ?
Al O1 H1WA . . 127(3) ?
Al O1 H1WB . . 120(3) ?
H1WA O1 H1WB . . 109(3) ?
H2WA O2 H2WB . . 115(3) ?
C1 N1 C3 . . 116.6(3) ?
C1 N1 H1A . . 108.1 ?
C3 N1 H1A . . 108.1 ?
C1 N1 H1B . . 108.1 ?
C3 N1 H1B . . 108.1 ?
H1A N1 H1B . . 107.3 ?
C5 N2 C4 . . 114.6(3) ?
C5 N2 H2A . . 108.6 ?
C4 N2 H2A . . 108.6 ?
C5 N2 H2B . . 108.6 ?
C4 N2 H2B . . 108.6 ?
H2A N2 H2B . . 107.6 ?
N1 C1 C4 . . 113.8(3) ?
N1 C1 H1C . . 108.8 ?
C4 C1 H1C . . 108.8 ?
N1 C1 H1D . . 108.8 ?
C4 C1 H1D . . 108.8 ?
H1C C1 H1D . . 107.7 ?
C3 C2 C5 3_656 . 110.6(3) ?
C3 C2 H2C 3_656 . 109.5 ?
C5 C2 H2C . . 109.5 ?
C3 C2 H2D 3_656 . 109.5 ?
C5 C2 H2D . . 109.5 ?
H2C C2 H2D . . 108.1 ?
C2 C3 N1 3_656 . 114.3(3) ?
C2 C3 H3A 3_656 . 108.7 ?
N1 C3 H3A . . 108.7 ?
C2 C3 H3B 3_656 . 108.7 ?
N1 C3 H3B . . 108.7 ?
H3A C3 H3B . . 107.6 ?
N2 C4 C1 . . 116.1(3) ?
N2 C4 H4A . . 108.3 ?
C1 C4 H4A . . 108.3 ?
N2 C4 H4B . . 108.3 ?
C1 C4 H4B . . 108.3 ?
H4A C4 H4B . . 107.4 ?
N2 C5 C2 . . 110.7(3) ?
N2 C5 H5A . . 109.5 ?
C2 C5 H5A . . 109.5 ?
N2 C5 H5B . . 109.5 ?
C2 C5 H5B . . 109.5 ?
H5A C5 H5B . . 108.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al F4 . 1.713(2) y
Al F5 . 1.741(2) y
Al F2 . 1.762(2) y
Al F3 . 1.781(2) y
Al F1 . 1.804(2) y
Al O1 . 1.933(3) y
O1 H1WA . 0.83(2) ?
O1 H1WB . 0.82(2) ?
O2 H2WA . 0.82(4) ?
O2 H2WB . 0.81(2) ?
N1 C1 . 1.478(4) y
N1 C3 . 1.497(4) y
N1 H1A . 0.9000 ?
N1 H1B . 0.9000 ?
N2 C5 . 1.407(4) y
N2 C4 . 1.491(5) y
N2 H2A . 0.9000 ?
N2 H2B . 0.9000 ?
C1 C4 . 1.506(5) y
C1 H1C . 0.9700 ?
C1 H1D . 0.9700 ?
C2 C3 3_656 1.454(5) y
C2 C5 . 1.503(5) y
C2 H2C . 0.9700 ?
C2 H2D . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1WA F4 3_655 0.83(2) 1.676(18) 2.501(3) 172(4)
O1 H1WB O2 1_554 0.82(2) 1.84(2) 2.626(4) 161(4)
O2 H2WA F3 3_556 0.82(4) 1.92(4) 2.610(4) 141(5)
O2 H2WB F1 4_566 0.81(2) 1.92(2) 2.718(4) 166(4)
N1 H1A F5 2_545 0.90 1.89 2.787(4) 173
N1 H1A F2 2_545 0.90 2.34 2.789(4) 111
N1 H1B F2 4_566 0.90 1.61 2.478(3) 161
N2 H2A F1 2_545 0.90 1.97 2.732(4) 141
N2 H2A F5 2_545 0.90 2.07 2.842(4) 144
N2 H2B F3 . 0.90 1.76 2.655(4) 173
|
1100119.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 18:21:52 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100119.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_1100119
loop_
_publ_author_name
'K. Adil'
'M. Leblanc'
'V. Maisonneuve'
_publ_contact_author_address
;
Laboratoire des Oxydes et Fluorures - UMR 6010 CNRS,
Facult\'e des Sciences, Universit\'e du Maine,
Avenue Olivier Messiaen, 72085 Le Mans Cedex 9,
France
;
_publ_contact_author_email vincent.maisonneuve@univ-lemans.fr
_publ_contact_author_fax '(33) 2 43 83 35 06'
_publ_contact_author_name 'Vincent MAISONNEUVE'
_publ_contact_author_phone '(33) 2 43 83 35 61'
_publ_section_title
;
[H~4~tren].(Al~2~F~10~).H~2~O
;
_journal_issue 10
_journal_name_full 'Acta Crystallographica, Section E'
_journal_page_first m1379
_journal_page_last m1381
_journal_paper_category EM
_journal_paper_doi 10.1107/S1600536804020203
_journal_volume 60
_journal_year 2004
_chemical_formula_iupac 'C6 H22 N4 4+, Al2 F10 4- , H2 O'
_chemical_formula_moiety 'C6 H22 N4, Al2 F10, H2 O'
_chemical_formula_sum 'C6 H24 Al2 F10 N4 O'
_chemical_formula_weight 412.23
_chemical_name_common '[HN(CH2CH2NH3)3].(Al2F10).H2O'
_space_group_IT_number 2
_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
_audit_creation_method SHELXL97
_cell_angle_alpha 105.87(2)
_cell_angle_beta 97.74(3)
_cell_angle_gamma 106.317(15)
_cell_formula_units_Z 2
_cell_length_a 7.6996(16)
_cell_length_b 8.838(2)
_cell_length_c 12.197(4)
_cell_measurement_reflns_used 32
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 32
_cell_measurement_theta_min 28
_cell_volume 745.8(4)
_computing_cell_refinement Stadi4
_computing_data_collection 'Stadi4 (Stoe, 1998)'
_computing_data_reduction 'XRED32 (Stoe, 1998)'
_computing_molecular_graphics 'DIAMOND (Brandenburg, 2001)'
_computing_publication_material 'ENCIFER (Allen et al. (2004)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type 'Siemens AED2 diffractometer'
_diffrn_measurement_method '2\q/\w scans'
_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 0.0384
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4283
_diffrn_reflns_theta_full 29.96
_diffrn_reflns_theta_max 29.96
_diffrn_reflns_theta_min 1.78
_diffrn_standards_decay_% 15
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.313
_exptl_absorpt_correction_T_max 0.967
_exptl_absorpt_correction_T_min 0.934
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details '(SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.836
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'parallepiped '
_exptl_crystal_F_000 424.0
_exptl_crystal_size_max 0.135
_exptl_crystal_size_mid 0.095
_exptl_crystal_size_min 0.086
_refine_diff_density_max 1.217
_refine_diff_density_min -0.730
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.053
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 212
_refine_ls_number_reflns 4269
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0749
_refine_ls_R_factor_gt 0.0432
_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^)+(0.0562P)^2^+0.5017P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1075
_refine_ls_wR_factor_ref 0.1233
_reflns_number_gt 3119
_reflns_number_total 4283
_reflns_threshold_expression >2\s(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.
Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius
;
_cod_database_code 1100119
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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Al1 0.64711(9) 0.10387(8) -0.03968(6) 0.01633(14) Uani d . 1 . . Al
Al2 0.13806(9) 0.16839(8) -0.43328(6) 0.01701(14) Uani d . 1 . . Al
F1 0.50347(17) 0.11929(15) 0.07394(11) 0.0185(3) Uani d . 1 . . F
F2 0.47946(19) 0.13192(18) -0.13743(12) 0.0237(3) Uani d . 1 . . F
F3 0.7706(2) 0.05726(19) -0.15113(13) 0.0284(3) Uani d . 1 . . F
F4 0.7824(2) 0.31966(17) 0.01730(13) 0.0276(3) Uani d . 1 . . F
F5 0.81633(18) 0.07178(17) 0.06038(12) 0.0239(3) Uani d . 1 . . F
F6 -0.02659(17) -0.01903(16) -0.41057(11) 0.0197(3) Uani d . 1 . . F
F7 0.2119(2) 0.27790(18) -0.28188(12) 0.0295(3) Uani d . 1 . . F
F8 0.2803(2) 0.32431(19) -0.47908(13) 0.0295(3) Uani d . 1 . . F
F9 0.30964(18) 0.06826(18) -0.43321(13) 0.0265(3) Uani d . 1 . . F
F10 -0.04581(19) 0.25217(17) -0.44759(12) 0.0240(3) Uani d . 1 . . F
N1 0.0976(2) 0.3777(2) 0.17887(16) 0.0179(3) Uani d . 1 . . N
H1A -0.0065 0.3262 0.1199 0.0400(18) Uiso calc R 1 . . H
C1 0.2498(3) 0.3213(3) 0.1338(2) 0.0236(4) Uani d . 1 . . C
H1B 0.2190 0.2027 0.1213 0.0400(18) Uiso calc R 1 . . H
H1C 0.3646 0.3784 0.1935 0.0400(18) Uiso calc R 1 . . H
C2 0.2821(3) 0.3530(3) 0.0209(2) 0.0245(5) Uani d . 1 . . C
H2D 0.2606 0.4559 0.0205 0.0400(18) Uiso calc R 1 . . H
H2E 0.4106 0.3670 0.0177 0.0400(18) Uiso calc R 1 . . H
N2 0.1587(3) 0.2149(3) -0.08402(18) 0.0241(4) Uani d . 1 . . N
H2A 0.1776 0.1202 -0.0838 0.0400(18) Uiso calc R 1 . . H
H2B 0.1837 0.2370 -0.1483 0.0400(18) Uiso calc R 1 . . H
H2C 0.0406 0.2047 -0.0830 0.0400(18) Uiso calc R 1 . . H
C3 0.1333(3) 0.5622(3) 0.20895(19) 0.0186(4) Uani d . 1 . . C
H3D 0.0367 0.5900 0.2452 0.0400(18) Uiso calc R 1 . . H
H3E 0.1270 0.5907 0.1375 0.0400(18) Uiso calc R 1 . . H
C4 0.3216(3) 0.6652(3) 0.2914(2) 0.0256(5) Uani d . 1 . . C
H4D 0.3398 0.6215 0.3552 0.0400(18) Uiso calc R 1 . . H
H4E 0.4193 0.6585 0.2497 0.0400(18) Uiso calc R 1 . . H
N3 0.3309(3) 0.8409(2) 0.33845(17) 0.0219(4) Uani d . 1 . . N
H3A 0.2514 0.8483 0.3847 0.0400(18) Uiso calc R 1 . . H
H3B 0.3013 0.8770 0.2795 0.0400(18) Uiso calc R 1 . . H
H3C 0.4457 0.9033 0.3795 0.0400(18) Uiso calc R 1 . . H
C5 0.0564(3) 0.3155(3) 0.2787(2) 0.0256(5) Uani d . 1 . . C
H5A 0.1567 0.3792 0.3475 0.0400(18) Uiso calc R 1 . . H
H5B 0.0491 0.1994 0.2585 0.0400(18) Uiso calc R 1 . . H
C6 -0.1256(4) 0.3314(3) 0.3062(2) 0.0282(5) Uani d . 1 . . C
H6A -0.0996 0.4212 0.3793 0.0400(18) Uiso calc R 1 . . H
H6B -0.1902 0.3598 0.2449 0.0400(18) Uiso calc R 1 . . H
N4 -0.2461(3) 0.1757(3) 0.31569(19) 0.0263(4) Uani d . 1 . . N
H4A -0.2815 0.0961 0.2462 0.0400(18) Uiso calc R 1 . . H
H4B -0.3459 0.1922 0.3390 0.0400(18) Uiso calc R 1 . . H
H4C -0.1837 0.1448 0.3676 0.0400(18) Uiso calc R 1 . . H
OW 0.5195(4) 0.3353(4) 0.3911(3) 0.0755(9) Uani d . 1 . . O
H1W 0.4355 0.3238 0.4350 0.0400(18) Uiso d . 1 . . H
H2W 0.5840 0.4481 0.4103 0.0400(18) Uiso d . 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Al1 0.0143(3) 0.0191(3) 0.0176(3) 0.0061(2) 0.0036(2) 0.0085(2)
Al2 0.0152(3) 0.0213(3) 0.0151(3) 0.0058(2) 0.0041(2) 0.0068(2)
F1 0.0195(6) 0.0174(6) 0.0183(6) 0.0063(5) 0.0056(5) 0.0045(5)
F2 0.0230(7) 0.0311(7) 0.0227(7) 0.0131(6) 0.0040(5) 0.0140(6)
F3 0.0264(7) 0.0383(8) 0.0298(7) 0.0155(6) 0.0147(6) 0.0170(6)
F4 0.0266(7) 0.0207(7) 0.0325(8) 0.0028(6) -0.0011(6) 0.0130(6)
F5 0.0181(6) 0.0242(7) 0.0304(7) 0.0074(5) -0.0006(5) 0.0131(6)
F6 0.0198(6) 0.0233(6) 0.0157(6) 0.0052(5) 0.0053(5) 0.0075(5)
F7 0.0346(8) 0.0326(8) 0.0159(6) 0.0067(6) 0.0027(6) 0.0058(6)
F8 0.0283(7) 0.0301(8) 0.0297(8) 0.0031(6) 0.0118(6) 0.0138(6)
F9 0.0165(6) 0.0298(7) 0.0317(8) 0.0089(6) 0.0022(5) 0.0080(6)
F10 0.0233(7) 0.0255(7) 0.0261(7) 0.0114(6) 0.0069(5) 0.0089(6)
N1 0.0178(8) 0.0198(8) 0.0174(8) 0.0070(7) 0.0040(7) 0.0071(7)
C1 0.0241(11) 0.0259(11) 0.0262(11) 0.0143(9) 0.0082(9) 0.0092(9)
C2 0.0262(11) 0.0231(11) 0.0305(12) 0.0118(9) 0.0140(9) 0.0111(9)
N2 0.0263(10) 0.0282(10) 0.0259(10) 0.0142(8) 0.0101(8) 0.0140(8)
C3 0.0180(9) 0.0188(10) 0.0199(10) 0.0071(8) 0.0039(8) 0.0072(8)
C4 0.0175(10) 0.0216(11) 0.0327(12) 0.0044(8) 0.0010(9) 0.0058(9)
N3 0.0181(9) 0.0237(9) 0.0204(9) 0.0049(7) 0.0038(7) 0.0042(7)
C5 0.0272(11) 0.0308(12) 0.0266(12) 0.0113(10) 0.0094(9) 0.0182(10)
C6 0.0309(12) 0.0253(11) 0.0329(13) 0.0090(10) 0.0162(10) 0.0130(10)
N4 0.0253(10) 0.0262(10) 0.0277(10) 0.0055(8) 0.0060(8) 0.0123(8)
OW 0.0619(18) 0.077(2) 0.087(2) 0.0266(15) 0.0436(17) 0.0093(17)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0560 0.0520 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0140 0.0100 '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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
F2 Al1 F4 . . 94.02(8) ?
F2 Al1 F3 . . 90.91(8) ?
F4 Al1 F3 . . 94.33(8) ?
F2 Al1 F5 . . 179.04(7) ?
F4 Al1 F5 . . 86.89(7) ?
F3 Al1 F5 . . 89.34(8) ?
F2 Al1 F1 . 2_655 90.03(7) ?
F4 Al1 F1 . 2_655 170.15(7) ?
F3 Al1 F1 . 2_655 94.58(7) ?
F5 Al1 F1 . 2_655 89.02(7) ?
F2 Al1 F1 . . 90.88(7) ?
F4 Al1 F1 . . 93.69(7) ?
F3 Al1 F1 . . 171.64(7) ?
F5 Al1 F1 . . 88.75(7) ?
F1 Al1 F1 2_655 . 77.26(7) ?
F7 Al2 F8 . . 96.81(8) ?
F7 Al2 F10 . . 91.94(8) ?
F8 Al2 F10 . . 90.26(7) ?
F7 Al2 F9 . . 93.71(8) ?
F8 Al2 F9 . . 90.88(8) ?
F10 Al2 F9 . . 174.06(8) ?
F7 Al2 F6 . . 92.51(7) ?
F8 Al2 F6 . . 170.67(7) ?
F10 Al2 F6 . . 89.78(7) ?
F9 Al2 F6 . . 88.15(7) ?
F7 Al2 F6 . 2_554 169.37(7) ?
F8 Al2 F6 . 2_554 93.79(7) ?
F10 Al2 F6 . 2_554 87.26(7) ?
F9 Al2 F6 . 2_554 86.85(7) ?
F6 Al2 F6 . 2_554 76.89(7) ?
C5 N1 C3 . . 112.54(18) ?
C5 N1 C1 . . 109.66(17) ?
C3 N1 C1 . . 114.30(17) ?
C5 N1 H1A . . 106.6 ?
C3 N1 H1A . . 106.6 ?
C1 N1 H1A . . 106.6 ?
N1 C1 C2 . . 114.29(18) ?
N1 C1 H1B . . 108.7 ?
C2 C1 H1B . . 108.7 ?
N1 C1 H1C . . 108.7 ?
C2 C1 H1C . . 108.7 ?
H1B C1 H1C . . 107.6 ?
N2 C2 C1 . . 112.21(19) ?
N2 C2 H2D . . 109.2 ?
C1 C2 H2D . . 109.2 ?
N2 C2 H2E . . 109.2 ?
C1 C2 H2E . . 109.2 ?
H2D C2 H2E . . 107.9 ?
C2 N2 H2A . . 109.5 ?
C2 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
C2 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
N1 C3 C4 . . 112.31(18) ?
N1 C3 H3D . . 109.1 ?
C4 C3 H3D . . 109.1 ?
N1 C3 H3E . . 109.1 ?
C4 C3 H3E . . 109.1 ?
H3D C3 H3E . . 107.9 ?
N3 C4 C3 . . 109.57(19) ?
N3 C4 H4D . . 109.8 ?
C3 C4 H4D . . 109.8 ?
N3 C4 H4E . . 109.8 ?
C3 C4 H4E . . 109.8 ?
H4D C4 H4E . . 108.2 ?
C4 N3 H3A . . 109.5 ?
C4 N3 H3B . . 109.5 ?
H3A N3 H3B . . 109.5 ?
C4 N3 H3C . . 109.5 ?
H3A N3 H3C . . 109.5 ?
H3B N3 H3C . . 109.5 ?
N1 C5 C6 . . 111.04(19) ?
N1 C5 H5A . . 109.4 ?
C6 C5 H5A . . 109.4 ?
N1 C5 H5B . . 109.4 ?
C6 C5 H5B . . 109.4 ?
H5A C5 H5B . . 108.0 ?
N4 C6 C5 . . 111.6(2) ?
N4 C6 H6A . . 109.3 ?
C5 C6 H6A . . 109.3 ?
N4 C6 H6B . . 109.3 ?
C5 C6 H6B . . 109.3 ?
H6A C6 H6B . . 108.0 ?
C6 N4 H4A . . 109.5 ?
C6 N4 H4B . . 109.5 ?
H4A N4 H4B . . 109.5 ?
C6 N4 H4C . . 109.5 ?
H4A N4 H4C . . 109.5 ?
H4B N4 H4C . . 109.5 ?
H1W OW H2W . . 108.0(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 F2 . 1.7538(15) y
Al1 F4 . 1.7802(16) y
Al1 F3 . 1.7842(16) y
Al1 F5 . 1.7989(15) y
Al1 F1 2_655 1.8821(15) y
Al1 F1 . 1.8859(15) y
Al2 F7 . 1.7610(17) y
Al2 F8 . 1.7742(15) y
Al2 F10 . 1.7822(15) y
Al2 F9 . 1.7848(15) y
Al2 F6 . 1.8955(15) y
Al2 F6 2_554 1.9117(16) ?
F1 Al1 2_655 1.8821(15) ?
F1 F1 2_655 2.352(3) ?
F1 F2 2_655 2.5734(19) ?
F1 F5 . 2.5776(19) ?
F1 F5 2_655 2.581(2) ?
F1 F2 . 2.595(2) ?
F1 F4 . 2.675(2) ?
F1 F3 2_655 2.695(2) ?
F2 F3 . 2.522(2) ?
F2 F1 2_655 2.5734(19) ?
F2 F4 . 2.585(2) ?
F2 F5 2_655 2.917(2) ?
F3 F5 . 2.519(2) ?
F3 F4 . 2.614(2) ?
F3 F1 2_655 2.695(2) ?
F4 F5 . 2.4611(19) ?
F5 F1 2_655 2.581(2) ?
F5 F2 2_655 2.917(2) ?
F6 Al2 2_554 1.9117(16) ?
F6 F6 2_554 2.367(3) ?
F6 F9 2_554 2.543(2) ?
F6 F10 2_554 2.550(2) ?
F6 F9 . 2.5613(19) ?
F6 F10 . 2.597(2) ?
F6 F7 . 2.643(2) ?
F6 F8 2_554 2.693(2) ?
F7 F10 . 2.547(2) ?
F7 F9 . 2.587(2) ?
F7 F8 . 2.644(2) ?
F8 F10 . 2.520(2) ?
F8 F9 . 2.536(2) ?
F8 F6 2_554 2.693(2) ?
F9 F6 2_554 2.543(2) ?
F9 F10 2_554 2.825(2) ?
F10 F6 2_554 2.550(2) ?
F10 F9 2_554 2.825(2) ?
N1 C5 . 1.502(3) y
N1 C3 . 1.505(3) y
N1 C1 . 1.508(3) y
N1 H1A . 0.9100 ?
C1 C2 . 1.517(3) y
C1 H1B . 0.9700 ?
C1 H1C . 0.9700 ?
C2 N2 . 1.482(3) y
C2 H2D . 0.9700 ?
C2 H2E . 0.9700 ?
N2 H2A . 0.8900 ?
N2 H2B . 0.8900 ?
N2 H2C . 0.8900 ?
C3 C4 . 1.519(3) y
C3 H3D . 0.9700 ?
C3 H3E . 0.9700 ?
C4 N3 . 1.478(3) y
C4 H4D . 0.9700 ?
C4 H4E . 0.9700 ?
N3 H3A . 0.8900 ?
N3 H3B . 0.8900 ?
N3 H3C . 0.8900 ?
C5 C6 . 1.520(3) y
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 N4 . 1.472(3) y
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
N4 H4A . 0.8900 ?
N4 H4B . 0.8900 ?
N4 H4C . 0.8900 ?
OW H1W . 0.895(3) ?
OW H2W . 0.927(3) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A F4 1_455 0.91 1.89 2.738(2) 154.3
N1 H1A F5 1_455 0.91 2.14 2.796(2) 128.7
N2 H2A F5 2_655 0.89 1.81 2.683(2) 167.3
N2 H2B F7 . 0.89 1.79 2.678(3) 174.8
N2 H2C F3 1_455 0.89 2.03 2.814(3) 145.9
N3 H3A F10 2_565 0.89 1.95 2.764(2) 151.7
N3 H3B F3 2_665 0.89 1.88 2.771(3) 177.2
N3 H3C F9 2_665 0.89 1.83 2.650(2) 152.0
N4 H4A F2 2 0.89 2.10 2.884(3) 146.4
N4 H4B OW 1_455 0.89 1.88 2.694(4) 150.4
N4 H4C F10 1_556 0.89 2.17 2.884(3) 136.3
N4 H4C F9 2 0.89 2.27 2.869(3) 124.8
OW H1W F8 1_556 0.895(3) 1.6924(15) 2.584(3) 173.8(2)
OW H2W F8 2_665 0.927(3) 1.8713(16) 2.786(4) 168.8(2)
|
1100120.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100120.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_1100120
loop_
_publ_author_name
'Ben Ali, A.'
'Maisonneuve, V.'
'Kodjikian, S.'
'Smiri, L. S.'
'Leblanc, M.'
_publ_section_title
;
Synthesis, crystal structure and magnetic properties of a new
fluoride carbonate Ba~2~Co(CO~3~)~2~F~2~
;
_journal_coden_ASTM SSSCFJ
_journal_issue 4
_journal_name_full 'Solid State Sciences'
_journal_page_first 503
_journal_page_last 506
_journal_paper_doi 10.1016/S1293-2558(02)01274-8
_journal_volume 4
_journal_year 2002
_chemical_formula_structural 'Ba2 Co (C O3)2 F2'
_chemical_formula_sum 'C2 Ba2 Co F2 O6'
_chemical_name_systematic 'Dibarium Cobalt Dicarbonate Difluoride'
_space_group_IT_number 61
_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 4
_cell_length_a 6.6226(6)
_cell_length_b 11.494(2)
_cell_length_c 9.021(2)
_cell_volume 686.68
_refine_ls_R_factor_all 0.034
_cod_original_formula_sum 'C2 Ba2 Co1 F2 O6'
_cod_database_code 1100120
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x+1/2, y, -z+1/2'
2 'x, -y+1/2, z+1/2'
3 '-x+1/2, y+1/2, z'
4 '-x, -y, -z'
5 '-x+1/2, -y, z+1/2'
6 '-x, y+1/2, -z+1/2'
7 'x+1/2, -y+1/2, -z'
8 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Ba1 Ba2+ 8 c 0.01427(4) 0.32801(2) 0.10795(3) 1. 0 0.791(8)
Co1 Co2+ 4 a 0. 0. 0. 1. 0 0.62(2)
C1 C4+ 8 c 0.2488(8) 0.5902(4) 0.2413(6) 1. 0 0.80(6)
O1 O2- 8 c 0.2626(7) 0.5874(4) 0.0974(4) 1. 0 1.29(6)
O2 O2- 8 c 0.3049(6) 0.6779(4) 0.3121(5) 1. 0 1.13(5)
O3 O2- 8 c 0.1797(6) 0.4979(4) 0.3068(5) 1. 0 1.24(6)
F1 F1- 8 c 0.4085(5) 0.3451(3) 0.0893(4) 1. 0 0.95(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba2+ 2
C4+ 4
Co2+ 2
F1- -1
O2- -2
|
1100121.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100121.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_1100121
loop_
_publ_author_name
'Ben Ali, A.'
'Maisonneuve, V.'
'Smiri, L.S.'
'Leblanc, M.'
_publ_section_title
;
Synthesis and crystal structure of Ba Zn (C O3) F2; revision of the
structure of Ba Mn (C O3) F2
;
_journal_coden_ASTM SSSCFJ
_journal_issue 7
_journal_name_full 'Solid State Sciences'
_journal_page_first 891
_journal_page_last 894
_journal_paper_doi 10.1016/S1293-2558(02)01339-0
_journal_volume 4
_journal_year 2002
_chemical_formula_structural 'Ba Mn (C O3) F2'
_chemical_formula_sum 'C Ba F2 Mn O3'
_chemical_name_systematic
;
Barium Manganese Carbonate Difluoride
;
_space_group_IT_number 176
_symmetry_Int_Tables_number 176
_symmetry_space_group_name_Hall '-P 6c'
_symmetry_space_group_name_H-M 'P 63/m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 2
_cell_length_a 4.9120(8)
_cell_length_b 4.9120(8)
_cell_length_c 9.919(1)
_cell_volume 207.26
_refine_ls_R_factor_all 0.019
_cod_original_formula_sum 'C1 Ba1 F2 Mn1 O3'
_cod_database_code 1100121
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 '-x+y, -x, -z+1/2'
2 '-y, x-y, -z+1/2'
3 'x, y, -z+1/2'
4 'x-y, x, -z'
5 'y, -x+y, -z'
6 '-x, -y, -z'
7 'x-y, x, z+1/2'
8 'y, -x+y, z+1/2'
9 '-x, -y, z+1/2'
10 '-x+y, -x, z'
11 '-y, x-y, z'
12 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Ba1 Ba2+ 2 b 0. 0. 0. 1. 0 0.86(1)
Mn1 Mn2+ 2 c 0.3333 0.6667 0.250 1. 0 0.90(2)
C1 C4+ 2 d 0.6667 0.3333 0.250 1. 0 0.76(6)
O1 O2- 6 h 0.3705(7) 0.2389(6) 0.250 1. 0 1.11(4)
F1 F1- 4 f 0.3333 0.6667 0.0447(2) 1. 0 1.42(3)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba2+ 2
C4+ 4
F1- -1
Mn2+ 2
O2- -2
|
1100122.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100122.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_1100122
loop_
_publ_author_name
'Ben Ali, A.'
'Maisonneuve, V.'
'Smiri, L.S.'
'Leblanc, M.'
_publ_section_title
;
Synthesis and crystal structure of Ba Zn (C O3) F2; revision of the
structure of Ba Mn (C O3) F2
;
_journal_coden_ASTM SSSCFJ
_journal_issue 7
_journal_name_full 'Solid State Sciences'
_journal_page_first 891
_journal_page_last 894
_journal_paper_doi 10.1016/S1293-2558(02)01339-0
_journal_volume 4
_journal_year 2002
_chemical_formula_structural 'Ba Zn (C O3) F2'
_chemical_formula_sum 'C Ba F2 O3 Zn'
_chemical_name_systematic 'Barium Zinc Carbonate Difluoride'
_space_group_IT_number 176
_symmetry_Int_Tables_number 176
_symmetry_space_group_name_Hall '-P 6c'
_symmetry_space_group_name_H-M 'P 63/m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 2
_cell_length_a 4.8523(8)
_cell_length_b 4.8523(8)
_cell_length_c 9.854(1)
_cell_volume 200.93
_refine_ls_R_factor_all 0.016
_cod_original_formula_sum 'C1 Ba1 F2 O3 Zn1'
_cod_database_code 1100122
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 '-x+y, -x, -z+1/2'
2 '-y, x-y, -z+1/2'
3 'x, y, -z+1/2'
4 'x-y, x, -z'
5 'y, -x+y, -z'
6 '-x, -y, -z'
7 'x-y, x, z+1/2'
8 'y, -x+y, z+1/2'
9 '-x, -y, z+1/2'
10 '-x+y, -x, z'
11 '-y, x-y, z'
12 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Ba1 Ba2+ 2 b 0. 0. 0. 1. 0 0.83(1)
Zn1 Zn2+ 2 c 0.3333 0.6667 0.250 1. 0 0.79(2)
C1 C4+ 2 d 0.6667 0.3333 0.250 1. 0 0.8(1)
O1 O2- 6 h 0.3759(8) 0.2711(8) 0.250 1. 0 0.99(4)
F1 F1- 4 f 0.3333 0.6667 0.0472(3) 1. 0 1.26(5)
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ba2+ 2
C4+ 4
F1- -1
O2- -2
Zn2+ 2
|
1100123.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100123.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_1100123
loop_
_publ_author_name
'A. Martel'
'V. Maisonneuve'
'E. Brown'
'G. Dujardin'
_journal_issue 4
_journal_name_full Synthesis
_journal_page_first 539
_journal_page_last 544
_journal_paper_doi 10.1055/s-2003-37657
_journal_year 2003
_chemical_formula_moiety 'C21 H31 I1 O4'
_chemical_formula_sum 'C21 H31 I O4'
_chemical_melting_point 348.15
_chemical_name_systematic
;
(7R*,8R*,10R*)-(+-)-10-Benzyloxymethyl-8-t-butoxy-7-iodo-1-oxacyclodecan-2-one
;
_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 91.7(2)
_cell_angle_beta 90.51(4)
_cell_angle_gamma 93.21(7)
_cell_formula_units_Z 2
_cell_length_a 6.150(3)
_cell_length_b 12.32(5)
_cell_length_c 14.549(14)
_cell_volume 1100.073
_diffrn_ambient_temperature 293
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.432
_exptl_crystal_description needle
_refine_ls_R_factor_gt 0.1189
_refine_ls_wR_factor_gt 0.1189
_cod_original_formula_sum 'C21 H31 I1 O4'
_cod_database_code 1100123
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 0.761(4) -0.0576(17) 0.3927(14)
C2 C 0.724(4) 0.0598(18) 0.4194(15)
H1 H 0.85540 0.10350 0.40650
H2 H 0.70180 0.06440 0.48530
C3 C 0.532(3) 0.1110(19) 0.3722(14)
H3 H 0.50580 0.17960 0.40350
H4 H 0.40210 0.06330 0.37820
C4 C 0.570(4) 0.1313(19) 0.2691(15)
H5 H 0.44400 0.16520 0.24510
H6 H 0.69360 0.18350 0.26460
C5 C 0.612(3) 0.0360(17) 0.2077(15)
H7 H 0.74070 0.00300 0.23050
H8 H 0.64550 0.06240 0.14710
C6 C 0.418(3) -0.0579(14) 0.1970(12)
H9 H 0.34730 -0.06780 0.25650
C7 C 0.489(3) -0.1621(16) 0.1621(13)
H10 H 0.56100 -0.15130 0.10300
C8 C 0.651(3) -0.2137(16) 0.2301(12)
H11 H 0.67770 -0.28620 0.20650
H12 H 0.78870 -0.17120 0.22860
C9 C 0.584(3) -0.2229(17) 0.3320(13)
H13 H 0.69440 -0.26180 0.36460
C10 C 0.365(3) -0.2790(17) 0.3478(14)
H14 H 0.24990 -0.23190 0.33160
H15 H 0.34750 -0.34520 0.31010
O1 O 0.352(2) -0.3034(11) 0.4412(8)
C11 C 0.151(4) -0.345(2) 0.4637(16)
H16 H 0.11650 -0.41060 0.42700
H17 H 0.04400 -0.29270 0.44900
C12 C 0.134(3) -0.3701(17) 0.5628(14)
C13 C 0.282(3) -0.4238(17) 0.6064(14)
H18 H 0.40290 -0.44370 0.57340
C14 C 0.270(5) -0.452(2) 0.698(2)
H19 H 0.37990 -0.48900 0.72550
C15 C 0.089(5) -0.425(2) 0.745(2)
H20 H 0.07490 -0.44460 0.80560
C16 C -0.066(5) -0.371(2) 0.7058(19)
H21 H -0.18550 -0.35160 0.74040
C17 C -0.053(4) -0.342(2) 0.6129(18)
H22 H -0.16370 -0.30560 0.58520
O2 O 0.5734(18) -0.1158(11) 0.3742(8)
O3 O 0.936(2) -0.0967(13) 0.3873(11)
I1 I 0.1899(2) 0.01191(16) 0.10077(11)
O4 O 0.2964(19) -0.2305(10) 0.1471(8)
C18 C 0.278(3) -0.3116(18) 0.0716(14)
C19 C 0.387(5) -0.267(2) -0.015(2)
H23 H 0.29820 -0.21390 -0.04120
H24 H 0.40350 -0.32550 -0.05900
H25 H 0.52750 -0.23370 0.00110
C20 C 0.031(4) -0.322(2) 0.0563(19)
H26 H -0.04090 -0.29810 0.11090
H27 H -0.01370 -0.39690 0.04230
H28 H -0.00810 -0.27830 0.00590
C21 C 0.370(5) -0.419(2) 0.097(2)
H29 H 0.52380 -0.40870 0.10750
H30 H 0.34240 -0.47170 0.04740
H31 H 0.30080 -0.44520 0.15160
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
I 1.40
O 0.68
|
1100124.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100124.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_1100124
_chemical_formula_moiety ?
_chemical_formula_sum 'C26 H22 N9 O11 Pr'
_chemical_formula_weight 777.44
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_space_group_IT_number 2
_symmetry_cell_setting ?
_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 90.61
_cell_angle_beta 96.13
_cell_angle_gamma 103.19
_cell_formula_units_Z 2
_cell_length_a 7.780
_cell_length_b 11.326
_cell_length_c 17.873
_cell_measurement_reflns_used ?
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1523.6
_computing_cell_refinement ?
_computing_data_collection ?
_computing_data_reduction ?
_computing_molecular_graphics ?
_computing_publication_material ?
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution ?
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 0.71070
_diffrn_reflns_av_R_equivalents 0.0310
_diffrn_reflns_av_sigmaI/netI 0.0330
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 6556
_diffrn_reflns_theta_full 21.02
_diffrn_reflns_theta_max 21.02
_diffrn_reflns_theta_min 1.15
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.673
_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 1.695
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 776
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_refine_diff_density_max 0.610
_refine_diff_density_min -1.166
_refine_diff_density_rms 0.122
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.120
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 525
_refine_ls_number_reflns 3279
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.120
_refine_ls_R_factor_all 0.0291
_refine_ls_R_factor_gt 0.0264
_refine_ls_shift/su_max 0.030
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+1.9831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0615
_refine_ls_wR_factor_ref 0.0648
_reflns_number_gt 3135
_reflns_number_total 3279
_reflns_threshold_expression >2sigma(I)
_cod_database_code 1100124
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
Pr Pr 0.37530(3) 0.279253(18) 0.736020(12) 0.02953(13) Uani 1 1 d . . .
O2 O 0.7956(5) 0.1159(4) 0.8139(3) 0.0822(13) Uani 1 1 d . . .
O5 O 0.3632(4) 0.4830(3) 0.79011(17) 0.0426(8) Uani 1 1 d . . .
O6 O 0.4003(5) 0.2442(3) 0.60103(17) 0.0493(8) Uani 1 1 d . . .
O7 O 0.6428(5) 0.4364(3) 0.6951(2) 0.0539(9) Uani 1 1 d . . .
O8 O 0.5364(5) 0.1463(3) 0.8267(2) 0.0618(10) Uani 1 1 d . . .
O9 O 0.6433(5) 0.1817(3) 0.7226(2) 0.0561(9) Uani 1 1 d . . .
N10 N 0.3023(5) 0.2995(3) 0.8823(2) 0.0414(9) Uani 1 1 d . . .
O11 O 0.6836(5) 0.3943(3) 0.81102(19) 0.0523(8) Uani 1 1 d . . .
O12 O 0.3040(5) 0.4179(3) 0.9064(2) 0.0627(10) Uani 1 1 d . . .
O13 O 0.1698(5) 0.0803(3) 0.7835(2) 0.0560(9) Uani 1 1 d . . .
O21 O 0.2197(9) 0.0718(4) 0.6716(3) 0.128(2) Uani 1 1 d . . .
O22 O 0.9032(5) 0.4925(3) 0.7549(2) 0.0712(11) Uani 1 1 d . . .
O32 O 0.0730(6) -0.0863(3) 0.7200(2) 0.0823(13) Uani 1 1 d . . .
N14 N 0.7478(5) 0.4434(3) 0.7495(3) 0.0373(9) Uani 1 1 d . . .
N16 N 0.6611(6) 0.1464(3) 0.7888(3) 0.0496(11) Uani 1 1 d . . .
N17 N 0.3048(5) 0.3995(4) 0.5523(2) 0.0363(9) Uani 1 1 d . . .
H14 H 0.278(5) 0.438(4) 0.519(3) 0.027(13) Uiso 1 1 d . . .
N18 N 0.3376(6) 0.5040(4) 0.8550(3) 0.0566(11) Uani 1 1 d . . .
C19 C 0.3434(6) 0.6310(4) 0.8847(2) 0.0373(11) Uani 1 1 d . . .
O20 O 0.0566(6) 0.2839(5) 0.7301(3) 0.0602(12) Uani 1 1 d . . .
H20A H 0.035(10) 0.328(6) 0.741(4) 0.07(3) Uiso 1 1 d . . .
H20B H -0.020(11) 0.236(7) 0.754(4) 0.11(3) Uiso 1 1 d . . .
N25 N 0.1537(5) 0.0205(3) 0.7245(2) 0.0390(9) Uani 1 1 d . . .
N30 N 0.2816(5) 0.4380(3) 0.6236(2) 0.0403(9) Uani 1 1 d . . .
N15 N 0.2034(5) 0.5951(3) 0.4989(2) 0.0417(9) Uani 1 1 d . . .
N23 N 0.1892(5) 0.3371(3) 1.0308(2) 0.0458(10) Uani 1 1 d . . .
C24 C 0.2589(7) 0.2179(5) 0.9299(3) 0.0447(12) Uani 1 1 d . . .
H13 H 0.263(7) 0.143(5) 0.914(3) 0.062(16) Uiso 1 1 d . . .
C27 C 0.3863(8) 0.0824(5) 0.3892(3) 0.0627(15) Uani 1 1 d . . .
H13 H 0.399(8) 0.003(6) 0.380(3) 0.078(18) Uiso 1 1 d . . .
C28 C 0.2027(6) 0.2275(4) 1.0043(2) 0.0396(11) Uani 1 1 d . . .
C29 C 0.3787(7) 0.7234(4) 0.8350(3) 0.0492(12) Uani 1 1 d . . .
H29 H 0.394(6) 0.707(4) 0.784(3) 0.045(13) Uiso 1 1 d . . .
C31 C 0.1890(6) 0.6201(4) 0.5724(3) 0.0401(11) Uani 1 1 d . . .
C34 C 0.3436(6) 0.3152(5) 0.4051(3) 0.0427(12) Uani 1 1 d . . .
H12 H 0.325(6) 0.391(5) 0.408(3) 0.051(14) Uiso 1 1 d . . .
C35 C 0.1324(7) 0.3424(5) 1.0981(3) 0.0510(13) Uani 1 1 d . . .
H18 H 0.118(8) 0.414(6) 1.111(3) 0.08(2) Uiso 1 1 d . . .
C36 C 0.3640(6) 0.2503(4) 0.4677(2) 0.0360(11) Uani 1 1 d . . .
C37 C 0.1076(8) 0.8047(5) 0.5421(4) 0.0601(15) Uani 1 1 d . . .
H4 H 0.082(8) 0.879(6) 0.566(4) 0.09(2) Uiso 1 1 d . . .
C38 C 0.1399(7) 0.7246(5) 0.5947(3) 0.0490(13) Uani 1 1 d . . .
H25 H 0.137(7) 0.737(5) 0.645(3) 0.063(16) Uiso 1 1 d . . .
C42 C 0.3593(6) 0.2976(4) 0.5456(3) 0.0394(11) Uani 1 1 d . . .
C43 C 0.1619(7) 0.1249(5) 1.0469(3) 0.0462(12) Uani 1 1 d . . .
H15 H 0.170(6) 0.054(5) 1.028(3) 0.051(14) Uiso 1 1 d . . .
C44 C 0.1697(6) 0.6763(5) 0.4494(3) 0.0453(12) Uani 1 1 d . . .
H18 H 0.187(6) 0.663(4) 0.401(3) 0.042(13) Uiso 1 1 d . . .
C45 C 0.1218(7) 0.7809(5) 0.4690(4) 0.0560(14) Uani 1 1 d . . .
H9 H 0.095(6) 0.829(5) 0.433(3) 0.048(14) Uiso 1 1 d . . .
C46 C 0.3631(8) 0.8672(5) 0.9305(4) 0.0638(17) Uani 1 1 d . . .
H2 H 0.375(10) 0.944(7) 0.951(4) 0.11(2) Uiso 1 1 d . . .
C47 C 0.3447(7) 0.2654(5) 0.3353(3) 0.0512(13) Uani 1 1 d . . .
H10 H 0.332(6) 0.310(5) 0.293(3) 0.053(14) Uiso 1 1 d . . .
C48 C 0.1057(7) 0.1352(6) 1.1161(3) 0.0525(15) Uani 1 1 d . . .
H8 H 0.074(6) 0.077(5) 1.140(3) 0.044(15) Uiso 1 1 d . . .
C49 C 0.3871(8) 0.8406(5) 0.8590(4) 0.0619(15) Uani 1 1 d . . .
H12 H 0.423(8) 0.898(6) 0.828(4) 0.08(2) Uiso 1 1 d . . .
C50 C 0.0897(7) 0.2453(5) 1.1414(3) 0.0492(13) Uani 1 1 d . . .
H24 H 0.055(7) 0.252(5) 1.185(4) 0.063(17) Uiso 1 1 d . . .
C51 C 0.3860(8) 0.1342(5) 0.4598(3) 0.0532(14) Uani 1 1 d . . .
H7 H 0.396(7) 0.097(5) 0.496(3) 0.054(17) Uiso 1 1 d . . .
C52 C 0.3272(8) 0.7753(6) 0.9804(4) 0.0638(17) Uani 1 1 d . . .
H21 H 0.320(8) 0.788(6) 1.025(4) 0.07(2) Uiso 1 1 d . . .
C54 C 0.3172(7) 0.6564(5) 0.9572(3) 0.0484(13) Uani 1 1 d . . .
H19 H 0.296(6) 0.602(4) 0.991(3) 0.045(15) Uiso 1 1 d . . .
C55 C 0.2281(6) 0.5357(4) 0.6298(3) 0.0424(11) Uani 1 1 d . . .
H5 H 0.216(6) 0.559(4) 0.683(3) 0.045(12) Uiso 1 1 d . . .
C56 C 0.3630(8) 0.1487(5) 0.3265(3) 0.0561(14) Uani 1 1 d . . .
H10 H 0.361(7) 0.111(5) 0.275(3) 0.072(16) 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
Pr 0.03894(18) 0.02514(17) 0.02758(17) 0.00285(10) 0.01276(11) 0.00949(11)
O2 0.058(2) 0.080(3) 0.122(4) 0.035(2) 0.010(2) 0.040(2)
O5 0.067(2) 0.0386(18) 0.0289(18) 0.0036(14) 0.0238(15) 0.0178(15)
O6 0.078(2) 0.0437(19) 0.0299(18) 0.0071(16) 0.0140(16) 0.0185(17)
O7 0.066(3) 0.040(2) 0.057(2) 0.0078(16) 0.021(2) 0.0093(17)
O8 0.057(2) 0.061(2) 0.075(3) 0.0269(19) 0.028(2) 0.0184(18)
O9 0.072(2) 0.052(2) 0.054(2) -0.0041(18) 0.0173(18) 0.0296(18)
N10 0.063(3) 0.026(2) 0.039(2) 0.0022(19) 0.0152(19) 0.0153(18)
O11 0.065(2) 0.0374(18) 0.054(2) -0.0018(16) 0.0079(18) 0.0085(16)
O12 0.094(3) 0.044(2) 0.054(2) 0.0071(18) 0.022(2) 0.0177(19)
O13 0.080(3) 0.0400(19) 0.048(2) 0.0022(18) 0.0143(18) 0.0099(17)
O21 0.202(6) 0.078(3) 0.071(3) -0.030(3) 0.076(4) -0.064(3)
O22 0.055(3) 0.054(2) 0.103(3) -0.017(2) 0.023(2) 0.003(2)
O32 0.115(3) 0.042(2) 0.079(3) -0.0131(19) 0.041(2) -0.018(2)
N14 0.027(2) 0.0122(18) 0.073(3) -0.0090(19) 0.005(2) 0.0047(17)
N16 0.054(3) 0.027(2) 0.071(3) 0.007(2) 0.014(3) 0.013(2)
N17 0.052(2) 0.038(2) 0.022(2) 0.0022(19) 0.0119(18) 0.0135(19)
N18 0.060(3) 0.051(3) 0.062(3) 0.010(2) 0.013(2) 0.015(2)
C19 0.043(3) 0.029(3) 0.043(3) -0.002(2) 0.008(2) 0.013(2)
O20 0.046(2) 0.054(3) 0.089(3) 0.023(3) 0.024(2) 0.020(2)
N25 0.054(2) 0.024(2) 0.037(2) -0.007(2) 0.0236(19) -0.0043(18)
N30 0.043(2) 0.036(2) 0.043(2) -0.0014(18) 0.0127(18) 0.0074(18)
N15 0.046(2) 0.043(2) 0.037(2) 0.0038(19) 0.0078(17) 0.0102(18)
N23 0.064(3) 0.039(2) 0.038(2) 0.0011(18) 0.019(2) 0.0115(19)
C24 0.067(3) 0.030(3) 0.043(3) 0.003(3) 0.018(2) 0.016(2)
C27 0.089(4) 0.039(3) 0.063(4) -0.008(3) 0.018(3) 0.017(3)
C28 0.049(3) 0.042(3) 0.030(3) 0.002(2) 0.010(2) 0.012(2)
C29 0.057(3) 0.034(3) 0.058(4) -0.001(3) 0.011(3) 0.009(2)
C31 0.036(3) 0.043(3) 0.039(3) 0.005(2) 0.007(2) 0.003(2)
C34 0.053(3) 0.037(3) 0.039(3) -0.003(2) 0.011(2) 0.010(2)
C35 0.063(3) 0.050(4) 0.040(3) -0.007(3) 0.014(3) 0.011(3)
C36 0.038(3) 0.036(3) 0.033(3) -0.003(2) 0.0093(19) 0.004(2)
C37 0.068(4) 0.045(3) 0.070(4) -0.003(3) 0.005(3) 0.019(3)
C38 0.055(3) 0.050(3) 0.046(3) -0.008(3) 0.009(3) 0.017(2)
C42 0.043(3) 0.031(3) 0.044(3) 0.002(2) 0.011(2) 0.004(2)
C43 0.056(3) 0.039(3) 0.047(3) 0.004(3) 0.014(2) 0.014(2)
C44 0.049(3) 0.052(3) 0.036(3) 0.005(3) 0.006(2) 0.014(2)
C45 0.058(3) 0.050(3) 0.061(4) 0.015(3) 0.005(3) 0.016(3)
C46 0.062(4) 0.038(3) 0.091(5) -0.021(4) -0.010(3) 0.018(3)
C47 0.069(4) 0.052(3) 0.032(3) 0.006(3) 0.006(2) 0.012(3)
C48 0.055(3) 0.056(4) 0.046(3) 0.025(3) 0.016(3) 0.006(3)
C49 0.067(4) 0.037(3) 0.082(5) 0.002(3) 0.013(3) 0.012(3)
C50 0.052(3) 0.062(4) 0.034(3) 0.004(3) 0.015(2) 0.009(3)
C51 0.073(4) 0.051(4) 0.035(3) 0.009(3) 0.007(3) 0.012(3)
C52 0.068(4) 0.070(5) 0.058(4) -0.030(4) -0.006(3) 0.031(3)
C54 0.071(4) 0.041(3) 0.039(3) -0.006(3) 0.008(3) 0.024(3)
C55 0.049(3) 0.041(3) 0.037(3) -0.001(2) 0.010(2) 0.009(2)
C56 0.080(4) 0.054(4) 0.034(3) -0.010(3) 0.013(3) 0.012(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'
Pr Pr -0.2180 2.8214 '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
O6 Pr O20 100.42(15) . . ?
O6 Pr O5 122.60(10) . . ?
O20 Pr O5 73.09(16) . . ?
O6 Pr O21 60.81(13) . . ?
O20 Pr O21 77.7(2) . . ?
O5 Pr O21 150.73(19) . . ?
O6 Pr O7 70.23(12) . . ?
O20 Pr O7 130.52(15) . . ?
O5 Pr O7 72.84(10) . . ?
O21 Pr O7 127.74(13) . . ?
O6 Pr O9 70.29(11) . . ?
O20 Pr O9 155.77(16) . . ?
O5 Pr O9 130.99(11) . . ?
O21 Pr O9 78.28(18) . . ?
O7 Pr O9 68.77(11) . . ?
O6 Pr O8 113.76(12) . . ?
O20 Pr O8 125.34(14) . . ?
O5 Pr O8 115.51(11) . . ?
O21 Pr O8 83.26(18) . . ?
O7 Pr O8 101.47(12) . . ?
O9 Pr O8 47.81(11) . . ?
O6 Pr O13 107.63(11) . . ?
O20 Pr O13 65.77(15) . . ?
O5 Pr O13 119.22(11) . . ?
O21 Pr O13 46.85(12) . . ?
O7 Pr O13 163.59(12) . . ?
O9 Pr O13 95.02(12) . . ?
O8 Pr O13 63.91(11) . . ?
O6 Pr O11 112.24(11) . . ?
O20 Pr O11 138.15(16) . . ?
O5 Pr O11 67.56(10) . . ?
O21 Pr O11 141.04(19) . . ?
O7 Pr O11 48.03(11) . . ?
O9 Pr O11 64.30(10) . . ?
O8 Pr O11 64.05(11) . . ?
O13 Pr O11 123.43(11) . . ?
O6 Pr N10 172.37(11) . . ?
O20 Pr N10 73.27(14) . . ?
O5 Pr N10 60.31(10) . . ?
O21 Pr N10 112.91(13) . . ?
O7 Pr N10 117.06(11) . . ?
O9 Pr N10 113.72(11) . . ?
O8 Pr N10 68.11(11) . . ?
O13 Pr N10 66.10(11) . . ?
O11 Pr N10 75.33(11) . . ?
O6 Pr N30 58.11(10) . . ?
O20 Pr N30 68.48(13) . . ?
O5 Pr N30 67.23(10) . . ?
O21 Pr N30 100.16(16) . . ?
O7 Pr N30 65.74(11) . . ?
O9 Pr N30 119.41(11) . . ?
O8 Pr N30 166.14(11) . . ?
O13 Pr N30 127.84(11) . . ?
O11 Pr N30 107.16(10) . . ?
N10 Pr N30 121.59(10) . . ?
N18 O5 Pr 125.6(3) . . ?
C42 O6 Pr 131.1(3) . . ?
N14 O7 Pr 101.0(3) . . ?
N16 O8 Pr 96.4(3) . . ?
N16 O9 Pr 97.5(3) . . ?
C24 N10 O12 115.4(4) . . ?
C24 N10 Pr 130.3(3) . . ?
O12 N10 Pr 114.2(2) . . ?
N14 O11 Pr 93.4(2) . . ?
N18 O12 N10 116.1(4) . . ?
N25 O13 Pr 95.9(2) . . ?
N25 O21 Pr 99.9(3) . . ?
O7 N14 O22 126.9(5) . . ?
O7 N14 O11 115.8(4) . . ?
O22 N14 O11 117.2(4) . . ?
O2 N16 O8 122.6(5) . . ?
O2 N16 O9 121.0(5) . . ?
O8 N16 O9 116.4(4) . . ?
C42 N17 N30 118.2(4) . . ?
O5 N18 O12 123.6(4) . . ?
O5 N18 C19 122.4(4) . . ?
O12 N18 C19 113.9(4) . . ?
C54 C19 C29 120.0(4) . . ?
C54 C19 N18 123.3(4) . . ?
C29 C19 N18 116.7(4) . . ?
O21 N25 O13 117.1(4) . . ?
O21 N25 O32 122.2(4) . . ?
O13 N25 O32 120.6(4) . . ?
C55 N30 N17 118.1(4) . . ?
C55 N30 Pr 130.4(3) . . ?
N17 N30 Pr 111.5(3) . . ?
C44 N15 C31 116.7(4) . . ?
C35 N23 C28 117.7(4) . . ?
N10 C24 C28 130.1(4) . . ?
C56 C27 C51 119.2(5) . . ?
N23 C28 C43 120.9(4) . . ?
N23 C28 C24 119.1(4) . . ?
C43 C28 C24 120.1(4) . . ?
C49 C29 C19 119.4(6) . . ?
N15 C31 C38 121.7(4) . . ?
N15 C31 C55 119.3(4) . . ?
C38 C31 C55 119.0(4) . . ?
C36 C34 C47 120.5(5) . . ?
N23 C35 C50 123.8(5) . . ?
C34 C36 C51 119.1(4) . . ?
C34 C36 C42 123.4(4) . . ?
C51 C36 C42 117.5(4) . . ?
C45 C37 C38 119.5(5) . . ?
C37 C38 C31 119.2(5) . . ?
O6 C42 N17 120.8(4) . . ?
O6 C42 C36 121.8(4) . . ?
N17 C42 C36 117.3(4) . . ?
C48 C43 C28 119.2(5) . . ?
N15 C44 C45 123.4(5) . . ?
C37 C45 C44 119.3(5) . . ?
C49 C46 C52 119.6(5) . . ?
C34 C47 C56 121.0(5) . . ?
C50 C48 C43 119.2(5) . . ?
C46 C49 C29 121.3(6) . . ?
C35 C50 C48 119.2(5) . . ?
C36 C51 C27 120.9(5) . . ?
C46 C52 C54 119.9(6) . . ?
C19 C54 C52 119.8(6) . . ?
N30 C55 C31 130.3(4) . . ?
C27 C56 C47 119.3(5) . . ?
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
Pr O6 2.476(3) . ?
Pr O20 2.484(4) . ?
Pr O5 2.518(3) . ?
Pr O21 2.580(4) . ?
Pr O7 2.588(3) . ?
Pr O9 2.603(3) . ?
Pr O8 2.635(3) . ?
Pr O13 2.653(3) . ?
Pr O11 2.664(3) . ?
Pr N10 2.753(4) . ?
Pr N30 2.858(4) . ?
O2 N16 1.218(5) . ?
O5 N18 1.227(5) . ?
O6 C42 1.218(5) . ?
O7 N14 1.192(5) . ?
O8 N16 1.240(5) . ?
O9 N16 1.257(5) . ?
N10 C24 1.276(6) . ?
N10 O12 1.400(5) . ?
O11 N14 1.331(5) . ?
O12 N18 1.349(6) . ?
O13 N25 1.225(5) . ?
O21 N25 1.214(6) . ?
O22 N14 1.203(5) . ?
O32 N25 1.227(5) . ?
N17 C42 1.325(6) . ?
N17 N30 1.385(5) . ?
N18 C19 1.517(6) . ?
C19 C54 1.370(7) . ?
C19 C29 1.378(7) . ?
N30 C55 1.275(6) . ?
N15 C44 1.333(6) . ?
N15 C31 1.363(6) . ?
N23 C35 1.330(6) . ?
N23 C28 1.354(6) . ?
C24 C28 1.454(7) . ?
C27 C56 1.374(8) . ?
C27 C51 1.387(8) . ?
C28 C43 1.390(7) . ?
C29 C49 1.376(8) . ?
C31 C38 1.391(7) . ?
C31 C55 1.464(7) . ?
C34 C36 1.361(7) . ?
C34 C47 1.365(7) . ?
C35 C50 1.351(8) . ?
C36 C51 1.372(7) . ?
C36 C42 1.493(6) . ?
C37 C45 1.352(8) . ?
C37 C38 1.357(8) . ?
C43 C48 1.368(7) . ?
C44 C45 1.373(7) . ?
C46 C49 1.352(9) . ?
C46 C52 1.378(9) . ?
C47 C56 1.371(7) . ?
C48 C50 1.359(8) . ?
C52 C54 1.387(8) . ?
|
1100125.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100125.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_1100125
loop_
_publ_author_name
'Ito, T'
'West, J'
_publ_section_title
;
The Structure of Hemimorphite (H2 Zn2 Si O5)
;
_journal_coden_ASTM ZEKGAX
_journal_name_full
;
Zeitschrift fuer Kristallographie, Kristallgeometrie, Kristallphysik,
Kristallchemie (-144,1977)
;
_journal_page_first 1
_journal_page_last 8
_journal_volume 83
_journal_year 1932
_chemical_compound_source 'from Altenberg, Harz, Germany'
_chemical_formula_structural 'Zn4 (O H)2 (H2 O) (Si2 O7)'
_chemical_formula_sum 'H4 O10 Si2 Zn4'
_chemical_name_mineral Hemimorphite
_chemical_name_systematic 'Tetrazinc dihydroxide hydrate disilicate *'
_space_group_IT_number 44
_symmetry_cell_setting orthorhombic
_symmetry_Int_Tables_number 44
_symmetry_space_group_name_Hall 'I 2 -2'
_symmetry_space_group_name_H-M 'I m m 2'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.38
_cell_length_b 10.7
_cell_length_c 5.11
_cell_volume 458.2
_exptl_crystal_density_meas 3.45
_cod_duplicate_entry 1011257
_cod_database_code 1100125
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,z
-x,y,z
x,-y,z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2+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_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Si1 Si4+ 4 d 0. 0.16 0. 1. 0 d
Zn1 Zn2+ 8 e 0.3 0.342 0.01 1. 0 d
O1 O2- 2 a 0. 0. 0. 1. 0 d
O2 O2- 8 e 0.161 0.187 0.85 1. 0 d
O3 O2- 4 d 0. 0.187 0.305 1. 0 d
O4 O2- 4 c 0.25 0.5 0.85 1. 1 d
O5 O2- 2 b 0. 0.5 0.35 1. 2 d
H1 H1+ 8 e -1. -1. -1. 1. 0 dum
loop_
_atom_type_symbol
_atom_type_oxidation_number
Si4+ 4.000
Zn2+ 2.000
O2- -2.000
H1+ 1.000
|
1100126.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100126.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_1100126
loop_
_publ_author_name
'Saada, M.A.'
'Hemon-Ribaud, A.'
'Maisonneuve, V.'
'Smiri, L.S.'
'Leblanc, M.'
_publ_section_title
;
K2 Zr3 O F12: microwave-assisted hydrothermal synthesis and powder
diffraction study
;
_journal_coden_ASTM ACSEBH
_journal_issue 9
_journal_name_full
'Acta Crystallographica E, Structure Reports Online'
_journal_page_first i131
_journal_page_last i133
_journal_paper_doi 10.1107/S1600536803018567
_journal_volume 59
_journal_year 2003
_chemical_formula_structural 'K2 Zr3 O F12'
_chemical_formula_sum 'F12 K2 O Zr3'
_chemical_name_systematic
;
Dipotassium Trizirconium Oxide Dodecafluoride
;
_space_group_IT_number 166
_symmetry_space_group_name_Hall '-R 3 2"'
_symmetry_space_group_name_H-M 'R -3 m :H'
_cell_angle_alpha 90.
_cell_angle_beta 90.
_cell_angle_gamma 120.
_cell_formula_units_Z 6
_cell_length_a 7.6887(3)
_cell_length_b 7.6887(3)
_cell_length_c 28.870(1)
_cell_volume 1478.03
_refine_ls_R_factor_all 0.057
_cod_original_sg_symbol_H-M 'R -3 m'
_cod_original_formula_sum 'F12 K2 O1 Zr3'
_cod_database_code 1100126
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x-y, -y, -z'
2 '-x, -x+y, -z'
3 'y, x, -z'
4 'x-y, x, -z'
5 'y, -x+y, -z'
6 '-x, -y, -z'
7 '-x+y, y, z'
8 'x, x-y, z'
9 '-y, -x, z'
10 '-x+y, -x, z'
11 '-y, x-y, z'
12 'x, y, z'
13 'x-y+2/3, -y+1/3, -z+1/3'
14 'x-y+1/3, -y+2/3, -z+2/3'
15 '-x+2/3, -x+y+1/3, -z+1/3'
16 '-x+1/3, -x+y+2/3, -z+2/3'
17 'y+2/3, x+1/3, -z+1/3'
18 'y+1/3, x+2/3, -z+2/3'
19 'x-y+2/3, x+1/3, -z+1/3'
20 'x-y+1/3, x+2/3, -z+2/3'
21 'y+2/3, -x+y+1/3, -z+1/3'
22 'y+1/3, -x+y+2/3, -z+2/3'
23 '-x+2/3, -y+1/3, -z+1/3'
24 '-x+1/3, -y+2/3, -z+2/3'
25 '-x+y+2/3, y+1/3, z+1/3'
26 '-x+y+1/3, y+2/3, z+2/3'
27 'x+2/3, x-y+1/3, z+1/3'
28 'x+1/3, x-y+2/3, z+2/3'
29 '-y+2/3, -x+1/3, z+1/3'
30 '-y+1/3, -x+2/3, z+2/3'
31 '-x+y+2/3, -x+1/3, z+1/3'
32 '-x+y+1/3, -x+2/3, z+2/3'
33 '-y+2/3, x-y+1/3, z+1/3'
34 '-y+1/3, x-y+2/3, z+2/3'
35 'x+2/3, y+1/3, z+1/3'
36 'x+1/3, y+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_U_iso_or_equiv
K1 K1+ 3 a 0 0 0 1. 0 0.021(1)
K2 K1+ 3 b 0 0 0.5 1. 0 0.021(1)
K3 K1+ 6 c 0 0 0.1364(2) 1. 0 0.0211(11)
Zr1 Zr4+ 18 h 0.51535(9) -.51535(9) 0.06227(5) 1. 0 0.0110(4)
F1 F1- 18 f 0.3376(7) 0 0 1. 0 0.0129(9)
F2 F1- 18 h 0.1473(4) -.1473(4) 0.2019(2) 1. 0 0.0129(9)
F3 F1- 18 h 0.1574(4) -.1574(4) 0.9233(2) 1. 0 0.0129(9)
F4 F1- 18 h 0.2214(4) -.2214(4) 0.0727(2) 1. 0 0.0129(9)
O1 O2- 6 c 0 0 0.2830(4) 1. 0 0.0129(9)
loop_
_atom_type_symbol
_atom_type_oxidation_number
F1- -1
K1+ 1
O2- -2
Zr4+ 4
|
1100127.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100127.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_1100127
loop_
_publ_author_name
'Ben Ali, A.'
'Maisonneuve, V.'
'Leblanc, M.'
_publ_section_title
;
Phase stability regions in the (Na2 C O3) - (Yb F3) - (H2 O) system
at 190 C. Crystal structures of two new fluoride carbonates, Na2 Yb
(C O3)2 F and Na3 Yb (C O3)2 F2
;
_journal_coden_ASTM SSSCFJ
_journal_issue 11-12
_journal_name_full 'Solid State Sciences'
_journal_page_first 1367
_journal_page_last 1375
_journal_paper_doi 10.1016/S1293-2558(02)00024-9
_journal_volume 4
_journal_year 2002
_chemical_formula_structural 'Na2 Yb (C O3)2 F'
_chemical_formula_sum 'C2 F Na2 O6 Yb'
_chemical_name_systematic
;
Disodium Ytterbium Dicarbonate Fluoride
;
_space_group_IT_number 15
_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 95.64(3)
_cell_angle_gamma 90.
_cell_formula_units_Z 8
_cell_length_a 17.440(6)
_cell_length_b 6.1003(17)
_cell_length_c 11.2366(14)
_cell_volume 1189.67
_refine_ls_R_factor_all 0.034
_cod_original_formula_sum 'C2 F1 Na2 O6 Yb1'
_cod_database_code 1100127
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x, -y, z+1/2'
2 '-x, -y, -z'
3 '-x, y, -z+1/2'
4 'x, y, z'
5 'x+1/2, -y+1/2, z+1/2'
6 '-x+1/2, -y+1/2, -z'
7 '-x+1/2, y+1/2, -z+1/2'
8 'x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_U_iso_or_equiv
Yb1 Yb3+ 8 f 0.560193(18) 0.34289(5) 0.63128(2) 1. 0 0.00872(14)
Na1 Na1+ 8 f 0.6099(2) 0.0966(6) 0.3818(3) 1. 0 0.0174(7)
Na2 Na1+ 8 f 0.7360(3) -.0883(6) 0.6440(3) 1. 0 0.0255(8)
C1 C4+ 8 f 0.5639(5) -.2039(13) 0.6167(6) 1. 0 0.0112(13)
C2 C4+ 8 f 0.7932(5) 0.0762(12) 0.4223(6) 1. 0 0.0118(14)
O1 O2- 8 f 0.5060(3) 0.6869(9) 0.5650(5) 1. 0 0.0117(10)
O2 O2- 8 f 0.6065(4) 0.2996(10) 0.2009(5) 1. 0 0.0168(11)
O3 O2- 8 f 0.8037(4) -.1906(10) 0.8271(5) 1. 0 0.0154(11)
O4 O2- 8 f 0.5784(3) -.0088(9) 0.5847(5) 1. 0 0.0144(11)
O5 O2- 8 f 0.7314(3) -.0249(11) 0.4345(5) 1. 0 0.0190(12)
O6 O2- 8 f 0.6489(3) 0.4309(10) 0.4970(5) 1. 0 0.0144(11)
F1 F1- 8 f 0.4387(3) 0.2695(10) 0.6738(4) 1. 0 0.0245(11)
loop_
_atom_type_symbol
_atom_type_oxidation_number
C4+ 4
F1- -1
Na1+ 1
O2- -2
Yb3+ 3
|
1100128.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100128.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_1100128
loop_
_publ_author_name
'Ben Ali, A.'
'Maisonneuve, V.'
'Leblanc, M.'
_publ_section_title
;
Phase stability regions in the (Na2 C O3) - (Yb F3) - (H2 O) system
at 190 C. Crystal structures of two new fluoride carbonates, Na2 Yb
(C O3)2 F and Na3 Yb (C O3)2 F2
;
_journal_coden_ASTM SSSCFJ
_journal_issue 11-12
_journal_name_full 'Solid State Sciences'
_journal_page_first 1367
_journal_page_last 1375
_journal_paper_doi 10.1016/S1293-2558(02)00024-9
_journal_volume 4
_journal_year 2002
_chemical_formula_structural 'Na3 Yb (C O3)2 F2'
_chemical_formula_sum 'C2 F2 Na3 O6 Yb'
_chemical_name_systematic
;
Trisodium Ytterbium Dicarbonate Difluoride
;
_space_group_IT_number 9
_symmetry_Int_Tables_number 9
_symmetry_space_group_name_Hall 'C -2yc'
_symmetry_space_group_name_H-M 'C 1 c 1'
_cell_angle_alpha 90.
_cell_angle_beta 112.56(3)
_cell_angle_gamma 90.
_cell_formula_units_Z 8
_cell_length_a 7.127(2)
_cell_length_b 29.816(9)
_cell_length_c 6.9280(4)
_cell_volume 1359.54
_refine_ls_R_factor_all 0.074
_cod_original_formula_sum 'C2 F2 Na3 O6 Yb1'
_cod_database_code 1100128
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x, -y, z+1/2'
2 'x, y, z'
3 'x+1/2, -y+1/2, z+1/2'
4 'x+1/2, y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_U_iso_or_equiv
Yb1 Yb3+ 4 a 0.62432(17) 0.02453(13) 0.50007(18) 0.5 0 0.0205(7)
Yb2 Yb3+ 4 a 0.1300(2) 0.01921(16) 0.4985(2) 0.5 0 0.0254(6)
Yb3 Yb3+ 4 a 0.8775(3) 0.22886(3) 0.9989(3) 1. 0 0.0200(4)
Na1 Na1+ 4 a 0.62432(17) 0.02453(13) 0.50007(18) 0.5 0 0.0205(7)
Na2 Na1+ 4 a 0.1300(2) 0.01921(16) 0.4985(2) 0.5 0 0.0254(6)
Na3 Na1+ 4 a 0.368(4) 0.2174(5) 0.980(3) 1. 0 0.039(3)
Na4 Na1+ 4 a 0.999(2) 0.1276(5) 0.738(3) 1. 0 0.030(3)
Na5 Na1+ 4 a 0.760(2) 0.1201(5) 0.246(2) 1. 0 0.030(3)
Na6 Na1+ 4 a 0.252(2) 0.1212(5) 0.243(2) 1. 0 0.029(3)
Na7 Na1+ 4 a 0.517(3) 0.1306(5) 0.748(3) 1. 0 0.040(4)
C1 C4+ 4 a 0.143(3) 0.1940(5) 0.483(3) 1. 0 0.006(3)
C2 C4+ 4 a 0.887(7) 0.9462(9) 0.504(7) 1. 0 0.030(5)
C3 C4+ 4 a 0.385(7) 0.9435(8) 0.494(8) 1. 0 0.040(7)
C4 C4+ 4 a 0.631(5) 0.1956(12) 0.489(5) 1. 0 0.036(8)
O1 O2- 4 a 0.080(2) 0.1537(5) 0.466(2) 1. 0 0.011(3)
O2 O2- 4 a 0.056(3) 0.2258(4) 0.360(3) 1. 0 0.014(3)
O3 O2- 4 a 0.783(4) 0.9735(9) 0.362(4) 1. 0 0.043(6)
O4 O2- 4 a 0.336(4) 0.9026(7) 0.460(4) 1. 0 0.035(5)
O5 O2- 4 a 0.314(3) 0.2055(6) 0.653(3) 1. 0 0.017(3)
O6 O2- 4 a 0.552(4) 0.9521(11) 0.661(5) 1. 0 0.057(7)
O7 O2- 4 a 0.059(4) 0.9556(10) 0.663(5) 1. 0 0.051(7)
O8 O2- 4 a 0.843(4) 0.9031(8) 0.469(4) 1. 0 0.039(5)
O9 O2- 4 a 0.310(4) 0.9766(11) 0.373(5) 1. 0 0.048(7)
O10 O2- 4 a 0.488(5) 0.2141(11) 0.339(5) 1. 0 0.053(7)
O11 O2- 4 a 0.779(5) 0.2041(11) 0.678(5) 1. 0 0.060
O12 O2- 4 a 0.607(5) 0.1531(13) 0.467(6) 1. 0 0.066(9)
F1 F1- 4 a 0.674(3) 0.1825(6) 0.038(3) 1. 0 0.029(4)
F2 F1- 4 a 0.100(3) 0.1785(6) 0.011(3) 1. 0 0.023(4)
F3 F1- 4 a 0.399(4) 0.0715(7) 0.527(4) 1. 0 0.045(5)
F4 F1- 4 a 0.894(5) 0.0692(8) 0.533(4) 1. 0 0.049(6)
loop_
_atom_type_symbol
_atom_type_oxidation_number
C4+ 4
F1- -1
Na1+ 1
O2- -2
Yb3+ 3
|
1100129.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100129.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_1100129
loop_
_publ_author_name
'Awaleh, M.O.'
'Ben Ali, A.'
'Maisonneuve, V.'
'Leblanc, M.'
_publ_section_title
;
Microwave-assisted synthesis, crystal structures and thermal
behaviour of Na5 Y (C O3)4 and Na5 Yb (C O3)4 * 2(H2 O)
;
_journal_coden_ASTM JALCEU
_journal_issue 1-2
_journal_name_full 'Journal of Alloys Compd.'
_journal_page_first 114
_journal_page_last 120
_journal_paper_doi 10.1016/S0925-8388(02)00910-6
_journal_volume 349
_journal_year 2003
_chemical_formula_structural 'Na5 Y (C O3)4'
_chemical_formula_sum 'C4 Na5 O12 Y'
_chemical_name_systematic 'Pentasodium Yttrium Tetracarbonate'
_space_group_IT_number 14
_symmetry_Int_Tables_number 14
_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 90.39(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.209(3)
_cell_length_b 10.085(4)
_cell_length_c 8.783(4)
_cell_volume 1081.41
_refine_ls_R_factor_all 0.065
_cod_original_formula_sum 'C4 Na5 O12 Y1'
_cod_database_code 1100129
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x, -y+1/2, z+1/2'
2 '-x, -y, -z'
3 '-x, y+1/2, -z+1/2'
4 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Y1 Y3+ 4 e 0.27554(6) 0.12411(8) 0.21440(8) 1. 0 0.80(1)
Na1 Na1+ 4 e 0.2122(2) 0.8742(4) 0.6964(4) 1. 0 1.66(6)
Na2 Na1+ 4 e 0.1033(3) 0.3737(4) 0.0847(4) 1. 0 1.57(5)
Na3 Na1+ 4 e 0.0745(3) 0.8750(5) 0.0458(3) 1. 0 1.96(6)
Na4 Na1+ 4 e 0.4015(3) 0.4203(4) 0.0771(4) 1. 0 1.58(6)
Na5 Na1+ 4 e 0.3664(3) 0.8243(4) 0.0141(4) 1. 0 1.84(6)
C1 C4+ 4 e 0.0128(6) 0.1083(8) 0.2552(8) 1. 0 0.9(1)
C2 C4+ 4 e 0.2182(6) 0.881(1) 0.3590(8) 1. 0 1.1(1)
C3 C4+ 4 e 0.2768(6) 0.3663(9) 0.3874(8) 1. 0 1.0(1)
C4 C4+ 4 e 0.5043(6) 0.134(1) 0.2613(9) 1. 0 1.2(1)
O1 O2- 4 e 0.2684(4) 0.3672(6) 0.2432(5) 1. 0 1.23(9)
O2 O2- 4 e 0.2297(4) 0.8934(6) 0.2124(6) 1. 0 1.3(1)
O3 O2- 4 e 0.2713(5) 0.2456(7) 0.9573(7) 1. 0 1.32(9)
O4 O2- 4 e 0.2228(5) 0.9896(6) 0.4351(6) 1. 0 1.1(1)
O5 O2- 4 e 0.0952(4) 0.1515(6) 0.1751(6) 1. 0 1.6(1)
O6 O2- 4 e 0.3998(4) 0.8483(6) 0.6894(7) 1. 0 2.0(1)
O7 O2- 4 e 0.4401(4) 0.0448(6) 0.3226(7) 1. 0 1.5(1)
O8 O2- 4 e 0.4618(5) 0.2010(6) 0.1511(7) 1. 0 1.8(1)
O9 O2- 4 e 0.9573(5) 0.0106(6) 0.2008(7) 1. 0 1.8(1)
O10 O2- 4 e 0.9875(5) 0.1635(7) 0.3791(7) 1. 0 2.3(1)
O11 O2- 4 e 0.2054(5) 0.7677(6) 0.4193(7) 1. 0 1.5(1)
O12 O2- 4 e 0.2920(5) 0.0288(6) 0.9675(7) 1. 0 1.7(1)
loop_
_atom_type_symbol
_atom_type_oxidation_number
C4+ 4
Na1+ 1
O2- -2
Y3+ 3
|
1100130.cif | #------------------------------------------------------------------------------
#$Date: 2016-09-13 15:04:05 +0300 (Tue, 13 Sep 2016) $
#$Revision: 186542 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100130.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_1100130
loop_
_publ_author_name
'Awaleh, M.O.'
'Ben Ali, A.'
'Maisonneuve, V.'
'Leblanc, M.'
_publ_section_title
;
Microwave-assisted synthesis, crystal structures and thermal
behaviour of Na5 Y (C O3)4 and Na5 Yb (C O3)4 * 2(H2 O)
;
_journal_coden_ASTM JALCEU
_journal_issue 1-2
_journal_name_full 'Journal of Alloys Compd.'
_journal_page_first 114
_journal_page_last 120
_journal_paper_doi 10.1016/S0925-8388(02)00910-6
_journal_volume 349
_journal_year 2003
_chemical_formula_structural 'Na5 Yb (C O3)4 (H2 O)2'
_chemical_formula_sum 'C4 H4 Na5 O14 Yb'
_chemical_name_systematic
;
Pentasodium Ytterbium Tetracarbonate Dihydrate
;
_space_group_IT_number 114
_symmetry_Int_Tables_number 114
_symmetry_space_group_name_Hall 'P -4 2n'
_symmetry_space_group_name_H-M 'P -4 21 c'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.593(2)
_cell_length_b 7.593(2)
_cell_length_c 11.528(8)
_cell_volume 664.63
_refine_ls_R_factor_all 0.023
_cod_original_formula_sum 'C4 H4 Na5 O14 Yb1'
_cod_database_code 1100130
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'y+1/2, x+1/2, z+1/2'
2 'y, -x, -z'
3 '-y+1/2, -x+1/2, z+1/2'
4 '-y, x, -z'
5 'x+1/2, -y+1/2, -z+1/2'
6 '-x, -y, z'
7 '-x+1/2, y+1/2, -z+1/2'
8 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Yb1 Yb3+ 2 a 0. 0. 0. 1. 0 1.060(7)
Na1 Na1+ 2 b 0.5 0.5 0. 1. 0 2.18(5)
Na2 Na1+ 8 e 0.3230(2) 0.1815(2) 0.2075(1) 1. 0 1.92(2)
C1 C4+ 8 e 0.1824(4) 0.2861(3) -0.0795(2) 1. 0 1.39(3)
O1 O2- 8 e 0.0954(3) 0.1796(3) 0.8525(2) 1. 0 1.46(3)
O2 O2- 8 e 0.1702(3) 0.2527(3) 0.0315(2) 1. 0 1.61(3)
O3 O2- 8 e 0.2745(3) 0.4092(3) 0.8803(2) 1. 0 2.29(4)
O4 O2- 4 d 0. 0.5 0.1673(3) 1. 0 2.03(4)
H1 H1+ 8 e 0.056(8) 0.438(8) 0.115(4) 1. 0 2.03(4)
loop_
_atom_type_symbol
_atom_type_oxidation_number
C4+ 4
H1+ 1
Na1+ 1
O2- -2
Yb3+ 3
|
1100131.cif | #------------------------------------------------------------------------------
#$Date: 2016-09-18 01:35:58 +0300 (Sun, 18 Sep 2016) $
#$Revision: 186632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100131.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_1100131
loop_
_publ_author_name
'Ben Ali, A.'
'Smiri, L.'
'Maisonneuve, V.'
_publ_section_title
;
Crystal structure of Na Rb B4 O5 (O H)4 * 4(H2 O): comparison with
other tetraborate hydrates
;
_journal_coden_ASTM JALCEU
_journal_issue 1-2
_journal_name_full 'Journal of Alloys and Compounds'
_journal_page_first 153
_journal_page_last 159
_journal_paper_doi 10.1016/S0925-8388(01)01259-2
_journal_volume 322
_journal_year 2001
_chemical_formula_structural 'Na Rb (B4 O5 (O H)4) (H2 O)4'
_chemical_formula_sum 'B4 H12 Na O13 Rb'
_chemical_name_systematic
;
Sodium Rubidium Tetrahydroxopentaoxotetraborate Tetrahydrate
;
_space_group_IT_number 14
_symmetry_Int_Tables_number 14
_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 91.91(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.1138(5)
_cell_length_b 11.471(1)
_cell_length_c 12.8233(9)
_cell_volume 1192.85
_refine_ls_R_factor_all 0.045
_cod_original_formula_sum 'H12 B4 Na1 O13 Rb1'
_cod_database_code 1100131
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 'x, -y+1/2, z+1/2'
2 '-x, -y, -z'
3 '-x, y+1/2, -z+1/2'
4 'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_B_iso_or_equiv
Rb1 Rb1+ 4 e 0.03366(5) 0.10923(4) 0.13288(3) 1. 0 0
Na1 Na1+ 4 e 0.1502(2) 0.0909(1) 0.4633(1) 1. 0 0
B1 B3+ 4 e 0.6405(4) 0.0980(3) 0.9066(3) 1. 0 0
B2 B3+ 4 e 0.3929(4) 0.3182(3) 0.7902(3) 1. 0 0
B3 B3+ 4 e 0.3877(4) 0.1074(3) 0.7882(3) 1. 0 0
B4 B3+ 4 e 0.6394(4) 0.2031(3) 0.7421(2) 1. 0 0
O1 O2- 4 e 0.5136(2) 0.1181(2) 0.7093(2) 1. 0 0
O2 O2- 4 e 0.5568(2) 0.3156(2) 0.7684(2) 1. 0 0
O3 O2- 4 e 0.7288(2) 0.1594(2) 0.8369(2) 1. 0 0
O4 O2- 4 e 0.4743(2) 0.0797(2) 0.8922(2) 1. 0 0
O5 O2- 4 e 0.3012(2) 0.2190(2) 0.7981(2) 1. 0 0
O6 O2- 4 e 0.2655(2) 0.0187(2) 0.7656(2) 1. 0 0
O7 O2- 4 e 0.7239(3) 0.0565(3) 0.9933(2) 1. 0 0
O8 O2- 4 e 0.7605(3) 0.2226(2) 0.6637(2) 1. 0 0
O9 O2- 4 e 0.3119(3) 0.4212(2) 0.8057(2) 1. 0 0
O10 O2- 4 e 0.0268(3) 0.2259(3) 0.9179(3) 1. 2 0
O11 O2- 4 e 0.6621(4) 0.0673(4) 0.4814(2) 1. 2 0
O12 O2- 4 e 0.3285(3) 0.2355(3) 0.5485(2) 1. 2 0
O13 O2- 4 e 0.0146(3) 0.0595(3) 0.6223(2) 1. 2 0
H1 H1+ 4 e 0.674(7) 0.042(5) 0.249(4) 1. 0 5.5
H2 H1+ 4 e 0.656(7) 0.017(5) 0.037(5) 1. 0 5.5
H3 H1+ 4 e 0.700(7) 0.255(5) 0.112(5) 1. 0 5.5
H4 H1+ 4 e 0.374(5) 0.487(3) 0.805(4) 1. 0 5.5
loop_
_atom_type_symbol
_atom_type_oxidation_number
B3+ 3
H1+ 1
Na1+ 1
O2- -2
Rb1+ 1
|
1100132.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100132.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_1100132
_publ_contact_author_name 'Luca Lutterotti'
_chemical_formula_sum 'Ni Ti'
_chemical_name_common austenite
_symmetry_cell_setting cubic
_symmetry_space_group_name_H-M Pm-3m
_audit_creation_date 'Mon Oct 12 15:11:53 PDT 1998'
_audit_creation_method 'Maud, version 1.9992'
_audit_update_record 'Last update Wed May 04 13:16:22 CEST 2005'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 1
_cell_length_a 3.015
_cell_length_b 3.015
_cell_length_c 3.015
_computing_structure_refinement 'Maud, version 1.9992'
_refine_ls_goodness_of_fit_all 0
_refine_ls_R_factor_all 0
_refine_ls_wR_factor_all 0
_cod_original_formula_sum NiTi
_cod_database_code 1100132
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_B_iso_or_equiv
Ni Ni 1.0 0.0 0.0 0.0 0.0
Ti Ti 1.0 0.5 0.5 0.5 0.0
|
1100133.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100133.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_1100133
loop_
_publ_author_name
'Rademeyer, M.'
_publ_section_title
;
Bis(p-toluidinium) tetrachlorozincate(II)
;
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m304
_journal_page_last m306
_journal_paper_doi 10.1107/S1600536805000747
_journal_volume 61
_journal_year 2005
_chemical_formula_moiety '2(C7 H10 N), Cl4 Zn'
_chemical_formula_sum 'C14 H20 Cl4 N2 Zn'
_chemical_formula_weight 423.35
_chemical_melting_point ?
_chemical_name_common 'Bis(p-toluidinium) tetrachlorozincate(II)'
_chemical_name_systematic 'Bis(p-toluidinium) tetrachlorozincate(II)'
_space_group_IT_number 2
_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
_audit_creation_method SHELXL-97
_cell_angle_alpha 107.14(5)
_cell_angle_beta 95.43(7)
_cell_angle_gamma 92.03(6)
_cell_formula_units_Z 2
_cell_length_a 7.119(8)
_cell_length_b 11.532(6)
_cell_length_c 12.490(7)
_cell_measurement_reflns_used 195
_cell_measurement_temperature 280(2)
_cell_measurement_theta_max 31
_cell_measurement_theta_min 2
_cell_volume 973.3(13)
_computing_cell_refinement
'CrysAlis CCD 170 (Oxford Diffraction Ltd., 2003)'
_computing_data_collection
'CrysAlis CCD 170 (Oxford Diffraction Ltd., 2003)'
_computing_data_reduction
'CrysAlis RED 170 (Oxford Diffraction Ltd., 2003)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2000)'
_computing_publication_material
'WinGX (Farrugia, 1999) and PLATON (Spek, 2000)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature 280(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type 'Oxford Excalibur2'
_diffrn_measurement_method 'omega-2theta 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 0.0327
_diffrn_reflns_av_sigmaI/netI 0.0612
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 9806
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 31.73
_diffrn_reflns_theta_min 4.54
_diffrn_standards_decay_% <2
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time n/a
_diffrn_standards_number n/a
_exptl_absorpt_coefficient_mu 1.805
_exptl_absorpt_correction_T_max 0.6998
_exptl_absorpt_correction_T_min 0.6012
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(Blessing, 1995)'
_exptl_crystal_colour 'dark brown'
_exptl_crystal_density_diffrn 1.445
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 432
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_diff_density_max 0.610
_refine_diff_density_min -0.706
_refine_diff_density_rms 0.079
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.895
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 202
_refine_ls_number_reflns 5949
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.895
_refine_ls_R_factor_all 0.0789
_refine_ls_R_factor_gt 0.0436
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0940
_refine_ls_wR_factor_ref 0.1060
_reflns_number_gt 3404
_reflns_number_total 5949
_reflns_threshold_expression >2sigma(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
;
_cod_database_code 1100133
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 0.2586(3) 0.1681(2) -0.00008(18) 0.0459(5) Uani 1 1 d . . .
H1A H 0.1702 0.1720 -0.0540 0.069 Uiso 1 1 calc R . .
H1B H 0.2054 0.1406 0.0502 0.069 Uiso 1 1 calc R . .
H1C H 0.3445 0.1178 -0.0303 0.069 Uiso 1 1 calc R . .
C1 C 0.3502(4) 0.2894(2) 0.0557(2) 0.0428(6) Uani 1 1 d . . .
C2 C 0.2417(4) 0.3883(3) 0.0708(2) 0.0552(7) Uani 1 1 d . . .
H2 H 0.1137 0.3777 0.0444 0.060(9) Uiso 1 1 d R . .
C6 C 0.5389(4) 0.3029(3) 0.0915(3) 0.0556(7) Uani 1 1 d . . .
H6 H 0.6111 0.2356 0.0799 0.064(9) Uiso 1 1 d R . .
C5 C 0.6200(5) 0.4179(3) 0.1463(3) 0.0677(9) Uani 1 1 d . . .
H5 H 0.7481 0.4278 0.1720 0.118(15) Uiso 1 1 d R . .
C4 C 0.5140(5) 0.5191(3) 0.1648(3) 0.0636(8) Uani 1 1 d . . .
C3 C 0.3250(5) 0.5026(3) 0.1253(3) 0.0636(8) Uani 1 1 d . . .
H3 H 0.2523 0.5697 0.1363 0.089(12) Uiso 1 1 d R . .
C7 C 0.6004(6) 0.6437(4) 0.2280(4) 0.0961(13) Uani 1 1 d . . .
H71 H 0.7325 0.6478 0.2185 0.144 Uiso 1 1 calc R . .
H72 H 0.5857 0.6605 0.3066 0.144 Uiso 1 1 calc R . .
H73 H 0.5384 0.7028 0.1993 0.144 Uiso 1 1 calc R . .
N2 N 0.7517(3) 0.0977(2) 0.39762(19) 0.0487(5) Uani 1 1 d . . .
H2A H 0.6543 0.0777 0.3440 0.073 Uiso 1 1 calc R . .
H2B H 0.7363 0.0581 0.4479 0.073 Uiso 1 1 calc R . .
H2C H 0.8582 0.0775 0.3669 0.073 Uiso 1 1 calc R . .
C8 C 0.7620(3) 0.2290(2) 0.4537(2) 0.0405(6) Uani 1 1 d . . .
C9 C 0.6871(4) 0.3051(3) 0.3968(2) 0.0495(6) Uani 1 1 d . . .
H9 H 0.6284 0.2741 0.3236 0.058(8) Uiso 1 1 d R . .
C13 C 0.8521(4) 0.2735(3) 0.5599(2) 0.0583(8) Uani 1 1 d . . .
H13 H 0.9041 0.2212 0.5969 0.077(11) Uiso 1 1 d R . .
C12 C 0.8648(5) 0.3964(3) 0.6120(3) 0.0615(8) Uani 1 1 d . . .
H12 H 0.9240 0.4267 0.6853 0.092(12) Uiso 1 1 d R . .
C11 C 0.7899(4) 0.4767(3) 0.5589(3) 0.0521(7) Uani 1 1 d . . .
C10 C 0.7014(4) 0.4284(3) 0.4509(3) 0.0557(7) Uani 1 1 d . . .
H10 H 0.6488 0.4804 0.4136 0.070(10) Uiso 1 1 d R . .
C14 C 0.8055(5) 0.6109(3) 0.6170(3) 0.0770(11) Uani 1 1 d . . .
H14A H 0.9340 0.6363 0.6483 0.116 Uiso 1 1 calc R . .
H14B H 0.7247 0.6292 0.6764 0.116 Uiso 1 1 calc R . .
H14C H 0.7676 0.6532 0.5637 0.116 Uiso 1 1 calc R . .
Zn Zn 0.80950(4) 0.01269(3) 0.76682(3) 0.04276(10) Uani 1 1 d . . .
Cl1 Cl 0.93243(12) 0.20514(7) 0.82409(8) 0.0714(2) Uani 1 1 d . . .
Cl2 Cl 0.75839(12) -0.05935(7) 0.57535(6) 0.0618(2) Uani 1 1 d . . .
Cl3 Cl 0.53242(9) -0.00867(7) 0.83740(6) 0.05383(19) Uani 1 1 d . . .
Cl4 Cl 1.02362(9) -0.10044(6) 0.83165(6) 0.04822(17) 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
N1 0.0474(12) 0.0489(13) 0.0413(12) 0.0133(10) 0.0052(10) 0.0043(10)
C1 0.0485(14) 0.0463(15) 0.0339(13) 0.0123(11) 0.0057(11) 0.0020(12)
C2 0.0552(17) 0.0526(18) 0.0547(17) 0.0119(14) 0.0011(14) 0.0090(14)
C6 0.0489(15) 0.0565(19) 0.0615(19) 0.0192(15) -0.0005(14) 0.0067(14)
C5 0.0562(19) 0.074(2) 0.070(2) 0.0218(19) -0.0006(16) -0.0131(17)
C4 0.080(2) 0.056(2) 0.0545(18) 0.0183(16) 0.0058(17) -0.0147(17)
C3 0.084(2) 0.0470(18) 0.0588(19) 0.0132(15) 0.0074(17) 0.0085(17)
C7 0.114(3) 0.072(3) 0.093(3) 0.019(2) -0.001(3) -0.033(2)
N2 0.0574(13) 0.0474(14) 0.0435(12) 0.0161(11) 0.0092(11) 0.0007(10)
C8 0.0389(12) 0.0445(15) 0.0380(13) 0.0117(11) 0.0071(10) 0.0007(11)
C9 0.0516(15) 0.0500(17) 0.0441(15) 0.0119(13) -0.0035(12) 0.0054(12)
C13 0.070(2) 0.063(2) 0.0407(15) 0.0169(15) -0.0030(14) 0.0032(16)
C12 0.067(2) 0.063(2) 0.0435(17) 0.0032(15) -0.0001(15) -0.0039(16)
C11 0.0415(14) 0.0495(17) 0.0591(18) 0.0042(14) 0.0163(13) -0.0025(12)
C10 0.0561(17) 0.0526(18) 0.0622(19) 0.0220(16) 0.0066(15) 0.0107(14)
C14 0.064(2) 0.053(2) 0.099(3) -0.0040(19) 0.0242(19) -0.0045(16)
Zn 0.03820(16) 0.04319(18) 0.04655(19) 0.01376(14) 0.00325(13) -0.00089(12)
Cl1 0.0840(5) 0.0473(4) 0.0793(6) 0.0286(4) -0.0325(4) -0.0166(4)
Cl2 0.0895(5) 0.0534(4) 0.0424(4) 0.0159(3) 0.0037(4) 0.0012(4)
Cl3 0.0378(3) 0.0685(5) 0.0545(4) 0.0153(4) 0.0110(3) 0.0052(3)
Cl4 0.0401(3) 0.0520(4) 0.0552(4) 0.0191(3) 0.0067(3) 0.0085(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2840 1.4300 '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 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 C1 C2 121.4(3) . . ?
C6 C1 N1 120.1(3) . . ?
C2 C1 N1 118.5(3) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.3 . . ?
C1 C6 C5 118.7(3) . . ?
C1 C6 H6 120.6 . . ?
C5 C6 H6 120.7 . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 C7 120.2(3) . . ?
C5 C4 C7 121.4(4) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C4 C7 H71 109.5 . . ?
C4 C7 H72 109.5 . . ?
H71 C7 H72 109.5 . . ?
C4 C7 H73 109.5 . . ?
H71 C7 H73 109.5 . . ?
H72 C7 H73 109.5 . . ?
C8 N2 H2A 109.5 . . ?
C8 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C8 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C13 C8 C9 121.3(3) . . ?
C13 C8 N2 119.1(2) . . ?
C9 C8 N2 119.6(2) . . ?
C8 C9 C10 118.4(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.9 . . ?
C8 C13 C12 119.3(3) . . ?
C8 C13 H13 120.4 . . ?
C12 C13 H13 120.3 . . ?
C13 C12 C11 121.6(3) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.0 . . ?
C10 C11 C12 117.4(3) . . ?
C10 C11 C14 121.6(3) . . ?
C12 C11 C14 121.0(3) . . ?
C9 C10 C11 121.9(3) . . ?
C9 C10 H10 119.0 . . ?
C11 C10 H10 119.1 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Cl1 Zn Cl3 112.49(7) . . ?
Cl1 Zn Cl2 111.36(6) . . ?
Cl3 Zn Cl2 108.28(8) . . ?
Cl1 Zn Cl4 106.91(7) . . ?
Cl3 Zn Cl4 108.31(7) . . ?
Cl2 Zn Cl4 109.41(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
N1 C1 1.464(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C6 1.363(4) . ?
C1 C2 1.377(4) . ?
C2 C3 1.376(4) . ?
C2 H2 0.9300 . ?
C6 C5 1.377(4) . ?
C6 H6 0.9289 . ?
C5 C4 1.386(5) . ?
C5 H5 0.9292 . ?
C4 C3 1.375(5) . ?
C4 C7 1.498(5) . ?
C3 H3 0.9292 . ?
C7 H71 0.9600 . ?
C7 H72 0.9600 . ?
C7 H73 0.9600 . ?
N2 C8 1.465(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C8 C13 1.360(4) . ?
C8 C9 1.375(4) . ?
C9 C10 1.378(4) . ?
C9 H9 0.9293 . ?
C13 C12 1.370(4) . ?
C13 H13 0.9279 . ?
C12 C11 1.383(5) . ?
C12 H12 0.9298 . ?
C11 C10 1.378(4) . ?
C11 C14 1.498(4) . ?
C10 H10 0.9297 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
Zn Cl1 2.2386(18) . ?
Zn Cl3 2.270(2) . ?
Zn Cl2 2.2769(17) . ?
Zn Cl4 2.2828(18) . ?
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
N1 H1A Cl1 0.89 2.29 3.171(4) 172.4 1_454
N1 H1B Cl4 0.89 2.42 3.275(3) 161.3 2_656
N1 H1C Cl3 0.89 2.40 3.266(4) 162.9 1_554
N2 H2A Cl3 0.89 2.41 3.273(4) 162.4 2_656
N2 H2B Cl2 0.89 2.37 3.250(3) 168.4 .
N2 H2C Cl2 0.89 2.79 3.528(5) 141.5 2_756
N2 H2C Cl4 0.89 2.77 3.417(3) 130.3 2_756
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
C6 C1 C2 C3 -1.4(4) . . . . ?
N1 C1 C2 C3 178.6(3) . . . . ?
C2 C1 C6 C5 1.6(4) . . . . ?
N1 C1 C6 C5 -178.3(3) . . . . ?
C1 C6 C5 C4 -0.3(5) . . . . ?
C6 C5 C4 C3 -1.1(5) . . . . ?
C6 C5 C4 C7 177.8(3) . . . . ?
C5 C4 C3 C2 1.4(5) . . . . ?
C7 C4 C3 C2 -177.6(3) . . . . ?
C1 C2 C3 C4 -0.1(5) . . . . ?
C13 C8 C9 C10 -1.5(4) . . . . ?
N2 C8 C9 C10 -179.0(2) . . . . ?
C9 C8 C13 C12 1.5(4) . . . . ?
N2 C8 C13 C12 179.0(3) . . . . ?
C8 C13 C12 C11 -0.7(5) . . . . ?
C13 C12 C11 C10 0.0(4) . . . . ?
C13 C12 C11 C14 -179.8(3) . . . . ?
C8 C9 C10 C11 0.8(4) . . . . ?
C12 C11 C10 C9 0.0(4) . . . . ?
C14 C11 C10 C9 179.8(3) . . . . ?
|
1100134.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100134.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_1100134
loop_
_publ_author_name
'Carballo, Rosa'
'V\'azquez-L\'opez, Ezequiel M.'
'Covelo, Berta'
'Casti\~neiras, Alfonso'
_publ_section_title
;
Coordination polymers of Copper(II) based on mixed N- and O-donor
ligands: The crystal structures of [CuL~2~(4,4'-bipy)]~n~
(L = lactate or 2-methyllactate)'
;
_journal_issue 9-10
_journal_name_full Polyhedron
_journal_page_first 899
_journal_page_last 904
_journal_paper_doi 10.1016/S0277-5387(01)00749-5
_journal_volume 20
_journal_year 2001
_chemical_formula_moiety ?
_chemical_formula_sum 'C18 H22 Cu N2 O6'
_chemical_formula_weight 425.92
_chemical_melting_point ?
_chemical_name_systematic
;
catena-(\mu-4,4'-Bipyridyl)-bis(2-methyllactate-O,O')-copper(II)
;
_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_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 115.974(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 16.5140(16)
_cell_length_b 11.1559(11)
_cell_length_c 11.2834(11)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1868.8(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_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 0.0490
_diffrn_reflns_av_sigmaI/netI 0.0681
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 5749
_diffrn_reflns_theta_max 28.00
_diffrn_reflns_theta_min 2.28
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.206
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min .8117
_exptl_absorpt_process_details ?
_exptl_crystal_colour Blue
_exptl_crystal_density_diffrn 1.514
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 884
_exptl_crystal_size_max .21
_exptl_crystal_size_mid .15
_exptl_crystal_size_min .05
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.967
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 128
_refine_ls_number_reflns 2196
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.967
_refine_ls_R_factor_all 0.0757
_refine_ls_R_factor_gt 0.0497
_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^)+(0.0618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1114
_refine_ls_wR_factor_ref 0.1203
_reflns_number_gt 1567
_reflns_number_total 2196
_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 C2/c
_cod_database_code 1100134
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
Cu Cu 0.5000 0.54970(5) 0.7500 0.02353(19) Uani 1 2 d S . .
N1 N 0.5000 0.3666(3) 0.7500 0.0242(8) Uani 1 2 d S . .
N2 N 0.5000 0.7332(3) 0.7500 0.0269(9) Uani 1 2 d S . .
O11 O 0.58241(17) 0.5520(2) 0.9380(2) 0.0359(6) Uani 1 1 d . . .
O12 O 0.64009(17) 0.53682(19) 0.7535(2) 0.0347(6) Uani 1 1 d . . .
O13 O 0.7182(2) 0.5292(3) 1.1024(3) 0.0621(9) Uani 1 1 d . . .
C1 C 0.6654(3) 0.5374(3) 0.9791(4) 0.0356(8) Uani 1 1 d . . .
C2 C 0.7094(2) 0.5210(3) 0.8855(3) 0.0292(8) Uani 1 1 d . . .
C3 C 0.4455(2) 0.7963(3) 0.7861(4) 0.0357(9) Uani 1 1 d . . .
H3 H 0.4068 0.7546 0.8112 0.043 Uiso 1 1 calc R . .
C4 C 0.4438(2) 0.9187(3) 0.7881(4) 0.0343(9) Uani 1 1 d . . .
H4 H 0.4051 0.9581 0.8150 0.041 Uiso 1 1 calc R . .
C5 C 0.5000 0.9842(4) 0.7500 0.0264(10) Uani 1 2 d S . .
C11 C 0.4891(2) 0.3055(3) 0.8439(3) 0.0313(8) Uani 1 1 d . . .
H11 H 0.4816 0.3477 0.9095 0.038 Uiso 1 1 calc R . .
C12 C 0.4885(2) 0.1815(3) 0.8468(3) 0.0311(8) Uani 1 1 d . . .
H12 H 0.4804 0.1418 0.9133 0.037 Uiso 1 1 calc R . .
C13 C 0.5000 0.1161(4) 0.7500 0.0272(10) Uani 1 2 d S . .
C21 C 0.7483(3) 0.3956(4) 0.9054(4) 0.0502(11) Uani 1 1 d . . .
H21A H 0.7017 0.3383 0.8917 0.075 Uiso 1 1 calc R . .
H21B H 0.7952 0.3880 0.9936 0.075 Uiso 1 1 calc R . .
H21C H 0.7727 0.3812 0.8436 0.075 Uiso 1 1 calc R . .
C22 C 0.7816(3) 0.6165(4) 0.9144(4) 0.0436(10) Uani 1 1 d . . .
H22A H 0.8019 0.6154 0.8467 0.065 Uiso 1 1 calc R . .
H22B H 0.8315 0.6004 0.9982 0.065 Uiso 1 1 calc R . .
H22C H 0.7569 0.6940 0.9167 0.065 Uiso 1 1 calc R . .
H12 H 0.6713 0.5085 0.7100 0.022(8) Uiso 1 1 d 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
Cu 0.0286(3) 0.0163(3) 0.0273(3) 0.000 0.0137(3) 0.000
N1 0.029(2) 0.0197(19) 0.027(2) 0.000 0.0146(18) 0.000
N2 0.029(2) 0.023(2) 0.030(2) 0.000 0.0147(19) 0.000
O11 0.0416(15) 0.0380(14) 0.0342(13) -0.0035(11) 0.0221(12) -0.0012(12)
O12 0.0416(15) 0.0364(14) 0.0317(13) 0.0006(10) 0.0212(12) 0.0013(11)
O13 0.0437(18) 0.110(3) 0.0303(16) 0.0016(15) 0.0145(14) -0.0091(17)
C1 0.038(2) 0.034(2) 0.046(2) -0.0049(16) 0.0283(19) -0.0075(16)
C2 0.0276(19) 0.037(2) 0.0241(17) 0.0017(13) 0.0124(15) -0.0004(14)
C3 0.042(2) 0.0233(18) 0.051(2) -0.0001(15) 0.029(2) -0.0051(15)
C4 0.039(2) 0.0231(17) 0.052(2) -0.0053(15) 0.030(2) -0.0003(14)
C5 0.030(3) 0.017(2) 0.032(3) 0.000 0.014(2) 0.000
C11 0.041(2) 0.0250(17) 0.033(2) -0.0004(14) 0.0212(18) 0.0017(15)
C12 0.043(2) 0.0238(17) 0.0320(19) 0.0011(13) 0.0213(18) -0.0031(15)
C13 0.026(3) 0.024(2) 0.035(3) 0.000 0.016(2) 0.000
C21 0.043(3) 0.048(2) 0.060(3) 0.014(2) 0.022(2) 0.017(2)
C22 0.038(2) 0.057(3) 0.040(2) -0.0052(18) 0.0209(19) -0.0130(18)
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
|
1100135.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100135.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_1100135
loop_
_publ_author_name
'Carballo, Rosa'
'V\'azquez-L\'opez, Ezequiel M.'
'Covelo, Berta'
'Casti\~neiras, Alfonso'
_publ_section_title
;
Coordination polymers of Copper(II) based on mixed N- and O-donor
ligands: The crystal structures of [CuL~2~(4,4'-bipy)]~n~
(L = lactate or 2-methyllactate)'
;
_journal_issue 9-10
_journal_name_full Polyhedron
_journal_page_first 899
_journal_page_last 904
_journal_paper_doi 10.1016/S0277-5387(01)00749-5
_journal_volume 20
_journal_year 2001
_chemical_formula_moiety ?
_chemical_formula_sum 'C16 H18 Cu N2 O6'
_chemical_formula_weight 397.86
_chemical_melting_point ?
_chemical_name_systematic
;
catena-(\mu-4,4'-Bipyridyl)-bis(lactate-O,O')-copper(II)
;
_space_group_IT_number 12
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2y'
_symmetry_space_group_name_H-M 'C 1 2/m 1'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 104.854(2)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 14.443(2)
_cell_length_b 11.2031(16)
_cell_length_c 5.3902(8)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 843.0(2)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_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 0.0326
_diffrn_reflns_av_sigmaI/netI 0.0312
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 7
_diffrn_reflns_limit_l_min -4
_diffrn_reflns_number 2791
_diffrn_reflns_theta_max 28.00
_diffrn_reflns_theta_min 2.33
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.331
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min .8033
_exptl_absorpt_process_details ?
_exptl_crystal_colour Blue
_exptl_crystal_density_diffrn 1.567
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Prism
_exptl_crystal_F_000 410
_exptl_crystal_size_max .26
_exptl_crystal_size_mid .22
_exptl_crystal_size_min .04
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.118
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 78
_refine_ls_number_reflns 1055
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.118
_refine_ls_R_factor_all 0.0366
_refine_ls_R_factor_gt 0.0345
_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^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0877
_refine_ls_wR_factor_ref 0.0885
_reflns_number_gt 992
_reflns_number_total 1055
_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 C2/m
_cod_database_code 1100135
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'
'x, -y, z'
'-x+1/2, -y+1/2, -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
Cu Cu 0.0000 0.0000 0.5000 0.02584(18) Uani 1 4 d S . .
O11 O 0.12267(13) 0.0000 0.7559(3) 0.0288(4) Uani 1 2 d S . .
O12 O 0.11563(17) 0.0000 0.2586(4) 0.0506(7) Uani 1 2 d S . .
O13 O 0.28123(17) 0.0000 0.8646(5) 0.0650(9) Uani 1 2 d S . .
N1 N 0.0000 0.1829(2) 0.5000 0.0283(5) Uani 1 2 d S . .
C1 C 0.04136(17) 0.2459(2) 0.7108(4) 0.0388(5) Uani 1 1 d . . .
H1 H 0.0704 0.2044 0.8599 0.047 Uiso 1 1 calc R . .
C2 C 0.04318(17) 0.36838(19) 0.7181(4) 0.0388(5) Uani 1 1 d . . .
H2 H 0.0734 0.4075 0.8694 0.047 Uiso 1 1 calc R . .
C3 C 0.0000 0.4345(2) 0.5000 0.0277(6) Uani 1 2 d S . .
C11 C 0.2043(2) 0.0000 0.7035(6) 0.0406(7) Uani 1 2 d S . .
C12 C 0.2072(3) 0.0333(5) 0.4261(8) 0.0437(14) Uani 0.50 1 d P . .
H12A H 0.2559 -0.0171 0.3813 0.052 Uiso 0.50 1 calc PR . .
C13 C 0.2346(4) 0.1633(6) 0.3934(12) 0.0651(17) Uani 0.50 1 d P . .
H13A H 0.1900 0.2154 0.4445 0.098 Uiso 0.50 1 calc PR . .
H13B H 0.2329 0.1778 0.2168 0.098 Uiso 0.50 1 calc PR . .
H13C H 0.2980 0.1782 0.4985 0.098 Uiso 0.50 1 calc PR . .
H12 H 0.122(2) 0.0000 0.121(7) 0.033(9) Uiso 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
Cu 0.0327(3) 0.0204(2) 0.0212(3) 0.000 0.00113(17) 0.000
O11 0.0326(10) 0.0307(10) 0.0203(9) 0.000 0.0017(7) 0.000
O12 0.0399(13) 0.090(2) 0.0215(11) 0.000 0.0068(9) 0.000
O13 0.0347(13) 0.111(3) 0.0407(14) 0.000 -0.0051(10) 0.000
N1 0.0347(12) 0.0226(11) 0.0252(11) 0.000 0.0031(9) 0.000
C1 0.0540(13) 0.0273(10) 0.0280(10) 0.0011(8) -0.0027(9) 0.0031(9)
C2 0.0573(14) 0.0263(10) 0.0253(10) -0.0027(8) -0.0029(9) 0.0015(9)
C3 0.0309(13) 0.0252(14) 0.0260(13) 0.000 0.0057(10) 0.000
C11 0.0397(17) 0.054(2) 0.0246(14) 0.000 0.0015(12) 0.000
C12 0.034(2) 0.066(4) 0.0308(19) -0.0024(18) 0.0072(15) 0.0008(18)
C13 0.052(3) 0.087(5) 0.058(3) 0.008(3) 0.016(3) -0.021(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'
Cu Cu 0.3201 1.2651 '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'
|
1100136.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-16 01:16:12 +0300 (Mon, 16 Oct 2017) $
#$Revision: 202026 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100136.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_1100136
loop_
_publ_author_name
'Spreadborough, J'
'Christian, J W'
_publ_section_title 'High-temperature X-ray diffractometer'
_journal_name_full 'Journal of Scientific Instruments'
_journal_page_first 116
_journal_page_last 118
_journal_paper_doi 10.1088/0950-7671/36/3/302
_journal_volume 36
_journal_year 1959
_chemical_formula_structural Ag
_chemical_formula_sum Ag
_chemical_name_mineral Silver
_chemical_name_systematic 'Silver - 3C'
_space_group_IT_number 225
_symmetry_cell_setting cubic
_symmetry_Int_Tables_number 225
_symmetry_space_group_name_Hall '-F 4 2 3'
_symmetry_space_group_name_H-M 'F m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.0855(1)
_cell_length_b 4.0855(1)
_cell_length_c 4.0855(1)
_cell_volume 68.2
_cod_database_code 1100136
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
y,z,x
z,x,y
x,z,y
y,x,z
z,y,x
x,-y,-z
y,-z,-x
z,-x,-y
x,-z,-y
y,-x,-z
z,-y,-x
-x,y,-z
-y,z,-x
-z,x,-y
-x,z,-y
-y,x,-z
-z,y,-x
-x,-y,z
-y,-z,x
-z,-x,y
-x,-z,y
-y,-x,z
-z,-y,x
-x,-y,-z
-y,-z,-x
-z,-x,-y
-x,-z,-y
-y,-x,-z
-z,-y,-x
-x,y,z
-y,z,x
-z,x,y
-x,z,y
-y,x,z
-z,y,x
x,-y,z
y,-z,x
z,-x,y
x,-z,y
y,-x,z
z,-y,x
x,y,-z
y,z,-x
z,x,-y
x,z,-y
y,x,-z
z,y,-x
x,1/2+y,1/2+z
1/2+x,y,1/2+z
1/2+x,1/2+y,z
y,1/2+z,1/2+x
1/2+y,z,1/2+x
1/2+y,1/2+z,x
z,1/2+x,1/2+y
1/2+z,x,1/2+y
1/2+z,1/2+x,y
x,1/2+z,1/2+y
1/2+x,z,1/2+y
1/2+x,1/2+z,y
y,1/2+x,1/2+z
1/2+y,x,1/2+z
1/2+y,1/2+x,z
z,1/2+y,1/2+x
1/2+z,y,1/2+x
1/2+z,1/2+y,x
x,1/2-y,1/2-z
1/2+x,-y,1/2-z
1/2+x,1/2-y,-z
y,1/2-z,1/2-x
1/2+y,-z,1/2-x
1/2+y,1/2-z,-x
z,1/2-x,1/2-y
1/2+z,-x,1/2-y
1/2+z,1/2-x,-y
x,1/2-z,1/2-y
1/2+x,-z,1/2-y
1/2+x,1/2-z,-y
y,1/2-x,1/2-z
1/2+y,-x,1/2-z
1/2+y,1/2-x,-z
z,1/2-y,1/2-x
1/2+z,-y,1/2-x
1/2+z,1/2-y,-x
-x,1/2+y,1/2-z
1/2-x,y,1/2-z
1/2-x,1/2+y,-z
-y,1/2+z,1/2-x
1/2-y,z,1/2-x
1/2-y,1/2+z,-x
-z,1/2+x,1/2-y
1/2-z,x,1/2-y
1/2-z,1/2+x,-y
-x,1/2+z,1/2-y
1/2-x,z,1/2-y
1/2-x,1/2+z,-y
-y,1/2+x,1/2-z
1/2-y,x,1/2-z
1/2-y,1/2+x,-z
-z,1/2+y,1/2-x
1/2-z,y,1/2-x
1/2-z,1/2+y,-x
-x,1/2-y,1/2+z
1/2-x,-y,1/2+z
1/2-x,1/2-y,z
-y,1/2-z,1/2+x
1/2-y,-z,1/2+x
1/2-y,1/2-z,x
-z,1/2-x,1/2+y
1/2-z,-x,1/2+y
1/2-z,1/2-x,y
-x,1/2-z,1/2+y
1/2-x,-z,1/2+y
1/2-x,1/2-z,y
-y,1/2-x,1/2+z
1/2-y,-x,1/2+z
1/2-y,1/2-x,z
-z,1/2-y,1/2+x
1/2-z,-y,1/2+x
1/2-z,1/2-y,x
-x,1/2-y,1/2-z
1/2-x,-y,1/2-z
1/2-x,1/2-y,-z
-y,1/2-z,1/2-x
1/2-y,-z,1/2-x
1/2-y,1/2-z,-x
-z,1/2-x,1/2-y
1/2-z,-x,1/2-y
1/2-z,1/2-x,-y
-x,1/2-z,1/2-y
1/2-x,-z,1/2-y
1/2-x,1/2-z,-y
-y,1/2-x,1/2-z
1/2-y,-x,1/2-z
1/2-y,1/2-x,-z
-z,1/2-y,1/2-x
1/2-z,-y,1/2-x
1/2-z,1/2-y,-x
-x,1/2+y,1/2+z
1/2-x,y,1/2+z
1/2-x,1/2+y,z
-y,1/2+z,1/2+x
1/2-y,z,1/2+x
1/2-y,1/2+z,x
-z,1/2+x,1/2+y
1/2-z,x,1/2+y
1/2-z,1/2+x,y
-x,1/2+z,1/2+y
1/2-x,z,1/2+y
1/2-x,1/2+z,y
-y,1/2+x,1/2+z
1/2-y,x,1/2+z
1/2-y,1/2+x,z
-z,1/2+y,1/2+x
1/2-z,y,1/2+x
1/2-z,1/2+y,x
x,1/2-y,1/2+z
1/2+x,-y,1/2+z
1/2+x,1/2-y,z
y,1/2-z,1/2+x
1/2+y,-z,1/2+x
1/2+y,1/2-z,x
z,1/2-x,1/2+y
1/2+z,-x,1/2+y
1/2+z,1/2-x,y
x,1/2-z,1/2+y
1/2+x,-z,1/2+y
1/2+x,1/2-z,y
y,1/2-x,1/2+z
1/2+y,-x,1/2+z
1/2+y,1/2-x,z
z,1/2-y,1/2+x
1/2+z,-y,1/2+x
1/2+z,1/2-y,x
x,1/2+y,1/2-z
1/2+x,y,1/2-z
1/2+x,1/2+y,-z
y,1/2+z,1/2-x
1/2+y,z,1/2-x
1/2+y,1/2+z,-x
z,1/2+x,1/2-y
1/2+z,x,1/2-y
1/2+z,1/2+x,-y
x,1/2+z,1/2-y
1/2+x,z,1/2-y
1/2+x,1/2+z,-y
y,1/2+x,1/2-z
1/2+y,x,1/2-z
1/2+y,1/2+x,-z
z,1/2+y,1/2-x
1/2+z,y,1/2-x
1/2+z,1/2+y,-x
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Ag1 Ag0 4 a 0. 0. 0. 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Ag0 0.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 22394
2 AMCSD 0018275
|
1100137.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100137.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_1100137
loop_
_publ_author_name
'Sawsan Salameh'
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 824
_journal_page_last 827
_journal_paper_doi 10.1016/j.ica.2004.09.025
_journal_volume 358
_journal_year 2005
_chemical_formula_sum 'C10 H12 Ag2 N10 O10'
_chemical_formula_weight 648.04
_chemical_name_systematic
;
Di(nitrate)bis(mu-7,8-dihydro-7-oxo-1,2,4-triazolo[4,3-a]pyrimidine-N1,N2)
disilver(I) dihydrate
;
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 94.7820(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 10.5297(6)
_cell_length_b 12.6897(8)
_cell_length_c 6.9432(4)
_cell_measurement_reflns_used 3774
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 28.01
_cell_measurement_theta_min 2.52
_cell_volume 924.51(9)
_diffrn_ambient_temperature 298(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0155
_diffrn_reflns_av_sigmaI/netI 0.0183
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_limit_l_min -5
_diffrn_reflns_number 5595
_diffrn_reflns_theta_full 28.14
_diffrn_reflns_theta_max 28.14
_diffrn_reflns_theta_min 1.94
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.199
_exptl_absorpt_correction_T_max 0.6930
_exptl_absorpt_correction_T_min 0.4965
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.328
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'trapezoidal prism'
_exptl_crystal_F_000 632
_exptl_crystal_size_max 0.49
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.18
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.599
_refine_diff_density_min -0.405
_refine_diff_density_rms 0.073
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.067
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 151
_refine_ls_number_reflns 2080
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.066
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0232
_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^)+(0.0300P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0582
_refine_ls_wR_factor_ref 0.0592
_reflns_number_gt 1912
_reflns_number_total 2080
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100137
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
Ag Ag -0.034602(16) 0.366253(14) 0.47882(3) 0.04028(9) Uani 1 1 d . . .
N1 N 0.15620(17) 0.41571(14) 0.3890(3) 0.0311(4) Uani 1 1 d . . .
N2 N 0.18306(18) 0.52354(15) 0.4143(3) 0.0345(4) Uani 1 1 d . . .
C3 C 0.2960(2) 0.54148(17) 0.3607(3) 0.0323(5) Uani 1 1 d . . .
H3 H 0.3362 0.6068 0.3644 0.039 Uiso 1 1 calc R . .
N4 N 0.34725(17) 0.44956(13) 0.2983(3) 0.0278(4) Uani 1 1 d . . .
C5 C 0.4636(2) 0.42561(18) 0.2279(3) 0.0326(5) Uani 1 1 d . . .
H5 H 0.5234 0.4780 0.2104 0.039 Uiso 1 1 calc R . .
C6 C 0.4873(2) 0.32501(19) 0.1866(4) 0.0351(5) Uani 1 1 d . . .
H6 H 0.5644 0.3079 0.1381 0.042 Uiso 1 1 calc R . .
C7 C 0.3965(2) 0.24136(17) 0.2140(3) 0.0299(4) Uani 1 1 d . . .
O7 O 0.41724(18) 0.14841(12) 0.1839(3) 0.0391(4) Uani 1 1 d . . .
N8 N 0.28107(17) 0.27263(14) 0.2769(3) 0.0299(4) Uani 1 1 d . . .
H8 H 0.2228 0.2261 0.2885 0.036 Uiso 1 1 calc R . .
C8A C 0.2569(2) 0.37471(15) 0.3210(3) 0.0263(4) Uani 1 1 d . . .
N1N N -0.18750(19) 0.16666(16) 0.5373(3) 0.0340(4) Uani 1 1 d . . .
O1N O -0.07156(17) 0.18332(16) 0.5922(3) 0.0480(4) Uani 1 1 d . . .
O2N O -0.24949(19) 0.23627(14) 0.4477(3) 0.0484(4) Uani 1 1 d . . .
O3N O -0.2380(2) 0.08141(14) 0.5736(3) 0.0508(5) Uani 1 1 d . . .
O1W O 0.1119(2) 0.11319(15) 0.3519(3) 0.0483(5) Uani 1 1 d D . .
H11W H 0.059(3) 0.115(3) 0.438(4) 0.058 Uiso 1 1 d D . .
H12W H 0.142(3) 0.0506(13) 0.369(5) 0.058 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
Ag 0.03116(12) 0.03170(12) 0.05990(15) -0.00673(8) 0.01517(9) -0.00173(7)
N1 0.0279(9) 0.0223(9) 0.0441(11) -0.0045(8) 0.0088(8) -0.0015(7)
N2 0.0322(9) 0.0231(9) 0.0493(12) -0.0051(8) 0.0099(8) 0.0014(7)
C3 0.0317(11) 0.0210(10) 0.0448(13) -0.0012(9) 0.0064(9) 0.0011(8)
N4 0.0260(9) 0.0212(8) 0.0368(10) 0.0014(7) 0.0062(7) -0.0001(7)
C5 0.0262(11) 0.0298(11) 0.0432(13) 0.0015(9) 0.0107(9) -0.0021(8)
C6 0.0276(11) 0.0353(12) 0.0438(13) -0.0030(10) 0.0116(9) 0.0020(9)
C7 0.0308(11) 0.0269(10) 0.0321(11) -0.0018(8) 0.0037(9) 0.0050(8)
O7 0.0421(10) 0.0262(8) 0.0494(10) -0.0063(7) 0.0059(8) 0.0080(7)
N8 0.0287(9) 0.0209(8) 0.0408(10) -0.0032(7) 0.0070(7) -0.0016(7)
C8A 0.0263(10) 0.0221(10) 0.0310(11) 0.0003(8) 0.0047(8) -0.0006(7)
N1N 0.0350(10) 0.0288(9) 0.0395(11) -0.0023(8) 0.0112(8) 0.0003(8)
O1N 0.0328(9) 0.0547(12) 0.0571(12) -0.0004(9) 0.0074(8) -0.0028(8)
O2N 0.0527(11) 0.0334(9) 0.0587(12) 0.0067(8) 0.0027(9) 0.0060(8)
O3N 0.0523(11) 0.0296(9) 0.0721(13) 0.0072(9) 0.0143(10) -0.0054(8)
O1W 0.0492(11) 0.0317(9) 0.0674(13) 0.0017(9) 0.0251(10) -0.0025(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'
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'
Ag Ag -0.8971 1.1015 '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 Ag N2 125.20(6) . 3_566 ?
N1 Ag O1N 121.04(6) . . ?
N2 Ag O1N 109.94(7) 3_566 . ?
C8A N1 N2 105.80(17) . . ?
C8A N1 Ag 139.76(15) . . ?
N2 N1 Ag 114.42(13) . . ?
C3 N2 N1 108.38(18) . . ?
C3 N2 Ag 131.29(15) . 3_566 ?
N1 N2 Ag 120.28(14) . 3_566 ?
N2 C3 N4 109.65(19) . . ?
N2 C3 H3 125.1 . . ?
N4 C3 H3 125.2 . . ?
C8A N4 C3 105.04(17) . . ?
C8A N4 C5 122.17(18) . . ?
C3 N4 C5 132.78(19) . . ?
C6 C5 N4 118.0(2) . . ?
C6 C5 H5 121.0 . . ?
N4 C5 H5 121.0 . . ?
C5 C6 C7 122.3(2) . . ?
C5 C6 H6 119.0 . . ?
C7 C6 H6 118.7 . . ?
O7 C7 N8 120.3(2) . . ?
O7 C7 C6 123.7(2) . . ?
N8 C7 C6 115.91(19) . . ?
C8A N8 C7 122.00(18) . . ?
C8A N8 H8 119.0 . . ?
C7 N8 H8 119.0 . . ?
N1 C8A N8 129.4(2) . . ?
N1 C8A N4 111.12(18) . . ?
N8 C8A N4 119.50(19) . . ?
O2N N1N O3N 120.6(2) . . ?
O2N N1N O1N 119.2(2) . . ?
O3N N1N O1N 120.2(2) . . ?
N1N O1N Ag 103.45(15) . . ?
H11W O1W H12W 101(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
Ag N1 2.2423(18) . ?
Ag N2 2.2680(19) 3_566 ?
Ag O1N 2.492(2) . ?
N1 C8A 1.304(3) . ?
N1 N2 1.405(3) . ?
N2 C3 1.295(3) . ?
N2 Ag 2.2679(19) 3_566 ?
C3 N4 1.371(3) . ?
C3 H3 0.9300 . ?
N4 C8A 1.363(3) . ?
N4 C5 1.390(3) . ?
C5 C6 1.336(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.451(3) . ?
C6 H6 0.9300 . ?
C7 O7 1.221(3) . ?
C7 N8 1.384(3) . ?
N8 C8A 1.360(3) . ?
N8 H8 0.8600 . ?
N1N O2N 1.235(3) . ?
N1N O3N 1.240(3) . ?
N1N O1N 1.266(3) . ?
O1W H11W 0.856(10) . ?
O1W H12W 0.860(10) . ?
|
1100138.cif | #------------------------------------------------------------------------------
#$Date: 2017-10-13 02:32:00 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201954 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100138.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_1100138
loop_
_publ_author_name
'J. Spreadborough'
'J. W. Christian'
_publ_section_title 'High-temperature X-ray diffractometer'
_journal_name_full 'Journal of Scientific Instruments'
_journal_page_first 116
_journal_page_last 118
_journal_paper_doi 10.1088/0950-7671/36/3/302
_journal_volume 36
_journal_year 1959
_chemical_formula_structural Au
_chemical_formula_sum Au
_chemical_name_mineral Gold
_chemical_name_systematic 'Gold - 3C'
_space_group_IT_number 225
_symmetry_cell_setting cubic
_symmetry_Int_Tables_number 225
_symmetry_space_group_name_Hall '-F 4 2 3'
_symmetry_space_group_name_H-M 'F m -3 m'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.07(1)
_cell_length_b 4.07(1)
_cell_length_c 4.07(1)
_cell_volume 67.42
_cod_database_code 1100138
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
y,z,x
z,x,y
x,z,y
y,x,z
z,y,x
x,-y,-z
y,-z,-x
z,-x,-y
x,-z,-y
y,-x,-z
z,-y,-x
-x,y,-z
-y,z,-x
-z,x,-y
-x,z,-y
-y,x,-z
-z,y,-x
-x,-y,z
-y,-z,x
-z,-x,y
-x,-z,y
-y,-x,z
-z,-y,x
-x,-y,-z
-y,-z,-x
-z,-x,-y
-x,-z,-y
-y,-x,-z
-z,-y,-x
-x,y,z
-y,z,x
-z,x,y
-x,z,y
-y,x,z
-z,y,x
x,-y,z
y,-z,x
z,-x,y
x,-z,y
y,-x,z
z,-y,x
x,y,-z
y,z,-x
z,x,-y
x,z,-y
y,x,-z
z,y,-x
x,1/2+y,1/2+z
1/2+x,y,1/2+z
1/2+x,1/2+y,z
y,1/2+z,1/2+x
1/2+y,z,1/2+x
1/2+y,1/2+z,x
z,1/2+x,1/2+y
1/2+z,x,1/2+y
1/2+z,1/2+x,y
x,1/2+z,1/2+y
1/2+x,z,1/2+y
1/2+x,1/2+z,y
y,1/2+x,1/2+z
1/2+y,x,1/2+z
1/2+y,1/2+x,z
z,1/2+y,1/2+x
1/2+z,y,1/2+x
1/2+z,1/2+y,x
x,1/2-y,1/2-z
1/2+x,-y,1/2-z
1/2+x,1/2-y,-z
y,1/2-z,1/2-x
1/2+y,-z,1/2-x
1/2+y,1/2-z,-x
z,1/2-x,1/2-y
1/2+z,-x,1/2-y
1/2+z,1/2-x,-y
x,1/2-z,1/2-y
1/2+x,-z,1/2-y
1/2+x,1/2-z,-y
y,1/2-x,1/2-z
1/2+y,-x,1/2-z
1/2+y,1/2-x,-z
z,1/2-y,1/2-x
1/2+z,-y,1/2-x
1/2+z,1/2-y,-x
-x,1/2+y,1/2-z
1/2-x,y,1/2-z
1/2-x,1/2+y,-z
-y,1/2+z,1/2-x
1/2-y,z,1/2-x
1/2-y,1/2+z,-x
-z,1/2+x,1/2-y
1/2-z,x,1/2-y
1/2-z,1/2+x,-y
-x,1/2+z,1/2-y
1/2-x,z,1/2-y
1/2-x,1/2+z,-y
-y,1/2+x,1/2-z
1/2-y,x,1/2-z
1/2-y,1/2+x,-z
-z,1/2+y,1/2-x
1/2-z,y,1/2-x
1/2-z,1/2+y,-x
-x,1/2-y,1/2+z
1/2-x,-y,1/2+z
1/2-x,1/2-y,z
-y,1/2-z,1/2+x
1/2-y,-z,1/2+x
1/2-y,1/2-z,x
-z,1/2-x,1/2+y
1/2-z,-x,1/2+y
1/2-z,1/2-x,y
-x,1/2-z,1/2+y
1/2-x,-z,1/2+y
1/2-x,1/2-z,y
-y,1/2-x,1/2+z
1/2-y,-x,1/2+z
1/2-y,1/2-x,z
-z,1/2-y,1/2+x
1/2-z,-y,1/2+x
1/2-z,1/2-y,x
-x,1/2-y,1/2-z
1/2-x,-y,1/2-z
1/2-x,1/2-y,-z
-y,1/2-z,1/2-x
1/2-y,-z,1/2-x
1/2-y,1/2-z,-x
-z,1/2-x,1/2-y
1/2-z,-x,1/2-y
1/2-z,1/2-x,-y
-x,1/2-z,1/2-y
1/2-x,-z,1/2-y
1/2-x,1/2-z,-y
-y,1/2-x,1/2-z
1/2-y,-x,1/2-z
1/2-y,1/2-x,-z
-z,1/2-y,1/2-x
1/2-z,-y,1/2-x
1/2-z,1/2-y,-x
-x,1/2+y,1/2+z
1/2-x,y,1/2+z
1/2-x,1/2+y,z
-y,1/2+z,1/2+x
1/2-y,z,1/2+x
1/2-y,1/2+z,x
-z,1/2+x,1/2+y
1/2-z,x,1/2+y
1/2-z,1/2+x,y
-x,1/2+z,1/2+y
1/2-x,z,1/2+y
1/2-x,1/2+z,y
-y,1/2+x,1/2+z
1/2-y,x,1/2+z
1/2-y,1/2+x,z
-z,1/2+y,1/2+x
1/2-z,y,1/2+x
1/2-z,1/2+y,x
x,1/2-y,1/2+z
1/2+x,-y,1/2+z
1/2+x,1/2-y,z
y,1/2-z,1/2+x
1/2+y,-z,1/2+x
1/2+y,1/2-z,x
z,1/2-x,1/2+y
1/2+z,-x,1/2+y
1/2+z,1/2-x,y
x,1/2-z,1/2+y
1/2+x,-z,1/2+y
1/2+x,1/2-z,y
y,1/2-x,1/2+z
1/2+y,-x,1/2+z
1/2+y,1/2-x,z
z,1/2-y,1/2+x
1/2+z,-y,1/2+x
1/2+z,1/2-y,x
x,1/2+y,1/2-z
1/2+x,y,1/2-z
1/2+x,1/2+y,-z
y,1/2+z,1/2-x
1/2+y,z,1/2-x
1/2+y,1/2+z,-x
z,1/2+x,1/2-y
1/2+z,x,1/2-y
1/2+z,1/2+x,-y
x,1/2+z,1/2-y
1/2+x,z,1/2-y
1/2+x,1/2+z,-y
y,1/2+x,1/2-z
1/2+y,x,1/2-z
1/2+y,1/2+x,-z
z,1/2+y,1/2-x
1/2+z,y,1/2-x
1/2+z,1/2+y,-x
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_attached_hydrogens
_atom_site_calc_flag
Au1 Au0 4 a 0. 0. 0. 1. 0 d
loop_
_atom_type_symbol
_atom_type_oxidation_number
Au0 0.000
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 22421
|
1100139.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100139.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_1100139
loop_
_publ_author_name
'Esther R. Acuna-Cueva'
'Sonia B. Jimenez-Pulido'
'Miguel N. Moreno-Carretero'
'Miguel Quiros'
_journal_name_full 'Structural Chemistry'
_journal_page_first 159
_journal_page_last 163
_journal_paper_doi 10.1023/B:STUC.0000011250.33484.84
_journal_volume 15
_journal_year 2004
_chemical_formula_moiety ?
_chemical_formula_sum 'C27 H37 Au Br4 N12 O9'
_chemical_formula_weight 1190.29
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_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 71.538(17)
_cell_angle_beta 71.675(7)
_cell_angle_gamma 78.681(13)
_cell_formula_units_Z 2
_cell_length_a 11.3215(10)
_cell_length_b 11.908(2)
_cell_length_c 16.4596(14)
_cell_measurement_reflns_used 29
_cell_measurement_temperature 295(1)
_cell_measurement_theta_max 14.7
_cell_measurement_theta_min 12.5
_cell_volume 1986.6(5)
_diffrn_ambient_temperature 295(1)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.82 - 1.48, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_radiation_collimation '0.8 mm'
_diffrn_radiation_detector 'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_polarisn_norm 90
_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 0.0453
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 6974
_diffrn_reflns_theta_full 24.97
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_min 1.82
_diffrn_standards_decay_% 6.3
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 7.788
_exptl_absorpt_correction_T_max 0.2691
_exptl_absorpt_correction_T_min 0.0613
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details
;
Psi Scan Reflections used Mu * R = 0.95
H K L 2Theta Chi Imin/Imax
1 1 6 15.0 79.9 0.235
2 0 6 16.0 78.2 0.264
2 1 7 17.6 80.6 0.255
1 0 7 18.4 83.6 0.324
1 1 8 20.3 80.5 0.270
3 1 8 20.8 75.0 0.271
2 0 8 21.1 84.1 0.308
1 0 8 21.1 82.5 0.335
1 -1 8 22.5 76.1 0.389
1 0 9 23.8 81.5 0.358
;
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.990
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 1148
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_min 0.050
_refine_diff_density_max 2.411
_refine_diff_density_min -2.998
_refine_diff_density_rms 0.220
_refine_ls_extinction_coef 0.0013(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 1.017
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 488
_refine_ls_number_reflns 6974
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.017
_refine_ls_R_factor_all 0.1194
_refine_ls_R_factor_gt 0.0890
_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^)+(0.1600P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2346
_refine_ls_wR_factor_ref 0.2771
_reflns_d_resolution_high 0.841
_reflns_d_resolution_low 11.207
_reflns_number_gt 4910
_reflns_number_total 6974
_reflns_threshold_expression >2sigma(I)
_cod_database_code 1100139
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
Au Au 0.25509(5) 0.26103(5) 0.24397(4) 0.0632(3) Uani 1 1 d . . .
Br1 Br 0.23408(17) 0.40227(19) 0.10580(12) 0.0867(6) Uani 1 1 d . . .
Br2 Br 0.2773(2) 0.1206(2) 0.38250(14) 0.1009(7) Uani 1 1 d . . .
Br3 Br 0.09194(19) 0.1565(2) 0.24434(16) 0.0955(6) Uani 1 1 d . . .
Br4 Br 0.4159(2) 0.3675(2) 0.24324(17) 0.1023(7) Uani 1 1 d . . .
N1A N 0.6147(10) 0.3422(9) 0.3818(7) 0.052(3) Uani 1 1 d . . .
C1A C 0.6053(15) 0.4671(13) 0.3798(9) 0.066(4) Uani 1 1 d . . .
H11A H 0.6291 0.4720 0.4295 0.079 Uiso 1 1 d R . .
H12A H 0.5207 0.5025 0.3832 0.079 Uiso 1 1 d R . .
H13A H 0.6601 0.5088 0.3254 0.079 Uiso 1 1 d R . .
C1AA C 0.6818(10) 0.2986(11) 0.3098(7) 0.043(3) Uani 1 1 d . . .
C2A C 0.5492(12) 0.2657(12) 0.4586(8) 0.051(3) Uani 1 1 d . . .
O2A O 0.4889(8) 0.3015(9) 0.5229(6) 0.061(2) Uani 1 1 d . . .
N3A N 0.5511(10) 0.1503(10) 0.4586(7) 0.055(3) Uani 1 1 d . . .
H3A H 0.5085 0.1046 0.5063 0.066 Uiso 1 1 d R . .
C4A C 0.6150(11) 0.0999(13) 0.3905(8) 0.052(3) Uani 1 1 d . . .
O4A O 0.6116(9) -0.0052(9) 0.3987(7) 0.069(3) Uani 1 1 d . . .
C4AA C 0.6854(11) 0.1812(11) 0.3115(8) 0.045(3) Uani 1 1 d . . .
N5A N 0.7490(10) 0.1408(10) 0.2422(7) 0.052(3) Uani 1 1 d . . .
C6A C 0.8099(12) 0.2186(13) 0.1686(8) 0.055(3) Uani 1 1 d . . .
C61A C 0.8813(18) 0.1729(16) 0.0904(11) 0.092(6) Uani 1 1 d . . .
H61A H 0.8669 0.0915 0.1032 0.110 Uiso 1 1 d R . .
H62A H 0.9691 0.1775 0.0785 0.110 Uiso 1 1 d R . .
H63A H 0.8532 0.2199 0.0394 0.110 Uiso 1 1 d R . .
C7A C 0.8071(12) 0.3356(12) 0.1703(8) 0.049(3) Uani 1 1 d . . .
C71A C 0.8823(15) 0.4189(14) 0.0878(9) 0.070(4) Uani 1 1 d . . .
H71A H 0.8725 0.4966 0.0966 0.084 Uiso 1 1 d R . .
H72A H 0.8532 0.4245 0.0377 0.084 Uiso 1 1 d R . .
H73A H 0.9691 0.3881 0.0768 0.084 Uiso 1 1 d R . .
N8A N 0.7444(9) 0.3769(9) 0.2372(7) 0.051(3) Uani 1 1 d . . .
N1B N 0.4133(11) -0.0350(12) 0.1712(9) 0.064(3) Uani 1 1 d . . .
C1B C 0.5073(16) -0.0407(15) 0.2168(12) 0.077(5) Uani 1 1 d . . .
H11B H 0.4987 -0.1088 0.2679 0.092 Uiso 1 1 d R . .
H12B H 0.4950 0.0303 0.2355 0.092 Uiso 1 1 d R . .
H13B H 0.5896 -0.0477 0.1772 0.092 Uiso 1 1 d R . .
C1AB C 0.4066(12) 0.0590(13) 0.0956(10) 0.059(4) Uani 1 1 d . . .
C2B C 0.3324(13) -0.1177(14) 0.2052(11) 0.061(4) Uani 1 1 d . . .
O2B O 0.3337(12) -0.2010(11) 0.2720(8) 0.082(3) Uani 1 1 d . . .
N3B N 0.2487(10) -0.1081(10) 0.1579(8) 0.061(3) Uani 1 1 d . . .
H3B H 0.1999 -0.1635 0.1778 0.073 Uiso 1 1 d R . .
C4B C 0.2322(14) -0.0204(12) 0.0817(9) 0.057(3) Uani 1 1 d . . .
O4B O 0.1517(10) -0.0215(9) 0.0466(7) 0.062(2) Uani 1 1 d . . .
C4AB C 0.3210(14) 0.0670(13) 0.0500(9) 0.059(4) Uani 1 1 d . . .
N5B N 0.3193(12) 0.1548(12) -0.0250(8) 0.073(4) Uani 1 1 d . . .
C6B C 0.4034(16) 0.2320(14) -0.0522(12) 0.078(5) Uani 1 1 d . . .
C61B C 0.395(2) 0.3315(19) -0.1356(14) 0.117(8) Uani 1 1 d . . .
H61B H 0.3263 0.3229 -0.1552 0.140 Uiso 1 1 d R . .
H62B H 0.4713 0.3272 -0.1815 0.140 Uiso 1 1 d R . .
H63B H 0.3811 0.4073 -0.1232 0.140 Uiso 1 1 d R . .
C7B C 0.4898(15) 0.2256(14) -0.0050(14) 0.079(5) Uani 1 1 d . . .
C71B C 0.5780(19) 0.3179(17) -0.0339(16) 0.110(8) Uani 1 1 d . . .
H71B H 0.6350 0.2957 0.0025 0.132 Uiso 1 1 d R . .
H72B H 0.5307 0.3927 -0.0284 0.132 Uiso 1 1 d R . .
H73B H 0.6243 0.3254 -0.0949 0.132 Uiso 1 1 d R . .
N8B N 0.4916(11) 0.1382(11) 0.0671(9) 0.069(4) Uani 1 1 d . . .
N1C N 0.0330(10) 0.5274(10) 0.3073(8) 0.056(3) Uani 1 1 d . . .
C1C C -0.0479(13) 0.5401(14) 0.2513(10) 0.062(4) Uani 1 1 d . . .
H11C H -0.0346 0.4699 0.2314 0.074 Uiso 1 1 d R . .
H12C H -0.0288 0.6080 0.2007 0.074 Uiso 1 1 d R . .
H13C H -0.1337 0.5516 0.2844 0.074 Uiso 1 1 d R . .
C1AC C 0.0276(11) 0.4325(12) 0.3840(9) 0.050(3) Uani 1 1 d . . .
C2C C 0.1120(13) 0.6134(14) 0.2835(10) 0.063(4) Uani 1 1 d . . .
O2C O 0.1145(11) 0.6981(10) 0.2202(7) 0.079(3) Uani 1 1 d . . .
N3C N 0.1863(11) 0.5974(10) 0.3408(8) 0.062(3) Uani 1 1 d . . .
H3C H 0.2352 0.6512 0.3276 0.074 Uiso 1 1 d R . .
C4C C 0.1907(13) 0.5055(13) 0.4150(9) 0.055(3) Uani 1 1 d . . .
O4C O 0.2612(11) 0.5025(10) 0.4601(8) 0.083(3) Uani 1 1 d . . .
C4AC C 0.1044(12) 0.4176(13) 0.4381(9) 0.055(3) Uani 1 1 d . . .
N5C N 0.0985(11) 0.3254(10) 0.5116(8) 0.061(3) Uani 1 1 d . . .
C6C C 0.0211(14) 0.2472(14) 0.5278(10) 0.063(4) Uani 1 1 d . . .
C61C C 0.0159(18) 0.1430(15) 0.6073(12) 0.091(6) Uani 1 1 d . . .
H61C H 0.0911 0.0898 0.5966 0.110 Uiso 1 1 d R . .
H62C H -0.0552 0.1023 0.6183 0.110 Uiso 1 1 d R . .
H63C H 0.0090 0.1694 0.6582 0.110 Uiso 1 1 d R . .
C7C C -0.0549(14) 0.2600(15) 0.4735(11) 0.067(4) Uani 1 1 d . . .
C71C C -0.1444(18) 0.1755(16) 0.4897(14) 0.095(6) Uani 1 1 d . . .
H71C H -0.2214 0.1943 0.5312 0.114 Uiso 1 1 d R . .
H72C H -0.1092 0.0963 0.5140 0.114 Uiso 1 1 d R . .
H73C H -0.1605 0.1801 0.4348 0.114 Uiso 1 1 d R . .
N8C N -0.0500(10) 0.3523(10) 0.3987(8) 0.056(3) Uani 1 1 d . . .
O1W O 0.2550(9) 0.2827(10) 0.6189(7) 0.067(3) Uani 1 1 d . . .
O2W O 0.2133(10) 0.1089(10) 0.7445(6) 0.074(3) Uani 1 1 d . . .
O3W O 0.0868(11) 0.1470(12) 0.8938(7) 0.088(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
Au 0.0590(4) 0.0578(4) 0.0690(4) -0.0202(3) -0.0142(3) 0.0016(3)
Br1 0.0810(11) 0.0882(13) 0.0759(11) -0.0082(10) -0.0234(8) 0.0046(9)
Br2 0.1075(14) 0.0859(14) 0.0829(12) -0.0010(10) -0.0237(10) 0.0093(11)
Br3 0.0858(12) 0.0904(14) 0.1177(16) -0.0397(12) -0.0156(11) -0.0273(10)
Br4 0.0911(13) 0.0932(15) 0.1365(18) -0.0210(13) -0.0536(12) -0.0213(11)
N1A 0.061(6) 0.032(5) 0.049(6) -0.004(5) -0.003(5) -0.005(4)
C1A 0.086(10) 0.050(9) 0.055(8) -0.006(7) -0.008(7) -0.021(7)
C1AA 0.040(6) 0.047(7) 0.040(6) -0.011(5) -0.006(5) -0.006(5)
C2A 0.055(7) 0.045(7) 0.045(7) -0.006(6) -0.005(5) -0.009(6)
O2A 0.064(5) 0.059(6) 0.053(5) -0.019(5) 0.002(4) -0.015(4)
N3A 0.056(6) 0.047(6) 0.054(6) -0.016(5) 0.005(5) -0.018(5)
C4A 0.050(7) 0.059(9) 0.037(6) -0.006(6) -0.001(5) -0.013(6)
O4A 0.078(6) 0.042(6) 0.072(6) -0.018(5) 0.010(5) -0.020(5)
C4AA 0.044(6) 0.043(7) 0.043(6) -0.010(5) -0.006(5) -0.006(5)
N5A 0.059(6) 0.047(6) 0.047(6) -0.012(5) -0.008(5) -0.012(5)
C6A 0.060(7) 0.054(8) 0.039(6) -0.001(6) -0.007(5) -0.009(6)
C61A 0.109(13) 0.066(11) 0.067(10) -0.016(9) 0.024(9) -0.019(10)
C7A 0.054(7) 0.046(7) 0.039(6) 0.001(6) -0.012(5) -0.009(6)
C71A 0.092(11) 0.049(9) 0.046(7) 0.006(7) -0.005(7) -0.011(7)
N8A 0.052(6) 0.040(6) 0.047(6) -0.003(5) 0.000(5) -0.009(5)
N1B 0.057(7) 0.060(8) 0.079(8) -0.014(7) -0.024(6) -0.011(6)
C1B 0.088(11) 0.056(10) 0.092(12) -0.002(9) -0.038(9) -0.028(8)
C1AB 0.049(7) 0.046(8) 0.067(9) -0.018(7) -0.001(6) 0.007(6)
C2B 0.049(7) 0.055(9) 0.076(10) -0.015(8) -0.017(7) -0.005(6)
O2B 0.109(9) 0.063(7) 0.077(7) 0.012(6) -0.048(6) -0.029(6)
N3B 0.060(7) 0.036(6) 0.084(8) 0.001(6) -0.028(6) -0.013(5)
C4B 0.066(8) 0.042(8) 0.053(8) -0.010(6) -0.008(6) -0.002(6)
O4B 0.083(7) 0.051(6) 0.065(6) -0.019(5) -0.031(5) -0.008(5)
C4AB 0.067(9) 0.046(8) 0.056(8) -0.013(7) -0.009(7) -0.002(6)
N5B 0.079(8) 0.068(9) 0.051(7) -0.002(6) -0.009(6) 0.001(7)
C6B 0.075(10) 0.051(9) 0.080(11) -0.019(8) 0.018(9) -0.004(8)
C61B 0.115(16) 0.081(15) 0.107(16) 0.000(12) 0.007(13) -0.010(12)
C7B 0.062(9) 0.043(9) 0.116(15) -0.025(10) 0.003(9) -0.007(7)
C71B 0.097(13) 0.067(12) 0.16(2) -0.028(13) 0.000(13) -0.046(11)
N8B 0.052(7) 0.047(7) 0.092(9) -0.014(7) 0.000(6) -0.009(5)
N1C 0.055(6) 0.046(7) 0.061(7) 0.000(5) -0.019(5) -0.008(5)
C1C 0.060(8) 0.061(9) 0.061(8) -0.003(7) -0.025(6) -0.009(7)
C1AC 0.044(6) 0.042(7) 0.061(8) -0.014(6) -0.012(5) -0.004(5)
C2C 0.059(8) 0.058(9) 0.066(9) -0.003(8) -0.023(7) -0.011(7)
O2C 0.099(8) 0.065(7) 0.072(7) 0.021(6) -0.045(6) -0.038(6)
N3C 0.068(7) 0.040(6) 0.078(8) 0.003(6) -0.034(6) -0.015(5)
C4C 0.059(8) 0.056(9) 0.052(7) -0.017(7) -0.014(6) -0.011(6)
O4C 0.101(8) 0.060(7) 0.092(8) 0.011(6) -0.050(7) -0.031(6)
C4AC 0.051(7) 0.055(8) 0.059(8) -0.010(7) -0.020(6) -0.004(6)
N5C 0.064(7) 0.042(7) 0.073(8) -0.008(6) -0.024(6) -0.004(5)
C6C 0.063(8) 0.053(9) 0.069(9) -0.005(7) -0.017(7) -0.014(7)
C61C 0.119(14) 0.046(9) 0.091(12) 0.035(9) -0.055(11) -0.017(9)
C7C 0.060(8) 0.064(10) 0.077(10) -0.022(8) -0.015(7) -0.012(7)
C71C 0.101(13) 0.064(11) 0.120(15) 0.013(11) -0.049(11) -0.041(10)
N8C 0.059(6) 0.043(6) 0.062(7) -0.009(6) -0.012(5) -0.013(5)
O1W 0.060(5) 0.069(7) 0.072(6) -0.026(5) -0.009(5) -0.013(5)
O2W 0.102(8) 0.059(7) 0.055(6) -0.022(5) -0.011(5) -0.002(6)
O3W 0.106(9) 0.092(9) 0.053(6) -0.017(6) -0.027(6) 0.019(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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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
Br4 Au Br1 89.53(8) . . ?
Br4 Au Br2 89.98(9) . . ?
Br1 Au Br2 179.51(8) . . ?
Br4 Au Br3 179.27(7) . . ?
Br1 Au Br3 89.99(8) . . ?
Br2 Au Br3 90.49(9) . . ?
C1AA N1A C2A 119.2(11) . . ?
C1AA N1A C1A 123.0(10) . . ?
C2A N1A C1A 117.8(11) . . ?
N8A C1AA C4AA 121.2(11) . . ?
N8A C1AA N1A 116.5(11) . . ?
C4AA C1AA N1A 122.3(10) . . ?
O2A C2A N3A 121.3(11) . . ?
O2A C2A N1A 120.7(12) . . ?
N3A C2A N1A 117.9(11) . . ?
C2A O2A O1W 131.2(9) . . ?
C2A N3A C4A 126.7(11) . . ?
O4A C4A N3A 120.9(11) . . ?
O4A C4A C4AA 124.7(12) . . ?
N3A C4A C4AA 114.3(12) . . ?
N5A C4AA C1AA 121.8(11) . . ?
N5A C4AA C4A 118.7(12) . . ?
C1AA C4AA C4A 119.6(11) . . ?
C4AA N5A C6A 117.7(12) . . ?
N5A C6A C7A 118.9(12) . . ?
N5A C6A C61A 117.6(13) . . ?
C7A C6A C61A 123.5(12) . . ?
N8A C7A C6A 124.2(11) . . ?
N8A C7A C71A 118.5(13) . . ?
C6A C7A C71A 117.4(12) . . ?
C7A N8A C1AA 116.2(11) . . ?
C2B N1B C1AB 121.6(13) . . ?
C2B N1B C1B 119.1(13) . . ?
C1AB N1B C1B 119.2(12) . . ?
N8B C1AB C4AB 121.7(14) . . ?
N8B C1AB N1B 117.1(14) . . ?
C4AB C1AB N1B 121.2(13) . . ?
O2B C2B N1B 123.9(14) . . ?
O2B C2B N3B 120.2(13) . . ?
N1B C2B N3B 115.8(14) . . ?
C2B N3B C4B 128.6(12) . . ?
O4B C4B N3B 121.9(13) . . ?
O4B C4B C4AB 125.7(13) . . ?
N3B C4B C4AB 112.4(13) . . ?
N5B C4AB C1AB 120.7(14) . . ?
N5B C4AB C4B 119.1(15) . . ?
C1AB C4AB C4B 120.3(13) . . ?
C6B N5B C4AB 116.9(16) . . ?
N5B C6B C7B 122.7(16) . . ?
N5B C6B C61B 114.7(19) . . ?
C7B C6B C61B 122.5(17) . . ?
N8B C7B C6B 119.5(15) . . ?
N8B C7B C71B 119(2) . . ?
C6B C7B C71B 121.5(19) . . ?
C7B N8B C1AB 118.5(16) . . ?
C2C N1C C1AC 121.6(12) . . ?
C2C N1C C1C 117.6(12) . . ?
C1AC N1C C1C 120.7(11) . . ?
N8C C1AC C4AC 121.8(13) . . ?
N8C C1AC N1C 116.2(12) . . ?
C4AC C1AC N1C 121.9(12) . . ?
O2C C2C N1C 122.8(14) . . ?
O2C C2C N3C 122.1(14) . . ?
N1C C2C N3C 115.1(13) . . ?
C4C N3C C2C 127.3(12) . . ?
O4C C4C N3C 120.6(13) . . ?
O4C C4C C4AC 123.8(13) . . ?
N3C C4C C4AC 115.5(12) . . ?
N5C C4AC C1AC 121.3(13) . . ?
N5C C4AC C4C 120.2(13) . . ?
C1AC C4AC C4C 118.5(13) . . ?
C6C N5C C4AC 117.4(13) . . ?
C6C N5C O1W 119.0(10) . . ?
C4AC N5C O1W 123.3(10) . . ?
N5C C6C C7C 121.9(14) . . ?
N5C C6C C61C 118.3(15) . . ?
C7C C6C C61C 119.9(14) . . ?
N8C C7C C6C 121.5(14) . . ?
N8C C7C C71C 114.7(14) . . ?
C6C C7C C71C 123.8(15) . . ?
C1AC N8C C7C 115.9(12) . . ?
O2W O1W O2A 117.5(5) . . ?
O2W O1W N5C 113.0(5) . . ?
O2A O1W N5C 110.8(5) . . ?
O1W O2W O3W 116.4(5) . . ?
O1W O2W N5A 132.3(5) . 2_656 ?
O3W O2W N5A 110.8(5) . 2_656 ?
O2W O3W O4B 114.8(5) . 1_556 ?
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
Au Br4 2.409(2) . ?
Au Br1 2.4120(19) . ?
Au Br2 2.416(2) . ?
Au Br3 2.419(2) . ?
N1A C1AA 1.385(15) . ?
N1A C2A 1.387(15) . ?
N1A C1A 1.460(17) . ?
C1AA N8A 1.350(15) . ?
C1AA C4AA 1.382(18) . ?
C2A O2A 1.218(15) . ?
C2A N3A 1.370(17) . ?
O2A O1W 2.634(12) . ?
N3A C4A 1.373(16) . ?
C4A O4A 1.223(17) . ?
C4A C4AA 1.455(16) . ?
C4AA N5A 1.321(16) . ?
N5A C6A 1.347(16) . ?
C6A C7A 1.397(19) . ?
C6A C61A 1.49(2) . ?
C7A N8A 1.293(16) . ?
C7A C71A 1.518(17) . ?
N1B C2B 1.344(19) . ?
N1B C1AB 1.40(2) . ?
N1B C1B 1.463(19) . ?
C1AB N8B 1.352(19) . ?
C1AB C4AB 1.37(2) . ?
C2B O2B 1.227(19) . ?
C2B N3B 1.373(19) . ?
N3B C4B 1.392(18) . ?
C4B O4B 1.227(17) . ?
C4B C4AB 1.45(2) . ?
C4AB N5B 1.345(19) . ?
N5B C6B 1.33(2) . ?
C6B C7B 1.41(3) . ?
C6B C61B 1.52(3) . ?
C7B N8B 1.31(2) . ?
C7B C71B 1.49(2) . ?
N1C C2C 1.374(19) . ?
N1C C1AC 1.396(18) . ?
N1C C1C 1.449(17) . ?
C1AC N8C 1.338(17) . ?
C1AC C4AC 1.381(19) . ?
C2C O2C 1.196(18) . ?
C2C N3C 1.398(19) . ?
N3C C4C 1.365(18) . ?
C4C O4C 1.238(17) . ?
C4C C4AC 1.45(2) . ?
C4AC N5C 1.346(19) . ?
N5C C6C 1.31(2) . ?
N5C O1W 2.749(16) . ?
C6C C7C 1.38(2) . ?
C6C C61C 1.49(2) . ?
C7C N8C 1.36(2) . ?
C7C C71C 1.47(2) . ?
O1W O2W 2.416(15) . ?
O2W O3W 2.557(14) . ?
O2W N5A 2.868(15) 2_656 ?
O3W O4B 2.877(15) 1_556 ?
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
N3A H3A O4A 0.86 1.95 2.803(13) 169.0 2_656
N3B H3B O2C 0.86 1.90 2.754(15) 171.4 1_545
N3C H3C O2B 0.86 2.07 2.915(16) 166.6 1_565
|
1100140.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100140.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_1100140
loop_
_publ_author_name
'Barea, Elisa'
'Quiros, Miguel'
'Navarro, Jorge A. R.'
'Salas, Juan M.'
_publ_section_title
;
Heteroleptic pyrimidine-2-olate and 4,4[prime or minute]-bipyridine
copper(II) layered metal-organic frameworks with swelling properties.
;
_journal_issue 9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 1743
_journal_page_last 1746
_journal_paper_doi 10.1039/b500942a
_journal_year 2005
_chemical_formula_sum 'C34 H41.5 Cl2 Cu3 N9 O12.25'
_chemical_formula_weight 1033.78
_chemical_name_common
(Cu3Cl2(OH)3(2-pymo)(4,4'-bpy)1.5)n(NO3)n.6.25nH2O
_chemical_name_systematic
;
?
;
_space_group_IT_number 34
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'P 2 -2n'
_symmetry_space_group_name_H-M 'P n n 2'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-97
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 17.076(3)
_cell_length_b 19.341(3)
_cell_length_c 13.481(2)
_cell_measurement_reflns_used 2098
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.7
_cell_measurement_theta_min 2.4
_cell_volume 4452.3(12)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0993
_diffrn_reflns_av_sigmaI/netI 0.1066
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 27660
_diffrn_reflns_theta_full 28.44
_diffrn_reflns_theta_max 28.44
_diffrn_reflns_theta_min 1.59
_exptl_absorpt_coefficient_mu 1.607
_exptl_absorpt_correction_T_max 0.9297
_exptl_absorpt_correction_T_min 0.6260
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.542
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 2110
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.05
_refine_diff_density_max 1.381
_refine_diff_density_min -0.807
_refine_diff_density_rms 0.177
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.38(3)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.099
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 532
_refine_ls_number_reflns 8792
_refine_ls_number_restraints 12
_refine_ls_restrained_S_all 1.098
_refine_ls_R_factor_all 0.1154
_refine_ls_R_factor_gt 0.0841
_refine_ls_shift/su_max 0.062
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2010
_refine_ls_wR_factor_ref 0.2176
_reflns_number_gt 6423
_reflns_number_total 8792
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file b500942a.txt
_cod_data_source_block cuel
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' tag value 'orthorrombic' was replaced with
'orthorhombic' value.
Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana
;
_cod_original_formula_sum 'C34 H41.50 Cl2 Cu3 N9 O12.25'
_cod_database_code 1100140
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'
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 0.74340(8) 0.39747(6) 0.5000 0.0191(3) Uani 1 1 d . . .
Cu2 Cu 0.78112(7) 0.53035(6) 0.63488(15) 0.0193(3) Uani 1 1 d . . .
Cu3 Cu 0.70975(7) 0.26090(6) 0.36270(15) 0.0178(3) Uani 1 1 d . . .
Cl2 Cl 0.59672(18) 0.33689(14) 0.4426(2) 0.0335(7) Uani 1 1 d . . .
Cl3 Cl 0.88731(15) 0.44800(12) 0.5623(2) 0.0218(5) Uani 1 1 d . . .
O2 O 0.6993(4) 0.4752(4) 0.5766(6) 0.0242(17) Uani 1 1 d . . .
O3 O 0.7847(4) 0.3205(4) 0.4245(5) 0.0206(16) Uani 1 1 d . . .
N1P N 0.6363(5) 0.1969(4) 0.2968(6) 0.0200(19) Uani 1 1 d . . .
C2P C 0.6795(6) 0.1463(6) 0.2496(8) 0.021(2) Uani 1 1 d . . .
O2P O 0.7518(4) 0.1468(4) 0.2498(6) 0.0212(14) Uani 1 1 d . . .
N3P N 0.6392(5) 0.0939(4) 0.1974(7) 0.0214(19) Uani 1 1 d . . .
C4P C 0.5631(7) 0.0941(5) 0.1939(10) 0.031(3) Uani 1 1 d . . .
H4P H 0.5368 0.0591 0.1574 0.037 Uiso 1 1 d R . .
C5P C 0.5198(7) 0.1449(7) 0.2394(11) 0.038(3) Uani 1 1 d . . .
H5P H 0.4642 0.1450 0.2375 0.045 Uiso 1 1 d R . .
C6P C 0.5602(6) 0.1964(5) 0.2919(9) 0.026(2) Uani 1 1 d . . .
H6P H 0.5315 0.2319 0.3243 0.032 Uiso 1 1 d R . .
N11 N 0.7471(5) 0.4572(4) 0.3744(7) 0.0207(19) Uani 1 1 d . . .
C12 C 0.6874(6) 0.4976(5) 0.3478(8) 0.021(2) Uani 1 1 d . . .
H12 H 0.6409 0.4968 0.3865 0.025 Uiso 1 1 d R . .
C13 C 0.6906(6) 0.5401(5) 0.2672(8) 0.020(2) Uani 1 1 d . . .
H13 H 0.6471 0.5683 0.2504 0.024 Uiso 1 1 d R . .
C14 C 0.7563(7) 0.5422(5) 0.2103(8) 0.023(2) Uani 1 1 d . . .
C15 C 0.8195(6) 0.4990(5) 0.2360(8) 0.019(2) Uani 1 1 d . . .
H15 H 0.8656 0.4977 0.1966 0.023 Uiso 1 1 d R . .
C16 C 0.8120(6) 0.4577(5) 0.3201(8) 0.022(2) Uani 1 1 d . . .
H16 H 0.8547 0.4292 0.3392 0.026 Uiso 1 1 d R . .
N21 N 0.7385(5) 0.3365(4) 0.6230(7) 0.024(2) Uani 1 1 d . . .
C22 C 0.6760(7) 0.3323(5) 0.6818(8) 0.023(2) Uani 1 1 d . . .
H22 H 0.6324 0.3610 0.6670 0.027 Uiso 1 1 d R . .
C23 C 0.6703(7) 0.2885(5) 0.7618(8) 0.026(2) Uani 1 1 d . . .
H23 H 0.6227 0.2852 0.7979 0.032 Uiso 1 1 d R . .
C24 C 0.7351(7) 0.2494(5) 0.7895(8) 0.020(2) Uani 1 1 d . . .
C25 C 0.8011(7) 0.2537(5) 0.7295(10) 0.028(3) Uani 1 1 d . . .
H25 H 0.8456 0.2260 0.7440 0.033 Uiso 1 1 d R . .
C26 C 0.8027(7) 0.2973(5) 0.6480(9) 0.024(2) Uani 1 1 d . . .
H26 H 0.8488 0.3003 0.6088 0.029 Uiso 1 1 d R . .
N31 N 0.7741(5) 0.6000(4) 0.5212(6) 0.022(2) Uani 1 1 d . . .
C32 C 0.8356(7) 0.6145(5) 0.4675(9) 0.032(3) Uani 1 1 d . . .
H32 H 0.8832 0.5912 0.4819 0.038 Uiso 1 1 d R . .
C33 C 0.8357(7) 0.6626(6) 0.3919(8) 0.030(3) Uani 1 1 d . . .
H33 H 0.8812 0.6698 0.3527 0.037 Uiso 1 1 d R . .
C34 C 0.7690(7) 0.7000(5) 0.3729(9) 0.025(2) Uani 1 1 d . . .
C35 C 0.7032(7) 0.6840(5) 0.4311(8) 0.026(2) Uani 1 1 d . . .
H35 H 0.6546 0.7065 0.4194 0.031 Uiso 1 1 d R . .
C36 C 0.7090(6) 0.6359(5) 0.5044(9) 0.022(2) Uani 1 1 d . . .
H36 H 0.6647 0.6272 0.5452 0.027 Uiso 1 1 d R . .
N41 N 0.7659(5) 0.4832(4) 0.7689(7) 0.0213(19) Uani 1 1 d . . .
C42 C 0.6987(7) 0.4784(6) 0.8123(9) 0.033(3) Uani 1 1 d . . .
H42 H 0.6550 0.4985 0.7797 0.040 Uiso 1 1 d R . .
C43 C 0.6855(8) 0.4468(6) 0.9038(9) 0.037(3) Uani 1 1 d . . .
H43 H 0.6343 0.4446 0.9311 0.045 Uiso 1 1 d R . .
C44 C 0.7482(7) 0.4177(5) 0.9528(8) 0.022(2) Uani 1 1 d . . .
C45 C 0.8220(8) 0.4248(7) 0.9093(10) 0.040(3) Uani 1 1 d . . .
H45 H 0.8676 0.4090 0.9426 0.048 Uiso 1 1 d R . .
C46 C 0.8278(8) 0.4565(7) 0.8195(9) 0.039(3) Uani 1 1 d . . .
H46 H 0.8782 0.4593 0.7898 0.046 Uiso 1 1 d R . .
N51 N 0.7218(5) 0.1893(4) 0.4736(6) 0.0184(19) Uani 1 1 d . . .
C52 C 0.6616(7) 0.1740(5) 0.5324(8) 0.025(2) Uani 1 1 d . . .
H52 H 0.6138 0.1982 0.5227 0.030 Uiso 1 1 d R . .
C53 C 0.6646(6) 0.1256(5) 0.6076(8) 0.025(2) Uani 1 1 d . . .
H53 H 0.6197 0.1155 0.6467 0.030 Uiso 1 1 d R . .
C54 C 0.7361(6) 0.0916(5) 0.6246(8) 0.019(2) Uani 1 1 d . . .
C55 C 0.7971(6) 0.1053(5) 0.5625(9) 0.026(2) Uani 1 1 d . . .
H55 H 0.8449 0.0808 0.5701 0.032 Uiso 1 1 d R . .
C56 C 0.7898(6) 0.1547(5) 0.4869(8) 0.020(2) Uani 1 1 d . . .
H56 H 0.8334 0.1642 0.4453 0.024 Uiso 1 1 d R . .
N61 N 0.7206(5) 0.3130(4) 0.2303(7) 0.0197(18) Uani 1 1 d . . .
C62 C 0.7841(8) 0.3073(7) 0.1773(10) 0.040(3) Uani 1 1 d . . .
H62 H 0.8250 0.2790 0.2023 0.048 Uiso 1 1 d R . .
C63 C 0.7957(8) 0.3385(6) 0.0885(10) 0.040(3) Uani 1 1 d . . .
H63 H 0.8432 0.3313 0.0535 0.048 Uiso 1 1 d R . .
C64 C 0.7393(7) 0.3818(5) 0.0488(9) 0.024(2) Uani 1 1 d . . .
C65 C 0.6712(7) 0.3871(7) 0.1064(9) 0.037(3) Uani 1 1 d . . .
H65 H 0.6296 0.4159 0.0844 0.044 Uiso 1 1 d R . .
C66 C 0.6643(7) 0.3524(6) 0.1931(9) 0.037(3) Uani 1 1 d . . .
H66 H 0.6172 0.3566 0.2300 0.044 Uiso 1 1 d R . .
N1N N 0.996(2) 0.4504(9) 0.0161(15) 0.122(14) Uiso 0.50 1 d PD . .
O1N O 1.003(2) 0.4866(12) -0.0568(12) 0.071(7) Uiso 0.50 1 d PD . .
O2N O 0.988(3) 0.3879(9) 0.007(2) 0.175(18) Uiso 0.50 1 d PD . .
O3N O 0.9832(17) 0.4764(11) 0.0971(13) 0.099(9) Uiso 0.50 1 d PD . .
N2N N 0.493(2) 0.3580(14) 0.0239(19) 0.119(14) Uiso 0.50 1 d PD . .
O4N O 0.4780(16) 0.3393(12) 0.108(2) 0.089(8) Uiso 0.50 1 d PD . .
O5N O 0.487(3) 0.4194(17) 0.001(3) 0.179(17) Uiso 0.50 1 d PD . .
O6N O 0.498(7) 0.315(2) -0.042(3) 0.57(8) Uiso 0.50 1 d PD . .
O1W O 1.0000 0.5000 0.3946(10) 0.048(3) Uani 1 2 d S . .
O2W O 0.4637(7) 0.2677(6) 0.5684(11) 0.085(4) Uani 1 1 d . . .
O3W O 0.9099(7) 0.1581(10) 0.2336(10) 0.114(6) Uani 1 1 d . . .
O4W O 0.9986(8) 0.3807(9) 0.2488(14) 0.129(7) Uani 1 1 d . . .
O5W O 0.5000 0.5000 0.163(2) 0.089(8) Uiso 0.70 2 d SP . .
O6W O 0.9410(13) 0.2833(12) 0.3806(18) 0.117(8) Uiso 0.70 1 d P . .
O7W O 0.4887(15) 0.4352(13) 0.337(2) 0.138(9) Uiso 0.70 1 d P . .
O8W O 0.9713(14) 0.3666(12) 0.066(2) 0.071(6) Uiso 0.50 1 d P . .
O9W O 0.525(7) 0.512(6) 0.603(5) 0.36(5) Uiso 0.50 1 d P . .
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 0.0320(7) 0.0170(5) 0.0082(5) 0.0050(4) -0.0006(5) -0.0020(4)
Cu2 0.0326(7) 0.0160(6) 0.0094(6) 0.0041(5) 0.0018(6) 0.0000(5)
Cu3 0.0296(7) 0.0152(5) 0.0086(6) 0.0033(5) -0.0015(5) -0.0025(5)
Cl2 0.0436(18) 0.0342(15) 0.0226(16) 0.0043(12) 0.0041(12) -0.0026(11)
Cl3 0.0306(14) 0.0198(11) 0.0151(13) 0.0014(10) 0.0002(10) 0.0006(9)
O2 0.031(5) 0.026(4) 0.015(4) 0.004(3) 0.000(3) -0.001(3)
O3 0.033(4) 0.021(4) 0.008(4) 0.000(3) -0.005(3) -0.004(3)
N1P 0.034(5) 0.011(4) 0.015(5) 0.006(3) 0.003(4) 0.000(3)
C2P 0.048(7) 0.012(4) 0.002(4) 0.011(3) -0.005(5) -0.010(5)
O2P 0.025(4) 0.024(3) 0.014(3) 0.000(2) -0.003(3) -0.001(3)
N3P 0.032(5) 0.013(4) 0.019(5) 0.010(4) -0.003(4) -0.003(3)
C4P 0.030(6) 0.020(5) 0.044(8) 0.003(5) -0.008(5) 0.000(4)
C5P 0.044(7) 0.028(5) 0.041(8) -0.009(5) 0.004(6) 0.002(5)
C6P 0.025(6) 0.022(5) 0.032(7) 0.002(5) 0.004(5) 0.004(4)
N11 0.031(5) 0.018(4) 0.014(5) 0.003(4) 0.003(4) -0.001(3)
C12 0.027(6) 0.023(5) 0.013(6) 0.007(4) 0.000(4) -0.001(4)
C13 0.024(5) 0.021(5) 0.014(6) 0.003(4) 0.001(4) -0.004(4)
C14 0.043(7) 0.017(5) 0.010(6) 0.006(4) -0.012(5) -0.009(4)
C15 0.026(5) 0.014(5) 0.019(6) 0.004(4) 0.000(4) 0.002(4)
C16 0.030(6) 0.022(5) 0.014(5) 0.006(4) 0.000(4) -0.002(4)
N21 0.042(6) 0.018(4) 0.011(5) 0.006(4) -0.009(4) -0.003(4)
C22 0.038(6) 0.014(5) 0.016(5) 0.009(4) -0.001(5) -0.002(4)
C23 0.039(7) 0.026(6) 0.014(6) 0.011(4) 0.005(5) 0.000(5)
C24 0.035(6) 0.015(5) 0.011(6) 0.001(4) -0.003(5) 0.002(4)
C25 0.043(7) 0.016(5) 0.024(7) 0.002(5) -0.009(6) 0.005(5)
C26 0.037(6) 0.019(5) 0.016(6) 0.004(4) -0.004(5) -0.002(4)
N31 0.036(5) 0.022(4) 0.009(5) 0.006(4) 0.004(4) 0.005(4)
C32 0.047(8) 0.022(6) 0.027(7) 0.010(5) 0.001(5) 0.005(5)
C33 0.038(7) 0.037(6) 0.016(6) 0.014(5) 0.006(5) 0.004(5)
C34 0.050(7) 0.012(5) 0.014(6) 0.005(4) 0.011(5) 0.004(4)
C35 0.044(7) 0.022(5) 0.013(5) 0.009(4) -0.003(5) 0.009(5)
C36 0.022(5) 0.030(6) 0.015(5) 0.002(5) -0.003(5) -0.006(4)
N41 0.031(5) 0.016(4) 0.016(5) -0.003(4) 0.002(4) 0.001(4)
C42 0.027(6) 0.048(8) 0.024(7) 0.017(6) 0.004(5) 0.014(5)
C43 0.044(8) 0.045(7) 0.022(7) 0.025(6) 0.009(5) 0.005(6)
C44 0.043(7) 0.011(4) 0.012(5) 0.005(4) 0.006(5) -0.003(4)
C45 0.038(7) 0.057(8) 0.026(7) 0.029(6) 0.001(6) 0.009(6)
C46 0.053(8) 0.050(8) 0.013(6) 0.014(6) 0.005(6) 0.008(6)
N51 0.032(5) 0.020(4) 0.003(4) 0.001(3) -0.001(3) -0.008(3)
C52 0.028(6) 0.026(6) 0.021(6) 0.010(4) 0.000(4) 0.001(4)
C53 0.020(6) 0.027(5) 0.027(7) 0.009(5) 0.001(4) -0.002(4)
C54 0.031(6) 0.019(5) 0.007(5) 0.005(4) 0.000(4) -0.002(4)
C55 0.024(6) 0.025(5) 0.030(7) 0.012(5) -0.001(5) -0.002(4)
C56 0.028(6) 0.015(5) 0.017(6) 0.008(4) -0.002(4) -0.001(4)
N61 0.026(5) 0.027(5) 0.006(4) 0.003(4) 0.002(4) -0.004(4)
C62 0.040(7) 0.043(7) 0.037(8) 0.023(6) 0.010(6) 0.005(6)
C63 0.058(9) 0.039(7) 0.024(7) 0.017(6) 0.019(6) 0.009(6)
C64 0.037(7) 0.017(5) 0.017(6) -0.002(4) -0.005(5) -0.003(4)
C65 0.035(7) 0.056(8) 0.019(7) 0.020(6) 0.002(5) -0.004(6)
C66 0.034(7) 0.049(7) 0.027(7) 0.016(6) 0.004(5) 0.005(5)
O1W 0.057(9) 0.056(8) 0.032(7) 0.000 0.000 -0.015(6)
O2W 0.076(9) 0.082(8) 0.098(11) 0.018(8) 0.024(8) 0.013(7)
O3W 0.053(7) 0.227(18) 0.061(9) 0.052(10) 0.004(7) -0.015(9)
O4W 0.066(9) 0.169(15) 0.152(15) 0.079(13) 0.020(10) 0.032(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'
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'
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
O3 Cu1 O2 178.9(3) . . ?
O3 Cu1 N21 89.9(3) . . ?
O2 Cu1 N21 90.0(3) . . ?
O3 Cu1 N11 89.3(3) . . ?
O2 Cu1 N11 90.8(3) . . ?
N21 Cu1 N11 178.8(4) . . ?
O3 Cu1 Cl3 96.2(2) . . ?
O2 Cu1 Cl3 84.9(2) . . ?
N21 Cu1 Cl3 89.6(3) . . ?
N11 Cu1 Cl3 91.4(3) . . ?
O3 Cu1 Cl2 82.1(2) . . ?
O2 Cu1 Cl2 96.8(2) . . ?
N21 Cu1 Cl2 87.0(3) . . ?
N11 Cu1 Cl2 92.0(3) . . ?
Cl3 Cu1 Cl2 176.20(9) . . ?
O2 Cu2 N3P 175.6(3) . 4_655 ?
O2 Cu2 N41 91.2(3) . . ?
N3P Cu2 N41 89.3(3) 4_655 . ?
O2 Cu2 N31 91.0(3) . . ?
N3P Cu2 N31 87.2(3) 4_655 . ?
N41 Cu2 N31 162.0(3) . . ?
O2 Cu2 Cl3 90.7(2) . . ?
N3P Cu2 Cl3 93.4(3) 4_655 . ?
N41 Cu2 Cl3 98.5(3) . . ?
N31 Cu2 Cl3 99.3(3) . . ?
O3 Cu3 N1P 177.5(4) . . ?
O3 Cu3 N51 91.3(3) . . ?
N1P Cu3 N51 88.2(3) . . ?
O3 Cu3 N61 91.3(3) . . ?
N1P Cu3 N61 88.5(3) . . ?
N51 Cu3 N61 162.7(3) . . ?
O3 Cu3 Cl2 88.6(2) . . ?
N1P Cu3 Cl2 93.9(3) . . ?
N51 Cu3 Cl2 98.7(3) . . ?
N61 Cu3 Cl2 98.4(3) . . ?
Cu3 Cl2 Cu1 72.61(9) . . ?
Cu2 Cl3 Cu1 73.29(8) . . ?
Cu2 O2 Cu1 111.0(4) . . ?
Cu3 O3 Cu1 116.7(4) . . ?
C6P N1P C2P 120.3(9) . . ?
C6P N1P Cu3 131.5(7) . . ?
C2P N1P Cu3 108.2(7) . . ?
O2P C2P N1P 121.8(10) . . ?
O2P C2P N3P 119.6(11) . . ?
N1P C2P N3P 118.6(9) . . ?
C4P N3P C2P 120.1(10) . . ?
C4P N3P Cu2 131.3(8) . 4_644 ?
C2P N3P Cu2 108.5(7) . 4_644 ?
N3P C4P C5P 121.6(11) . . ?
C4P C5P C6P 117.9(11) . . ?
N1P C6P C5P 121.5(10) . . ?
C16 N11 C12 119.1(9) . . ?
C16 N11 Cu1 118.9(7) . . ?
C12 N11 Cu1 121.9(7) . . ?
N11 C12 C13 122.5(10) . . ?
C14 C13 C12 120.1(10) . . ?
C13 C14 C15 118.4(10) . . ?
C13 C14 C54 121.6(10) . 4_654 ?
C15 C14 C54 120.0(10) . 4_654 ?
C16 C15 C14 118.0(10) . . ?
N11 C16 C15 121.9(10) . . ?
C22 N21 C26 117.4(9) . . ?
C22 N21 Cu1 123.5(7) . . ?
C26 N21 Cu1 119.1(8) . . ?
N21 C22 C23 124.1(10) . . ?
C22 C23 C24 119.3(11) . . ?
C25 C24 C23 117.1(10) . . ?
C25 C24 C34 121.4(10) . 4_645 ?
C23 C24 C34 121.2(10) . 4_645 ?
C26 C25 C24 121.0(10) . . ?
N21 C26 C25 120.9(11) . . ?
C32 N31 C36 117.7(9) . . ?
C32 N31 Cu2 120.7(7) . . ?
C36 N31 Cu2 121.3(7) . . ?
N31 C32 C33 123.8(11) . . ?
C34 C33 C32 119.4(11) . . ?
C33 C34 C35 116.3(9) . . ?
C33 C34 C24 121.4(10) . 4_654 ?
C35 C34 C24 122.0(10) . 4_654 ?
C36 C35 C34 119.9(10) . . ?
N31 C36 C35 122.7(10) . . ?
C42 N41 C46 115.8(10) . . ?
C42 N41 Cu2 123.2(8) . . ?
C46 N41 Cu2 121.0(8) . . ?
N41 C42 C43 125.2(11) . . ?
C44 C43 C42 118.5(11) . . ?
C43 C44 C45 117.3(10) . . ?
C43 C44 C64 122.2(10) . 1_556 ?
C45 C44 C64 120.5(10) . 1_556 ?
C46 C45 C44 119.0(12) . . ?
C45 C46 N41 124.1(13) . . ?
C52 N51 C56 118.3(9) . . ?
C52 N51 Cu3 120.4(7) . . ?
C56 N51 Cu3 121.2(7) . . ?
N51 C52 C53 124.0(10) . . ?
C52 C53 C54 118.0(10) . . ?
C55 C54 C53 118.3(9) . . ?
C55 C54 C14 122.0(9) . 4_645 ?
C53 C54 C14 119.8(9) . 4_645 ?
C54 C55 C56 120.7(10) . . ?
N51 C56 C55 120.7(10) . . ?
C62 N61 C66 116.4(10) . . ?
C62 N61 Cu3 120.6(8) . . ?
C66 N61 Cu3 123.0(8) . . ?
N61 C62 C63 124.7(12) . . ?
C62 C63 C64 120.6(12) . . ?
C63 C64 C65 114.1(11) . . ?
C63 C64 C44 123.5(10) . 1_554 ?
C65 C64 C44 122.4(10) . 1_554 ?
C66 C65 C64 120.9(12) . . ?
N61 C66 C65 123.3(12) . . ?
O1N N1N O3N 120.3(11) . . ?
O1N N1N O2N 120.0(11) . . ?
O3N N1N O2N 118.7(11) . . ?
O1N N1N O8W 148(2) . . ?
O3N N1N O8W 89.9(15) . . ?
O2N N1N O8W 28.8(15) . . ?
O8W O2N N1N 112(2) . . ?
O4N N2N O6N 119.4(13) . . ?
O4N N2N O5N 120.1(13) . . ?
O6N N2N O5N 118.9(13) . . ?
O2N O8W N1N 38.8(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
Cu1 O3 1.936(7) . ?
Cu1 O2 1.973(8) . ?
Cu1 N21 2.037(9) . ?
Cu1 N11 2.051(9) . ?
Cu1 Cl3 2.775(3) . ?
Cu1 Cl2 2.872(3) . ?
Cu2 O2 1.925(8) . ?
Cu2 N3P 2.018(9) 4_655 ?
Cu2 N41 2.040(9) . ?
Cu2 N31 2.044(8) . ?
Cu2 Cl3 2.604(3) . ?
Cu3 O3 1.913(7) . ?
Cu3 N1P 1.973(9) . ?
Cu3 N51 2.049(8) . ?
Cu3 N61 2.059(9) . ?
Cu3 Cl2 2.654(3) . ?
N1P C6P 1.302(14) . ?
N1P C2P 1.381(14) . ?
C2P O2P 1.235(11) . ?
C2P N3P 1.412(14) . ?
N3P C4P 1.301(14) . ?
N3P Cu2 2.018(9) 4_644 ?
C4P C5P 1.374(16) . ?
C5P C6P 1.403(16) . ?
N11 C16 1.328(13) . ?
N11 C12 1.333(13) . ?
C12 C13 1.363(14) . ?
C13 C14 1.359(15) . ?
C14 C15 1.409(14) . ?
C14 C54 1.505(14) 4_654 ?
C15 C16 1.394(14) . ?
N21 C22 1.332(14) . ?
N21 C26 1.375(14) . ?
C22 C23 1.374(13) . ?
C23 C24 1.392(15) . ?
C24 C25 1.390(16) . ?
C24 C34 1.477(13) 4_645 ?
C25 C26 1.384(16) . ?
N31 C32 1.305(15) . ?
N31 C36 1.331(13) . ?
C32 C33 1.380(15) . ?
C33 C34 1.373(15) . ?
C34 C35 1.405(15) . ?
C34 C24 1.477(13) 4_654 ?
C35 C36 1.361(15) . ?
N41 C42 1.292(14) . ?
N41 C46 1.361(15) . ?
C42 C43 1.394(15) . ?
C43 C44 1.378(16) . ?
C44 C45 1.397(16) . ?
C44 C64 1.477(12) 1_556 ?
C45 C46 1.360(15) . ?
N51 C52 1.332(13) . ?
N51 C56 1.351(13) . ?
C52 C53 1.381(14) . ?
C53 C54 1.406(14) . ?
C54 C55 1.361(15) . ?
C54 C14 1.505(14) 4_645 ?
C55 C56 1.403(14) . ?
N61 C62 1.303(15) . ?
N61 C66 1.324(14) . ?
C62 C63 1.354(16) . ?
C63 C64 1.383(17) . ?
C64 C65 1.402(17) . ?
C64 C44 1.477(12) 1_554 ?
C65 C66 1.354(15) . ?
N1N O1N 1.214(9) . ?
N1N O3N 1.221(9) . ?
N1N O2N 1.222(9) . ?
N1N O8W 1.80(3) . ?
O2N O8W 0.94(4) . ?
N2N O4N 1.219(9) . ?
N2N O6N 1.223(9) . ?
N2N O5N 1.230(9) . ?
O9W O9W 1.0(2) 2_665 ?
|
1100141.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100141.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_1100141
_chemical_formula_moiety ?
_chemical_formula_sum 'C18 H16 O3'
_chemical_formula_weight 280.31
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_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 4
_cell_length_a 7.4026(11)
_cell_length_b 15.023(2)
_cell_length_c 12.3080(18)
_cell_measurement_reflns_used 369
_cell_measurement_temperature 153(2)
_cell_measurement_theta_max 17.69
_cell_measurement_theta_min 3.31
_cell_volume 1368.8(3)
_diffrn_ambient_temperature 153(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 0.0855
_diffrn_reflns_av_sigmaI/netI 0.1077
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 6715
_diffrn_reflns_theta_full 25.37
_diffrn_reflns_theta_max 25.37
_diffrn_reflns_theta_min 2.14
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.092
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.360
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description needle
_exptl_crystal_F_000 592
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.01
_exptl_crystal_size_min 0.01
_refine_diff_density_max 0.222
_refine_diff_density_min -0.193
_refine_diff_density_rms 0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0(2)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.983
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 191
_refine_ls_number_reflns 2496
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 0.983
_refine_ls_R_factor_all 0.1067
_refine_ls_R_factor_gt 0.0545
_refine_ls_shift/su_max 0.786
_refine_ls_shift/su_mean 0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0887
_refine_ls_wR_factor_ref 0.1060
_reflns_number_gt 1613
_reflns_number_total 2496
_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
;
_cod_original_sg_symbol_H-M Pna2(1)
_cod_database_code 1100141
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'
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 0.8283(3) 0.49282(15) 0.4305(2) 0.0253(7) Uani 1 1 d . . .
O2 O 1.0978(4) 0.50481(16) 0.5044(2) 0.0305(7) Uani 1 1 d . . .
O3 O 0.5090(4) 0.72697(18) 0.1313(2) 0.0409(8) Uani 1 1 d . . .
C1 C 0.6411(5) 0.5250(2) 0.4281(3) 0.0208(9) Uani 1 1 d . . .
H1 H 0.5818 0.5271 0.5112 0.025 Uiso 1 1 d R . .
C2 C 0.5321(5) 0.4576(3) 0.3651(3) 0.0268(10) Uani 1 1 d . . .
H2A H 0.4018 0.4681 0.3779 0.032 Uiso 1 1 calc R . .
H2B H 0.5615 0.3970 0.3912 0.032 Uiso 1 1 calc R . .
C3 C 0.5718(5) 0.4640(2) 0.2438(3) 0.0296(10) Uani 1 1 d . . .
H3A H 0.5023 0.4179 0.2044 0.036 Uiso 1 1 calc R . .
H3B H 0.7019 0.4532 0.2307 0.036 Uiso 1 1 calc R . .
C4 C 0.5203(6) 0.5562(2) 0.2010(3) 0.0296(10) Uani 1 1 d . . .
H4A H 0.5751 0.5646 0.1283 0.036 Uiso 1 1 calc R . .
H4B H 0.3875 0.5591 0.1924 0.036 Uiso 1 1 calc R . .
C5 C 0.5805(5) 0.6314(3) 0.2745(3) 0.0250(10) Uani 1 1 d . . .
C6 C 0.6413(5) 0.6165(2) 0.3798(3) 0.0202(9) Uani 1 1 d . . .
C7 C 0.7027(5) 0.6881(2) 0.4453(3) 0.0199(9) Uani 1 1 d . . .
C8 C 0.6929(5) 0.7738(2) 0.4036(3) 0.0224(9) Uani 1 1 d . . .
H8 H 0.7306 0.8226 0.4472 0.027 Uiso 1 1 calc R . .
C9 C 0.6292(5) 0.7893(3) 0.3001(3) 0.0278(10) Uani 1 1 d . . .
H9 H 0.6234 0.8483 0.2727 0.033 Uiso 1 1 calc R . .
C10 C 0.5738(6) 0.7188(3) 0.2362(3) 0.0290(10) Uani 1 1 d . . .
C11 C 0.4956(7) 0.8152(3) 0.0873(4) 0.0513(14) Uani 1 1 d . . .
H11A H 0.4360 0.8070 -0.0001 0.062 Uiso 1 1 d R . .
H11B H 0.4318 0.8577 0.1493 0.062 Uiso 1 1 d R . .
H11C H 0.6288 0.8432 0.0706 0.062 Uiso 1 1 d R . .
C12 C 0.7686(5) 0.6705(2) 0.5573(3) 0.0218(10) Uani 1 1 d . . .
C13 C 0.7307(5) 0.7318(2) 0.6400(3) 0.0241(9) Uani 1 1 d . . .
H13 H 0.6676 0.7851 0.6228 0.029 Uiso 1 1 calc R . .
C14 C 0.7836(5) 0.7161(2) 0.7467(3) 0.0260(10) Uani 1 1 d . . .
H14 H 0.7552 0.7581 0.8019 0.031 Uiso 1 1 calc R . .
C15 C 0.8768(5) 0.6400(3) 0.7725(3) 0.0279(10) Uani 1 1 d . . .
H15 H 0.9099 0.6286 0.8457 0.033 Uiso 1 1 calc R . .
C16 C 0.9224(5) 0.5801(2) 0.6924(3) 0.0244(10) Uani 1 1 d . . .
H16 H 0.9900 0.5284 0.7105 0.029 Uiso 1 1 calc R . .
C17 C 0.8695(5) 0.5947(2) 0.5837(3) 0.0195(9) Uani 1 1 d . . .
C18 C 0.9422(6) 0.5294(2) 0.5038(3) 0.0232(9) 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
O1 0.0252(16) 0.0237(15) 0.0270(15) -0.0037(13) -0.0033(13) 0.0029(12)
O2 0.0199(17) 0.0308(17) 0.0406(16) -0.0007(14) -0.0023(14) 0.0070(13)
O3 0.056(2) 0.0351(18) 0.0316(18) 0.0132(15) -0.0101(17) -0.0075(14)
C1 0.016(2) 0.021(2) 0.025(2) 0.000(2) 0.0005(19) -0.0023(17)
C2 0.030(3) 0.026(2) 0.025(2) -0.0016(18) -0.0001(19) -0.0018(19)
C3 0.025(2) 0.029(3) 0.035(3) -0.005(2) -0.003(2) -0.0028(18)
C4 0.029(3) 0.034(2) 0.026(2) 0.001(2) -0.004(2) -0.003(2)
C5 0.026(2) 0.028(3) 0.021(2) -0.0022(19) -0.001(2) -0.0007(17)
C6 0.016(2) 0.021(2) 0.023(2) 0.0031(18) 0.0042(18) 0.0006(17)
C7 0.019(2) 0.021(2) 0.020(2) 0.0020(19) 0.0009(19) -0.0010(16)
C8 0.023(2) 0.018(2) 0.027(2) -0.0046(19) 0.0001(18) 0.0002(17)
C9 0.032(3) 0.019(2) 0.032(3) 0.006(2) -0.001(2) -0.0005(19)
C10 0.032(3) 0.033(3) 0.021(2) 0.009(2) -0.003(2) 0.0000(19)
C11 0.073(4) 0.042(3) 0.040(3) 0.018(3) -0.013(3) -0.009(3)
C12 0.020(2) 0.022(2) 0.022(2) -0.0007(19) -0.0022(19) -0.0036(18)
C13 0.021(2) 0.023(2) 0.029(2) 0.000(2) -0.001(2) -0.0010(17)
C14 0.025(2) 0.027(2) 0.026(2) -0.005(2) -0.002(2) -0.0034(19)
C15 0.026(3) 0.035(3) 0.023(2) 0.004(2) -0.003(2) -0.007(2)
C16 0.020(2) 0.022(2) 0.032(2) 0.003(2) -0.002(2) -0.0038(17)
C17 0.017(2) 0.019(2) 0.023(2) 0.0007(18) -0.0019(18) 0.0005(17)
C18 0.028(3) 0.016(2) 0.025(2) 0.006(2) -0.006(2) -0.0020(18)
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'
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
C18 O1 C1 118.0(3) . . ?
C10 O3 C11 117.3(3) . . ?
O1 C1 C6 108.1(3) . . ?
O1 C1 C2 107.1(3) . . ?
C6 C1 C2 114.4(3) . . ?
C1 C2 C3 110.9(3) . . ?
C2 C3 C4 110.2(3) . . ?
C5 C4 C3 113.4(3) . . ?
C6 C5 C10 118.5(3) . . ?
C6 C5 C4 122.1(3) . . ?
C10 C5 C4 119.4(3) . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 C1 121.2(3) . . ?
C7 C6 C1 118.1(3) . . ?
C8 C7 C6 118.5(3) . . ?
C8 C7 C12 121.6(3) . . ?
C6 C7 C12 119.9(3) . . ?
C9 C8 C7 121.0(3) . . ?
C8 C9 C10 119.9(3) . . ?
C9 C10 O3 124.5(4) . . ?
C9 C10 C5 121.3(3) . . ?
O3 C10 C5 114.3(4) . . ?
C17 C12 C13 118.2(3) . . ?
C17 C12 C7 122.3(3) . . ?
C13 C12 C7 119.4(3) . . ?
C14 C13 C12 121.2(4) . . ?
C15 C14 C13 120.0(4) . . ?
C14 C15 C16 120.2(4) . . ?
C15 C16 C17 120.6(3) . . ?
C12 C17 C16 119.6(3) . . ?
C12 C17 C18 125.1(3) . . ?
C16 C17 C18 115.0(3) . . ?
O2 C18 O1 118.3(4) . . ?
O2 C18 C17 122.8(4) . . ?
O1 C18 C17 118.8(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
O1 C18 1.351(4) . ?
O1 C1 1.468(4) . ?
O2 C18 1.209(4) . ?
O3 C10 1.383(4) . ?
O3 C11 1.435(5) . ?
C1 C6 1.497(4) . ?
C1 C2 1.509(5) . ?
C2 C3 1.526(5) . ?
C3 C4 1.530(5) . ?
C4 C5 1.515(5) . ?
C5 C6 1.391(5) . ?
C5 C10 1.395(5) . ?
C6 C7 1.418(5) . ?
C7 C8 1.388(5) . ?
C7 C12 1.486(5) . ?
C8 C9 1.379(5) . ?
C9 C10 1.381(5) . ?
C12 C17 1.400(5) . ?
C12 C13 1.401(5) . ?
C13 C14 1.391(5) . ?
C14 C15 1.373(5) . ?
C15 C16 1.376(5) . ?
C16 C17 1.412(5) . ?
C17 C18 1.490(5) . ?
|
1100142.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100142.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_1100142
loop_
_publ_author_name
'Raj Pal Sharma'
'Ritu Bala'
'Rajni Sharma'
'Juan M. Salas'
'Miguel Quiros'
_journal_name_full 'Journal of Coordination Chemistry'
_journal_page_first 217
_journal_page_last 223
_journal_paper_doi 10.1080/0095897042000327888
_journal_volume 58
_journal_year 2005
_chemical_formula_sum 'Cl Co Cr2 H20 N6 O8'
_chemical_formula_weight 430.60
_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 112.962(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.0218(9)
_cell_length_b 9.3216(8)
_cell_length_c 16.2203(13)
_cell_measurement_reflns_used 27
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 17.14
_cell_measurement_theta_min 12.76
_cell_volume 1395.2(2)
_diffrn_ambient_temperature 293(2)
_diffrn_measurement_device 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0307
_diffrn_reflns_av_sigmaI/netI 0.0268
_diffrn_reflns_limit_h_max 1
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 1
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 5167
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 2.21
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 2.935
_exptl_absorpt_correction_T_max 0.5074
_exptl_absorpt_correction_T_min 0.3052
_exptl_absorpt_correction_type empirical
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 2.050
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description ?
_exptl_crystal_F_000 872
_exptl_crystal_size_max 0.1
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.4
_refine_diff_density_max 0.558
_refine_diff_density_min -1.005
_refine_diff_density_rms 0.138
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_all 1.072
_refine_ls_goodness_of_fit_obs 1.091
_refine_ls_hydrogen_treatment
;
Riding on their parent atoms, thermal parameters 1.2 times those of their
parent atoms
;
_refine_ls_matrix_type full
_refine_ls_number_parameters 175
_refine_ls_number_reflns 4018
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.071
_refine_ls_restrained_S_obs 1.091
_refine_ls_R_factor_all 0.0373
_refine_ls_R_factor_obs 0.0326
_refine_ls_shift/esd_max 0.002
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_all 0.0949
_refine_ls_wR_factor_obs 0.0906
_reflns_number_observed 3547
_reflns_number_total 4018
_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:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.6000P] 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^)+(0.0550P)^2^+0.6000P] 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 2(1)/c'
_cod_original_formula_sum 'H20 Cl Co Cr2 N6 O8'
_cod_database_code 1100142
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_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
Co 0.01540(13) 0.01464(12) 0.01375(12) 0.00005(7) 0.00651(9) -0.00015(7)
N1 0.0243(7) 0.0203(7) 0.0231(7) -0.0026(6) 0.0086(6) -0.0045(6)
N2 0.0238(8) 0.0306(8) 0.0174(7) -0.0003(5) 0.0111(6) -0.0016(6)
N3 0.0307(8) 0.0204(7) 0.0238(7) 0.0044(6) 0.0107(6) 0.0072(6)
N4 0.0281(9) 0.0305(8) 0.0212(7) -0.0035(6) 0.0148(7) -0.0027(6)
N5 0.0297(8) 0.0316(8) 0.0236(7) -0.0092(6) 0.0131(6) -0.0142(7)
N6 0.0251(8) 0.0310(8) 0.0266(8) 0.0067(7) 0.0086(6) 0.0109(7)
Cr1 0.0357(2) 0.02113(15) 0.01768(14) 0.00206(10) 0.00897(12) 0.00023(12)
Cr2 0.0186(2) 0.0226(2) 0.01703(15) 0.00170(9) 0.00752(12) 0.00121(9)
O1 0.0587(12) 0.0243(7) 0.0179(6) 0.0019(5) 0.0087(7) 0.0068(6)
O2 0.0672(13) 0.0493(10) 0.0324(8) 0.0159(8) 0.0281(9) 0.0089(9)
O3 0.0803(15) 0.0260(8) 0.0329(9) -0.0046(6) 0.0075(9) 0.0017(8)
O4 0.0381(10) 0.0562(12) 0.0560(12) 0.0101(9) 0.0109(9) -0.0026(8)
O5 0.0280(7) 0.0300(7) 0.0279(7) -0.0046(6) 0.0079(6) -0.0042(6)
O6 0.0320(8) 0.0267(7) 0.0318(7) 0.0072(6) 0.0128(6) 0.0066(6)
O7 0.0268(9) 0.0528(11) 0.0444(10) 0.0019(7) 0.0216(8) 0.0000(6)
Cl 0.0383(3) 0.0329(3) 0.0227(2) 0.0001(2) 0.0069(2) 0.0007(2)
O1W 0.0650(13) 0.0463(11) 0.0495(11) -0.0223(9) 0.0336(10) -0.0186(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
Co Co 0.29027(3) 0.25163(2) 0.062146(15) 0.01434(8) Uani 1 d . .
N1 N 0.4369(2) 0.4004(2) 0.11970(11) 0.0227(3) Uani 1 d . .
H11 H 0.3936(2) 0.4854(2) 0.11371(11) 0.027 Uiso 1 d R .
H12 H 0.5005(2) 0.4029(2) 0.09380(11) 0.027 Uiso 1 d R .
H13 H 0.4827(2) 0.3802(2) 0.17760(11) 0.027 Uiso 1 d R .
N2 N 0.3462(2) 0.2423(2) -0.04192(11) 0.0230(3) Uani 1 d . .
H21 H 0.4418(3) 0.2520(15) -0.02338(15) 0.028 Uiso 1 d R .
H22 H 0.3025(12) 0.3127(9) -0.0800(4) 0.028 Uiso 1 d R .
H23 H 0.3194(13) 0.1581(6) -0.0692(6) 0.028 Uiso 1 d R .
N3 N 0.4348(2) 0.1053(2) 0.12564(11) 0.0249(3) Uani 1 d . .
H31 H 0.4808(2) 0.1312(2) 0.18260(11) 0.030 Uiso 1 d R .
H32 H 0.4984(2) 0.0967(2) 0.10003(11) 0.030 Uiso 1 d R .
H33 H 0.3906(2) 0.0216(2) 0.12309(11) 0.030 Uiso 1 d R .
N4 N 0.2307(2) 0.2609(2) 0.16393(12) 0.0250(3) Uani 1 d . .
H41 H 0.1888(2) 0.3452(2) 0.16372(12) 0.030 Uiso 1 d R .
H42 H 0.3082(2) 0.2512(2) 0.21481(12) 0.030 Uiso 1 d R .
H43 H 0.1682(2) 0.1906(2) 0.15941(12) 0.030 Uiso 1 d R .
N5 N 0.1468(2) 0.1014(2) 0.00745(12) 0.0275(3) Uani 1 d . .
H51 H 0.1479(2) 0.0391(2) 0.04930(12) 0.033 Uiso 1 d R .
H52 H 0.1681(2) 0.0560(2) -0.03415(12) 0.033 Uiso 1 d R .
H53 H 0.0592(2) 0.1406(2) -0.01770(12) 0.033 Uiso 1 d R .
N6 N 0.1460(2) 0.3988(2) 0.00127(12) 0.0280(3) Uani 1 d . .
H61 H 0.1688(2) 0.4405(2) -0.04088(12) 0.034 Uiso 1 d R .
H62 H 0.1448(2) 0.4644(2) 0.04082(12) 0.034 Uiso 1 d R .
H63 H 0.0589(2) 0.3584(2) -0.02381(12) 0.034 Uiso 1 d R .
Cr1 Cr 0.08247(4) 0.92583(3) 0.24259(2) 0.02526(9) Uani 1 d . .
Cr2 Cr 0.23661(3) 0.74715(3) 0.42025(2) 0.01921(9) Uani 1 d . .
O1 O 0.1746(2) 0.7693(2) 0.30304(10) 0.0356(4) Uani 1 d . .
O2 O 0.1270(2) 0.9470(2) 0.15801(12) 0.0470(5) Uani 1 d . .
O3 O 0.1307(3) 1.0617(2) 0.30840(13) 0.0508(5) Uani 1 d . .
O4 O -0.0900(2) 0.9025(2) 0.2073(2) 0.0524(5) Uani 1 d . .
O5 O 0.3425(2) 0.8821(2) 0.46518(10) 0.0296(3) Uani 1 d . .
O6 O 0.3283(2) 0.5983(2) 0.44588(11) 0.0301(3) Uani 1 d . .
O7 O 0.1018(2) 0.7441(2) 0.45110(14) 0.0389(4) Uani 1 d . .
Cl Cl 0.55198(7) 0.25924(5) 0.32599(3) 0.03285(13) Uani 1 d . .
O1W O 0.1606(3) 0.5909(2) 0.15014(14) 0.0502(5) Uani 1 d D .
H11W H 0.2274(31) 0.6531(33) 0.1593(24) 0.060 Uiso 1 d D .
H12W H 0.1639(41) 0.6002(39) 0.2038(15) 0.060 Uiso 1 d D .
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'
O O 0.0106 0.0060 '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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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
N5 Co N6 90.31(9) . . ?
N5 Co N3 90.10(8) . . ?
N6 Co N3 178.78(7) . . ?
N5 Co N4 90.14(7) . . ?
N6 Co N4 89.21(8) . . ?
N3 Co N4 89.64(7) . . ?
N5 Co N1 178.72(7) . . ?
N6 Co N1 90.76(8) . . ?
N3 Co N1 88.82(8) . . ?
N4 Co N1 89.17(7) . . ?
N5 Co N2 89.10(7) . . ?
N6 Co N2 89.97(7) . . ?
N3 Co N2 91.18(7) . . ?
N4 Co N2 178.88(7) . . ?
N1 Co N2 91.61(7) . . ?
Co N1 O5 106.64(7) . 2_645 ?
Co N1 Cl 95.69(6) . . ?
O5 N1 Cl 113.78(6) 2_645 . ?
Co N3 O6 110.04(7) . 2_645 ?
Co N3 Cl 138.98(8) . 2_645 ?
O6 N3 Cl 96.04(5) 2_645 2_645 ?
Co N3 Cl 96.89(6) . . ?
O6 N3 Cl 110.74(6) 2_645 . ?
Cl N3 Cl 102.89(4) 2_645 . ?
Co N4 Cl 98.56(7) . . ?
Co N5 O2 104.63(8) . 1_545 ?
Co N5 O6 99.21(7) . 4_565 ?
O2 N5 O6 102.66(8) 1_545 4_565 ?
Co N5 O2 139.47(9) . 3_565 ?
O2 N5 O2 109.57(7) 1_545 3_565 ?
O6 N5 O2 93.97(7) 4_565 3_565 ?
Co N6 O1W 102.73(8) . . ?
O3 Cr1 O4 110.26(13) . . ?
O3 Cr1 O2 110.96(11) . . ?
O4 Cr1 O2 109.25(12) . . ?
O3 Cr1 O1 108.68(9) . . ?
O4 Cr1 O1 109.61(10) . . ?
O2 Cr1 O1 108.05(9) . . ?
O7 Cr2 O5 110.74(9) . . ?
O7 Cr2 O6 111.34(9) . . ?
O5 Cr2 O6 109.93(9) . . ?
O7 Cr2 O1 110.49(11) . . ?
O5 Cr2 O1 106.65(8) . . ?
O6 Cr2 O1 107.54(8) . . ?
Cr2 O1 Cr1 124.86(9) . . ?
Cr2 O1 O1W 136.20(9) . . ?
Cr1 O1 O1W 98.82(8) . . ?
N4 Cl N3 49.70(4) . . ?
N4 Cl N1 49.30(4) . . ?
N3 Cl N1 48.73(4) . . ?
O1 O1W N6 177.22(10) . . ?
O1 O1W Cl 82.83(6) . 2_655 ?
N6 O1W Cl 98.77(7) . 2_655 ?
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
Co N5 1.954(2) . ?
Co N6 1.958(2) . ?
Co N3 1.964(2) . ?
Co N4 1.964(2) . ?
Co N1 1.971(2) . ?
Co N2 1.977(2) . ?
N1 O5 3.031(2) 2_645 ?
N1 Cl 3.354(2) . ?
N3 O6 3.022(2) 2_645 ?
N3 Cl 3.310(2) 2_645 ?
N3 Cl 3.320(2) . ?
N4 Cl 3.267(2) . ?
N5 O2 2.908(2) 1_545 ?
N5 O6 3.031(2) 4_565 ?
N5 O2 3.032(3) 3_565 ?
N6 O1W 2.964(3) . ?
Cr1 O3 1.605(2) . ?
Cr1 O4 1.609(2) . ?
Cr1 O2 1.612(2) . ?
Cr1 O1 1.799(2) . ?
Cr2 O7 1.614(2) . ?
Cr2 O5 1.624(2) . ?
Cr2 O6 1.6260(15) . ?
Cr2 O1 1.767(2) . ?
O1 O1W 2.944(2) . ?
O1W Cl 3.168(2) 2_655 ?
|
1100143.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100143.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_1100143
loop_
_publ_author_name
'Raj Pal Sharma'
'Rajni Sharma'
'Ritu Bala'
'Miguel Quiros'
'Juan M. Salas'
_journal_name_full 'Journal of Coordination Chemistry'
_journal_page_first 1581
_journal_page_last 1586
_journal_paper_doi 10.1080/00958970310001641673
_journal_volume 56
_journal_year 2003
_chemical_formula_moiety ?
_chemical_formula_sum 'C5 H16 Co N11 S'
_chemical_formula_weight 321.28
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_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 113.4190(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 12.1950(6)
_cell_length_b 9.0317(5)
_cell_length_c 12.6017(7)
_cell_measurement_reflns_used 4678
_cell_measurement_temperature 295(2)
_cell_measurement_theta_max 25.019
_cell_measurement_theta_min 2.861
_cell_volume 1273.63(12)
_diffrn_ambient_temperature 295(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_diffrn_measurement_method '\w rotations with narrow frames'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'normal-focus sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0292
_diffrn_reflns_av_sigmaI/netI 0.0216
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 12953
_diffrn_reflns_theta_full 25.92
_diffrn_reflns_theta_max 25.92
_diffrn_reflns_theta_min 1.82
_diffrn_standards_decay_% 0.0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.515
_exptl_absorpt_correction_T_max 0.9336
_exptl_absorpt_correction_T_min 0.7605
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS
within SAINT+ package, v. 6.22.
;
_exptl_crystal_colour brown
_exptl_crystal_density_diffrn 1.676
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'irregular block'
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.05
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.422
_refine_diff_density_min -0.209
_refine_diff_density_rms 0.056
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 163
_refine_ls_number_reflns 2253
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.039
_refine_ls_R_factor_all 0.0297
_refine_ls_R_factor_gt 0.0262
_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^)+(0.0400P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0678
_refine_ls_wR_factor_ref 0.0697
_reflns_number_gt 2047
_reflns_number_total 2253
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 2(1)/c'
_cod_database_code 1100143
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
Co Co 0.17300(2) 0.46590(3) 0.31515(2) 0.02106(11) Uani 1 1 d . . .
N1A N 0.02113(15) 0.56148(19) 0.24018(15) 0.0286(4) Uani 1 1 d . . .
N2A N -0.03974(15) 0.53110(19) 0.13850(16) 0.0275(4) Uani 1 1 d . . .
N3A N -0.10125(18) 0.5073(2) 0.04063(18) 0.0425(5) Uani 1 1 d . . .
N4A N 0.12370(15) 0.3545(2) 0.42313(15) 0.0312(4) Uani 1 1 d . . .
N5A N 0.02892(16) 0.35343(19) 0.42268(14) 0.0278(4) Uani 1 1 d . . .
N6A N -0.06020(17) 0.3438(2) 0.42829(18) 0.0428(5) Uani 1 1 d . . .
N1E N 0.23250(15) 0.5878(2) 0.21923(15) 0.0278(4) Uani 1 1 d . . .
H11E H 0.2778 0.5327 0.1927 0.033 Uiso 1 1 d R . .
H12E H 0.1710 0.6254 0.1583 0.033 Uiso 1 1 d R . .
C1E C 0.3046(2) 0.7088(3) 0.2943(2) 0.0395(5) Uani 1 1 d . . .
H13E H 0.3111 0.7901 0.2469 0.047 Uiso 1 1 d R . .
H14E H 0.3844 0.6731 0.3406 0.047 Uiso 1 1 d R . .
C2E C 0.2457(2) 0.7618(3) 0.3724(2) 0.0401(5) Uani 1 1 d . . .
H23E H 0.2981 0.8293 0.4301 0.048 Uiso 1 1 d R . .
H24E H 0.1718 0.8132 0.3277 0.048 Uiso 1 1 d R . .
N2E N 0.22099(15) 0.6288(2) 0.42939(14) 0.0295(4) Uani 1 1 d . . .
H21E H 0.1620 0.6483 0.4532 0.035 Uiso 1 1 d R . .
H22E H 0.2868 0.6031 0.4914 0.035 Uiso 1 1 d R . .
N3E N 0.13067(14) 0.30238(19) 0.19910(14) 0.0269(4) Uani 1 1 d . . .
H31E H 0.0707 0.2484 0.2038 0.032 Uiso 1 1 d R . .
H32E H 0.1051 0.3411 0.1275 0.032 Uiso 1 1 d R . .
C3E C 0.2326(2) 0.2074(3) 0.21870(19) 0.0361(5) Uani 1 1 d . . .
H33E H 0.2811 0.2467 0.1801 0.043 Uiso 1 1 d R . .
H34E H 0.2066 0.1085 0.1896 0.043 Uiso 1 1 d R . .
C4E C 0.3043(2) 0.2046(2) 0.35062(19) 0.0363(5) Uani 1 1 d . . .
H43E H 0.2614 0.1485 0.3876 0.044 Uiso 1 1 d R . .
H44E H 0.3815 0.1582 0.3690 0.044 Uiso 1 1 d R . .
N4E N 0.32039(14) 0.3604(2) 0.39237(14) 0.0291(4) Uani 1 1 d . . .
H41E H 0.3791 0.4036 0.3772 0.035 Uiso 1 1 d R . .
H42E H 0.3410 0.3624 0.4693 0.035 Uiso 1 1 d R . .
S S 0.43865(6) 0.45395(8) 0.12585(5) 0.04896(19) Uani 1 1 d . . .
C1T C 0.5128(2) 0.4608(3) 0.2697(2) 0.0380(6) Uani 1 1 d . . .
N1T N 0.5622(2) 0.4653(3) 0.3719(2) 0.0616(7) 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
Co 0.01696(15) 0.02456(17) 0.02102(17) -0.00081(10) 0.00686(11) 0.00012(10)
N1A 0.0214(8) 0.0335(10) 0.0289(10) 0.0008(8) 0.0077(8) 0.0039(7)
N2A 0.0210(8) 0.0279(9) 0.0350(11) 0.0028(8) 0.0126(8) 0.0026(7)
N3A 0.0324(11) 0.0520(13) 0.0350(12) -0.0058(9) 0.0047(9) 0.0022(9)
N4A 0.0249(9) 0.0392(11) 0.0319(9) 0.0067(8) 0.0138(8) 0.0022(8)
N5A 0.0322(10) 0.0256(9) 0.0272(9) -0.0021(7) 0.0134(8) -0.0021(7)
N6A 0.0336(11) 0.0473(12) 0.0577(13) -0.0089(10) 0.0290(10) -0.0071(9)
N1E 0.0239(8) 0.0292(9) 0.0319(9) -0.0001(8) 0.0129(7) -0.0003(7)
C1E 0.0352(12) 0.0344(12) 0.0508(14) -0.0038(11) 0.0190(11) -0.0107(10)
C2E 0.0412(13) 0.0308(12) 0.0466(13) -0.0109(10) 0.0156(11) -0.0065(10)
N2E 0.0226(8) 0.0347(10) 0.0307(9) -0.0061(8) 0.0100(7) 0.0005(7)
N3E 0.0256(9) 0.0272(9) 0.0245(8) 0.0001(7) 0.0065(7) 0.0000(7)
C3E 0.0352(12) 0.0316(12) 0.0417(12) -0.0072(10) 0.0155(10) 0.0045(9)
C4E 0.0315(12) 0.0349(12) 0.0408(13) 0.0021(10) 0.0127(10) 0.0090(10)
N4E 0.0197(8) 0.0374(10) 0.0282(9) -0.0001(8) 0.0074(7) 0.0026(7)
S 0.0374(3) 0.0716(5) 0.0344(3) -0.0008(3) 0.0106(3) 0.0032(3)
C1T 0.0238(11) 0.0477(14) 0.0445(15) -0.0024(11) 0.0157(11) 0.0043(10)
N1T 0.0471(14) 0.085(2) 0.0396(14) -0.0082(12) 0.0036(11) 0.0164(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Co Co 0.3494 0.9721 '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
N1A Co N4E 176.60(7) . . ?
N1A Co N4A 94.02(7) . . ?
N4E Co N4A 82.98(7) . . ?
N1A Co N1E 88.02(7) . . ?
N4E Co N1E 95.11(7) . . ?
N4A Co N1E 174.76(7) . . ?
N1A Co N2E 88.41(7) . . ?
N4E Co N2E 93.08(7) . . ?
N4A Co N2E 87.73(7) . . ?
N1E Co N2E 87.51(7) . . ?
N1A Co N3E 93.11(7) . . ?
N4E Co N3E 85.51(7) . . ?
N4A Co N3E 93.85(7) . . ?
N1E Co N3E 90.85(7) . . ?
N2E Co N3E 177.73(7) . . ?
N2A N1A Co 118.54(14) . . ?
N3A N2A N1A 177.1(2) . . ?
N5A N4A Co 125.56(15) . . ?
N6A N5A N4A 174.7(2) . . ?
C1E N1E Co 106.80(13) . . ?
N1E C1E C2E 109.55(18) . . ?
N2E C2E C1E 107.37(18) . . ?
C2E N2E Co 107.86(13) . . ?
C3E N3E Co 111.01(13) . . ?
N3E C3E C4E 105.92(16) . . ?
N4E C4E C3E 107.71(17) . . ?
C4E N4E Co 108.94(12) . . ?
N1T C1T S 178.1(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
Co N1A 1.9175(17) . ?
Co N4E 1.9223(16) . ?
Co N4A 1.9686(17) . ?
Co N1E 1.9739(17) . ?
Co N2E 1.9773(17) . ?
Co N3E 1.9966(17) . ?
N1A N2A 1.230(2) . ?
N2A N3A 1.181(3) . ?
N4A N5A 1.154(2) . ?
N5A N6A 1.120(2) . ?
N1E C1E 1.484(3) . ?
C1E C2E 1.508(3) . ?
C2E N2E 1.490(3) . ?
N3E C3E 1.449(3) . ?
C3E C4E 1.541(3) . ?
C4E N4E 1.488(3) . ?
S C1T 1.675(3) . ?
C1T N1T 1.185(3) . ?
|
1100144.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100144.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_1100144
loop_
_publ_author_name
'Esther R. Acuna-Cueva'
'Rene Faure'
'Nuria A. Illan-Cabeza'
'Sonia B. Jimenez-Pulido'
'Miguel N. Moreno-Carretero'
'Miguel Quiros'
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 209
_journal_page_last 218
_journal_paper_doi 10.1016/S0020-1693(02)01165-9
_journal_volume 342
_journal_year 2003
_chemical_formula_moiety ?
_chemical_formula_sum 'C18 H24 Co N10 O12'
_chemical_formula_weight 631.40
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_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 109.305(5)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 13.2319(9)
_cell_length_b 8.1677(7)
_cell_length_c 12.9061(9)
_cell_measurement_reflns_used 37
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.06
_cell_measurement_theta_min 4.99
_cell_volume 1316.39(17)
_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 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0312
_diffrn_reflns_av_sigmaI/netI 0.0624
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 1
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 4853
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 1.63
_diffrn_standards_decay_% 5.91
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.732
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.593
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 650
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.07
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.359
_refine_diff_density_min -0.287
_refine_diff_density_rms 0.063
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.991
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 196
_refine_ls_number_reflns 3844
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 0.991
_refine_ls_R_factor_all 0.1266
_refine_ls_R_factor_gt 0.0571
_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^)+(0.0700P)^2^+0.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1248
_refine_ls_wR_factor_ref 0.1540
_reflns_number_gt 2016
_reflns_number_total 3844
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100144
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
Co Co 0.5000 0.5000 0.5000 0.03881(19) Uani 1 2 d S . .
N1 N 0.0826(2) 0.5954(4) 0.3632(2) 0.0497(7) Uani 1 1 d . . .
C1 C -0.0273(3) 0.6165(6) 0.2878(4) 0.0749(13) Uani 1 1 d . . .
H11 H -0.0255 0.6577 0.2187 0.090 Uiso 1 1 d R . .
H12 H -0.0646 0.6927 0.3187 0.090 Uiso 1 1 d R . .
H13 H -0.0635 0.5129 0.2766 0.090 Uiso 1 1 d R . .
C1A C 0.1631(2) 0.5482(4) 0.3232(3) 0.0415(7) Uani 1 1 d . . .
C2 C 0.1022(3) 0.6263(5) 0.4739(3) 0.0518(9) Uani 1 1 d . . .
O2 O 0.0351(2) 0.6752(4) 0.5109(2) 0.0684(8) Uani 1 1 d . . .
N3 N 0.2072(2) 0.5977(4) 0.5420(2) 0.0504(7) Uani 1 1 d . . .
H3 H 0.2197 0.6079 0.6114 0.060 Uiso 1 1 d R . .
C4 C 0.2916(2) 0.5569(4) 0.5100(3) 0.0427(7) Uani 1 1 d . . .
O4 O 0.38286(16) 0.5391(3) 0.57649(18) 0.0546(7) Uani 1 1 d . . .
C4A C 0.2676(2) 0.5351(3) 0.3942(3) 0.0380(7) Uani 1 1 d . . .
N5 N 0.35001(18) 0.5036(3) 0.35665(19) 0.0395(5) Uani 1 1 d . . .
C6 C 0.3275(2) 0.4799(4) 0.2503(2) 0.0430(7) Uani 1 1 d . . .
C61 C 0.4154(3) 0.4500(6) 0.2058(3) 0.0700(13) Uani 1 1 d . . .
H61 H 0.4829 0.4583 0.2639 0.084 Uiso 1 1 d R . .
H62 H 0.4124 0.5299 0.1503 0.084 Uiso 1 1 d R . .
H63 H 0.4082 0.3423 0.1743 0.084 Uiso 1 1 d R . .
C7 C 0.2181(3) 0.4819(4) 0.1798(3) 0.0459(8) Uani 1 1 d . . .
C71 C 0.1883(3) 0.4381(5) 0.0607(3) 0.0649(11) Uani 1 1 d . . .
H71 H 0.1122 0.4476 0.0259 0.078 Uiso 1 1 d R . .
H72 H 0.2100 0.3275 0.0541 0.078 Uiso 1 1 d R . .
H73 H 0.2240 0.5109 0.0257 0.078 Uiso 1 1 d R . .
N8 N 0.1380(2) 0.5175(4) 0.2160(2) 0.0470(7) Uani 1 1 d . . .
O1W O 0.4852(2) 0.2546(3) 0.5092(2) 0.0611(7) Uani 1 1 d D . .
H11W H 0.542(2) 0.199(4) 0.539(3) 0.073 Uiso 1 1 d D . .
H12W H 0.430(2) 0.210(5) 0.463(3) 0.073 Uiso 1 1 d D . .
N1N N 0.6950(2) 0.0089(4) 0.6779(2) 0.0526(7) Uani 1 1 d . . .
O1N O 0.6361(2) 0.0190(4) 0.5813(2) 0.0891(11) Uani 1 1 d . . .
O2N O 0.7147(3) -0.1238(4) 0.7226(3) 0.1006(12) Uani 1 1 d . . .
O3N O 0.7348(2) 0.1348(3) 0.7288(2) 0.0680(8) 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
Co 0.0335(3) 0.0450(3) 0.0386(3) 0.0032(3) 0.0128(2) 0.0020(3)
N1 0.0337(13) 0.0582(19) 0.0556(17) 0.0015(15) 0.0127(12) 0.0063(13)
C1 0.0376(18) 0.100(4) 0.078(3) -0.003(3) 0.0065(18) 0.016(2)
C1A 0.0383(15) 0.0383(17) 0.0471(17) 0.0054(13) 0.0129(13) 0.0000(12)
C2 0.0441(18) 0.053(2) 0.058(2) -0.0010(18) 0.0163(16) 0.0042(16)
O2 0.0478(13) 0.086(2) 0.0766(19) -0.0091(16) 0.0273(14) 0.0149(14)
N3 0.0429(14) 0.069(2) 0.0415(14) 0.0001(14) 0.0175(12) 0.0067(14)
C4 0.0390(15) 0.0480(18) 0.0424(16) 0.0026(14) 0.0152(13) 0.0007(14)
O4 0.0369(11) 0.086(2) 0.0403(11) 0.0000(12) 0.0127(9) 0.0085(11)
C4A 0.0368(14) 0.0349(18) 0.0423(15) 0.0038(12) 0.0130(12) -0.0004(11)
N5 0.0376(11) 0.0413(13) 0.0404(12) 0.0012(14) 0.0141(10) 0.0015(13)
C6 0.0475(16) 0.0435(19) 0.0382(15) 0.0013(15) 0.0144(13) 0.0023(15)
C61 0.057(2) 0.113(4) 0.0428(18) -0.003(2) 0.0199(16) 0.013(2)
C7 0.0499(16) 0.045(2) 0.0405(15) 0.0022(16) 0.0117(13) -0.0046(16)
C71 0.065(2) 0.080(3) 0.046(2) -0.0115(19) 0.0134(17) -0.012(2)
N8 0.0445(13) 0.0484(17) 0.0437(14) 0.0031(14) 0.0084(11) -0.0027(13)
O1W 0.0586(17) 0.0473(15) 0.0661(18) 0.0074(14) 0.0055(13) -0.0012(12)
N1N 0.0403(14) 0.0566(19) 0.0568(16) -0.0054(18) 0.0105(12) 0.0043(16)
O1N 0.0774(19) 0.112(3) 0.0566(16) -0.0201(18) -0.0059(14) 0.0281(19)
O2N 0.095(2) 0.0460(18) 0.146(3) 0.020(2) 0.020(2) -0.0046(17)
O3N 0.094(2) 0.0476(16) 0.0537(15) -0.0010(13) 0.0132(14) -0.0185(14)
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'
Co Co 0.3494 0.9721 '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 Co O4 91.26(11) . . ?
O1W Co N5 89.13(10) . . ?
O4 Co N5 78.25(8) . . ?
C1A N1 C2 122.0(3) . . ?
C1A N1 C1 120.1(3) . . ?
C2 N1 C1 117.9(3) . . ?
N8 C1A N1 118.8(3) . . ?
N8 C1A C4A 121.4(3) . . ?
N1 C1A C4A 119.8(3) . . ?
O2 C2 N1 123.8(3) . . ?
O2 C2 N3 121.1(3) . . ?
N1 C2 N3 115.2(3) . . ?
C4 N3 C2 126.8(3) . . ?
O4 C4 N3 122.1(3) . . ?
O4 C4 C4A 122.5(3) . . ?
N3 C4 C4A 115.4(3) . . ?
C4 O4 Co 113.0(2) . . ?
N5 C4A C1A 121.5(3) . . ?
N5 C4A C4 118.0(3) . . ?
C1A C4A C4 120.5(3) . . ?
C6 N5 C4A 117.9(2) . . ?
C6 N5 Co 134.2(2) . . ?
C4A N5 Co 107.90(18) . . ?
N5 C6 C7 119.6(3) . . ?
N5 C6 C61 119.5(3) . . ?
C7 C6 C61 120.9(3) . . ?
N8 C7 C6 122.4(3) . . ?
N8 C7 C71 116.4(3) . . ?
C6 C7 C71 121.1(3) . . ?
C7 N8 C1A 117.0(3) . . ?
O2N N1N O1N 120.2(4) . . ?
O2N N1N O3N 120.1(3) . . ?
O1N N1N O3N 119.7(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
Co O1W 2.021(3) . ?
Co O4 2.119(2) . ?
Co N5 2.221(2) . ?
N1 C1A 1.384(4) . ?
N1 C2 1.389(4) . ?
N1 C1 1.468(4) . ?
C1A N8 1.336(4) . ?
C1A C4A 1.388(4) . ?
C2 O2 1.206(4) . ?
C2 N3 1.397(4) . ?
N3 C4 1.354(4) . ?
C4 O4 1.237(4) . ?
C4 C4A 1.433(4) . ?
C4A N5 1.356(4) . ?
N5 C6 1.318(4) . ?
C6 C7 1.433(4) . ?
C6 C61 1.480(5) . ?
C7 N8 1.323(4) . ?
C7 C71 1.499(5) . ?
N1N O2N 1.215(4) . ?
N1N O1N 1.235(4) . ?
N1N O3N 1.239(4) . ?
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
O1W H11W O1N 0.857(10) 1.885(18) 2.707(4) 160(4) .
O1W H12W O1N 0.855(10) 2.07(3) 2.774(4) 140(4) 3_656
|
1100145.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100145.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_1100145
loop_
_publ_author_name
'Esther R. Acuna-Cueva'
'Rene Faure'
'Nuria A. Illan-Cabeza'
'Sonia B. Jimenez-Pulido'
'Miguel N. Moreno-Carretero'
'Miguel Quiros'
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 209
_journal_page_last 218
_journal_paper_doi 10.1016/S0020-1693(02)01165-9
_journal_volume 342
_journal_year 2003
_chemical_formula_moiety ?
_chemical_formula_sum 'C14 H16 Cu N10 O12'
_chemical_formula_weight 579.91
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 103.022(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 15.1701(10)
_cell_length_b 8.0805(6)
_cell_length_c 17.7233(17)
_cell_measurement_reflns_used 39
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.52
_cell_measurement_theta_min 4.98
_cell_volume 2116.7(3)
_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 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0338
_diffrn_reflns_av_sigmaI/netI 0.0363
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 3865
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 2.36
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time ?
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.122
_exptl_absorpt_correction_T_max 0.6767
_exptl_absorpt_correction_T_min 0.6052
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.820
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 1180
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.1
_refine_diff_density_max 0.332
_refine_diff_density_min -0.587
_refine_diff_density_rms 0.084
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.073
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 175
_refine_ls_number_reflns 3087
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.074
_refine_ls_R_factor_all 0.0446
_refine_ls_R_factor_gt 0.0359
_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^)+(0.0500P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0959
_refine_ls_wR_factor_ref 0.1014
_reflns_number_gt 2642
_reflns_number_total 3087
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
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
;
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100145
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
Cu Cu 0.0000 0.17538(4) 0.2500 0.02700(10) Uani 1 2 d S . .
N1 N 0.24657(10) 0.5063(2) 0.44732(8) 0.0307(3) Uani 1 1 d . . .
C1 C 0.32855(15) 0.6079(3) 0.47158(12) 0.0427(5) Uani 1 1 d . . .
H11 H 0.3758 0.5638 0.4495 0.051 Uiso 1 1 d R . .
H12 H 0.3476 0.6068 0.5270 0.051 Uiso 1 1 d R . .
H13 H 0.3157 0.7196 0.4540 0.051 Uiso 1 1 d R . .
C1A C 0.20911(11) 0.4828(2) 0.36978(9) 0.0257(3) Uani 1 1 d . . .
C2 C 0.20854(13) 0.4357(3) 0.50393(10) 0.0326(4) Uani 1 1 d . . .
O2 O 0.23823(12) 0.4592(2) 0.57250(8) 0.0484(4) Uani 1 1 d . . .
N3 N 0.13505(11) 0.3320(2) 0.47881(8) 0.0320(3) Uani 1 1 d . . .
H3 H 0.1129 0.2857 0.5142 0.038 Uiso 1 1 d R . .
C4 C 0.09401(12) 0.2953(2) 0.40392(9) 0.0278(3) Uani 1 1 d . . .
C4A C 0.13608(11) 0.3765(2) 0.34684(9) 0.0251(3) Uani 1 1 d . . .
O4 O 0.02823(10) 0.20454(19) 0.38582(8) 0.0371(3) Uani 1 1 d . . .
N5 N 0.09954(10) 0.34816(19) 0.27153(8) 0.0269(3) Uani 1 1 d . . .
C6 C 0.13476(12) 0.4278(3) 0.21958(10) 0.0321(4) Uani 1 1 d . . .
H6 H 0.1111 0.4112 0.1670 0.039 Uiso 1 1 d R . .
C7 C 0.20722(13) 0.5363(3) 0.24406(10) 0.0347(4) Uani 1 1 d . . .
H7 H 0.2299 0.5920 0.2066 0.042 Uiso 1 1 d R . .
N8 N 0.24548(10) 0.5643(2) 0.31809(9) 0.0330(3) Uani 1 1 d . . .
O1W O 0.09317(9) 0.00104(19) 0.25903(9) 0.0357(3) Uani 1 1 d D . .
H11W H 0.0902(18) -0.051(3) 0.2168(9) 0.043 Uiso 1 1 d D . .
H12W H 0.0845(18) -0.065(3) 0.2935(12) 0.043 Uiso 1 1 d D . .
N1N N 0.00181(12) 0.2711(2) 0.61487(10) 0.0369(3) Uani 1 1 d . . .
O1N O 0.07028(13) 0.1802(2) 0.62564(12) 0.0546(4) Uani 1 1 d . . .
O2N O -0.05574(13) 0.2554(2) 0.65458(12) 0.0576(5) Uani 1 1 d . . .
O3N O -0.00817(15) 0.3781(3) 0.56482(12) 0.0675(6) 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
Cu 0.02280(15) 0.03152(16) 0.02535(15) 0.000 0.00260(10) 0.000
N1 0.0300(7) 0.0382(8) 0.0229(6) -0.0030(6) 0.0038(5) -0.0045(6)
C1 0.0395(10) 0.0507(12) 0.0364(9) -0.0099(9) 0.0052(8) -0.0159(9)
C1A 0.0244(7) 0.0305(8) 0.0220(6) 0.0002(6) 0.0048(5) 0.0018(6)
C2 0.0338(8) 0.0406(10) 0.0234(7) -0.0019(7) 0.0063(6) 0.0010(8)
O2 0.0543(9) 0.0682(11) 0.0215(6) -0.0072(7) 0.0060(6) -0.0134(8)
N3 0.0354(8) 0.0415(8) 0.0204(6) 0.0005(6) 0.0091(5) -0.0038(7)
C4 0.0273(7) 0.0327(8) 0.0235(7) 0.0020(6) 0.0056(6) 0.0012(6)
C4A 0.0249(7) 0.0295(7) 0.0206(6) 0.0012(6) 0.0046(5) 0.0027(6)
O4 0.0349(7) 0.0474(8) 0.0292(6) 0.0012(6) 0.0075(5) -0.0108(6)
N5 0.0249(6) 0.0327(7) 0.0220(6) 0.0011(5) 0.0030(5) -0.0002(5)
C6 0.0304(8) 0.0436(10) 0.0217(7) 0.0036(7) 0.0048(6) 0.0004(7)
C7 0.0310(8) 0.0471(11) 0.0270(8) 0.0069(7) 0.0087(6) -0.0021(8)
N8 0.0284(7) 0.0421(9) 0.0287(7) 0.0022(6) 0.0069(6) -0.0047(6)
O1W 0.0297(6) 0.0376(7) 0.0412(7) 0.0052(6) 0.0108(5) 0.0027(5)
N1N 0.0409(9) 0.0359(8) 0.0359(8) 0.0002(7) 0.0126(7) -0.0014(7)
O1N 0.0503(10) 0.0506(10) 0.0693(11) 0.0048(9) 0.0270(9) 0.0128(8)
O2N 0.0601(11) 0.0573(11) 0.0670(11) 0.0231(9) 0.0389(9) 0.0184(9)
O3N 0.0763(14) 0.0694(12) 0.0649(12) 0.0351(11) 0.0327(11) 0.0138(11)
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'
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
O1W Cu O1W 89.07(9) . 2 ?
O1W Cu N5 89.25(6) . . ?
O1W Cu N5 173.84(6) . 2 ?
N5 Cu N5 93.03(8) . 2 ?
O1W Cu O4 96.65(5) . 2 ?
O1W Cu O4 91.52(6) . . ?
N5 Cu O4 77.47(5) . . ?
N5 Cu O4 94.56(6) . 2 ?
O4 Cu O4 168.54(8) . 2 ?
C1A N1 C2 121.33(15) . . ?
C1A N1 C1 119.99(15) . . ?
C2 N1 C1 118.68(15) . . ?
N8 C1A N1 118.22(15) . . ?
N8 C1A C4A 121.79(15) . . ?
N1 C1A C4A 119.99(15) . . ?
O2 C2 N3 120.48(17) . . ?
O2 C2 N1 122.65(18) . . ?
N3 C2 N1 116.86(15) . . ?
C4 N3 C2 126.95(15) . . ?
C4 N3 O3N 107.61(12) . . ?
C2 N3 O3N 113.02(12) . . ?
O4 C4 N3 123.51(16) . . ?
O4 C4 C4A 122.95(15) . . ?
N3 C4 C4A 113.53(15) . . ?
N5 C4A C1A 121.27(15) . . ?
N5 C4A C4 117.54(15) . . ?
C1A C4A C4 121.16(14) . . ?
C4 O4 Cu 106.12(11) . . ?
C6 N5 C4A 117.70(15) . . ?
C6 N5 Cu 126.93(12) . . ?
C4A N5 Cu 115.26(11) . . ?
N5 C6 C7 119.97(15) . . ?
N8 C7 C6 123.46(16) . . ?
C7 N8 C1A 115.78(16) . . ?
Cu O1W O2N 110.70(7) . 5_556 ?
Cu O1W O1N 111.25(7) . 6 ?
O2N O1W O1N 94.42(8) 5_556 6 ?
O3N N1N O2N 119.61(19) . . ?
O3N N1N O1N 119.23(19) . . ?
O2N N1N O1N 121.16(19) . . ?
N1N O3N N3 107.50(15) . . ?
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
Cu O1W 1.9763(14) . ?
Cu N5 2.0287(15) . ?
Cu O4 2.3598(14) . ?
N1 C1A 1.377(2) . ?
N1 C2 1.388(2) . ?
N1 C1 1.472(2) . ?
C1A N8 1.343(2) . ?
C1A C4A 1.389(2) . ?
C2 O2 1.212(2) . ?
C2 N3 1.386(2) . ?
N3 C4 1.366(2) . ?
N3 O3N 2.945(3) . ?
C4 O4 1.221(2) . ?
C4 C4A 1.467(2) . ?
C4A N5 1.345(2) . ?
N5 C6 1.330(2) . ?
C6 C7 1.397(3) . ?
C7 N8 1.329(2) . ?
O1W O2N 2.711(2) 5_556 ?
O1W O1N 2.736(3) 6 ?
N1N O3N 1.223(2) . ?
N1N O2N 1.245(2) . ?
N1N O1N 1.251(2) . ?
|
1100146.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100146.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_1100146
loop_
_publ_author_name
'Esther R. Acuna-Cueva'
'Rene Faure'
'Nuria A. Illan-Cabeza'
'Sonia B. Jimenez-Pulido'
'Miguel N. Moreno-Carretero'
'Miguel Quiros'
_journal_name_full 'Inorganica Chimica Acta'
_journal_page_first 356
_journal_page_last 362
_journal_paper_doi 10.1016/S0020-1693(03)00172-5
_journal_volume 351
_journal_year 2003
_chemical_formula_moiety ?
_chemical_formula_sum 'C9 H12 Cl2 Cu N4 O3'
_chemical_formula_weight 358.67
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_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 90.00
_cell_angle_beta 91.521(9)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 8.8152(10)
_cell_length_b 10.0526(12)
_cell_length_c 15.344(2)
_cell_measurement_reflns_used 39
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.50
_cell_measurement_theta_min 5.05
_cell_volume 1359.3(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0665
_diffrn_reflns_av_sigmaI/netI 0.0489
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 5152
_diffrn_reflns_theta_full 30.00
_diffrn_reflns_theta_max 30.00
_diffrn_reflns_theta_min 2.42
_diffrn_standards_decay_% 21.64
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 2.008
_exptl_absorpt_correction_T_max 0.8319
_exptl_absorpt_correction_T_min 0.4755
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.753
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 724
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.1
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.904
_refine_diff_density_min -0.757
_refine_diff_density_rms 0.089
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 181
_refine_ls_number_reflns 3958
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.0504
_refine_ls_R_factor_gt 0.0411
_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^)+(0.0600P)^2^+0.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1111
_refine_ls_wR_factor_ref 0.1178
_reflns_number_gt 3330
_reflns_number_total 3958
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 2(1)/n'
_cod_database_code 1100146
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
Cu Cu 0.35109(3) 0.21134(3) 0.402136(17) 0.03049(10) Uani 1 1 d . . .
Cl1 Cl 0.16476(7) 0.36401(7) 0.42076(4) 0.03879(15) Uani 1 1 d . . .
Cl2 Cl 0.47076(9) 0.02221(7) 0.36180(5) 0.04615(17) Uani 1 1 d . . .
N1 N 0.6450(2) 0.59668(19) 0.25277(12) 0.0289(4) Uani 1 1 d . . .
C1 C 0.6703(3) 0.6950(3) 0.18370(17) 0.0404(6) Uani 1 1 d . . .
H11 H 0.6891 0.7808 0.2093 0.049 Uiso 1 1 d R . .
H12 H 0.5822 0.6996 0.1457 0.049 Uiso 1 1 d R . .
H13 H 0.7565 0.6684 0.1509 0.049 Uiso 1 1 d R . .
C1A C 0.5517(2) 0.4879(2) 0.23703(13) 0.0238(4) Uani 1 1 d . . .
C2 C 0.7088(3) 0.6200(2) 0.33401(15) 0.0301(4) Uani 1 1 d . . .
O2 O 0.7908(2) 0.71622(19) 0.34879(13) 0.0406(4) Uani 1 1 d . . .
N3 N 0.6753(2) 0.5302(2) 0.39899(12) 0.0321(4) Uani 1 1 d . . .
H3 H 0.7211 0.5416 0.4486 0.039 Uiso 1 1 d R . .
C4 C 0.5772(2) 0.4254(2) 0.39270(14) 0.0264(4) Uani 1 1 d . . .
O4 O 0.5479(2) 0.35334(18) 0.45487(11) 0.0348(4) Uani 1 1 d . . .
C4A C 0.5118(2) 0.4063(2) 0.30543(13) 0.0239(4) Uani 1 1 d . . .
N5 N 0.4108(2) 0.30680(18) 0.29203(12) 0.0262(3) Uani 1 1 d . . .
C6 C 0.3547(3) 0.2858(2) 0.21218(14) 0.0281(4) Uani 1 1 d . . .
C61 C 0.2373(3) 0.1799(3) 0.19899(19) 0.0430(6) Uani 1 1 d . . .
H61 H 0.2837 0.1007 0.1771 0.052 Uiso 1 1 d R . .
H62 H 0.1610 0.2105 0.1579 0.052 Uiso 1 1 d R . .
H63 H 0.1912 0.1608 0.2536 0.052 Uiso 1 1 d R . .
C7 C 0.4076(2) 0.3646(2) 0.14184(13) 0.0264(4) Uani 1 1 d . . .
C71 C 0.3623(3) 0.3331(3) 0.04978(15) 0.0375(5) Uani 1 1 d . . .
H71 H 0.4065 0.3972 0.0117 0.045 Uiso 1 1 d R . .
H72 H 0.2537 0.3364 0.0432 0.045 Uiso 1 1 d R . .
H73 H 0.3973 0.2457 0.0352 0.045 Uiso 1 1 d R . .
N8 N 0.5008(2) 0.46672(18) 0.15516(11) 0.0268(3) Uani 1 1 d . . .
O1W O 0.2999(3) 0.1289(2) 0.51296(13) 0.0446(5) Uani 1 1 d D . .
H11W H 0.259(4) 0.176(3) 0.551(2) 0.054 Uiso 1 1 d D . .
H12W H 0.366(3) 0.079(3) 0.536(2) 0.054 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
Cu 0.04165(18) 0.02633(15) 0.02366(15) 0.00389(10) 0.00383(10) -0.00530(11)
Cl1 0.0413(3) 0.0432(3) 0.0318(3) 0.0004(2) 0.0004(2) 0.0012(2)
Cl2 0.0666(4) 0.0334(3) 0.0388(3) 0.0035(2) 0.0071(3) 0.0058(3)
N1 0.0340(9) 0.0285(9) 0.0243(8) 0.0023(7) 0.0040(7) -0.0076(7)
C1 0.0481(14) 0.0403(13) 0.0330(12) 0.0116(10) 0.0008(10) -0.0155(11)
C1A 0.0250(9) 0.0232(8) 0.0235(9) 0.0001(7) 0.0033(7) -0.0008(7)
C2 0.0338(10) 0.0303(10) 0.0264(10) -0.0021(8) 0.0051(8) -0.0053(8)
O2 0.0489(10) 0.0399(10) 0.0331(9) -0.0031(7) 0.0041(7) -0.0202(8)
N3 0.0401(10) 0.0339(10) 0.0223(8) -0.0003(7) -0.0013(7) -0.0099(8)
C4 0.0306(10) 0.0256(9) 0.0231(9) 0.0009(7) 0.0014(7) -0.0008(8)
O4 0.0473(10) 0.0337(8) 0.0233(7) 0.0053(6) -0.0009(6) -0.0071(7)
C4A 0.0285(9) 0.0226(8) 0.0208(8) -0.0001(7) 0.0020(7) -0.0006(7)
N5 0.0320(9) 0.0227(8) 0.0238(8) 0.0006(6) 0.0012(6) -0.0029(6)
C6 0.0347(10) 0.0245(9) 0.0250(9) -0.0032(8) 0.0012(8) -0.0025(8)
C61 0.0523(15) 0.0410(13) 0.0356(12) -0.0019(10) -0.0033(11) -0.0194(11)
C7 0.0295(9) 0.0288(10) 0.0209(9) -0.0011(7) 0.0015(7) 0.0019(8)
C71 0.0483(14) 0.0425(13) 0.0216(10) -0.0039(9) -0.0006(9) -0.0047(11)
N8 0.0311(9) 0.0277(8) 0.0217(8) 0.0018(7) 0.0031(6) -0.0007(7)
O1W 0.0677(13) 0.0369(10) 0.0298(9) 0.0073(8) 0.0127(8) 0.0012(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'
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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.0500
1.00 0.00 -1.00 0.0500
1.00 0.00 2.00 0.2000
0.00 -1.00 -1.00 0.2000
0.00 -1.00 1.00 0.2000
-1.00 0.00 0.00 0.1500
-1.00 1.00 0.00 0.2000
1.00 1.00 0.00 0.2000
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 Cu N5 176.14(8) . . ?
O1W Cu Cl2 90.09(7) . . ?
N5 Cu Cl2 92.09(6) . . ?
O1W Cu Cl1 89.59(7) . . ?
N5 Cu Cl1 89.41(6) . . ?
Cl2 Cu Cl1 160.68(3) . . ?
O1W Cu O4 98.16(8) . . ?
N5 Cu O4 78.20(7) . . ?
Cl2 Cu O4 104.84(5) . . ?
Cl1 Cu O4 94.32(5) . . ?
C2 N1 C1A 121.30(18) . . ?
C2 N1 C1 118.24(19) . . ?
C1A N1 C1 120.35(19) . . ?
N8 C1A C4A 122.08(18) . . ?
N8 C1A N1 118.11(18) . . ?
C4A C1A N1 119.80(18) . . ?
O2 C2 N1 121.9(2) . . ?
O2 C2 N3 121.2(2) . . ?
N1 C2 N3 116.90(19) . . ?
C4 N3 C2 126.87(19) . . ?
O4 C4 N3 123.0(2) . . ?
O4 C4 C4A 123.3(2) . . ?
N3 C4 C4A 113.68(18) . . ?
C4 O4 Cu 104.84(14) . . ?
N5 C4A C1A 120.19(18) . . ?
N5 C4A C4 118.74(18) . . ?
C1A C4A C4 121.07(18) . . ?
C6 N5 C4A 119.13(19) . . ?
C6 N5 Cu 126.63(15) . . ?
C4A N5 Cu 114.12(14) . . ?
N5 C6 C7 119.28(19) . . ?
N5 C6 C61 118.6(2) . . ?
C7 C6 C61 122.1(2) . . ?
N8 C7 C6 121.75(19) . . ?
N8 C7 C71 117.3(2) . . ?
C6 C7 C71 120.9(2) . . ?
C7 N8 C1A 117.24(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
Cu O1W 1.9552(19) . ?
Cu N5 2.0248(19) . ?
Cu Cl2 2.2684(8) . ?
Cu Cl1 2.2715(7) . ?
Cu O4 2.3725(18) . ?
N1 C2 1.374(3) . ?
N1 C1A 1.386(3) . ?
N1 C1 1.470(3) . ?
C1A N8 1.340(3) . ?
C1A C4A 1.385(3) . ?
C2 O2 1.225(3) . ?
C2 N3 1.383(3) . ?
N3 C4 1.365(3) . ?
C4 O4 1.231(3) . ?
C4 C4A 1.456(3) . ?
C4A N5 1.351(3) . ?
N5 C6 1.326(3) . ?
C6 C7 1.427(3) . ?
C6 C61 1.494(3) . ?
C7 N8 1.328(3) . ?
C7 C71 1.492(3) . ?
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
O1W H11W O2 0.839(18) 1.94(2) 2.767(3) 167(4) 3_666
O1W H12W Cl2 0.836(18) 2.34(2) 3.143(2) 162(4) 3_656
N3 H3 Cl1 0.86 2.41 3.250(2) 164.4 3_666
|
1100147.cif | #------------------------------------------------------------------------------
#$Date: 2017-07-12 10:07:33 +0300 (Wed, 12 Jul 2017) $
#$Revision: 198667 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100147.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_1100147
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Garcia-Martinez, Emilia'
'Covelo, Berta'
'Castineiras, Alfonso'
_publ_section_title
;
An X-Ray Study of the Crystal Structure of a new stepped-
cubane tetranuclear copper(II) compound, [Cu~4~(\m~2~-OH)
~2~(\m~3~-OH)~2~Cl~2~(bipy)~4~]Cl~2~.6H~2~O
;
_journal_name_full 'Z. Anorg. Allg. Chem.'
_journal_page_first 907
_journal_page_last 908
_journal_paper_doi
10.1002/1521-3749(200206)628:5<907::AID-ZAAC907>3.0.CO;2-K
_journal_volume 628
_journal_year 2002
_chemical_formula_sum 'C40 H48 Cl4 Cu4 N8 O10'
_chemical_formula_weight 1196.82
_chemical_name_systematic
;
Tetrakis(2,2'-bipyridine-N,N')-dichloro-bis(mu!3$-hydroxo)
-bis(mu!2$-hydroxo)-tetracopper(II) dichloride hexahydrate
;
_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, H of hydroxo ligands, difmap'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 85.760(2)
_cell_angle_beta 75.915(2)
_cell_angle_gamma 73.000(2)
_cell_formula_units_Z 1
_cell_length_a 9.2608(10)
_cell_length_b 10.3755(11)
_cell_length_c 12.9865(14)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1157.4(2)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.865
_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 0.0477
_diffrn_reflns_av_sigmaI/netI 0.1699
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 6967
_diffrn_reflns_theta_full 28.04
_diffrn_reflns_theta_max 28.04
_diffrn_reflns_theta_min 1.62
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.108
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.78607
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.717
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 608
_exptl_crystal_size_max .23
_exptl_crystal_size_mid .05
_exptl_crystal_size_min .04
_refine_diff_density_max 0.537
_refine_diff_density_min -0.393
_refine_diff_density_rms 0.099
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.832
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 300
_refine_ls_number_reflns 4866
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.832
_refine_ls_R_factor_all 0.1255
_refine_ls_R_factor_gt 0.0529
_refine_ls_shift/su_max 0.053
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0908
_refine_ls_wR_factor_ref 0.1055
_reflns_number_gt 2359
_reflns_number_total 4866
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
Marking attached hydrogen atoms.
Antanas Vaitkus,
2017-07-12
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.
'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-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 P-1
_cod_database_code 1100147
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
_atom_site_attached_hydrogens
Cu2 Cu 0.04423(9) 0.05488(7) 0.27590(6) 0.0298(2) Uani 1 1 d . . . 0
Cu1 Cu 0.13968(8) 0.06569(7) 0.47418(5) 0.0277(2) Uani 1 1 d . . . 0
O1 O 0.0516(4) 0.1864(4) 0.3712(3) 0.0298(10) Uani 1 1 d . . . 0
O2 O 0.0850(4) -0.0634(4) 0.3984(3) 0.0255(10) Uani 1 1 d . . . 0
N1 N 0.2027(5) 0.1969(4) 0.5454(4) 0.0258(12) Uani 1 1 d . . . 0
N2 N 0.2814(5) -0.0632(4) 0.5542(4) 0.0267(12) Uani 1 1 d . . . 0
C1 C 0.1513(7) 0.3310(6) 0.5379(5) 0.0373(17) Uani 1 1 d . . . 0
H1 H 0.0764 0.3689 0.4994 0.045 Uiso 1 1 calc R . . 0
C2 C 0.2081(8) 0.4156(7) 0.5869(5) 0.0424(18) Uani 1 1 d . . . 0
H2 H 0.1697 0.5087 0.5824 0.051 Uiso 1 1 calc R . . 0
C3 C 0.3198(8) 0.3597(7) 0.6410(5) 0.0451(19) Uani 1 1 d . . . 0
H3 H 0.3618 0.4144 0.6713 0.054 Uiso 1 1 calc R . . 0
C4 C 0.3710(7) 0.2211(6) 0.6508(5) 0.0369(17) Uani 1 1 d . . . 0
H4 H 0.4451 0.1818 0.6896 0.044 Uiso 1 1 calc R . . 0
C5 C 0.3104(7) 0.1420(6) 0.6024(4) 0.0279(15) Uani 1 1 d . . . 0
C6 C 0.3551(7) -0.0060(6) 0.6095(5) 0.0277(15) Uani 1 1 d . . . 0
C7 C 0.4589(7) -0.0814(6) 0.6642(5) 0.0368(17) Uani 1 1 d . . . 0
H7 H 0.5068 -0.0395 0.7013 0.044 Uiso 1 1 calc R . . 0
C8 C 0.4933(7) -0.2211(7) 0.6644(5) 0.0434(19) Uani 1 1 d . . . 0
H8 H 0.5635 -0.2739 0.7018 0.052 Uiso 1 1 calc R . . 0
C9 C 0.4217(7) -0.2789(6) 0.6084(5) 0.0418(18) Uani 1 1 d . . . 0
H9 H 0.4450 -0.3723 0.6056 0.050 Uiso 1 1 calc R . . 0
C10 C 0.3156(7) -0.1993(6) 0.5562(5) 0.0369(17) Uani 1 1 d . . . 0
H10 H 0.2649 -0.2404 0.5208 0.044 Uiso 1 1 calc R . . 0
N3 N -0.0179(5) -0.0738(5) 0.1979(4) 0.0282(13) Uani 1 1 d . . . 0
N4 N -0.0854(5) 0.1869(5) 0.1882(4) 0.0276(12) Uani 1 1 d . . . 0
C11 C 0.0295(7) -0.2102(6) 0.2055(4) 0.0339(16) Uani 1 1 d . . . 0
H11 H 0.0969 -0.2499 0.2489 0.041 Uiso 1 1 calc R . . 0
C12 C -0.0197(7) -0.2911(6) 0.1504(5) 0.0382(17) Uani 1 1 d . . . 0
H12 H 0.0147 -0.3843 0.1566 0.046 Uiso 1 1 calc R . . 0
C13 C -0.1182(8) -0.2344(6) 0.0872(5) 0.0435(18) Uani 1 1 d . . . 0
H13 H -0.1526 -0.2884 0.0502 0.052 Uiso 1 1 calc R . . 0
C14 C -0.1682(7) -0.0937(6) 0.0778(5) 0.0385(17) Uani 1 1 d . . . 0
H14 H -0.2357 -0.0528 0.0347 0.046 Uiso 1 1 calc R . . 0
C15 C -0.1145(7) -0.0175(6) 0.1344(5) 0.0286(15) Uani 1 1 d . . . 0
C16 C -0.1544(7) 0.1325(6) 0.1298(5) 0.0281(15) Uani 1 1 d . . . 0
C17 C -0.2548(7) 0.2086(6) 0.0722(5) 0.0413(17) Uani 1 1 d . . . 0
H17 H -0.3021 0.1681 0.0337 0.050 Uiso 1 1 calc R . . 0
C18 C -0.2846(8) 0.3485(7) 0.0725(5) 0.052(2) Uani 1 1 d . . . 0
H18 H -0.3511 0.4030 0.0333 0.062 Uiso 1 1 calc R . . 0
C19 C -0.2143(8) 0.4039(7) 0.1316(5) 0.0475(19) Uani 1 1 d . . . 0
H19 H -0.2332 0.4968 0.1342 0.057 Uiso 1 1 calc R . . 0
C20 C -0.1163(7) 0.3203(6) 0.1863(5) 0.0372(17) Uani 1 1 d . . . 0
H20 H -0.0676 0.3590 0.2251 0.045 Uiso 1 1 calc R . . 0
Cl2 Cl 0.3053(2) -0.38930(16) 0.34869(14) 0.0512(5) Uani 1 1 d . . . 0
Cl1 Cl 0.3214(2) 0.00890(17) 0.16049(13) 0.0501(5) Uani 1 1 d . . . 0
O3 O 0.1603(5) 0.4127(4) 0.2676(3) 0.0508(13) Uani 1 1 d . . . 2
O4 O 0.3312(6) 0.3023(5) 0.0739(4) 0.0726(16) Uani 1 1 d . . . 2
O5 O 0.4795(6) 0.6981(5) 0.1270(4) 0.0766(17) Uani 1 1 d . . . 2
H100 H 0.1196 0.2472 0.3492 0.07(2) Uiso 1 1 d . . . 0
H200 H 0.1770 -0.1306 0.3838 0.030(17) Uiso 1 1 d . . . 0
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
Cu2 0.0347(5) 0.0329(4) 0.0262(5) 0.0008(4) -0.0143(4) -0.0106(4)
Cu1 0.0309(5) 0.0303(4) 0.0261(5) -0.0010(4) -0.0131(4) -0.0096(4)
O1 0.037(3) 0.027(2) 0.034(3) 0.003(2) -0.020(2) -0.014(2)
O2 0.023(2) 0.033(2) 0.026(2) -0.0034(19) -0.0109(19) -0.011(2)
N1 0.026(3) 0.025(3) 0.029(3) -0.003(2) -0.011(2) -0.007(2)
N2 0.026(3) 0.028(3) 0.023(3) 0.001(2) -0.004(2) -0.004(2)
C1 0.039(4) 0.032(4) 0.039(4) -0.007(3) -0.008(3) -0.005(3)
C2 0.051(5) 0.040(4) 0.041(4) -0.011(4) -0.004(4) -0.022(4)
C3 0.050(5) 0.053(5) 0.042(5) -0.011(4) -0.008(4) -0.029(4)
C4 0.038(4) 0.045(4) 0.033(4) -0.005(3) -0.011(3) -0.018(3)
C5 0.027(4) 0.031(4) 0.021(4) -0.007(3) 0.003(3) -0.008(3)
C6 0.016(3) 0.045(4) 0.024(4) -0.007(3) -0.004(3) -0.010(3)
C7 0.029(4) 0.044(4) 0.035(4) -0.005(3) -0.008(3) -0.006(3)
C8 0.027(4) 0.065(5) 0.036(4) 0.010(4) -0.015(3) -0.006(4)
C9 0.035(4) 0.033(4) 0.046(5) 0.007(4) -0.006(4) 0.003(3)
C10 0.034(4) 0.039(4) 0.038(4) -0.004(3) -0.009(3) -0.010(3)
N3 0.028(3) 0.032(3) 0.025(3) -0.001(3) -0.006(3) -0.008(3)
N4 0.034(3) 0.027(3) 0.023(3) 0.000(2) -0.012(2) -0.005(2)
C11 0.039(4) 0.037(4) 0.022(4) 0.000(3) -0.008(3) -0.006(3)
C12 0.041(4) 0.032(4) 0.041(4) -0.007(3) -0.011(4) -0.006(3)
C13 0.058(5) 0.044(4) 0.043(4) -0.001(4) -0.028(4) -0.023(4)
C14 0.041(4) 0.050(4) 0.037(4) 0.004(4) -0.024(3) -0.020(4)
C15 0.018(4) 0.042(4) 0.024(4) 0.000(3) -0.002(3) -0.008(3)
C16 0.027(4) 0.035(4) 0.021(3) 0.004(3) -0.008(3) -0.007(3)
C17 0.044(4) 0.044(4) 0.046(4) 0.006(4) -0.027(4) -0.015(4)
C18 0.056(5) 0.044(5) 0.053(5) 0.012(4) -0.024(4) -0.006(4)
C19 0.059(5) 0.030(4) 0.057(5) -0.002(4) -0.028(4) -0.008(4)
C20 0.045(4) 0.034(4) 0.036(4) -0.002(3) -0.019(3) -0.008(3)
Cl2 0.0560(12) 0.0452(10) 0.0569(12) 0.0004(9) -0.0255(10) -0.0111(9)
Cl1 0.0427(11) 0.0675(12) 0.0437(11) -0.0009(9) -0.0115(9) -0.0197(10)
O3 0.053(3) 0.046(3) 0.056(3) 0.005(2) -0.015(3) -0.017(2)
O4 0.085(4) 0.075(3) 0.064(4) -0.013(3) -0.016(3) -0.031(3)
O5 0.086(4) 0.067(3) 0.056(4) 0.005(3) -0.004(3) -0.002(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'
Cu Cu 0.3201 1.2651 '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
O1 Cu2 O2 80.46(15) . . ?
O1 Cu2 N3 165.79(17) . . ?
O2 Cu2 N3 97.37(17) . . ?
O1 Cu2 N4 96.50(18) . . ?
O2 Cu2 N4 156.57(17) . . ?
N3 Cu2 N4 79.9(2) . . ?
O1 Cu2 Cl1 98.85(12) . . ?
O2 Cu2 Cl1 99.85(12) . . ?
N3 Cu2 Cl1 95.36(13) . . ?
N4 Cu2 Cl1 103.57(14) . . ?
O1 Cu2 Cu1 40.34(11) . . ?
O2 Cu2 Cu1 41.58(10) . . ?
N3 Cu2 Cu1 138.94(14) . . ?
N4 Cu2 Cu1 135.98(14) . . ?
Cl1 Cu2 Cu1 93.81(5) . . ?
O1 Cu2 Cu2 59.94(11) . 2_556 ?
O2 Cu2 Cu2 27.71(10) . 2_556 ?
N3 Cu2 Cu2 112.77(13) . 2_556 ?
N4 Cu2 Cu2 132.94(13) . 2_556 ?
Cl1 Cu2 Cu2 119.07(5) . 2_556 ?
Cu1 Cu2 Cu2 31.670(16) . 2_556 ?
O1 Cu1 O2 81.07(15) . . ?
O1 Cu1 N1 98.10(18) . . ?
O2 Cu1 N1 177.45(17) . . ?
O1 Cu1 N2 165.58(17) . . ?
O2 Cu1 N2 99.63(18) . . ?
N1 Cu1 N2 80.6(2) . . ?
O1 Cu1 O2 100.24(15) . 2_556 ?
O2 Cu1 O2 84.86(14) . 2_556 ?
N1 Cu1 O2 97.67(16) . 2_556 ?
N2 Cu1 O2 94.17(16) . 2_556 ?
O1 Cu1 Cu2 40.56(11) . . ?
O2 Cu1 Cu2 41.99(11) . . ?
N1 Cu1 Cu2 136.62(14) . . ?
N2 Cu1 Cu2 135.21(14) . . ?
O2 Cu1 Cu2 101.85(9) 2_556 . ?
O1 Cu1 Cu1 91.97(11) . 2_556 ?
O2 Cu1 Cu1 46.87(10) . 2_556 ?
N1 Cu1 Cu1 135.66(13) . 2_556 ?
N2 Cu1 Cu1 99.01(14) . 2_556 ?
O2 Cu1 Cu1 37.99(9) 2_556 2_556 ?
Cu2 Cu1 Cu1 72.01(3) . 2_556 ?
O1 Cu1 Cu2 130.58(11) . 2_556 ?
O2 Cu1 Cu2 90.21(10) . 2_556 ?
N1 Cu1 Cu2 92.15(13) . 2_556 ?
N2 Cu1 Cu2 63.82(12) . 2_556 ?
O2 Cu1 Cu2 30.35(9) 2_556 2_556 ?
Cu2 Cu1 Cu2 122.95(3) . 2_556 ?
Cu1 Cu1 Cu2 50.94(2) 2_556 2_556 ?
Cu1 O1 Cu2 99.10(16) . . ?
Cu1 O1 O2 50.09(12) . . ?
Cu2 O1 O2 50.52(11) . . ?
Cu1 O1 O3 125.90(19) . . ?
Cu2 O1 O3 115.22(17) . . ?
O2 O1 O3 151.26(19) . . ?
Cu1 O1 O2 44.38(10) . 2_556 ?
Cu2 O1 O2 100.89(15) . 2_556 ?
O2 O1 O2 58.45(14) . 2_556 ?
O3 O1 O2 143.83(17) . 2_556 ?
Cu1 O1 O1 38.70(7) . 2_556 ?
Cu2 O1 O1 78.77(12) . 2_556 ?
O2 O1 O1 33.34(9) . 2_556 ?
O3 O1 O1 163.18(18) . 2_556 ?
O2 O1 O1 25.11(7) 2_556 2_556 ?
Cu1 O2 Cu2 96.43(15) . . ?
Cu1 O2 Cu1 95.14(14) . 2_556 ?
Cu2 O2 Cu1 113.19(17) . 2_556 ?
Cu1 O2 O1 48.84(11) . . ?
Cu2 O2 O1 49.02(12) . . ?
Cu1 O2 O1 101.83(16) 2_556 . ?
Cu1 O2 O2 52.88(11) . 2_556 ?
Cu2 O2 O2 113.0(2) . 2_556 ?
Cu1 O2 O2 42.26(9) 2_556 2_556 ?
O1 O2 O2 73.73(16) . 2_556 ?
Cu1 O2 O1 88.41(14) . 2_556 ?
Cu2 O2 O1 148.57(18) . 2_556 ?
Cu1 O2 O1 35.38(8) 2_556 2_556 ?
O1 O2 O1 121.55(14) . 2_556 ?
O2 O2 O1 47.82(12) 2_556 2_556 ?
Cu1 O2 Cl1 90.56(12) . . ?
Cu2 O2 Cl1 46.28(8) . . ?
Cu1 O2 Cl1 159.32(15) 2_556 . ?
O1 O2 Cl1 67.49(11) . . ?
O2 O2 Cl1 139.08(18) 2_556 . ?
O1 O2 Cl1 165.09(15) 2_556 . ?
C1 N1 C5 119.3(5) . . ?
C1 N1 Cu1 125.3(5) . . ?
C5 N1 Cu1 115.4(4) . . ?
C10 N2 C6 117.1(6) . . ?
C10 N2 Cu1 127.3(4) . . ?
C6 N2 Cu1 115.6(4) . . ?
N1 C1 C2 121.3(7) . . ?
C3 C2 C1 119.1(6) . . ?
C2 C3 C4 119.8(7) . . ?
C5 C4 C3 119.0(7) . . ?
N1 C5 C4 121.5(5) . . ?
N1 C5 C6 115.2(5) . . ?
C4 C5 C6 123.2(6) . . ?
C7 C6 N2 122.1(6) . . ?
C7 C6 C5 124.9(6) . . ?
N2 C6 C5 113.0(6) . . ?
C6 C7 C8 119.8(7) . . ?
C9 C8 C7 118.4(7) . . ?
C8 C9 C10 119.8(6) . . ?
N2 C10 C9 122.7(6) . . ?
C15 N3 C11 118.7(5) . . ?
C15 N3 Cu2 116.1(4) . . ?
C11 N3 Cu2 125.2(4) . . ?
C20 N4 C16 117.0(6) . . ?
C20 N4 Cu2 127.5(5) . . ?
C16 N4 Cu2 115.4(4) . . ?
N3 C11 C12 121.6(6) . . ?
C13 C12 C11 119.7(6) . . ?
C12 C13 C14 119.6(6) . . ?
C15 C14 C13 118.2(6) . . ?
N3 C15 C14 122.2(5) . . ?
N3 C15 C16 113.9(5) . . ?
C14 C15 C16 123.9(6) . . ?
N4 C16 C17 122.8(6) . . ?
N4 C16 C15 114.5(6) . . ?
C17 C16 C15 122.7(6) . . ?
C16 C17 C18 118.5(6) . . ?
C19 C18 C17 118.8(7) . . ?
C20 C19 C18 118.6(6) . . ?
N4 C20 C19 124.3(6) . . ?
O4 Cl2 O1 24.26(4) 2 2 ?
O4 Cl2 O5 32.08(4) 2 2_565 ?
O1 Cl2 O5 31.68(3) 2 2_565 ?
O4 Cl2 O2 31.04(3) 2 2 ?
O1 Cl2 O2 12.46(2) 2 2 ?
O5 Cl2 O2 23.68(3) 2_565 2 ?
Cu2 Cl1 O5 111.03(10) . 1_545 ?
Cu2 Cl1 O4 102.05(11) . . ?
O5 Cl1 O4 145.21(13) 1_545 . ?
Cu2 Cl1 O2 33.87(7) . . ?
O5 Cl1 O2 88.79(11) 1_545 . ?
O4 Cl1 O2 125.69(11) . . ?
Cu2 Cl1 O3 72.00(5) . 1_545 ?
O5 Cl1 O3 39.16(10) 1_545 1_545 ?
O4 Cl1 O3 164.95(11) . 1_545 ?
O2 Cl1 O3 56.18(7) . 1_545 ?
O4 O3 O1 101.30(17) . . ?
O4 O3 Cl2 112.31(16) . 1_565 ?
O1 O3 Cl2 131.62(17) . 1_565 ?
O3 O4 O5 155.0(2) . 2_665 ?
O3 O4 Cl1 90.64(15) . . ?
O5 O4 Cl1 113.50(18) 2_665 . ?
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
Cu2 O1 1.935(4) . ?
Cu2 O2 1.978(4) . ?
Cu2 N3 2.018(5) . ?
Cu2 N4 2.022(5) . ?
Cu2 Cl1 2.5650(18) . ?
Cu2 Cu1 2.9382(11) . ?
Cu2 Cu2 5.7525(15) 2_556 ?
Cu1 O1 1.926(4) . ?
Cu1 O2 1.962(4) . ?
Cu1 N1 1.991(5) . ?
Cu1 N2 2.006(5) . ?
Cu1 O2 2.327(4) 2_556 ?
Cu1 Cu1 3.1754(14) 2_556 ?
Cu1 Cu2 3.5992(10) 2_556 ?
O1 O2 2.527(5) . ?
O1 O3 2.931(5) . ?
O1 O2 3.274(5) 2_556 ?
O1 O1 5.076(7) 2_556 ?
O2 Cu1 2.327(4) 2_556 ?
O2 O2 2.906(7) 2_556 ?
O2 O1 3.274(5) 2_556 ?
O2 Cl1 3.497(4) . ?
N1 C1 1.336(7) . ?
N1 C5 1.354(7) . ?
N2 C10 1.353(7) . ?
N2 C6 1.369(7) . ?
C1 C2 1.403(8) . ?
C2 C3 1.358(9) . ?
C3 C4 1.383(8) . ?
C4 C5 1.379(8) . ?
C5 C6 1.471(8) . ?
C6 C7 1.361(8) . ?
C7 C8 1.390(8) . ?
C8 C9 1.364(8) . ?
C9 C10 1.369(8) . ?
N3 C15 1.343(7) . ?
N3 C11 1.357(7) . ?
N4 C20 1.329(7) . ?
N4 C16 1.347(7) . ?
C11 C12 1.376(7) . ?
C12 C13 1.354(8) . ?
C13 C14 1.402(8) . ?
C14 C15 1.380(8) . ?
C15 C16 1.491(8) . ?
C16 C17 1.367(8) . ?
C17 C18 1.396(8) . ?
C18 C19 1.367(9) . ?
C19 C20 1.358(8) . ?
Cl2 O4 8.809(6) 2 ?
Cl2 O1 10.527(4) 2 ?
Cl2 O5 11.280(5) 2_565 ?
Cl2 O2 11.387(4) 2 ?
Cl1 O5 3.141(5) 1_545 ?
Cl1 O4 3.185(5) . ?
Cl1 O3 6.748(4) 1_545 ?
O3 O4 2.751(6) . ?
O3 Cl2 3.124(5) 1_565 ?
O4 O5 2.766(6) 2_665 ?
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 H100 O3 0.997(4) 2.032(4) 2.931(5) 148.9(2) .
O2 H200 Cl2 0.917(4) 2.6223(16) 3.415(4) 145.1(2) .
C7 H7 Cl1 0.93 2.76 3.646(7) 159.2 2_656
C10 H10 Cl2 0.93 2.70 3.490(7) 143.3 .
C11 H11 Cl2 0.93 2.61 3.531(7) 171.4 .
C14 H14 Cl1 0.93 2.80 3.657(7) 153.0 2
C20 H20 O3 0.93 2.52 3.391(8) 155.2 .
|
1100148.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100148.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_1100148
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_publ_section_title
;
Diaquabis(nitrato-O)bis(4,7-dihydro-1,2,4-triazolo
[1,5-a]pyrimidine-7-one-N^3^)copper(II).
;
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m903
_journal_page_last m905
_journal_paper_doi 10.1107/S1600536803019974
_journal_volume 59
_journal_year 2003
_chemical_formula_moiety 'C10 H12 Cu N10 O10'
_chemical_formula_sum 'C10 H12 Cu N10 O10'
_chemical_formula_weight 495.84
_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'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary heavy
_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 14.4717(5)
_cell_length_b 6.4247(2)
_cell_length_c 18.4846(6)
_cell_measurement_reflns_used 40
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 17.6
_cell_measurement_theta_min 12.7
_cell_volume 1718.63(10)
_diffrn_ambient_temperature 295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
;
Scan width (\w) = 1.05 - 1.25, scan ratio 2\q:\w = 1.00
;
_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 0.0205
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 3096
_diffrn_reflns_theta_full 32.45
_diffrn_reflns_theta_max 32.45
_diffrn_reflns_theta_min 2.20
_diffrn_standards_decay_% 4.0
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.355
_exptl_absorpt_correction_T_max 0.7036
_exptl_absorpt_correction_T_min 0.5692
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details 'X-RED (Stoe, 1996)'
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.916
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description brick-shaped
_exptl_crystal_F_000 1004
_exptl_crystal_size_max 0.550
_exptl_crystal_size_mid 0.383
_exptl_crystal_size_min 0.250
_refine_diff_density_max 0.941
_refine_diff_density_min -0.654
_refine_diff_density_rms 0.106
_refine_ls_extinction_coef 0.0078(11)
_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_gt 1.113
_refine_ls_goodness_of_fit_ref 1.082
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 149
_refine_ls_number_reflns 3092
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.088
_refine_ls_restrained_S_gt 1.113
_refine_ls_R_factor_all 0.0802
_refine_ls_R_factor_gt 0.0570
_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^)+(0.0650P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme sigma
_refine_ls_wR_factor_gt 0.1398
_refine_ls_wR_factor_ref 0.1658
_reflns_number_gt 2141
_reflns_number_total 3096
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 2202376
_cod_database_code 1100148
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_group
Cu Cu 0.5000 0.5000 0.5000 0.0276(2) Uani 1 d S .
N1 N 0.5490(2) 0.0712(4) 0.33448(14) 0.0393(6) Uani 1 d . .
C2 C 0.5189(2) 0.1410(5) 0.3969(2) 0.0375(6) Uani 1 d . .
H2 H 0.4894 0.0560 0.4304 0.045 Uiso 1 calc RT .
N3 N 0.5341(2) 0.3490(4) 0.40906(12) 0.0307(5) Uani 1 d . .
C3A C 0.5769(2) 0.4102(4) 0.34914(15) 0.0311(5) Uani 1 d . .
N4 N 0.6091(2) 0.5978(4) 0.3301(2) 0.0415(6) Uani 1 d . .
H4 H 0.6048 0.7019 0.3592 0.050 Uiso 1 calc RT .
C5 C 0.6487(2) 0.6202(6) 0.2636(2) 0.0456(8) Uani 1 d . .
H5 H 0.6712 0.7502 0.2502 0.055 Uiso 1 calc RT .
C6 C 0.6564(3) 0.4609(6) 0.2165(2) 0.0451(7) Uani 1 d . .
H6 H 0.6849 0.4838 0.1721 0.054 Uiso 1 calc RT .
C7 C 0.6220(2) 0.2581(5) 0.2329(2) 0.0354(6) Uani 1 d . .
O7 O 0.6210(2) 0.1020(4) 0.19453(12) 0.0458(6) Uani 1 d . .
N8 N 0.5860(2) 0.2468(4) 0.30352(12) 0.0317(5) Uani 1 d . .
N1N N 0.3085(2) 0.2281(5) 0.5033(2) 0.0455(7) Uani 1 d . .
O1N O 0.3890(2) 0.2359(4) 0.53173(13) 0.0403(5) Uani 1 d . .
O2N O 0.2998(2) 0.2337(6) 0.4369(2) 0.0764(10) Uani 1 d . .
O3N O 0.2405(2) 0.2160(6) 0.5432(2) 0.0724(10) Uani 1 d . .
O1W O 0.59055(15) 0.3231(4) 0.55131(12) 0.0359(5) Uani 1 d D .
H11W H 0.6388(19) 0.2951(66) 0.5275(19) 0.043 Uiso 1 d DT .
H12W H 0.6026(27) 0.3639(60) 0.5942(12) 0.043 Uiso 1 d DT .
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
Cu 0.0306(3) 0.0281(2) 0.0242(2) -0.0024(2) 0.0003(2) 0.0033(2)
N1 0.056(2) 0.0270(11) 0.0348(12) -0.0016(10) 0.0075(11) -0.0019(11)
C2 0.052(2) 0.0283(13) 0.0324(13) 0.0012(11) 0.0044(12) 0.0004(12)
N3 0.0363(11) 0.0272(10) 0.0286(10) -0.0008(8) 0.0026(9) 0.0014(9)
C3A 0.0369(13) 0.0254(11) 0.0311(12) -0.0015(10) -0.0003(10) -0.0006(10)
N4 0.0485(15) 0.0299(12) 0.0462(14) -0.0032(11) 0.0080(12) -0.0062(11)
C5 0.047(2) 0.038(2) 0.052(2) 0.0102(14) 0.0090(15) -0.0041(14)
C6 0.049(2) 0.049(2) 0.037(2) 0.0069(14) 0.0081(14) -0.0034(15)
C7 0.0393(14) 0.040(2) 0.0265(11) 0.0006(11) -0.0001(10) 0.0033(12)
O7 0.063(2) 0.0453(13) 0.0295(10) -0.0071(9) 0.0037(10) 0.0042(12)
N8 0.0403(12) 0.0282(10) 0.0266(10) -0.0017(8) 0.0056(9) 0.0017(10)
N1N 0.0356(13) 0.0348(13) 0.066(2) -0.0082(13) -0.0011(13) -0.0054(11)
O1N 0.0351(10) 0.0405(12) 0.0454(12) -0.0002(10) -0.0016(9) -0.0035(9)
O2N 0.071(2) 0.100(3) 0.058(2) -0.009(2) -0.023(2) -0.006(2)
O3N 0.048(2) 0.085(2) 0.084(2) -0.012(2) 0.015(2) -0.012(2)
O1W 0.0361(10) 0.0394(11) 0.0321(10) -0.0022(9) -0.0018(8) 0.0065(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'
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'
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
O1W Cu N3 87.75(9) . . y
O1W Cu O1N 85.44(9) . . y
N3 Cu O1N 91.59(9) . . y
C2 N1 N8 102.4(2) . . n
N1 C2 N3 115.1(3) . . n
N1 C2 H2 122.5 . . n
N3 C2 H2 122.4 . . n
C3A N3 C2 103.1(2) . . n
C3A N3 Cu 132.2(2) . . n
C2 N3 Cu 124.7(2) . . n
N3 C3A N4 130.4(3) . . n
N3 C3A N8 109.6(2) . . n
N4 C3A N8 120.0(3) . . n
C3A N4 C5 118.6(3) . . n
C3A N4 H4 120.7 . . n
C5 N4 H4 120.7 . . n
C6 C5 N4 122.4(3) . . n
C6 C5 H5 118.7 . . n
N4 C5 H5 118.8 . . n
C5 C6 C7 121.8(3) . . n
C5 C6 H6 119.1 . . n
C7 C6 H6 119.0 . . n
O7 C7 N8 119.3(3) . . n
O7 C7 C6 128.9(3) . . n
N8 C7 C6 111.9(3) . . n
C3A N8 N1 109.9(2) . . n
C3A N8 C7 125.0(3) . . n
N1 N8 C7 125.0(2) . . n
O3N N1N O2N 121.0(3) . . n
O3N N1N O1N 119.0(3) . . n
O2N N1N O1N 120.1(3) . . n
N1N O1N Cu 122.3(2) . . y
Cu O1W H11W 115(3) . . n
Cu O1W H12W 114(3) . . n
H11W O1W H12W 113(4) . . n
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
Cu O1W 1.977(2) . y
Cu N3 2.003(2) . y
Cu O1N 2.410(2) . y
N1 C2 1.312(4) . n
N1 N8 1.374(4) . n
C2 N3 1.373(4) . n
C2 H2 0.9300 . n
N3 C3A 1.328(4) . n
C3A N4 1.339(4) . n
C3A N8 1.353(4) . n
N4 C5 1.364(4) . n
N4 H4 0.8600 . n
C5 C6 1.348(5) . n
C5 H5 0.9300 . n
C6 C7 1.427(5) . n
C6 H6 0.9300 . n
C7 O7 1.228(4) . n
C7 N8 1.408(4) . n
N1N O3N 1.232(4) . n
N1N O2N 1.234(4) . n
N1N O1N 1.278(4) . n
O1W H11W 0.844(18) . n
O1W H12W 0.853(18) . n
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
_geom_hbond_publ_flag
N4 H4 O1N 0.86 2.06 2.769(4) 139.5(2) 5_666 n
O1W H11W O3N 0.84(2) 1.97(2) 2.797(4) 166(3) 4_556 n
O1W H12W O7 0.85(2) 1.89(1) 2.727(3) 168(4) 7_566 n
|
1100149.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100149.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_1100149
loop_
_publ_author_name
'Carballo, Rosa'
'Covelo, Berta'
'Vazquez-Lopez, Ezequiel M.'
'Garcia-Martinez, Emilia'
_publ_section_title
;
Unexpected formation and crystal structures of the mixed ligand
complexes [Cu(OAc)(bipy)2]Cl.4H2O.1/2MeOH and [Co(OH2)2(phen)2](AcO)2.
6H2O
;
_journal_name_full 'Z. Anorg. Allg. Chem.'
_journal_page_first 244
_journal_page_last 248
_journal_paper_doi 10.1002/zaac.200390039
_journal_volume 629
_journal_year 2003
_chemical_formula_sum 'C28 H38 Co N4 O12'
_chemical_formula_weight 681.55
_chemical_name_systematic
;
Diaqua-bis(1,10-phenanthroline-N,N')cobalt(II) acetate hexahydrate
;
_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 108.097(4)
_cell_angle_beta 94.267(5)
_cell_angle_gamma 110.194(4)
_cell_formula_units_Z 2
_cell_length_a 9.5560(17)
_cell_length_b 13.408(3)
_cell_length_c 14.480(3)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1620.4(6)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.825
_diffrn_measured_fraction_theta_max 0.825
_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 0.0479
_diffrn_reflns_av_sigmaI/netI 0.2258
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 9185
_diffrn_reflns_theta_full 27.98
_diffrn_reflns_theta_max 27.98
_diffrn_reflns_theta_min 1.51
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.595
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8607
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour orange
_exptl_crystal_density_diffrn 1.397
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 714
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.11
_refine_diff_density_max 0.274
_refine_diff_density_min -0.218
_refine_diff_density_rms 0.052
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.724
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 424
_refine_ls_number_reflns 6450
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.724
_refine_ls_R_factor_all 0.1578
_refine_ls_R_factor_gt 0.0503
_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^)+(0.0163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0736
_refine_ls_wR_factor_ref 0.0923
_reflns_number_gt 2446
_reflns_number_total 6450
_reflns_threshold_expression >2sigma(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.
'_exptl_absorpt_correction_type' value 'MULTISCAN' changed to
'multi-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 P-1
_cod_database_code 1100149
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
Co Co 0.77190(7) -0.03302(6) 0.24906(5) 0.03610(18) Uani 1 1 d . . .
N4 N 0.6526(4) -0.0751(3) 0.1011(2) 0.0380(9) Uani 1 1 d . . .
N1 N 0.6917(4) 0.1022(3) 0.3145(2) 0.0395(10) Uani 1 1 d . . .
N2 N 0.5756(4) -0.1186(3) 0.3001(2) 0.0366(9) Uani 1 1 d . . .
N3 N 0.9360(4) 0.0768(3) 0.1966(3) 0.0393(10) Uani 1 1 d . . .
C5 C 0.5606(5) 0.0659(4) 0.3481(3) 0.0356(11) Uani 1 1 d . . .
C20 C 0.5397(7) -0.1138(5) -0.0956(4) 0.0672(17) Uani 1 1 d . . .
H20 H 0.5005 -0.1269 -0.1610 0.081 Uiso 1 1 calc R . .
C6 C 0.4987(5) -0.0518(4) 0.3417(3) 0.0375(12) Uani 1 1 d . . .
C18 C 0.7384(5) -0.0137(4) 0.0509(3) 0.0396(12) Uani 1 1 d . . .
C17 C 0.8896(5) 0.0684(4) 0.1026(4) 0.0408(12) Uani 1 1 d . . .
C23 C 0.9240(7) 0.1199(5) -0.0447(4) 0.0720(18) Uani 1 1 d . . .
H23 H 0.9842 0.1644 -0.0761 0.086 Uiso 1 1 calc R . .
C10 C 0.5218(5) -0.2252(4) 0.2986(3) 0.0493(13) Uani 1 1 d . . .
H10 H 0.5729 -0.2715 0.2714 0.059 Uiso 1 1 calc R . .
C14 C 1.1729(6) 0.2210(4) 0.2035(5) 0.0674(17) Uani 1 1 d . . .
H14 H 1.2698 0.2716 0.2396 0.081 Uiso 1 1 calc R . .
C4 C 0.4861(6) 0.1372(5) 0.3886(3) 0.0490(13) Uani 1 1 d . . .
C16 C 0.9805(6) 0.1352(4) 0.0552(4) 0.0529(14) Uani 1 1 d . . .
C13 C 1.0752(5) 0.1518(4) 0.2453(4) 0.0536(14) Uani 1 1 d . . .
H13 H 1.1083 0.1581 0.3096 0.064 Uiso 1 1 calc R . .
C24 C 0.7849(7) 0.0417(5) -0.0935(4) 0.0720(18) Uani 1 1 d . . .
H24 H 0.7519 0.0330 -0.1586 0.086 Uiso 1 1 calc R . .
C1 C 0.7496(5) 0.2100(4) 0.3205(3) 0.0517(14) Uani 1 1 d . . .
H1 H 0.8391 0.2358 0.2979 0.062 Uiso 1 1 calc R . .
C3 C 0.5492(6) 0.2510(5) 0.3930(4) 0.0649(16) Uani 1 1 d . . .
H3 H 0.5020 0.3008 0.4181 0.078 Uiso 1 1 calc R . .
C9 C 0.3939(5) -0.2713(4) 0.3352(3) 0.0578(15) Uani 1 1 d . . .
H9 H 0.3623 -0.3460 0.3330 0.069 Uiso 1 1 calc R . .
C22 C 0.5170(5) -0.1539(4) 0.0534(3) 0.0520(14) Uani 1 1 d . . .
H22 H 0.4589 -0.1963 0.0871 0.062 Uiso 1 1 calc R . .
C2 C 0.6803(6) 0.2862(4) 0.3599(4) 0.0630(15) Uani 1 1 d . . .
H2 H 0.7244 0.3612 0.3633 0.076 Uiso 1 1 calc R . .
C19 C 0.6841(7) -0.0298(5) -0.0491(4) 0.0554(15) Uani 1 1 d . . .
C7 C 0.3668(5) -0.0933(5) 0.3786(3) 0.0472(13) Uani 1 1 d . . .
C15 C 1.1263(6) 0.2148(5) 0.1089(5) 0.0681(18) Uani 1 1 d . . .
H15 H 1.1899 0.2622 0.0810 0.082 Uiso 1 1 calc R . .
C21 C 0.4553(6) -0.1770(5) -0.0469(4) 0.0622(15) Uani 1 1 d . . .
H21 H 0.3597 -0.2338 -0.0784 0.075 Uiso 1 1 calc R . .
C8 C 0.3154(5) -0.2063(5) 0.3744(4) 0.0618(16) Uani 1 1 d . . .
H8 H 0.2288 -0.2364 0.3981 0.074 Uiso 1 1 calc R . .
C11 C 0.3480(6) 0.0922(5) 0.4234(4) 0.0628(16) Uani 1 1 d . . .
H11 H 0.2967 0.1387 0.4494 0.075 Uiso 1 1 calc R . .
C12 C 0.2938(6) -0.0167(5) 0.4182(4) 0.0672(17) Uani 1 1 d . . .
H12 H 0.2052 -0.0435 0.4413 0.081 Uiso 1 1 calc R . .
O6 O 0.2053(4) 0.4867(3) 0.1311(3) 0.0735(11) Uani 1 1 d . . .
O5 O 0.3179(4) 0.5635(3) 0.0275(2) 0.0740(11) Uani 1 1 d . . .
O2 O 0.8217(3) -0.1763(3) 0.1921(2) 0.0449(8) Uani 1 1 d . . .
O1 O 0.9217(3) 0.0038(3) 0.3781(2) 0.0530(9) Uani 1 1 d . . .
C28 C 0.1331(5) 0.6273(4) 0.0989(4) 0.0709(16) Uani 1 1 d . . .
H28A H 0.1979 0.7045 0.1388 0.106 Uiso 1 1 calc R . .
H28B H 0.0518 0.5998 0.1312 0.106 Uiso 1 1 calc R . .
H28C H 0.0914 0.6243 0.0352 0.106 Uiso 1 1 calc R . .
O4 O 0.8705(4) 0.7069(3) 0.2989(2) 0.0719(11) Uani 1 1 d . . .
O3 O 0.9167(4) 0.8385(3) 0.4441(2) 0.0666(10) Uani 1 1 d . . .
C25 C 0.8827(5) 0.7382(5) 0.3913(4) 0.0467(13) Uani 1 1 d . . .
C27 C 0.2260(5) 0.5526(4) 0.0851(4) 0.0507(14) Uani 1 1 d . . .
C26 C 0.8579(6) 0.6507(4) 0.4366(4) 0.101(2) Uani 1 1 d . . .
H26A H 0.7510 0.6048 0.4231 0.151 Uiso 1 1 calc R . .
H26B H 0.8950 0.6869 0.5070 0.151 Uiso 1 1 calc R . .
H26C H 0.9114 0.6033 0.4091 0.151 Uiso 1 1 calc R . .
O1W O 0.7346(4) 0.4791(3) 0.1765(3) 0.0637(10) Uani 1 1 d . . .
O2W O 0.3672(4) 0.3546(3) 0.9685(3) 0.0656(10) Uani 1 1 d . . .
O3W O 0.4551(4) 0.4764(3) 0.2398(2) 0.0798(12) Uani 1 1 d . . .
O4W O 0.9616(4) 0.4021(3) 0.2231(3) 0.0813(12) Uani 1 1 d . . .
O5W O 0.3886(4) 0.4740(3) 0.4233(3) 0.0903(13) Uani 1 1 d . . .
O6W O 0.0997(4) 0.4950(4) 0.4248(3) 0.1195(18) Uani 1 1 d . . .
H2B H 0.7496 -0.2397 0.1394 0.020(11) Uiso 1 1 d . . .
H1A H 0.9723 0.0642 0.4248 0.07(2) Uiso 1 1 d . . .
H2A H 0.8478 -0.2046 0.2455 0.15(3) Uiso 1 1 d . . .
H1B H 0.9249 -0.0439 0.4064 0.14(3) Uiso 1 1 d . . .
H310 H 0.5330 0.4763 0.2056 0.13(2) Uiso 1 1 d . . .
H320 H 0.3629 0.4455 0.1860 0.13(2) Uiso 1 1 d . . .
H410 H 0.9033 0.4569 0.2177 0.12(2) Uiso 1 1 d . . .
H510 H 0.4083 0.4733 0.3643 0.09(2) Uiso 1 1 d . . .
H420 H 1.0076 0.4066 0.1708 0.11(2) Uiso 1 1 d . . .
H520 H 0.3080 0.4956 0.4187 0.13(3) Uiso 1 1 d . . .
H120 H 0.7230 0.4734 0.1166 0.15(3) Uiso 1 1 d . . .
H610 H 0.0588 0.5249 0.4551 0.49(10) Uiso 1 1 d . . .
H620 H 0.0574 0.4656 0.3594 0.08(2) Uiso 1 1 d . . .
H210 H 0.4657 0.3801 0.9697 0.14(3) Uiso 1 1 d . . .
H220 H 0.3642 0.4159 1.0083 0.15(3) Uiso 1 1 d . . .
H110 H 0.7774 0.5515 0.2155 0.12(3) 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
Co 0.0403(4) 0.0363(4) 0.0331(4) 0.0140(3) 0.0100(3) 0.0147(3)
N4 0.042(2) 0.038(3) 0.037(2) 0.015(2) 0.006(2) 0.020(2)
N1 0.044(2) 0.042(3) 0.035(2) 0.016(2) 0.0113(19) 0.017(2)
N2 0.042(2) 0.031(2) 0.035(2) 0.010(2) 0.0072(19) 0.013(2)
N3 0.046(2) 0.031(3) 0.038(3) 0.009(2) 0.012(2) 0.015(2)
C5 0.041(3) 0.042(3) 0.026(3) 0.010(3) 0.006(2) 0.021(3)
C20 0.086(5) 0.085(5) 0.038(3) 0.010(4) 0.005(3) 0.055(4)
C6 0.035(3) 0.052(4) 0.024(3) 0.013(3) 0.004(2) 0.017(3)
C18 0.058(3) 0.042(3) 0.037(3) 0.018(3) 0.021(3) 0.036(3)
C17 0.049(3) 0.043(3) 0.050(3) 0.023(3) 0.031(3) 0.031(3)
C23 0.106(5) 0.078(5) 0.078(5) 0.052(4) 0.060(4) 0.061(4)
C10 0.054(3) 0.047(4) 0.048(3) 0.020(3) 0.015(3) 0.018(3)
C14 0.051(3) 0.044(4) 0.105(5) 0.024(4) 0.039(4) 0.013(3)
C4 0.059(4) 0.066(4) 0.035(3) 0.014(3) 0.012(3) 0.042(3)
C16 0.066(4) 0.049(4) 0.072(4) 0.036(4) 0.043(3) 0.036(3)
C13 0.046(3) 0.041(3) 0.062(4) 0.012(3) 0.016(3) 0.008(3)
C24 0.121(5) 0.099(6) 0.045(4) 0.046(4) 0.043(4) 0.077(5)
C1 0.056(3) 0.044(4) 0.057(4) 0.018(3) 0.015(3) 0.021(3)
C3 0.081(4) 0.065(4) 0.061(4) 0.013(4) 0.014(3) 0.051(4)
C9 0.060(4) 0.047(4) 0.055(4) 0.022(3) 0.016(3) 0.004(3)
C22 0.053(3) 0.046(4) 0.048(4) 0.008(3) 0.001(3) 0.018(3)
C2 0.075(4) 0.044(4) 0.067(4) 0.010(3) 0.009(3) 0.030(4)
C19 0.087(4) 0.071(4) 0.043(3) 0.030(3) 0.027(3) 0.060(4)
C7 0.038(3) 0.063(4) 0.042(3) 0.019(3) 0.016(2) 0.020(3)
C15 0.075(4) 0.050(4) 0.110(5) 0.047(4) 0.065(4) 0.035(4)
C21 0.065(4) 0.057(4) 0.051(4) -0.001(3) -0.007(3) 0.029(3)
C8 0.049(3) 0.075(5) 0.059(4) 0.032(4) 0.020(3) 0.012(4)
C11 0.062(4) 0.089(5) 0.052(4) 0.019(4) 0.020(3) 0.051(4)
C12 0.052(4) 0.096(5) 0.069(4) 0.034(4) 0.027(3) 0.040(4)
O6 0.075(3) 0.075(3) 0.094(3) 0.046(3) 0.024(2) 0.041(2)
O5 0.066(2) 0.101(3) 0.059(2) 0.030(2) 0.024(2) 0.034(2)
O2 0.055(2) 0.038(2) 0.040(2) 0.009(2) 0.0059(18) 0.021(2)
O1 0.068(2) 0.044(2) 0.037(2) 0.011(2) -0.0045(19) 0.016(2)
C28 0.067(4) 0.066(4) 0.083(4) 0.024(4) 0.010(3) 0.033(4)
O4 0.118(3) 0.058(3) 0.050(2) 0.022(2) 0.016(2) 0.044(2)
O3 0.093(3) 0.040(2) 0.052(2) 0.009(2) -0.002(2) 0.020(2)
C25 0.054(3) 0.046(4) 0.044(4) 0.019(3) 0.014(3) 0.020(3)
C27 0.043(3) 0.045(4) 0.046(3) 0.002(3) -0.004(3) 0.012(3)
C26 0.169(6) 0.076(5) 0.088(5) 0.050(4) 0.045(4) 0.062(5)
O1W 0.070(2) 0.063(3) 0.060(3) 0.020(2) 0.0144(19) 0.029(2)
O2W 0.063(3) 0.045(2) 0.067(3) 0.001(2) 0.0045(19) 0.014(2)
O3W 0.060(2) 0.119(4) 0.057(2) 0.035(3) 0.016(2) 0.026(2)
O4W 0.101(3) 0.102(3) 0.078(3) 0.052(3) 0.037(2) 0.063(3)
O5W 0.091(3) 0.145(4) 0.057(3) 0.040(3) 0.026(2) 0.066(3)
O6W 0.109(3) 0.205(6) 0.071(3) 0.056(3) 0.025(3) 0.085(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co 0.3494 0.9721 '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
O2 Co O1 85.72(13) . . ?
O2 Co N3 97.98(12) . . ?
O1 Co N3 94.15(14) . . ?
O2 Co N2 94.49(13) . . ?
O1 Co N2 93.20(12) . . ?
N3 Co N2 165.95(13) . . ?
O2 Co N4 87.04(13) . . ?
O1 Co N4 168.69(12) . . ?
N3 Co N4 78.27(14) . . ?
N2 Co N4 96.02(13) . . ?
O2 Co N1 171.91(13) . . ?
O1 Co N1 94.91(13) . . ?
N3 Co N1 90.02(13) . . ?
N2 Co N1 77.42(14) . . ?
N4 Co N1 93.48(12) . . ?
C22 N4 C18 118.2(4) . . ?
C22 N4 Co 129.1(3) . . ?
C18 N4 Co 112.5(3) . . ?
C1 N1 C5 118.1(4) . . ?
C1 N1 Co 128.5(3) . . ?
C5 N1 Co 113.3(3) . . ?
C10 N2 C6 116.7(4) . . ?
C10 N2 Co 129.0(3) . . ?
C6 N2 Co 114.3(3) . . ?
C13 N3 C17 118.0(4) . . ?
C13 N3 Co 127.5(3) . . ?
C17 N3 Co 114.4(3) . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 C6 117.7(4) . . ?
C4 C5 C6 119.5(4) . . ?
C21 C20 C19 121.0(5) . . ?
N2 C6 C7 122.5(4) . . ?
N2 C6 C5 117.1(4) . . ?
C7 C6 C5 120.4(4) . . ?
N4 C18 C19 122.2(5) . . ?
N4 C18 C17 117.5(4) . . ?
C19 C18 C17 120.2(5) . . ?
N3 C17 C16 123.1(5) . . ?
N3 C17 C18 117.2(4) . . ?
C16 C17 C18 119.7(5) . . ?
C24 C23 C16 120.5(5) . . ?
N2 C10 C9 124.0(5) . . ?
C15 C14 C13 120.1(5) . . ?
C5 C4 C3 117.9(5) . . ?
C5 C4 C11 119.3(5) . . ?
C3 C4 C11 122.8(5) . . ?
C17 C16 C15 117.6(5) . . ?
C17 C16 C23 119.7(5) . . ?
C15 C16 C23 122.7(5) . . ?
N3 C13 C14 122.5(5) . . ?
C23 C24 C19 122.9(5) . . ?
N1 C1 C2 122.2(4) . . ?
C2 C3 C4 118.7(5) . . ?
C8 C9 C10 119.5(5) . . ?
N4 C22 C21 123.2(5) . . ?
C3 C2 C1 120.4(5) . . ?
C20 C19 C18 117.0(5) . . ?
C20 C19 C24 126.1(5) . . ?
C18 C19 C24 116.9(5) . . ?
C8 C7 C6 118.1(5) . . ?
C8 C7 C12 124.3(5) . . ?
C6 C7 C12 117.6(5) . . ?
C14 C15 C16 118.6(5) . . ?
C20 C21 C22 118.3(5) . . ?
C9 C8 C7 119.2(5) . . ?
C12 C11 C4 120.2(5) . . ?
C11 C12 C7 122.9(5) . . ?
O3 C25 O4 122.4(5) . . ?
O3 C25 C26 120.0(5) . . ?
O4 C25 C26 117.6(5) . . ?
O6 C27 O5 125.2(5) . . ?
O6 C27 C28 117.8(5) . . ?
O5 C27 C28 117.0(5) . . ?
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
Co O2 2.074(3) . ?
Co O1 2.080(3) . ?
Co N3 2.118(3) . ?
Co N2 2.151(3) . ?
Co N4 2.157(3) . ?
Co N1 2.184(4) . ?
N4 C22 1.319(5) . ?
N4 C18 1.369(5) . ?
N1 C1 1.328(5) . ?
N1 C5 1.364(4) . ?
N2 C10 1.334(5) . ?
N2 C6 1.374(5) . ?
N3 C13 1.332(5) . ?
N3 C17 1.357(5) . ?
C5 C4 1.397(5) . ?
C5 C6 1.450(5) . ?
C20 C21 1.360(6) . ?
C20 C19 1.394(6) . ?
C6 C7 1.410(5) . ?
C18 C19 1.425(5) . ?
C18 C17 1.445(5) . ?
C17 C16 1.401(5) . ?
C23 C24 1.343(6) . ?
C23 C16 1.431(6) . ?
C10 C9 1.391(5) . ?
C14 C15 1.376(6) . ?
C14 C13 1.390(6) . ?
C4 C3 1.412(6) . ?
C4 C11 1.448(6) . ?
C16 C15 1.408(6) . ?
C24 C19 1.447(6) . ?
C1 C2 1.403(6) . ?
C3 C2 1.358(6) . ?
C9 C8 1.361(6) . ?
C22 C21 1.421(6) . ?
C7 C8 1.401(6) . ?
C7 C12 1.434(6) . ?
C11 C12 1.345(6) . ?
O6 C27 1.236(5) . ?
O5 C27 1.259(5) . ?
C28 C27 1.532(6) . ?
O4 C25 1.254(5) . ?
O3 C25 1.233(5) . ?
C25 C26 1.475(6) . ?
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
O2 H2B O2W 0.945(3) 1.766(4) 2.706(5) 172.5(2) 2_656
O1 H1A O3 0.829(4) 1.907(3) 2.694(5) 157.9(2) 2_766
O2 H2A O4 1.012(3) 1.666(3) 2.639(4) 159.9(2) 1_545
O1 H1B O3 0.868(3) 1.802(3) 2.661(4) 170.1(3) 1_545
O3W H310 O1W 0.924(3) 1.992(3) 2.879(4) 160.2(2) .
O3W H320 O6 1.001(3) 1.969(3) 2.829(4) 142.5(2) .
O4W H410 O1W 1.080(3) 1.829(3) 2.826(4) 151.7(2) .
O5W H510 O3W 0.886(3) 1.898(3) 2.784(5) 178.3(3) .
O4W H420 O6 0.911(4) 2.048(3) 2.839(5) 144.4(2) 1_655
O5W H520 O6W 0.917(4) 1.996(4) 2.872(5) 159.1(3) .
O1W H120 O5 0.842(4) 1.963(3) 2.800(5) 171.8(3) 2_665
O6W H610 O6W 0.728(5) 2.407(4) 3.001(9) 140.0(2) 2_566
O6W H620 O4W 0.904(4) 1.900(3) 2.803(5) 178.0(3) 1_455
O2W H210 O5 0.880(4) 1.933(3) 2.813(5) 179.8(2) 2_666
O2W H220 O5 0.856(4) 2.114(3) 2.878(5) 148.2(2) 1_556
O2W H220 O6 0.856(4) 2.592(3) 3.305(5) 141.4(3) 1_556
C23 H23 O2 0.93 2.59 3.395(6) 145.2 2_755
O1W H110 O4 0.882(4) 1.894(3) 2.776(5) 179.6(2) .
|
1100150.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100150.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_1100150
loop_
_publ_author_name
'Carballo, Rosa'
'Covelo, Berta'
'Vazquez-Lopez, Ezequiel M.'
'Garcia-Martinez, Emilia'
_publ_section_title
;
Unexpected formation and crystal structures of the mixed ligand
complexes [Cu(OAc)(bipy)2]Cl.4H2O.1/2MeOH and [Co(OH2)2(phen)2](AcO)2.
6H2O
;
_journal_name_full 'Z. Anorg. Allg. Chem.'
_journal_page_first 244
_journal_page_last 248
_journal_paper_doi 10.1002/zaac.200390039
_journal_volume 629
_journal_year 2003
_chemical_formula_sum 'C22.5 H29 Cl Cu N4 O6.5'
_chemical_formula_weight 558.49
_chemical_name_systematic
;
(Acetato-O)-bis(2,2'-bipyridine-N,N')copper(II) chloride
tetrahydrate methanol hemisolvate
;
_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 96.512(2)
_cell_angle_beta 104.786(2)
_cell_angle_gamma 92.260(2)
_cell_formula_units_Z 2
_cell_length_a 8.8328(8)
_cell_length_b 10.5365(10)
_cell_length_c 14.4604(14)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1289.5(2)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_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 0.0452
_diffrn_reflns_av_sigmaI/netI 0.0641
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 7881
_diffrn_reflns_theta_full 28.04
_diffrn_reflns_theta_max 28.04
_diffrn_reflns_theta_min 1.47
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.996
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8284
_exptl_absorpt_correction_type SADABS
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.438
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 580
_exptl_crystal_size_max .38
_exptl_crystal_size_mid .34
_exptl_crystal_size_min .17
_refine_diff_density_max 1.126
_refine_diff_density_min -0.770
_refine_diff_density_rms 0.093
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.016
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 322
_refine_ls_number_reflns 5513
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.016
_refine_ls_R_factor_all 0.0812
_refine_ls_R_factor_gt 0.0611
_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^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1712
_refine_ls_wR_factor_ref 0.1822
_reflns_number_gt 3912
_reflns_number_total 5513
_reflns_threshold_expression >2sigma(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
;
_cod_original_sg_symbol_H-M P-1
_cod_original_formula_sum 'C22.50 H29 Cl Cu N4 O6.50'
_cod_database_code 1100150
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
Cu Cu 0.97199(6) 0.51543(4) 0.25564(3) 0.04067(18) Uani 1 1 d . . .
N1 N 0.9850(4) 0.3746(3) 0.1513(2) 0.0437(7) Uani 1 1 d . . .
N2 N 0.8033(4) 0.5710(3) 0.1282(2) 0.0445(8) Uani 1 1 d . . .
C1 C 1.0791(5) 0.2778(4) 0.1673(3) 0.0518(10) Uani 1 1 d . . .
H1 H 1.1355 0.2715 0.2302 0.062 Uiso 1 1 calc R . .
C2 C 1.0953(6) 0.1883(4) 0.0949(4) 0.0614(12) Uani 1 1 d . . .
H2 H 1.1620 0.1228 0.1083 0.074 Uiso 1 1 calc R . .
C3 C 1.0116(6) 0.1969(4) 0.0021(4) 0.0607(12) Uani 1 1 d . . .
H3 H 1.0206 0.1371 -0.0483 0.073 Uiso 1 1 calc R . .
C4 C 0.9146(6) 0.2947(4) -0.0153(3) 0.0533(10) Uani 1 1 d . . .
H4 H 0.8572 0.3015 -0.0779 0.064 Uiso 1 1 calc R . .
C5 C 0.9020(5) 0.3830(4) 0.0600(3) 0.0411(8) Uani 1 1 d . . .
C6 C 0.8007(5) 0.4912(4) 0.0475(3) 0.0427(9) Uani 1 1 d . . .
C7 C 0.7068(6) 0.5132(5) -0.0412(3) 0.0577(11) Uani 1 1 d . . .
H7 H 0.7068 0.4592 -0.0967 0.069 Uiso 1 1 calc R . .
C8 C 0.6141(6) 0.6146(6) -0.0466(4) 0.0719(14) Uani 1 1 d . . .
H8 H 0.5507 0.6299 -0.1057 0.086 Uiso 1 1 calc R . .
C9 C 0.6158(6) 0.6948(5) 0.0375(4) 0.0676(14) Uani 1 1 d . . .
H9 H 0.5521 0.7631 0.0358 0.081 Uiso 1 1 calc R . .
C10 C 0.7139(5) 0.6702(4) 0.1227(4) 0.0547(11) Uani 1 1 d . . .
H10 H 0.7180 0.7248 0.1787 0.066 Uiso 1 1 calc R . .
N3 N 0.9647(4) 0.6378(3) 0.3707(2) 0.0441(8) Uani 1 1 d . . .
N4 N 0.8150(4) 0.4155(3) 0.3049(2) 0.0416(7) Uani 1 1 d . . .
C11 C 1.0503(6) 0.7510(4) 0.3998(4) 0.0594(12) Uani 1 1 d . . .
H11 H 1.1119 0.7794 0.3618 0.071 Uiso 1 1 calc R . .
C12 C 1.0488(7) 0.8250(4) 0.4836(4) 0.0713(15) Uani 1 1 d . . .
H12 H 1.1080 0.9030 0.5018 0.086 Uiso 1 1 calc R . .
C13 C 0.9591(7) 0.7831(5) 0.5405(4) 0.0687(14) Uani 1 1 d . . .
H13 H 0.9592 0.8316 0.5984 0.082 Uiso 1 1 calc R . .
C14 C 0.8678(6) 0.6672(4) 0.5109(3) 0.0584(12) Uani 1 1 d . . .
H14 H 0.8042 0.6382 0.5475 0.070 Uiso 1 1 calc R . .
C15 C 0.8749(5) 0.5969(4) 0.4256(3) 0.0417(9) Uani 1 1 d . . .
C16 C 0.7876(5) 0.4732(4) 0.3871(3) 0.0422(9) Uani 1 1 d . . .
C17 C 0.6784(6) 0.4182(5) 0.4271(3) 0.0563(11) Uani 1 1 d . . .
H17 H 0.6619 0.4580 0.4841 0.068 Uiso 1 1 calc R . .
C18 C 0.5937(6) 0.3049(5) 0.3829(4) 0.0661(13) Uani 1 1 d . . .
H18 H 0.5190 0.2679 0.4088 0.079 Uiso 1 1 calc R . .
C19 C 0.6234(6) 0.2486(5) 0.2996(4) 0.0651(13) Uani 1 1 d . . .
H19 H 0.5692 0.1717 0.2685 0.078 Uiso 1 1 calc R . .
C20 C 0.7335(5) 0.3058(4) 0.2620(3) 0.0524(10) Uani 1 1 d . . .
H20 H 0.7514 0.2669 0.2051 0.063 Uiso 1 1 calc R . .
O1 O 1.1598(3) 0.6092(3) 0.2398(2) 0.0541(7) Uani 1 1 d . . .
O2 O 1.2801(4) 0.4855(3) 0.3440(2) 0.0656(9) Uani 1 1 d . . .
C21 C 1.2826(5) 0.5727(4) 0.2952(3) 0.0491(10) Uani 1 1 d . . .
C22 C 1.4349(6) 0.6474(6) 0.3003(5) 0.0818(17) Uani 1 1 d . . .
H22A H 1.4147 0.7123 0.2580 0.123 Uiso 1 1 calc R . .
H22B H 1.5065 0.5904 0.2809 0.123 Uiso 1 1 calc R . .
H22C H 1.4803 0.6870 0.3653 0.123 Uiso 1 1 calc R . .
Cl Cl 1.41041(18) 0.94836(16) 0.14508(11) 0.0850(4) Uani 1 1 d . . .
O3 O 0.6923(5) 0.9061(4) 0.3277(3) 0.0981(13) Uani 1 1 d . . .
O4 O 1.9181(6) 0.9976(5) 0.2423(4) 0.1106(16) Uani 1 1 d . . .
O5 O 0.6973(5) 0.0694(4) 0.0846(3) 0.0960(13) Uani 1 1 d . . .
O6 O 0.2396(8) 0.0172(8) 0.3040(5) 0.172(3) Uani 1 1 d . . .
C71 C 0.5000 0.0000 0.5000 0.124(4) Uani 1 2 d S . .
O7 O 0.3776(12) 0.0771(13) 0.4936(8) 0.128(4) Uani 0.50 1 d P . .
H70 H 0.3271 0.0730 0.4371 0.192 Uiso 0.50 1 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
Cu 0.0441(3) 0.0455(3) 0.0330(3) 0.00375(19) 0.0120(2) 0.0012(2)
N1 0.0473(19) 0.0475(17) 0.0392(18) 0.0076(14) 0.0157(15) 0.0046(15)
N2 0.0462(18) 0.0505(18) 0.0400(18) 0.0062(15) 0.0167(15) 0.0047(15)
C1 0.055(3) 0.052(2) 0.052(3) 0.013(2) 0.017(2) 0.009(2)
C2 0.069(3) 0.048(2) 0.075(3) 0.009(2) 0.031(3) 0.012(2)
C3 0.075(3) 0.050(2) 0.059(3) -0.009(2) 0.029(3) -0.001(2)
C4 0.061(3) 0.057(2) 0.041(2) -0.002(2) 0.019(2) -0.004(2)
C5 0.044(2) 0.0451(19) 0.037(2) 0.0030(16) 0.0160(17) -0.0035(16)
C6 0.040(2) 0.055(2) 0.0348(19) 0.0071(17) 0.0125(17) -0.0032(17)
C7 0.059(3) 0.073(3) 0.039(2) 0.009(2) 0.007(2) 0.002(2)
C8 0.056(3) 0.095(4) 0.064(3) 0.035(3) 0.004(3) 0.013(3)
C9 0.060(3) 0.065(3) 0.085(4) 0.028(3) 0.021(3) 0.024(2)
C10 0.055(3) 0.052(2) 0.062(3) 0.009(2) 0.022(2) 0.011(2)
N3 0.0443(18) 0.0428(17) 0.0420(18) -0.0006(15) 0.0083(15) 0.0022(14)
N4 0.0444(18) 0.0453(17) 0.0333(16) 0.0030(14) 0.0084(14) -0.0005(14)
C11 0.063(3) 0.048(2) 0.065(3) 0.004(2) 0.016(2) 0.002(2)
C12 0.080(4) 0.044(2) 0.074(4) -0.012(2) -0.001(3) 0.006(2)
C13 0.088(4) 0.062(3) 0.047(3) -0.010(2) 0.007(3) 0.017(3)
C14 0.076(3) 0.062(3) 0.039(2) 0.004(2) 0.017(2) 0.020(2)
C15 0.046(2) 0.046(2) 0.0298(18) 0.0023(16) 0.0043(17) 0.0113(17)
C16 0.042(2) 0.054(2) 0.0321(19) 0.0098(17) 0.0092(16) 0.0099(17)
C17 0.062(3) 0.069(3) 0.048(2) 0.011(2) 0.029(2) 0.011(2)
C18 0.061(3) 0.077(3) 0.068(3) 0.012(3) 0.031(3) -0.005(2)
C19 0.060(3) 0.060(3) 0.069(3) 0.007(2) 0.009(3) -0.015(2)
C20 0.056(3) 0.054(2) 0.044(2) 0.000(2) 0.013(2) -0.004(2)
O1 0.0497(17) 0.0678(19) 0.0455(16) 0.0128(15) 0.0121(14) 0.0001(14)
O2 0.075(2) 0.076(2) 0.0479(18) 0.0159(17) 0.0171(17) 0.0003(18)
C21 0.051(2) 0.060(2) 0.037(2) 0.003(2) 0.0152(19) 0.000(2)
C22 0.050(3) 0.107(4) 0.084(4) 0.027(4) 0.007(3) -0.014(3)
Cl 0.0760(9) 0.1021(11) 0.0744(9) 0.0003(8) 0.0207(8) 0.0004(8)
O3 0.089(3) 0.109(3) 0.098(3) 0.027(3) 0.021(3) 0.000(3)
O4 0.091(3) 0.129(4) 0.112(4) 0.023(3) 0.027(3) -0.004(3)
O5 0.089(3) 0.115(3) 0.075(3) 0.000(2) 0.016(2) -0.021(3)
O6 0.132(5) 0.270(9) 0.120(5) 0.047(6) 0.036(4) 0.023(6)
C71 0.138(11) 0.164(11) 0.065(6) 0.046(7) 0.009(7) -0.030(9)
O7 0.093(7) 0.217(13) 0.089(7) 0.036(8) 0.034(6) 0.067(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'
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'
Cu Cu 0.3201 1.2651 '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
O1 Cu N3 92.28(13) . . ?
O1 Cu N1 90.88(13) . . ?
N3 Cu N1 172.56(13) . . ?
O1 Cu N4 165.63(12) . . ?
N3 Cu N4 80.36(13) . . ?
N1 Cu N4 95.07(13) . . ?
O1 Cu N2 97.05(12) . . ?
N3 Cu N2 108.17(13) . . ?
N1 Cu N2 78.08(13) . . ?
N4 Cu N2 96.97(13) . . ?
O1 Cu O2 52.56(11) . . ?
N3 Cu O2 88.50(12) . . ?
N1 Cu O2 88.08(12) . . ?
N4 Cu O2 114.49(12) . . ?
N2 Cu O2 146.70(11) . . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Cu 123.3(3) . . ?
C5 N1 Cu 118.0(3) . . ?
C10 N2 C6 119.9(4) . . ?
C10 N2 Cu 128.7(3) . . ?
C6 N2 Cu 111.4(3) . . ?
N1 C1 C2 122.7(4) . . ?
C1 C2 C3 118.8(4) . . ?
C4 C3 C2 119.2(4) . . ?
C3 C4 C5 120.0(4) . . ?
N1 C5 C4 120.7(4) . . ?
N1 C5 C6 115.8(3) . . ?
C4 C5 C6 123.5(4) . . ?
N2 C6 C7 120.3(4) . . ?
N2 C6 C5 116.5(3) . . ?
C7 C6 C5 123.3(4) . . ?
C8 C7 C6 119.8(5) . . ?
C7 C8 C9 119.3(5) . . ?
C10 C9 C8 118.3(4) . . ?
N2 C10 C9 122.4(5) . . ?
C15 N3 C11 119.1(4) . . ?
C15 N3 Cu 115.7(3) . . ?
C11 N3 Cu 125.0(3) . . ?
C20 N4 C16 119.1(4) . . ?
C20 N4 Cu 126.6(3) . . ?
C16 N4 Cu 114.2(3) . . ?
N3 C11 C12 121.8(5) . . ?
C11 C12 C13 119.5(5) . . ?
C12 C13 C14 119.6(5) . . ?
C15 C14 C13 118.1(5) . . ?
N3 C15 C14 122.0(4) . . ?
N3 C15 C16 114.3(3) . . ?
C14 C15 C16 123.7(4) . . ?
N4 C16 C17 120.6(4) . . ?
N4 C16 C15 115.3(3) . . ?
C17 C16 C15 124.1(4) . . ?
C18 C17 C16 120.5(4) . . ?
C19 C18 C17 117.8(4) . . ?
C18 C19 C20 120.1(5) . . ?
N4 C20 C19 121.9(4) . . ?
C21 O1 Cu 109.5(3) . . ?
C21 O2 Cu 74.4(3) . . ?
O2 C21 O1 123.3(4) . . ?
O2 C21 C22 120.9(4) . . ?
O1 C21 C22 115.8(4) . . ?
O6 Cl O5 135.79(17) 1_665 1_665 ?
O6 Cl O5 132.82(16) 1_665 2_765 ?
O5 Cl O5 74.33(12) 1_665 2_765 ?
O6 Cl O3 82.24(16) 1_665 1_655 ?
O5 Cl O3 79.93(12) 1_665 1_655 ?
O5 Cl O3 144.89(13) 2_765 1_655 ?
O4 O3 O7 140.3(3) 1_455 2_666 ?
O6 O4 O5 134.9(3) 1_765 1_665 ?
O7 C71 O7 179.999(4) 2_656 . ?
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
Cu O1 1.974(3) . ?
Cu N3 2.002(3) . ?
Cu N1 2.021(3) . ?
Cu N4 2.024(3) . ?
Cu N2 2.207(3) . ?
Cu O2 2.742(4) . ?
N1 C1 1.344(5) . ?
N1 C5 1.351(5) . ?
N2 C10 1.332(5) . ?
N2 C6 1.353(5) . ?
C1 C2 1.367(6) . ?
C2 C3 1.371(7) . ?
C3 C4 1.371(7) . ?
C4 C5 1.379(6) . ?
C5 C6 1.476(6) . ?
C6 C7 1.388(6) . ?
C7 C8 1.368(7) . ?
C8 C9 1.396(8) . ?
C9 C10 1.371(7) . ?
N3 C15 1.347(5) . ?
N3 C11 1.350(6) . ?
N4 C20 1.335(5) . ?
N4 C16 1.355(5) . ?
C11 C12 1.368(7) . ?
C12 C13 1.374(8) . ?
C13 C14 1.397(7) . ?
C14 C15 1.382(6) . ?
C15 C16 1.463(6) . ?
C16 C17 1.384(6) . ?
C17 C18 1.381(7) . ?
C18 C19 1.372(7) . ?
C19 C20 1.380(7) . ?
O1 C21 1.276(5) . ?
O2 C21 1.222(5) . ?
C21 C22 1.513(6) . ?
Cl O6 3.092(7) 1_665 ?
Cl O5 3.153(5) 1_665 ?
Cl O5 3.194(5) 2_765 ?
Cl O3 3.220(5) 1_655 ?
O3 O4 2.794(7) 1_455 ?
O3 O7 2.795(11) 2_666 ?
O4 O6 2.742(8) 1_765 ?
O4 O5 2.796(7) 1_665 ?
C71 O7 1.368(10) 2_656 ?
C71 O7 1.368(10) . ?
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
O7 H70 O6 0.82 1.90 2.691(12) 162.9 .
C4 H4 O1 0.93 2.59 3.421(5) 148.7 2_765
C11 H11 O1 0.93 2.50 2.999(6) 114.1 .
C14 H14 O2 0.93 2.39 3.271(6) 158.7 2_766
C17 H17 O2 0.93 2.41 3.273(6) 155.2 2_766
C20 H20 O5 0.93 2.50 3.310(6) 145.1 .
|
1100151.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100151.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_1100151
loop_
_publ_author_name
'Carballo, Rosa'
'Covelo, Berta'
'VV\'azquez-L\'opez, Ezequiel M.'
'Casti\~neiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
Synthesis and structural characterization of the mixed ligand
complex [Cu(HmL)2(phen)].2H2O (H2mL = 2-methyllactic acid)
;
_journal_issue 1
_journal_name_full ' Zeitschrift f\"ur Naturforschung B'
_journal_page_first 151
_journal_page_last 154
_journal_paper_doi 10.1515/znb-2003-0122
_journal_volume 58
_journal_year 2003
_chemical_formula_sum 'C20 H26 Cu N2 O8'
_chemical_formula_weight 485.97
_chemical_name_systematic
;
Bis(2-methyllactato-O,O')(1,10-phenanthroline-N,N')
copper(II) dihydrate
;
_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 and located'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 111.758(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 12
_cell_length_a 29.437(4)
_cell_length_b 10.2477(14)
_cell_length_c 24.223(3)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 6786.5(16)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_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 0.0663
_diffrn_reflns_av_sigmaI/netI 0.1664
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 18260
_diffrn_reflns_theta_full 28.04
_diffrn_reflns_theta_max 28.04
_diffrn_reflns_theta_min 1.81
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.012
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.5775
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.427
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 3036
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.403
_refine_diff_density_min -0.575
_refine_diff_density_rms 0.062
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.756
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 462
_refine_ls_number_reflns 7590
_refine_ls_number_restraints 9
_refine_ls_restrained_S_all 0.758
_refine_ls_R_factor_all 0.1546
_refine_ls_R_factor_gt 0.0464
_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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0763
_refine_ls_wR_factor_ref 0.0933
_reflns_number_gt 3102
_reflns_number_total 7590
_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.
'_exptl_absorpt_correction_type' value 'MULTI SCAN' changed
to 'multi-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 C2/c
_cod_database_code 1100151
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
Cu1 Cu 0.0000 0.61440(6) 0.2500 0.0414(2) Uani 1 2 d S . .
O11 O 0.05295(9) 0.7440(2) 0.27246(12) 0.0452(7) Uani 1 1 d . . .
O12 O 0.10423(10) 0.8726(3) 0.33772(12) 0.0669(9) Uani 1 1 d . . .
O13 O 0.02679(10) 0.6289(3) 0.35128(11) 0.0504(7) Uani 1 1 d D . .
C11 C 0.07065(14) 0.7922(4) 0.32375(18) 0.0410(10) Uani 1 1 d . . .
C12 C 0.04917(13) 0.7526(4) 0.37018(16) 0.0389(10) Uani 1 1 d . . .
C13 C 0.01037(14) 0.8511(4) 0.36932(17) 0.0648(13) Uani 1 1 d . . .
H13A H -0.0156 0.8504 0.3309 0.097 Uiso 1 1 calc R . .
H13B H 0.0246 0.9366 0.3773 0.097 Uiso 1 1 calc R . .
H13C H -0.0025 0.8284 0.3992 0.097 Uiso 1 1 calc R . .
C14 C 0.08828(14) 0.7417(4) 0.43145(17) 0.0671(13) Uani 1 1 d . . .
H14A H 0.0744 0.7062 0.4583 0.101 Uiso 1 1 calc R . .
H14B H 0.1015 0.8266 0.4450 0.101 Uiso 1 1 calc R . .
H14C H 0.1139 0.6853 0.4301 0.101 Uiso 1 1 calc R . .
N1 N 0.04699(13) 0.4653(3) 0.25896(13) 0.0481(9) Uani 1 1 d . . .
C101 C 0.09466(16) 0.4692(5) 0.26963(18) 0.0654(13) Uani 1 1 d . . .
H101 H 0.1099 0.5499 0.2726 0.078 Uiso 1 1 calc R . .
C102 C 0.12233(19) 0.3570(6) 0.2764(2) 0.0923(18) Uani 1 1 d . . .
H102 H 0.1557 0.3632 0.2843 0.111 Uiso 1 1 calc R . .
C103 C 0.1012(2) 0.2385(6) 0.2715(2) 0.0895(19) Uani 1 1 d . . .
H103 H 0.1198 0.1632 0.2755 0.107 Uiso 1 1 calc R . .
C104 C 0.0508(2) 0.2295(5) 0.26050(18) 0.0661(14) Uani 1 1 d . . .
C105 C 0.02561(13) 0.3475(4) 0.25500(15) 0.0478(11) Uani 1 1 d . . .
Cu2 Cu 0.174854(15) 0.85660(4) 0.093654(19) 0.03946(15) Uani 1 1 d . . .
O21 O 0.11944(9) 0.7332(2) 0.07634(12) 0.0480(7) Uani 1 1 d . . .
O22 O 0.06154(10) 0.6134(3) 0.01332(11) 0.0643(9) Uani 1 1 d . . .
O23 O 0.14005(10) 0.8516(3) -0.00600(11) 0.0567(8) Uani 1 1 d D . .
C21 C 0.09505(14) 0.6941(4) 0.02477(19) 0.0394(10) Uani 1 1 d . . .
C22 C 0.10730(13) 0.7455(4) -0.02751(16) 0.0382(9) Uani 1 1 d . . .
C23 C 0.06139(14) 0.7958(4) -0.07625(19) 0.0831(16) Uani 1 1 d . . .
H23A H 0.0462 0.8606 -0.0602 0.125 Uiso 1 1 calc R . .
H23B H 0.0391 0.7248 -0.0921 0.125 Uiso 1 1 calc R . .
H23C H 0.0699 0.8338 -0.1074 0.125 Uiso 1 1 calc R . .
C24 C 0.13127(16) 0.6387(4) -0.04958(19) 0.0813(15) Uani 1 1 d . . .
H24A H 0.1395 0.6709 -0.0820 0.122 Uiso 1 1 calc R . .
H24B H 0.1092 0.5664 -0.0630 0.122 Uiso 1 1 calc R . .
H24C H 0.1605 0.6107 -0.0179 0.122 Uiso 1 1 calc R . .
O31 O 0.22443(9) 0.7220(2) 0.10397(11) 0.0434(7) Uani 1 1 d . . .
O32 O 0.27999(9) 0.5879(3) 0.16199(11) 0.0574(8) Uani 1 1 d . . .
O33 O 0.20623(9) 0.8217(3) 0.19277(11) 0.0433(7) Uani 1 1 d D . .
C31 C 0.24623(14) 0.6675(4) 0.15329(17) 0.0398(10) Uani 1 1 d . . .
C32 C 0.22979(13) 0.6977(3) 0.20529(16) 0.0369(9) Uani 1 1 d . . .
C33 C 0.19417(14) 0.5923(4) 0.20798(17) 0.0637(13) Uani 1 1 d . . .
H33A H 0.1838 0.6101 0.2404 0.096 Uiso 1 1 calc R . .
H33B H 0.2100 0.5088 0.2138 0.096 Uiso 1 1 calc R . .
H33C H 0.1662 0.5916 0.1714 0.096 Uiso 1 1 calc R . .
C34 C 0.27284(14) 0.7034(4) 0.26397(16) 0.0621(13) Uani 1 1 d . . .
H34A H 0.2955 0.7687 0.2618 0.093 Uiso 1 1 calc R . .
H34B H 0.2888 0.6200 0.2721 0.093 Uiso 1 1 calc R . .
H34C H 0.2615 0.7251 0.2952 0.093 Uiso 1 1 calc R . .
N3 N 0.21965(11) 1.0021(3) 0.08860(13) 0.0396(8) Uani 1 1 d . . .
N2 N 0.13505(11) 1.0114(3) 0.09991(13) 0.0426(8) Uani 1 1 d . . .
C201 C 0.09350(15) 1.0132(5) 0.10972(19) 0.0654(13) Uani 1 1 d . . .
H201 H 0.0799 0.9343 0.1148 0.078 Uiso 1 1 calc R . .
C202 C 0.06979(17) 1.1272(6) 0.1126(2) 0.0885(17) Uani 1 1 d . . .
H202 H 0.0417 1.1244 0.1216 0.106 Uiso 1 1 calc R . .
C203 C 0.08699(18) 1.2427(5) 0.1024(2) 0.0787(16) Uani 1 1 d . . .
H203 H 0.0699 1.3193 0.1021 0.094 Uiso 1 1 calc R . .
C204 C 0.13143(17) 1.2465(5) 0.09215(17) 0.0538(12) Uani 1 1 d . . .
C205 C 0.15347(13) 1.1271(4) 0.09208(14) 0.0381(9) Uani 1 1 d . . .
C206 C 0.20009(14) 1.1216(4) 0.08570(14) 0.0371(9) Uani 1 1 d . . .
C207 C 0.22295(17) 1.2357(4) 0.07877(17) 0.0528(12) Uani 1 1 d . . .
C208 C 0.26971(19) 1.2226(5) 0.0762(2) 0.0786(16) Uani 1 1 d . . .
H208 H 0.2871 1.2959 0.0726 0.094 Uiso 1 1 calc R . .
C209 C 0.28894(18) 1.1025(6) 0.0790(2) 0.0927(18) Uani 1 1 d . . .
H209 H 0.3197 1.0926 0.0770 0.111 Uiso 1 1 calc R . .
C210 C 0.26331(15) 0.9938(4) 0.08487(19) 0.0618(13) Uani 1 1 d . . .
H210 H 0.2772 0.9118 0.0863 0.074 Uiso 1 1 calc R . .
C211 C 0.15489(19) 1.3618(5) 0.08288(18) 0.0700(15) Uani 1 1 d . . .
H211 H 0.1397 1.4423 0.0809 0.084 Uiso 1 1 calc R . .
C212 C 0.1985(2) 1.3563(5) 0.07695(18) 0.0685(14) Uani 1 1 d . . .
H212 H 0.2130 1.4333 0.0715 0.082 Uiso 1 1 calc R . .
O2W O 0.01242(12) 0.5114(3) 0.07982(14) 0.0561(8) Uani 1 1 d D . .
O3W O 0.17217(13) 0.0354(4) 0.41604(15) 0.0679(9) Uani 1 1 d D . .
O1W O 0.16134(14) 0.8992(4) 0.26540(17) 0.0961(13) Uani 1 1 d D . .
C106 C 0.02369(18) 0.1118(4) 0.2549(3) 0.096(3) Uani 1 1 d . . .
H106 H 0.0398 0.0324 0.2581 0.115 Uiso 1 1 calc R . .
H13 H 0.0130(12) 0.596(3) 0.3738(14) 0.062(14) Uiso 1 1 d D . .
H23 H 0.1539(14) 0.877(4) -0.0307(15) 0.093(17) Uiso 1 1 d D . .
H33 H 0.1887(12) 0.838(4) 0.2134(15) 0.078(15) Uiso 1 1 d D . .
H1WA H 0.1402(13) 0.883(4) 0.2803(19) 0.101(18) Uiso 1 1 d D . .
H1WB H 0.1809(15) 0.959(4) 0.2894(18) 0.12(2) Uiso 1 1 d D . .
H2WA H 0.0313(13) 0.552(4) 0.0653(17) 0.085(17) Uiso 1 1 d D . .
H2WB H -0.0099(11) 0.477(4) 0.0505(13) 0.071(17) Uiso 1 1 d D . .
H3WA H 0.1907(15) 0.067(4) 0.399(2) 0.12(2) Uiso 1 1 d D . .
H3WB H 0.1489(12) -0.013(4) 0.3955(17) 0.09(2) 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
Cu1 0.0401(4) 0.0429(5) 0.0467(5) 0.000 0.0227(4) 0.000
O11 0.0465(17) 0.0563(19) 0.0401(18) 0.0004(14) 0.0246(15) -0.0109(14)
O12 0.0587(19) 0.084(2) 0.063(2) -0.0094(17) 0.0289(16) -0.0350(18)
O13 0.0683(19) 0.0486(19) 0.0483(18) -0.0008(15) 0.0380(16) -0.0106(16)
C11 0.035(2) 0.047(3) 0.043(3) 0.006(2) 0.017(2) 0.001(2)
C12 0.044(2) 0.037(2) 0.038(3) 0.0003(19) 0.018(2) 0.001(2)
C13 0.070(3) 0.069(3) 0.068(3) 0.000(3) 0.040(3) 0.019(3)
C14 0.058(3) 0.096(4) 0.043(3) 0.010(2) 0.013(2) 0.000(3)
N1 0.058(2) 0.045(2) 0.050(2) -0.0011(17) 0.029(2) 0.0087(19)
C101 0.047(3) 0.082(4) 0.073(4) 0.002(3) 0.029(3) 0.011(3)
C102 0.067(4) 0.119(5) 0.093(4) 0.005(4) 0.032(3) 0.043(4)
C103 0.106(5) 0.091(5) 0.067(4) 0.007(3) 0.027(4) 0.055(4)
C104 0.108(5) 0.052(4) 0.033(3) 0.000(2) 0.020(3) 0.026(3)
C105 0.077(3) 0.041(2) 0.027(2) 0.003(2) 0.020(3) 0.014(2)
Cu2 0.0333(3) 0.0436(3) 0.0440(3) 0.0020(3) 0.0174(2) -0.0018(3)
O21 0.0460(17) 0.0618(19) 0.0390(18) 0.0005(14) 0.0189(15) -0.0173(14)
O22 0.0608(19) 0.077(2) 0.059(2) -0.0074(16) 0.0272(16) -0.0362(17)
O23 0.0665(19) 0.069(2) 0.0358(17) 0.0038(15) 0.0205(15) -0.0274(17)
C21 0.037(3) 0.040(3) 0.046(3) 0.006(2) 0.021(2) 0.005(2)
C22 0.036(2) 0.039(2) 0.036(2) 0.0020(19) 0.009(2) -0.003(2)
C23 0.052(3) 0.113(4) 0.068(4) 0.034(3) 0.004(3) 0.000(3)
C24 0.116(4) 0.059(3) 0.099(4) -0.001(3) 0.074(3) 0.013(3)
O31 0.0506(17) 0.0492(18) 0.0354(17) 0.0024(13) 0.0216(14) 0.0098(14)
O32 0.0565(19) 0.066(2) 0.0525(19) 0.0090(15) 0.0236(15) 0.0270(16)
O33 0.0568(18) 0.0417(17) 0.0391(17) -0.0008(13) 0.0268(15) 0.0101(14)
C31 0.039(2) 0.041(3) 0.041(3) -0.006(2) 0.016(2) -0.007(2)
C32 0.041(2) 0.037(2) 0.036(2) 0.0009(18) 0.018(2) 0.0020(19)
C33 0.085(3) 0.057(3) 0.065(3) -0.005(2) 0.046(3) -0.016(3)
C34 0.067(3) 0.082(3) 0.034(3) -0.003(2) 0.015(2) 0.011(2)
N3 0.032(2) 0.048(2) 0.043(2) -0.0042(16) 0.0190(17) -0.0060(16)
N2 0.033(2) 0.049(2) 0.047(2) -0.0003(17) 0.0152(17) 0.0050(17)
C201 0.037(3) 0.074(4) 0.089(4) -0.003(3) 0.028(3) 0.004(2)
C202 0.048(3) 0.104(5) 0.115(5) -0.012(4) 0.032(3) 0.023(4)
C203 0.056(4) 0.085(4) 0.080(4) -0.011(3) 0.008(3) 0.036(3)
C204 0.060(3) 0.049(3) 0.034(3) -0.005(2) -0.004(2) 0.016(3)
C205 0.040(2) 0.040(3) 0.027(2) -0.0026(19) 0.0020(18) 0.002(2)
C206 0.047(3) 0.036(3) 0.023(2) -0.0030(18) 0.0072(18) -0.006(2)
C207 0.071(3) 0.045(3) 0.039(3) -0.002(2) 0.017(2) -0.011(3)
C208 0.085(4) 0.077(4) 0.092(4) -0.016(3) 0.054(3) -0.045(3)
C209 0.070(4) 0.088(4) 0.146(5) -0.013(4) 0.069(4) -0.029(3)
C210 0.044(3) 0.062(3) 0.092(4) -0.010(3) 0.038(3) -0.008(2)
C211 0.095(4) 0.043(3) 0.047(3) -0.010(2) -0.003(3) 0.018(3)
C212 0.107(4) 0.042(3) 0.044(3) -0.004(2) 0.012(3) -0.015(3)
O2W 0.058(2) 0.070(2) 0.051(2) -0.0134(18) 0.033(2) -0.0130(18)
O3W 0.065(2) 0.085(3) 0.068(2) -0.033(2) 0.041(2) -0.023(2)
O1W 0.104(3) 0.115(3) 0.107(3) -0.061(2) 0.084(3) -0.053(3)
C106 0.184(8) 0.044(3) 0.051(3) 0.001(3) 0.034(6) 0.026(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'
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
O11 Cu1 O11 94.96(15) . 2 ?
O11 Cu1 N1 169.52(12) . 2 ?
O11 Cu1 N1 92.29(13) 2 2 ?
O11 Cu1 N1 92.29(13) . . ?
O11 Cu1 N1 169.52(12) 2 . ?
N1 Cu1 N1 81.6(2) 2 . ?
O11 Cu1 O13 74.70(10) . . ?
O11 Cu1 O13 100.13(10) 2 . ?
N1 Cu1 O13 96.59(11) 2 . ?
N1 Cu1 O13 89.08(11) . . ?
O11 Cu1 O13 100.13(10) . 2 ?
O11 Cu1 O13 74.70(10) 2 2 ?
N1 Cu1 O13 89.08(11) 2 2 ?
N1 Cu1 O13 96.59(11) . 2 ?
O13 Cu1 O13 172.53(14) . 2 ?
C11 O11 Cu1 122.4(2) . . ?
C12 O13 Cu1 109.7(2) . . ?
O12 C11 O11 122.0(4) . . ?
O12 C11 C12 118.8(4) . . ?
O11 C11 C12 119.2(4) . . ?
O13 C12 C14 110.1(3) . . ?
O13 C12 C13 109.3(3) . . ?
C14 C12 C13 111.0(3) . . ?
O13 C12 C11 105.5(3) . . ?
C14 C12 C11 111.7(3) . . ?
C13 C12 C11 109.1(3) . . ?
C101 N1 C105 118.2(4) . . ?
C101 N1 Cu1 129.1(3) . . ?
C105 N1 Cu1 112.8(3) . . ?
N1 C101 C102 122.0(5) . . ?
C103 C102 C101 120.4(5) . . ?
C102 C103 C104 119.6(5) . . ?
C105 C104 C103 116.4(5) . . ?
C105 C104 C106 117.7(5) . . ?
C103 C104 C106 125.9(5) . . ?
N1 C105 C104 123.4(4) . . ?
N1 C105 C105 116.4(2) . 2 ?
C104 C105 C105 120.2(3) . 2 ?
O31 Cu2 O21 95.37(10) . . ?
O31 Cu2 N2 167.12(12) . . ?
O21 Cu2 N2 93.57(12) . . ?
O31 Cu2 N3 93.17(12) . . ?
O21 Cu2 N3 163.88(12) . . ?
N2 Cu2 N3 80.47(13) . . ?
O31 Cu2 O23 98.20(11) . . ?
O21 Cu2 O23 75.30(10) . . ?
N2 Cu2 O23 93.02(11) . . ?
N3 Cu2 O23 89.98(11) . . ?
O31 Cu2 O33 76.16(10) . . ?
O21 Cu2 O33 95.98(10) . . ?
N2 Cu2 O33 93.72(11) . . ?
N3 Cu2 O33 99.33(11) . . ?
O23 Cu2 O33 169.29(10) . . ?
C21 O21 Cu2 122.5(2) . . ?
C22 O23 Cu2 112.9(2) . . ?
O22 C21 O21 123.5(4) . . ?
O22 C21 C22 117.2(4) . . ?
O21 C21 C22 119.3(4) . . ?
O23 C22 C24 110.1(3) . . ?
O23 C22 C23 108.3(3) . . ?
C24 C22 C23 111.7(3) . . ?
O23 C22 C21 107.2(3) . . ?
C24 C22 C21 109.2(3) . . ?
C23 C22 C21 110.2(3) . . ?
C31 O31 Cu2 121.9(2) . . ?
C32 O33 Cu2 110.0(2) . . ?
O32 C31 O31 123.2(3) . . ?
O32 C31 C32 117.9(4) . . ?
O31 C31 C32 118.9(4) . . ?
O33 C32 C34 109.7(3) . . ?
O33 C32 C33 110.7(3) . . ?
C34 C32 C33 109.7(3) . . ?
O33 C32 C31 106.3(3) . . ?
C34 C32 C31 111.6(3) . . ?
C33 C32 C31 108.8(3) . . ?
C210 N3 C206 117.6(3) . . ?
C210 N3 Cu2 128.8(3) . . ?
C206 N3 Cu2 113.5(2) . . ?
C201 N2 C205 117.3(3) . . ?
C201 N2 Cu2 128.7(3) . . ?
C205 N2 Cu2 114.1(2) . . ?
N2 C201 C202 122.6(4) . . ?
C203 C202 C201 120.4(5) . . ?
C202 C203 C204 119.3(5) . . ?
C205 C204 C203 116.0(5) . . ?
C205 C204 C211 118.5(4) . . ?
C203 C204 C211 125.5(5) . . ?
N2 C205 C204 124.4(4) . . ?
N2 C205 C206 115.6(4) . . ?
C204 C205 C206 120.0(4) . . ?
N3 C206 C207 123.8(4) . . ?
N3 C206 C205 115.9(4) . . ?
C207 C206 C205 120.3(4) . . ?
C206 C207 C208 116.8(4) . . ?
C206 C207 C212 118.2(4) . . ?
C208 C207 C212 125.0(5) . . ?
C209 C208 C207 119.0(5) . . ?
C208 C209 C210 120.5(4) . . ?
N3 C210 C209 122.4(4) . . ?
C212 C211 C204 121.2(5) . . ?
C211 C212 C207 121.7(5) . . ?
C106 C106 C104 122.2(3) 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 O11 1.964(2) . ?
Cu1 O11 1.964(2) 2 ?
Cu1 N1 2.018(3) 2 ?
Cu1 N1 2.018(3) . ?
Cu1 O13 2.286(3) . ?
Cu1 O13 2.287(3) 2 ?
O11 C11 1.257(4) . ?
O12 C11 1.234(4) . ?
O13 C12 1.424(4) . ?
C11 C12 1.535(5) . ?
C12 C14 1.508(5) . ?
C12 C13 1.518(4) . ?
N1 C101 1.330(4) . ?
N1 C105 1.348(4) . ?
C101 C102 1.384(6) . ?
C102 C103 1.349(6) . ?
C103 C104 1.411(6) . ?
C104 C105 1.399(5) . ?
C104 C106 1.424(6) . ?
C105 C105 1.435(7) 2 ?
Cu2 O31 1.956(2) . ?
Cu2 O21 1.982(2) . ?
Cu2 N2 2.011(3) . ?
Cu2 N3 2.024(3) . ?
Cu2 O23 2.246(3) . ?
Cu2 O33 2.259(3) . ?
O21 C21 1.254(4) . ?
O22 C21 1.237(4) . ?
O23 C22 1.418(4) . ?
C21 C22 1.533(5) . ?
C22 C24 1.504(4) . ?
C22 C23 1.518(5) . ?
O31 C31 1.258(4) . ?
O32 C31 1.242(4) . ?
O33 C32 1.426(4) . ?
C31 C32 1.539(5) . ?
C32 C34 1.515(5) . ?
C32 C33 1.523(4) . ?
N3 C210 1.324(4) . ?
N3 C206 1.344(4) . ?
N2 C201 1.330(4) . ?
N2 C205 1.346(4) . ?
C201 C202 1.376(6) . ?
C202 C203 1.345(6) . ?
C203 C204 1.420(6) . ?
C204 C205 1.386(5) . ?
C204 C211 1.428(6) . ?
C205 C206 1.438(5) . ?
C206 C207 1.389(5) . ?
C207 C208 1.407(5) . ?
C207 C212 1.423(5) . ?
C208 C209 1.346(6) . ?
C209 C210 1.382(5) . ?
C211 C212 1.345(6) . ?
C106 C106 1.326(10) 2 ?
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
O13 H13 O2W 0.859(18) 1.790(19) 2.645(4) 173(4) 2
O23 H23 O3W 0.879(18) 1.81(2) 2.669(4) 166(4) 6_565
O33 H33 O1W 0.858(18) 1.84(2) 2.682(4) 168(4) .
O1W H1WA O12 0.843(18) 2.04(2) 2.855(4) 163(4) .
O1W H1WB O32 0.894(19) 1.86(2) 2.751(4) 178(5) 4
O2W H2WA O22 0.867(18) 1.90(2) 2.740(4) 163(4) .
O2W H2WB O22 0.847(18) 1.952(19) 2.798(4) 176(4) 5_565
O3W H3WA O32 0.863(19) 1.98(3) 2.796(4) 158(5) 4_545
O3W H3WB O12 0.841(19) 1.92(2) 2.751(4) 167(4) 1_545
C13 H13A O11 0.96 2.57 3.424(5) 147.6 2
C101 H101 O11 0.93 2.60 3.082(5) 112.9 .
C203 H203 O2W 0.93 2.52 3.437(6) 168.0 1_565
|
1100152.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100152.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_1100152
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_publ_section_title
;
Structure of the adduct of bis(2,2'biimidazole)copper(II) perchlorate
with 4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one
;
_journal_issue 8
_journal_name_full 'Journal of Chemical Crystallography'
_journal_page_first 549
_journal_page_last 552
_journal_paper_doi 10.1023/B:JOCC.0000042024.70444.a0
_journal_volume 34
_journal_year 2004
_chemical_formula_sum 'C22 H20 Cl2 Cu N16 O10'
_chemical_formula_weight 802.98
_chemical_name_systematic
'bis(2,2'-biimidazole)copper(II) perchlorate bis(4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one'
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 103.690(8)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 19.666(2)
_cell_length_b 11.7586(8)
_cell_length_c 13.4808(9)
_cell_measurement_reflns_used 33
_cell_measurement_temperature 295(1)
_cell_measurement_theta_max 20.1
_cell_measurement_theta_min 12.5
_cell_volume 3028.8(5)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.82 - 1.67, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_diffrn_radiation_collimation '0.8 mm'
_diffrn_radiation_detector 'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_polarisn_norm 90
_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 0.0477
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 4407
_diffrn_reflns_theta_full 29.98
_diffrn_reflns_theta_max 29.98
_diffrn_reflns_theta_min 2.03
_diffrn_standards_decay_% 7.3
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 0.983
_exptl_absorpt_correction_T_max 0.7873
_exptl_absorpt_correction_T_min 0.5556
_exptl_absorpt_correction_type empirical
_exptl_absorpt_process_details
;
Psi Scan Reflections used Mu * R = 0.16
H K L 2Theta Chi Imin/Imax
0 0 2 6.2 70.5 0.668
0 0 4 12.5 70.5 0.775
-5 1 6 19.6 75.4 0.822
-2 2 7 22.4 75.8 0.824
-6 2 7 23.7 71.5 0.803
-2 0 8 24.4 79.5 0.822
0 0 8 25.1 70.5 0.831
-2 0 10 30.8 77.7 0.832
;
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 1.761
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 1628
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.934
_refine_diff_density_min -1.016
_refine_diff_density_rms 0.109
_refine_ls_extinction_coef 0.0006(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 1.025
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 225
_refine_ls_number_reflns 4407
_refine_ls_number_restraints 20
_refine_ls_restrained_S_all 1.035
_refine_ls_R_factor_all 0.1388
_refine_ls_R_factor_gt 0.0806
_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^)+(0.0950P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1905
_refine_ls_wR_factor_ref 0.2456
_reflns_number_gt 2586
_reflns_number_total 4407
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100152
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
Cu Cu 0.5000 0.59382(7) 0.2500 0.0420(3) Uani 1 2 d S . .
N1I N 0.4693(2) 0.7034(4) 0.1342(3) 0.0436(10) Uani 1 1 d . . .
C2I C 0.4703(3) 0.8171(5) 0.1108(4) 0.0570(15) Uani 1 1 d . . .
H2I H 0.4908 0.8744 0.1554 0.068 Uiso 1 1 d R . .
C3I C 0.4364(3) 0.8307(5) 0.0115(4) 0.0565(14) Uani 1 1 d . . .
H3I H 0.4288 0.8992 -0.0239 0.068 Uiso 1 1 d R . .
N4I N 0.4154(2) 0.7262(4) -0.0263(3) 0.0491(11) Uani 1 1 d . . .
H4I H 0.3934 0.7109 -0.0879 0.059 Uiso 1 1 d R . .
C5I C 0.4357(3) 0.6517(4) 0.0486(3) 0.0410(11) Uani 1 1 d . . .
C6I C 0.4302(3) 0.5303(4) 0.0526(3) 0.0398(10) Uani 1 1 d . . .
N7I N 0.4035(2) 0.4529(4) -0.0174(3) 0.0473(10) Uani 1 1 d . . .
H7I H 0.3830 0.4664 -0.0800 0.057 Uiso 1 1 d R . .
C8I C 0.4139(3) 0.3477(5) 0.0278(4) 0.0541(14) Uani 1 1 d . . .
H8I H 0.4003 0.2779 -0.0030 0.065 Uiso 1 1 d R . .
C9I C 0.4474(3) 0.3663(5) 0.1268(4) 0.0519(13) Uani 1 1 d . . .
H9I H 0.4609 0.3102 0.1761 0.062 Uiso 1 1 d R . .
N10I N 0.4586(2) 0.4808(4) 0.1424(3) 0.0436(10) Uani 1 1 d . . .
N1 N 0.3496(3) 0.6636(4) 0.2746(3) 0.0500(11) Uani 1 1 d . . .
C2 C 0.3352(3) 0.7598(5) 0.2229(4) 0.0522(13) Uani 1 1 d . . .
H2 H 0.3516 0.8296 0.2510 0.063 Uiso 1 1 d R . .
N3 N 0.2947(2) 0.7513(4) 0.1261(3) 0.0487(11) Uani 1 1 d . . .
C3A C 0.2822(3) 0.6411(4) 0.1182(4) 0.0425(11) Uani 1 1 d . . .
N4 N 0.2457(3) 0.5787(4) 0.0391(3) 0.0505(11) Uani 1 1 d . . .
H4 H 0.2262 0.6109 -0.0179 0.061 Uiso 1 1 d R . .
C5 C 0.2406(3) 0.4650(5) 0.0514(4) 0.0516(13) Uani 1 1 d . . .
H5 H 0.2137 0.4227 -0.0020 0.062 Uiso 1 1 d R . .
C6 C 0.2721(3) 0.4103(5) 0.1374(4) 0.0509(13) Uani 1 1 d . . .
H6 H 0.2671 0.3318 0.1406 0.061 Uiso 1 1 d R . .
C7 C 0.3124(3) 0.4686(4) 0.2244(4) 0.0445(11) Uani 1 1 d . . .
O7 O 0.3443(2) 0.4307(3) 0.3062(3) 0.0540(10) Uani 1 1 d . . .
N8 N 0.3141(2) 0.5860(3) 0.2051(3) 0.0406(9) Uani 1 1 d . . .
Cl Cl 0.36980(9) 0.08321(11) 0.22556(11) 0.0587(4) Uani 1 1 d D . .
O1P O 0.4155(3) 0.0096(5) 0.2966(4) 0.0690(17) Uiso 0.67 1 d PD A 1
O2P O 0.3056(3) 0.0194(6) 0.1810(5) 0.0760(18) Uiso 0.67 1 d PD A 1
O3P O 0.4021(4) 0.1129(6) 0.1435(5) 0.100(2) Uiso 0.67 1 d PD A 1
O4P O 0.3498(4) 0.1805(5) 0.2740(5) 0.0789(19) Uiso 0.67 1 d PD A 1
O1P' O 0.3857(6) 0.0016(8) 0.3076(7) 0.0690(17) Uiso 0.33 1 d PD A 2
O2P' O 0.2957(3) 0.0927(12) 0.1868(9) 0.0760(18) Uiso 0.33 1 d PD A 2
O3P' O 0.4034(6) 0.0532(10) 0.1457(7) 0.100(2) Uiso 0.33 1 d PD A 2
O4P' O 0.3950(7) 0.1942(6) 0.2661(9) 0.0789(19) Uiso 0.33 1 d PD 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
Cu 0.0514(5) 0.0428(5) 0.0263(4) 0.000 -0.0019(3) 0.000
N1I 0.056(3) 0.040(2) 0.0299(18) 0.0014(16) -0.0006(17) 0.0000(19)
C2I 0.066(4) 0.050(3) 0.048(3) 0.007(2) -0.001(3) -0.009(3)
C3I 0.070(4) 0.046(3) 0.049(3) 0.011(2) 0.004(3) 0.002(3)
N4I 0.060(3) 0.053(3) 0.0291(19) 0.0079(18) -0.0006(18) 0.004(2)
C5I 0.044(3) 0.046(3) 0.029(2) 0.0013(19) 0.0004(18) 0.003(2)
C6I 0.045(3) 0.045(3) 0.027(2) 0.0014(19) 0.0023(18) 0.002(2)
N7I 0.054(3) 0.055(3) 0.0291(19) -0.0027(18) 0.0026(18) 0.002(2)
C8I 0.064(4) 0.049(3) 0.044(3) -0.010(2) 0.004(3) -0.003(3)
C9I 0.065(4) 0.044(3) 0.042(3) -0.003(2) 0.003(2) -0.001(3)
N10I 0.052(2) 0.044(2) 0.0299(18) -0.0004(16) 0.0004(17) 0.0002(19)
N1 0.067(3) 0.041(2) 0.033(2) 0.0031(18) -0.0062(19) -0.004(2)
C2 0.071(4) 0.039(3) 0.041(3) 0.005(2) 0.003(2) -0.005(3)
N3 0.059(3) 0.042(2) 0.040(2) 0.0082(18) 0.0022(19) 0.003(2)
C3A 0.043(3) 0.044(3) 0.037(2) 0.008(2) 0.002(2) 0.003(2)
N4 0.060(3) 0.052(3) 0.0296(19) 0.0066(18) -0.0077(18) 0.002(2)
C5 0.060(3) 0.048(3) 0.038(3) -0.001(2) -0.006(2) -0.005(3)
C6 0.065(3) 0.044(3) 0.037(2) 0.001(2) 0.000(2) -0.001(2)
C7 0.057(3) 0.041(3) 0.033(2) 0.006(2) 0.005(2) 0.005(2)
O7 0.079(3) 0.042(2) 0.0328(17) 0.0078(14) -0.0042(17) 0.0049(18)
N8 0.051(2) 0.036(2) 0.0291(18) 0.0050(15) -0.0022(16) 0.0031(17)
Cl 0.0831(10) 0.0411(7) 0.0455(7) -0.0040(5) 0.0023(7) 0.0033(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'
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'
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
N10I Cu N10I 96.4(2) . 2_655 ?
N10I Cu N1I 172.47(18) . 2_655 ?
N10I Cu N1I 82.30(17) . . ?
N1I Cu N1I 99.9(2) 2_655 . ?
C5I N1I C2I 106.0(4) . . ?
C5I N1I Cu 112.1(3) . . ?
C2I N1I Cu 141.9(4) . . ?
C3I C2I N1I 108.2(5) . . ?
C2I C3I N4I 107.3(5) . . ?
C5I N4I C3I 107.6(4) . . ?
N4I C5I N1I 110.9(5) . . ?
N4I C5I C6I 132.5(5) . . ?
N1I C5I C6I 116.6(4) . . ?
N7I C6I N10I 110.8(4) . . ?
N7I C6I C5I 132.6(4) . . ?
N10I C6I C5I 116.6(4) . . ?
C6I N7I C8I 108.1(4) . . ?
C9I C8I N7I 106.1(5) . . ?
C8I C9I N10I 109.4(5) . . ?
C6I N10I C9I 105.6(4) . . ?
C6I N10I Cu 112.3(3) . . ?
C9I N10I Cu 142.1(3) . . ?
C2 N1 N8 101.4(4) . . ?
N1 C2 N3 116.5(5) . . ?
C3A N3 C2 101.8(4) . . ?
N3 C3A N4 130.5(5) . . ?
N3 C3A N8 111.2(4) . . ?
N4 C3A N8 118.3(5) . . ?
C3A N4 C5 118.6(4) . . ?
C6 C5 N4 123.2(5) . . ?
C5 C6 C7 122.2(5) . . ?
O7 C7 N8 119.8(5) . . ?
O7 C7 C6 129.5(5) . . ?
N8 C7 C6 110.7(4) . . ?
C3A N8 N1 109.2(4) . . ?
C3A N8 C7 127.0(4) . . ?
N1 N8 C7 123.8(4) . . ?
O2P' Cl O3P' 110.8(4) . . ?
O4P Cl O1P 112.1(3) . . ?
O2P' Cl O1P' 110.4(4) . . ?
O3P' Cl O1P' 110.9(4) . . ?
O4P Cl O3P 112.2(3) . . ?
O1P Cl O3P 109.7(3) . . ?
O2P' Cl O4P' 107.1(8) . . ?
O3P' Cl O4P' 109.0(4) . . ?
O1P' Cl O4P' 108.4(4) . . ?
O4P Cl O2P 107.2(5) . . ?
O1P Cl O2P 107.8(3) . . ?
O3P Cl O2P 107.5(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
Cu N10I 1.993(4) . ?
Cu N1I 2.004(4) . ?
N1I C5I 1.333(6) . ?
N1I C2I 1.374(7) . ?
C2I C3I 1.356(8) . ?
C3I N4I 1.357(7) . ?
N4I C5I 1.325(6) . ?
C5I C6I 1.433(7) . ?
C6I N7I 1.327(6) . ?
C6I N10I 1.340(6) . ?
N7I C8I 1.372(7) . ?
C8I C9I 1.359(7) . ?
C9I N10I 1.373(7) . ?
N1 C2 1.324(6) . ?
N1 N8 1.374(6) . ?
C2 N3 1.362(7) . ?
N3 C3A 1.319(7) . ?
C3A N4 1.352(6) . ?
C3A N8 1.355(6) . ?
N4 C5 1.354(7) . ?
C5 C6 1.342(7) . ?
C6 C7 1.426(7) . ?
C7 O7 1.217(6) . ?
C7 N8 1.406(6) . ?
Cl O4P 1.418(5) . ?
Cl O2P' 1.432(6) . ?
Cl O3P' 1.433(5) . ?
Cl O1P 1.438(4) . ?
Cl O1P' 1.442(5) . ?
Cl O3P 1.442(5) . ?
Cl O4P' 1.456(6) . ?
Cl O2P 1.469(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
N4 H4 N3 0.86 2.15 2.957(6) 155.3 7_565
N4I H4I O7 0.86 2.26 2.995(6) 143.9 6_565
N4I H4I O4P 0.86 2.25 2.911(8) 133.2 6_565
N4I H4I O4P' 0.86 2.27 2.887(11) 128.8 6_565
N7I H7I O7 0.86 1.96 2.752(6) 152.6 6_565
|
1100153.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100153.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_1100153
loop_
_publ_author_name
'Kruger, Hannes'
'Kahlenberg, Volker'
_chemical_formula_sum 'Ca4 F2 O7 Si2'
_chemical_formula_weight 366.50
_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
_audit_contact_author_address
;
Institut fur Mineralogie und Petrographie
Leopold-Franzens-Universitat Innsbruck
Innrain 52
A-6020 Innsbruck
Austria
;
_audit_contact_author_email Hannes.Krueger@uibk.ac.at
_audit_contact_author_fax '+43 512 507 2926'
_audit_contact_author_name 'Kruger, Hannes'
_audit_contact_author_phone '+43 512 507 5502'
_cell_angle_alpha 90.00
_cell_angle_beta 109.557(17)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 7.5397(16)
_cell_length_b 10.5338(19)
_cell_length_c 10.907(2)
_cell_measurement_reflns_used 6855
_cell_measurement_temperature 300(2)
_cell_measurement_theta_max 29.41
_cell_measurement_theta_min 0.00
_cell_volume 816.3(3)
_diffrn_ambient_temperature 300(2)
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type STOE
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details ' 180 frames, detector distance = 100 mm'
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'STOE IPDS 2'
_diffrn_measurement_method 'rotation method'
_diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator 'plane graphite'
_diffrn_radiation_polarisn_norm 0
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0511
_diffrn_reflns_av_unetI/netI 0.0629
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 8019
_diffrn_reflns_theta_full 29.40
_diffrn_reflns_theta_max 29.40
_diffrn_reflns_theta_min 1.93
_diffrn_source
' sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current 40
_diffrn_source_power 2.00
_diffrn_source_voltage 50
_exptl_absorpt_coefficient_mu 2.994
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 2.982
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 728
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_refine_diff_density_max 0.482
_refine_diff_density_min -0.473
_refine_diff_density_rms 0.120
_refine_ls_extinction_coef 0.0154(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 1.045
_refine_ls_matrix_type full
_refine_ls_number_parameters 137
_refine_ls_number_reflns 2238
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0538
_refine_ls_R_factor_gt 0.0341
_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^)+(0.0293P)^2^+0.2638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0614
_refine_ls_wR_factor_ref 0.0664
_reflns_number_gt 1745
_reflns_number_total 2238
_reflns_threshold_expression I>2u(I)
_cod_database_code 1100153
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
Ca1 Ca -0.03011(8) 0.40475(6) 0.69828(5) 0.00849(13) Uani 1 1 d . . .
Ca2 Ca 0.66300(7) 0.13301(6) 0.58356(5) 0.00847(13) Uani 1 1 d . . .
Ca3 Ca 0.83067(8) 0.63499(6) 0.92406(5) 0.00882(13) Uani 1 1 d . . .
Ca4 Ca 0.47033(8) 0.41482(5) 0.68450(5) 0.00761(12) Uani 1 1 d . . .
Si5 Si 0.27271(10) 0.30739(8) 0.36755(6) 0.00571(15) Uani 1 1 d . . .
Si6 Si -0.15215(10) 0.30935(8) 0.37762(6) 0.00572(15) Uani 1 1 d . . .
F7 F 0.5742(2) 0.49984(17) 0.89674(15) 0.0106(3) Uani 1 1 d . . .
F8 F 0.9268(2) 0.49630(17) 1.10128(15) 0.0106(3) Uani 1 1 d . . .
O9 O 0.7224(3) 0.2789(2) 0.76016(18) 0.0120(4) Uani 1 1 d . . .
O10 O 0.0635(3) 0.2753(2) 0.3787(2) 0.0140(4) Uani 1 1 d . . .
O11 O -0.1390(3) 0.2670(2) 0.52267(18) 0.0109(4) Uani 1 1 d . . .
O12 O 0.7302(3) 0.7805(2) 0.75469(18) 0.0110(4) Uani 1 1 d . . .
O13 O 0.4103(3) 0.2652(2) 0.50919(19) 0.0118(4) Uani 1 1 d . . .
O14 O 0.1983(3) 0.5438(2) 0.6604(2) 0.0138(4) Uani 1 1 d . . .
O15 O -0.2831(3) 0.5462(2) 0.6703(2) 0.0151(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
Ca1 0.0084(2) 0.0079(3) 0.0093(2) -0.00168(19) 0.00315(18) -0.0003(2)
Ca2 0.0075(2) 0.0079(3) 0.0100(3) -0.00103(19) 0.00302(18) -0.0002(2)
Ca3 0.0092(2) 0.0089(3) 0.0084(2) 0.00200(19) 0.00306(18) 0.0007(2)
Ca4 0.0070(2) 0.0069(3) 0.0092(2) -0.00067(19) 0.00293(17) -0.0003(2)
Si5 0.0054(3) 0.0057(4) 0.0061(3) 0.0006(3) 0.0020(2) 0.0001(3)
Si6 0.0056(3) 0.0065(4) 0.0055(3) 0.0008(2) 0.0024(2) 0.0002(3)
F7 0.0095(7) 0.0114(9) 0.0104(7) -0.0010(6) 0.0029(6) 0.0000(6)
F8 0.0120(7) 0.0098(9) 0.0096(7) 0.0006(6) 0.0032(6) -0.0008(7)
O9 0.0134(9) 0.0121(11) 0.0081(8) 0.0002(7) 0.0005(7) 0.0034(8)
O10 0.0084(8) 0.0140(11) 0.0220(10) 0.0050(8) 0.0082(7) 0.0013(9)
O11 0.0141(10) 0.0131(11) 0.0064(8) 0.0000(7) 0.0048(7) -0.0030(8)
O12 0.0132(9) 0.0110(11) 0.0092(8) -0.0017(7) 0.0043(7) 0.0010(8)
O13 0.0111(9) 0.0134(11) 0.0083(8) -0.0003(7) -0.0003(7) 0.0031(8)
O14 0.0130(10) 0.0076(11) 0.0225(11) 0.0047(8) 0.0084(8) 0.0025(8)
O15 0.0119(9) 0.0105(11) 0.0245(11) 0.0037(8) 0.0083(8) -0.0003(9)
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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
F8 Ca1 O11 167.61(7) 3_667 . ?
F8 Ca1 O15 80.74(7) 3_667 . ?
O11 Ca1 O15 103.93(8) . . ?
F8 Ca1 O14 81.57(7) 3_667 . ?
O11 Ca1 O14 108.38(7) . . ?
O15 Ca1 O14 100.86(7) . . ?
F8 Ca1 O12 92.67(7) 3_667 2_646 ?
O11 Ca1 O12 83.59(7) . 2_646 ?
O15 Ca1 O12 171.57(8) . 2_646 ?
O14 Ca1 O12 72.80(7) . 2_646 ?
F8 Ca1 O9 91.65(7) 3_667 1_455 ?
O11 Ca1 O9 78.81(7) . 1_455 ?
O15 Ca1 O9 74.42(7) . 1_455 ?
O14 Ca1 O9 172.36(8) . 1_455 ?
O12 Ca1 O9 111.25(7) 2_646 1_455 ?
F8 Ca1 O10 72.46(7) 3_667 4_566 ?
O11 Ca1 O10 95.62(7) . 4_566 ?
O15 Ca1 O10 123.39(7) . 4_566 ?
O14 Ca1 O10 122.40(7) . 4_566 ?
O12 Ca1 O10 58.56(6) 2_646 4_566 ?
O9 Ca1 O10 57.99(7) 1_455 4_566 ?
F8 Ca1 Si5 79.88(5) 3_667 4_566 ?
O11 Ca1 Si5 91.48(6) . 4_566 ?
O15 Ca1 Si5 151.91(6) . 4_566 ?
O14 Ca1 Si5 96.19(6) . 4_566 ?
O12 Ca1 Si5 28.63(5) 2_646 4_566 ?
O9 Ca1 Si5 86.00(5) 1_455 4_566 ?
O10 Ca1 Si5 30.07(5) 4_566 4_566 ?
F8 Ca1 Si6 79.66(5) 3_667 4_566 ?
O11 Ca1 Si6 88.29(6) . 4_566 ?
O15 Ca1 Si6 97.70(6) . 4_566 ?
O14 Ca1 Si6 151.01(6) . 4_566 ?
O12 Ca1 Si6 86.19(5) 2_646 4_566 ?
O9 Ca1 Si6 28.27(5) 1_455 4_566 ?
O10 Ca1 Si6 29.82(5) 4_566 4_566 ?
Si5 Ca1 Si6 58.87(2) 4_566 4_566 ?
F8 Ca1 Si6 168.78(5) 3_667 . ?
O11 Ca1 Si6 23.46(5) . . ?
O15 Ca1 Si6 97.07(6) . . ?
O14 Ca1 Si6 88.09(6) . . ?
O12 Ca1 Si6 88.38(5) 2_646 . ?
O9 Ca1 Si6 98.38(5) 1_455 . ?
O10 Ca1 Si6 117.23(5) 4_566 . ?
Si5 Ca1 Si6 105.70(3) 4_566 . ?
Si6 Ca1 Si6 111.56(2) 4_566 . ?
F8 Ca1 Si5 77.88(5) 3_667 3_566 ?
O11 Ca1 Si5 110.91(6) . 3_566 ?
O15 Ca1 Si5 22.91(5) . 3_566 ?
O14 Ca1 Si5 77.96(6) . 3_566 ?
O12 Ca1 Si5 150.30(5) 2_646 3_566 ?
O9 Ca1 Si5 97.25(5) 1_455 3_566 ?
O10 Ca1 Si5 139.89(5) 4_566 3_566 ?
Si5 Ca1 Si5 157.60(2) 4_566 3_566 ?
Si6 Ca1 Si5 118.90(3) 4_566 3_566 ?
Si6 Ca1 Si5 95.79(2) . 3_566 ?
F8 Ca1 Si6 78.59(5) 3_667 3_566 ?
O11 Ca1 Si6 113.48(6) . 3_566 ?
O15 Ca1 Si6 77.98(6) . 3_566 ?
O14 Ca1 Si6 22.89(5) . 3_566 ?
O12 Ca1 Si6 95.64(5) 2_646 3_566 ?
O9 Ca1 Si6 151.88(5) 1_455 3_566 ?
O10 Ca1 Si6 139.27(5) 4_566 3_566 ?
Si5 Ca1 Si6 117.47(3) 4_566 3_566 ?
Si6 Ca1 Si6 158.23(2) 4_566 3_566 ?
Si6 Ca1 Si6 90.20(2) . 3_566 ?
Si5 Ca1 Si6 55.08(2) 3_566 3_566 ?
O13 Ca2 O11 93.91(8) . 1_655 ?
O13 Ca2 F7 79.93(7) . 2_646 ?
O11 Ca2 F7 168.97(7) 1_655 2_646 ?
O13 Ca2 F8 164.00(7) . 4_565 ?
O11 Ca2 F8 76.60(7) 1_655 4_565 ?
F7 Ca2 F8 107.17(7) 2_646 4_565 ?
O13 Ca2 F7 95.31(7) . 4_565 ?
O11 Ca2 F7 97.87(7) 1_655 4_565 ?
F7 Ca2 F7 73.80(7) 2_646 4_565 ?
F8 Ca2 F7 73.66(6) 4_565 4_565 ?
O13 Ca2 O9 78.61(7) . . ?
O11 Ca2 O9 82.75(7) 1_655 . ?
F7 Ca2 O9 104.76(7) 2_646 . ?
F8 Ca2 O9 112.31(7) 4_565 . ?
F7 Ca2 O9 173.92(7) 4_565 . ?
O13 Ca2 O14 123.34(7) . 2_646 ?
O11 Ca2 O14 115.56(7) 1_655 2_646 ?
F7 Ca2 O14 75.43(6) 2_646 2_646 ?
F8 Ca2 O14 72.64(6) 4_565 2_646 ?
F7 Ca2 O14 124.20(7) 4_565 2_646 ?
O9 Ca2 O14 60.27(7) . 2_646 ?
O13 Ca2 Si6 106.35(6) . 4_666 ?
O11 Ca2 Si6 93.90(5) 1_655 4_666 ?
F7 Ca2 Si6 96.62(5) 2_646 4_666 ?
F8 Ca2 Si6 87.35(5) 4_565 4_666 ?
F7 Ca2 Si6 154.54(5) 4_565 4_666 ?
O9 Ca2 Si6 30.76(5) . 4_666 ?
O14 Ca2 Si6 31.15(5) 2_646 4_666 ?
O13 Ca2 Si6 85.03(6) . 1_655 ?
O11 Ca2 Si6 21.02(5) 1_655 1_655 ?
F7 Ca2 Si6 148.05(5) 2_646 1_655 ?
F8 Ca2 Si6 81.66(5) 4_565 1_655 ?
F7 Ca2 Si6 79.78(5) 4_565 1_655 ?
O9 Ca2 Si6 99.61(6) . 1_655 ?
O14 Ca2 Si6 135.64(5) 2_646 1_655 ?
Si6 Ca2 Si6 114.69(3) 4_666 1_655 ?
O13 Ca2 Si5 18.50(5) . . ?
O11 Ca2 Si5 88.02(6) 1_655 . ?
F7 Ca2 Si5 83.30(5) 2_646 . ?
F8 Ca2 Si5 145.98(4) 4_565 . ?
F7 Ca2 Si5 78.77(5) 4_565 . ?
O9 Ca2 Si5 95.23(6) . . ?
O14 Ca2 Si5 140.90(5) 2_646 . ?
Si6 Ca2 Si5 124.30(3) 4_666 . ?
Si6 Ca2 Si5 74.10(2) 1_655 . ?
O13 Ca2 Ca1 90.08(6) . 1_655 ?
O11 Ca2 Ca1 38.54(5) 1_655 1_655 ?
F7 Ca2 Ca1 149.34(5) 2_646 1_655 ?
F8 Ca2 Ca1 90.25(5) 4_565 1_655 ?
F7 Ca2 Ca1 136.40(5) 4_565 1_655 ?
O9 Ca2 Ca1 44.62(5) . 1_655 ?
O14 Ca2 Ca1 86.49(5) 2_646 1_655 ?
Si6 Ca2 Ca1 58.32(2) 4_666 1_655 ?
Si6 Ca2 Ca1 57.59(2) 1_655 1_655 ?
Si5 Ca2 Ca1 96.34(3) . 1_655 ?
O13 Ca2 Ca4 40.30(5) . . ?
O11 Ca2 Ca4 87.16(6) 1_655 . ?
F7 Ca2 Ca4 93.82(5) 2_646 . ?
F8 Ca2 Ca4 148.92(5) 4_565 . ?
F7 Ca2 Ca4 135.61(5) 4_565 . ?
O9 Ca2 Ca4 38.32(5) . . ?
O14 Ca2 Ca4 91.48(5) 2_646 . ?
Si6 Ca2 Ca4 67.25(2) 4_666 . ?
Si6 Ca2 Ca4 92.63(3) 1_655 . ?
Si5 Ca2 Ca4 57.25(2) . . ?
Ca1 Ca2 Ca4 61.62(2) 1_655 . ?
O12 Ca3 F8 176.97(7) . . ?
O12 Ca3 F7 105.35(7) . . ?
F8 Ca3 F7 74.87(6) . . ?
O12 Ca3 F8 110.45(7) . 3_767 ?
F8 Ca3 F8 72.25(7) . 3_767 ?
F7 Ca3 F8 105.42(6) . 3_767 ?
O12 Ca3 O10 102.62(8) . 2_656 ?
F8 Ca3 O10 74.79(7) . 2_656 ?
F7 Ca3 O10 118.67(7) . 2_656 ?
F8 Ca3 O10 113.91(7) 3_767 2_656 ?
O12 Ca3 O13 78.46(7) . 2_656 ?
F8 Ca3 O13 98.76(6) . 2_656 ?
F7 Ca3 O13 74.21(7) . 2_656 ?
F8 Ca3 O13 170.56(6) 3_767 2_656 ?
O10 Ca3 O13 59.65(7) 2_656 2_656 ?
O12 Ca3 O11 81.62(7) . 2_656 ?
F8 Ca3 O11 98.21(6) . 2_656 ?
F7 Ca3 O11 173.00(7) . 2_656 ?
F8 Ca3 O11 70.91(7) 3_767 2_656 ?
O10 Ca3 O11 59.34(6) 2_656 2_656 ?
O13 Ca3 O11 108.39(7) 2_656 2_656 ?
O12 Ca3 O15 61.25(7) . 1_655 ?
F8 Ca3 O15 121.45(7) . 1_655 ?
F7 Ca3 O15 72.60(6) . 1_655 ?
F8 Ca3 O15 71.41(6) 3_767 1_655 ?
O10 Ca3 O15 163.32(7) 2_656 1_655 ?
O13 Ca3 O15 116.83(7) 2_656 1_655 ?
O11 Ca3 O15 110.99(6) 2_656 1_655 ?
O12 Ca3 Si5 31.14(5) . 3_666 ?
F8 Ca3 Si5 151.80(5) . 3_666 ?
F7 Ca3 Si5 94.36(5) . 3_666 ?
F8 Ca3 Si5 86.17(4) 3_767 3_666 ?
O10 Ca3 Si5 131.98(6) 2_656 3_666 ?
O13 Ca3 Si5 103.28(5) 2_656 3_666 ?
O11 Ca3 Si5 91.36(5) 2_656 3_666 ?
O15 Ca3 Si5 31.36(5) 1_655 3_666 ?
O12 Ca3 Si5 95.64(6) . 2_656 ?
F8 Ca3 Si5 81.33(5) . 2_656 ?
F7 Ca3 Si5 92.77(5) . 2_656 ?
F8 Ca3 Si5 142.22(5) 3_767 2_656 ?
O10 Ca3 Si5 30.79(5) 2_656 2_656 ?
O13 Ca3 Si5 29.87(5) 2_656 2_656 ?
O11 Ca3 Si5 87.14(5) 2_656 2_656 ?
O15 Ca3 Si5 146.36(5) 1_655 2_656 ?
Si5 Ca3 Si5 125.82(3) 3_666 2_656 ?
O12 Ca3 Si6 97.43(6) . 2_656 ?
F8 Ca3 Si6 81.14(5) . 2_656 ?
F7 Ca3 Si6 146.64(5) . 2_656 ?
F8 Ca3 Si6 88.55(5) 3_767 2_656 ?
O10 Ca3 Si6 30.52(5) 2_656 2_656 ?
O13 Ca3 Si6 87.14(5) 2_656 2_656 ?
O11 Ca3 Si6 29.76(4) 2_656 2_656 ?
O15 Ca3 Si6 140.66(5) 1_655 2_656 ?
Si5 Ca3 Si6 117.06(3) 3_666 2_656 ?
Si5 Ca3 Si6 60.55(2) 2_656 2_656 ?
O12 Ca3 Ca4 37.92(5) . 2_656 ?
F8 Ca3 Ca4 139.20(5) . 2_656 ?
F7 Ca3 Ca4 93.00(5) . 2_656 ?
F8 Ca3 Ca4 147.76(5) 3_767 2_656 ?
O10 Ca3 Ca4 77.77(6) 2_656 2_656 ?
O13 Ca3 Ca4 40.73(5) 2_656 2_656 ?
O11 Ca3 Ca4 93.02(5) 2_656 2_656 ?
O15 Ca3 Ca4 89.86(5) 1_655 2_656 ?
Si5 Ca3 Ca4 65.89(2) 3_666 2_656 ?
Si5 Ca3 Ca4 60.13(2) 2_656 2_656 ?
Si6 Ca3 Ca4 90.22(3) 2_656 2_656 ?
O9 Ca4 O12 93.27(8) . 2_646 ?
O9 Ca4 F7 85.48(7) . . ?
O12 Ca4 F7 89.15(7) 2_646 . ?
O9 Ca4 O15 79.31(8) . 1_655 ?
O12 Ca4 O15 167.50(8) 2_646 1_655 ?
F7 Ca4 O15 80.31(7) . 1_655 ?
O9 Ca4 O14 164.70(8) . . ?
O12 Ca4 O14 76.23(8) 2_646 . ?
F7 Ca4 O14 83.30(7) . . ?
O15 Ca4 O14 108.87(8) 1_655 . ?
O9 Ca4 O13 77.87(7) . . ?
O12 Ca4 O13 81.98(8) 2_646 . ?
F7 Ca4 O13 160.59(7) . . ?
O15 Ca4 O13 105.95(8) 1_655 . ?
O14 Ca4 O13 110.99(8) . . ?
O9 Ca4 Si5 100.51(5) . . ?
O12 Ca4 Si5 88.99(5) 2_646 . ?
F7 Ca4 Si5 173.82(5) . . ?
O15 Ca4 Si5 102.17(6) 1_655 . ?
O14 Ca4 Si5 90.54(6) . . ?
O13 Ca4 Si5 24.16(5) . . ?
O9 Ca4 Ca2 40.03(5) . . ?
O12 Ca4 Ca2 87.33(6) 2_646 . ?
F7 Ca4 Ca2 124.93(5) . . ?
O15 Ca4 Ca2 93.19(6) 1_655 . ?
O14 Ca4 Ca2 147.44(6) . . ?
O13 Ca4 Ca2 37.85(5) . . ?
Si5 Ca4 Ca2 60.85(2) . . ?
O9 Ca4 Ca3 87.89(6) . 2_646 ?
O12 Ca4 Ca3 37.91(5) 2_646 2_646 ?
F7 Ca4 Ca3 126.07(5) . 2_646 ?
O15 Ca4 Ca3 149.88(6) 1_655 2_646 ?
O14 Ca4 Ca3 90.33(6) . 2_646 ?
O13 Ca4 Ca3 44.26(5) . 2_646 ?
Si5 Ca4 Ca3 53.287(19) . 2_646 ?
Ca2 Ca4 Ca3 60.82(2) . 2_646 ?
O9 Ca4 Ca1 42.62(6) . 1_655 ?
O12 Ca4 Ca1 135.87(6) 2_646 1_655 ?
F7 Ca4 Ca1 88.40(5) . 1_655 ?
O15 Ca4 Ca1 37.97(6) 1_655 1_655 ?
O14 Ca4 Ca1 146.83(6) . 1_655 ?
O13 Ca4 Ca1 86.09(5) . 1_655 ?
Si5 Ca4 Ca1 97.03(3) . 1_655 ?
Ca2 Ca4 Ca1 59.135(17) . 1_655 ?
Ca3 Ca4 Ca1 119.93(2) 2_646 1_655 ?
O9 Ca4 Ca2 120.61(5) . 2_656 ?
O12 Ca4 Ca2 80.54(6) 2_646 2_656 ?
F7 Ca4 Ca2 35.95(4) . 2_656 ?
O15 Ca4 Ca2 94.51(6) 1_655 2_656 ?
O14 Ca4 Ca2 47.36(6) . 2_656 ?
O13 Ca4 Ca2 155.13(5) . 2_656 ?
Si5 Ca4 Ca2 137.88(2) . 2_656 ?
Ca2 Ca4 Ca2 156.762(19) . 2_656 ?
Ca3 Ca4 Ca2 115.40(2) 2_646 2_656 ?
Ca1 Ca4 Ca2 118.75(2) 1_655 2_656 ?
O9 Ca4 Ca1 132.49(6) . . ?
O12 Ca4 Ca1 39.44(5) 2_646 . ?
F7 Ca4 Ca1 88.85(5) . . ?
O15 Ca4 Ca1 145.68(6) 1_655 . ?
O14 Ca4 Ca1 37.10(5) . . ?
O13 Ca4 Ca1 95.03(6) . . ?
Si5 Ca4 Ca1 85.98(3) . . ?
Ca2 Ca4 Ca1 119.25(2) . . ?
Ca3 Ca4 Ca1 58.577(17) 2_646 . ?
Ca1 Ca4 Ca1 174.63(2) 1_655 . ?
Ca2 Ca4 Ca1 60.390(18) 2_656 . ?
O15 Si5 O13 116.19(12) 3_566 . ?
O15 Si5 O12 109.03(12) 3_566 3_666 ?
O13 Si5 O12 117.38(11) . 3_666 ?
O15 Si5 O10 110.16(11) 3_566 . ?
O13 Si5 O10 101.35(11) . . ?
O12 Si5 O10 101.15(11) 3_666 . ?
O15 Si5 Ca3 63.96(8) 3_566 3_666 ?
O13 Si5 Ca3 155.19(8) . 3_666 ?
O12 Si5 Ca3 47.98(8) 3_666 3_666 ?
O10 Si5 Ca3 101.46(8) . 3_666 ?
O15 Si5 Ca3 140.52(8) 3_566 2_646 ?
O13 Si5 Ca3 52.68(8) . 2_646 ?
O12 Si5 Ca3 108.73(8) 3_666 2_646 ?
O10 Si5 Ca3 50.83(8) . 2_646 ?
Ca3 Si5 Ca3 144.03(3) 3_666 2_646 ?
O15 Si5 Ca1 126.41(9) 3_566 4_565 ?
O13 Si5 Ca1 117.08(9) . 4_565 ?
O12 Si5 Ca1 48.10(8) 3_666 4_565 ?
O10 Si5 Ca1 53.35(8) . 4_565 ?
Ca3 Si5 Ca1 70.41(2) 3_666 4_565 ?
Ca3 Si5 Ca1 74.02(3) 2_646 4_565 ?
O15 Si5 Ca4 84.33(9) 3_566 . ?
O13 Si5 Ca4 37.66(8) . . ?
O12 Si5 Ca4 153.16(8) 3_666 . ?
O10 Si5 Ca4 95.46(8) . . ?
Ca3 Si5 Ca4 147.58(3) 3_666 . ?
Ca3 Si5 Ca4 66.58(2) 2_646 . ?
Ca1 Si5 Ca4 140.24(3) 4_565 . ?
O15 Si5 Ca1 34.88(8) 3_566 3_566 ?
O13 Si5 Ca1 124.26(8) . 3_566 ?
O12 Si5 Ca1 117.79(8) 3_666 3_566 ?
O10 Si5 Ca1 75.29(8) . 3_566 ?
Ca3 Si5 Ca1 71.42(2) 3_666 3_566 ?
Ca3 Si5 Ca1 113.79(3) 2_646 3_566 ?
Ca1 Si5 Ca1 104.93(3) 4_565 3_566 ?
Ca4 Si5 Ca1 86.69(2) . 3_566 ?
O15 Si5 Ca2 124.01(9) 3_566 . ?
O13 Si5 Ca2 26.71(8) . . ?
O12 Si5 Ca2 91.73(8) 3_666 . ?
O10 Si5 Ca2 115.96(8) . . ?
Ca3 Si5 Ca2 130.36(3) 3_666 . ?
Ca3 Si5 Ca2 65.53(2) 2_646 . ?
Ca1 Si5 Ca2 106.44(3) 4_565 . ?
Ca4 Si5 Ca2 61.90(2) . . ?
Ca1 Si5 Ca2 146.71(3) 3_566 . ?
O9 Si6 O14 109.34(12) 4_465 3_566 ?
O9 Si6 O11 116.57(12) 4_465 . ?
O14 Si6 O11 117.10(12) 3_566 . ?
O9 Si6 O10 101.20(12) 4_465 . ?
O14 Si6 O10 109.64(11) 3_566 . ?
O11 Si6 O10 101.21(11) . . ?
O9 Si6 Ca2 49.33(8) 4_465 4_465 ?
O14 Si6 Ca2 63.98(8) 3_566 4_465 ?
O11 Si6 Ca2 157.97(8) . 4_465 ?
O10 Si6 Ca2 98.62(8) . 4_465 ?
O9 Si6 Ca3 108.32(9) 4_465 2_646 ?
O14 Si6 Ca3 140.26(9) 3_566 2_646 ?
O11 Si6 Ca3 53.13(8) . 2_646 ?
O10 Si6 Ca3 50.11(8) . 2_646 ?
Ca2 Si6 Ca3 141.42(3) 4_465 2_646 ?
O9 Si6 Ca1 48.83(8) 4_465 4_565 ?
O14 Si6 Ca1 125.54(8) 3_566 4_565 ?
O11 Si6 Ca1 116.90(9) . 4_565 ?
O10 Si6 Ca1 52.59(8) . 4_565 ?
Ca2 Si6 Ca1 68.88(2) 4_465 4_565 ?
Ca3 Si6 Ca1 73.35(3) 2_646 4_565 ?
O9 Si6 Ca1 149.38(8) 4_465 . ?
O14 Si6 Ca1 86.72(8) 3_566 . ?
O11 Si6 Ca1 34.94(8) . . ?
O10 Si6 Ca1 97.30(8) . . ?
Ca2 Si6 Ca1 149.98(3) 4_465 . ?
Ca3 Si6 Ca1 66.50(2) 2_646 . ?
Ca1 Si6 Ca1 139.79(3) 4_565 . ?
O9 Si6 Ca1 118.58(8) 4_465 3_566 ?
O14 Si6 Ca1 35.43(7) 3_566 3_566 ?
O11 Si6 Ca1 124.47(8) . 3_566 ?
O10 Si6 Ca1 74.23(8) . 3_566 ?
Ca2 Si6 Ca1 70.42(2) 4_465 3_566 ?
Ca3 Si6 Ca1 112.30(3) 2_646 3_566 ?
Ca1 Si6 Ca1 103.65(2) 4_565 3_566 ?
Ca1 Si6 Ca1 89.80(2) . 3_566 ?
O9 Si6 Ca2 87.18(8) 4_465 1_455 ?
O14 Si6 Ca2 124.81(8) 3_566 1_455 ?
O11 Si6 Ca2 30.83(8) . 1_455 ?
O10 Si6 Ca2 118.32(8) . 1_455 ?
Ca2 Si6 Ca2 128.55(3) 4_465 1_455 ?
Ca3 Si6 Ca2 69.09(2) 2_646 1_455 ?
Ca1 Si6 Ca2 105.29(3) 4_565 1_455 ?
Ca1 Si6 Ca2 62.50(2) . 1_455 ?
Ca1 Si6 Ca2 149.90(3) 3_566 1_455 ?
Ca3 F7 Ca2 104.38(7) . 2_656 ?
Ca3 F7 Ca4 110.19(7) . . ?
Ca2 F7 Ca4 107.76(7) 2_656 . ?
Ca3 F7 Ca2 105.41(7) . 4_566 ?
Ca2 F7 Ca2 106.20(7) 2_656 4_566 ?
Ca4 F7 Ca2 121.59(8) . 4_566 ?
Ca1 F8 Ca3 114.45(8) 3_667 . ?
Ca1 F8 Ca2 110.20(7) 3_667 4_566 ?
Ca3 F8 Ca2 105.85(7) . 4_566 ?
Ca1 F8 Ca3 110.08(7) 3_667 3_767 ?
Ca3 F8 Ca3 107.75(7) . 3_767 ?
Ca2 F8 Ca3 108.27(7) 4_566 3_767 ?
Si6 O9 Ca4 147.14(12) 4_666 . ?
Si6 O9 Ca2 99.91(11) 4_666 . ?
Ca4 O9 Ca2 101.65(8) . . ?
Si6 O9 Ca1 102.90(10) 4_666 1_655 ?
Ca4 O9 Ca1 99.84(8) . 1_655 ?
Ca2 O9 Ca1 94.42(7) . 1_655 ?
Si5 O10 Si6 155.37(15) . . ?
Si5 O10 Ca3 98.39(10) . 2_646 ?
Si6 O10 Ca3 99.38(9) . 2_646 ?
Si5 O10 Ca1 96.58(9) . 4_565 ?
Si6 O10 Ca1 97.60(10) . 4_565 ?
Ca3 O10 Ca1 98.28(8) 2_646 4_565 ?
Si6 O11 Ca2 128.15(11) . 1_455 ?
Si6 O11 Ca1 121.60(12) . . ?
Ca2 O11 Ca1 103.23(7) 1_455 . ?
Si6 O11 Ca3 97.11(9) . 2_646 ?
Ca2 O11 Ca3 102.99(8) 1_455 2_646 ?
Ca1 O11 Ca3 96.14(7) . 2_646 ?
Si5 O12 Ca3 100.88(11) 3_666 . ?
Si5 O12 Ca4 138.87(12) 3_666 2_656 ?
Ca3 O12 Ca4 104.17(8) . 2_656 ?
Si5 O12 Ca1 103.27(10) 3_666 2_656 ?
Ca3 O12 Ca1 98.61(8) . 2_656 ?
Ca4 O12 Ca1 104.57(8) 2_656 2_656 ?
Si5 O13 Ca2 134.79(12) . . ?
Si5 O13 Ca4 118.18(12) . . ?
Ca2 O13 Ca4 101.85(8) . . ?
Si5 O13 Ca3 97.45(10) . 2_646 ?
Ca2 O13 Ca3 99.17(8) . 2_646 ?
Ca4 O13 Ca3 95.01(7) . 2_646 ?
Si6 O14 Ca1 121.68(11) 3_566 . ?
Si6 O14 Ca4 132.49(11) 3_566 . ?
Ca1 O14 Ca4 105.80(9) . . ?
Si6 O14 Ca2 84.87(10) 3_566 2_656 ?
Ca1 O14 Ca2 94.78(7) . 2_656 ?
Ca4 O14 Ca2 93.49(7) . 2_656 ?
Si5 O15 Ca1 122.21(11) 3_566 . ?
Si5 O15 Ca4 133.36(12) 3_566 1_455 ?
Ca1 O15 Ca4 103.97(9) . 1_455 ?
Si5 O15 Ca3 84.68(10) 3_566 1_455 ?
Ca1 O15 Ca3 96.74(8) . 1_455 ?
Ca4 O15 Ca3 96.87(7) 1_455 1_455 ?
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
Ca1 F8 2.3093(18) 3_667 ?
Ca1 O11 2.323(2) . ?
Ca1 O15 2.359(2) . ?
Ca1 O14 2.399(2) . ?
Ca1 O12 2.513(2) 2_646 ?
Ca1 O9 2.557(2) 1_455 ?
Ca1 O10 2.653(2) 4_566 ?
Ca1 Si5 3.2853(11) 4_566 ?
Ca1 Si6 3.3113(10) 4_566 ?
Ca1 Si6 3.4547(11) . ?
Ca1 Si5 3.4895(11) 3_566 ?
Ca1 Si6 3.5222(11) 3_566 ?
Ca2 O13 2.278(2) . ?
Ca2 O11 2.307(2) 1_655 ?
Ca2 F7 2.3388(18) 2_646 ?
Ca2 F8 2.3647(18) 4_565 ?
Ca2 F7 2.3761(18) 4_565 ?
Ca2 O9 2.386(2) . ?
Ca2 O14 2.796(2) 2_646 ?
Ca2 Si6 3.0993(11) 4_666 ?
Ca2 Si6 3.5403(10) 1_655 ?
Ca2 Si5 3.5976(11) . ?
Ca2 Ca1 3.6298(10) 1_655 ?
Ca2 Ca4 3.6339(9) . ?
Ca3 O12 2.323(2) . ?
Ca3 F8 2.3363(18) . ?
Ca3 F7 2.3384(19) . ?
Ca3 F8 2.3813(19) 3_767 ?
Ca3 O10 2.510(2) 2_656 ?
Ca3 O13 2.569(2) 2_656 ?
Ca3 O11 2.602(2) 2_656 ?
Ca3 O15 2.771(2) 1_655 ?
Ca3 Si5 3.0713(11) 3_666 ?
Ca3 Si5 3.2028(10) 2_656 ?
Ca3 Si6 3.2276(11) 2_656 ?
Ca3 Ca4 3.6663(10) 2_656 ?
Ca4 O9 2.301(2) . ?
Ca4 O12 2.324(2) 2_646 ?
Ca4 F7 2.3582(18) . ?
Ca4 O15 2.364(2) 1_655 ?
Ca4 O14 2.400(2) . ?
Ca4 O13 2.401(2) . ?
Ca4 Si5 3.4646(12) . ?
Ca4 Ca3 3.6663(10) 2_646 ?
Ca4 Ca1 3.7204(11) 1_655 ?
Ca4 Ca2 3.7942(10) 2_656 ?
Si5 O15 1.605(2) 3_566 ?
Si5 O13 1.609(2) . ?
Si5 O12 1.617(2) 3_666 ?
Si5 O10 1.657(2) . ?
Si5 Ca3 3.0713(11) 3_666 ?
Si5 Ca3 3.2028(10) 2_646 ?
Si5 Ca1 3.2853(11) 4_565 ?
Si5 Ca1 3.4895(11) 3_566 ?
Si6 O9 1.609(2) 4_465 ?
Si6 O14 1.610(2) 3_566 ?
Si6 O11 1.615(2) . ?
Si6 O10 1.661(2) . ?
Si6 Ca2 3.0993(11) 4_465 ?
Si6 Ca3 3.2276(11) 2_646 ?
Si6 Ca1 3.3113(10) 4_565 ?
Si6 Ca1 3.5222(11) 3_566 ?
Si6 Ca2 3.5403(10) 1_455 ?
F7 Ca2 2.3388(18) 2_656 ?
F7 Ca2 2.3761(18) 4_566 ?
F8 Ca1 2.3093(17) 3_667 ?
F8 Ca2 2.3647(18) 4_566 ?
F8 Ca3 2.3813(19) 3_767 ?
O9 Si6 1.609(2) 4_666 ?
O9 Ca1 2.557(2) 1_655 ?
O10 Ca3 2.510(2) 2_646 ?
O10 Ca1 2.653(2) 4_565 ?
O11 Ca2 2.307(2) 1_455 ?
O11 Ca3 2.602(2) 2_646 ?
O12 Si5 1.617(2) 3_666 ?
O12 Ca4 2.324(2) 2_656 ?
O12 Ca1 2.513(2) 2_656 ?
O13 Ca3 2.569(2) 2_646 ?
O14 Si6 1.610(2) 3_566 ?
O14 Ca2 2.796(2) 2_656 ?
O15 Si5 1.605(2) 3_566 ?
O15 Ca4 2.364(2) 1_455 ?
O15 Ca3 2.771(2) 1_455 ?
|
1100154.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100154.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_1100154
loop_
_publ_author_name
'Carlos Sanchez'
'Juan M. Salas'
'Miguel Quiros'
'M. Purificacion Sanchez'
_publ_section_title
;
trans-Dichloro bis(3-amino-1,2,4-triazolium-N^1^) copper(II)
tetrachlorocuprate(II) dihydrate.
;
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first m370
_journal_page_last m372
_journal_paper_doi 10.1107/S1600536804003812
_journal_volume 60
_journal_year 2004
_chemical_formula_moiety 'C4 H10 Cl2 Cu N8 2+, Cl4 Cu 2-, 2(H2 O)'
_chemical_formula_sum 'C4 H14 Cl6 Cu2 N8 O2'
_chemical_formula_weight 546.01
_chemical_name_systematic
;
trans-Dichloro bis(3-amino-1,2,4-triazolium-N^1^) copper(II)
tetrachlorocuprate(II) dihydrate.
;
_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 heavy
_atom_sites_solution_secondary difmap
_cell_angle_alpha 95.0132(15)
_cell_angle_beta 99.9045(15)
_cell_angle_gamma 110.2812(14)
_cell_formula_units_Z 1
_cell_length_a 6.1505(6)
_cell_length_b 7.6367(8)
_cell_length_c 9.7197(10)
_cell_measurement_reflns_used 3558
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.98
_cell_measurement_theta_min 3.62
_cell_volume 416.47(7)
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 66.06
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type 'Bruker SMART APEX CCD system'
_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 0.0148
_diffrn_reflns_av_sigmaI/netI 0.0163
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 4759
_diffrn_reflns_theta_full 25.00
_diffrn_reflns_theta_max 28.28
_diffrn_reflns_theta_min 2.15
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 3.531
_exptl_absorpt_correction_T_max 0.5105
_exptl_absorpt_correction_T_min 0.4216
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour green
_exptl_crystal_density_diffrn 2.177
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prismatic
_exptl_crystal_F_000 270
_exptl_crystal_size_max 0.26
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.22
_refine_diff_density_max 0.299
_refine_diff_density_min -0.331
_refine_diff_density_rms 0.062
_refine_ls_extinction_coef 0.079(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 1.083
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 110
_refine_ls_number_reflns 1867
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.086
_refine_ls_R_factor_all 0.0184
_refine_ls_R_factor_gt 0.0177
_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^)+(0.0200P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0457
_refine_ls_wR_factor_ref 0.0461
_reflns_number_gt 1800
_reflns_number_total 1867
_reflns_threshold_expression >2sigma(I)
_cod_duplicate_entry 2203434
_cod_database_code 1100154
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 0.5000 0.5000 0.0000 0.02586(9) Uani 1 2 d S . .
Cl1 Cl 0.70181(7) 0.54832(5) 0.23901(4) 0.02737(11) Uani 1 1 d . . .
Cl2 Cl 0.77967(7) 0.76437(6) -0.03392(4) 0.02997(11) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.5000 0.5000 0.02415(9) Uani 1 2 d S . .
Cl3 Cl 0.31753(7) 0.70168(5) 0.43559(4) 0.02755(11) Uani 1 1 d . . .
N1 N 0.2106(2) 0.27671(18) 0.39413(14) 0.0228(3) Uani 1 1 d . . .
N2 N 0.0043(2) 0.29145(18) 0.32524(14) 0.0233(3) Uani 1 1 d . . .
H2 H -0.0185 0.3961 0.3220 0.028 Uiso 1 1 d R . .
C3 C -0.1552(3) 0.1224(2) 0.26424(16) 0.0234(3) Uani 1 1 d . . .
N3 N -0.3714(3) 0.0830(2) 0.19151(17) 0.0338(3) Uani 1 1 d . . .
H31 H -0.4240 0.1724 0.1791 0.041 Uiso 1 1 d R . .
H32 H -0.4607 -0.0321 0.1563 0.041 Uiso 1 1 d R . .
N4 N -0.0499(2) -0.00194(19) 0.29491(15) 0.0274(3) Uani 1 1 d . . .
H4 H -0.1124 -0.1226 0.2697 0.033 Uiso 1 1 d R . .
C5 C 0.1719(3) 0.0977(2) 0.37260(18) 0.0268(3) Uani 1 1 d . . .
H5 H 0.2821 0.0447 0.4059 0.032 Uiso 1 1 d R . .
O1W O 0.2751(2) 0.7072(2) 0.09221(15) 0.0383(3) Uani 1 1 d D . .
H1W H 0.258(4) 0.672(3) 0.169(2) 0.046 Uiso 1 1 d D . .
H2W H 0.148(3) 0.708(3) 0.056(2) 0.046 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
Cu1 0.02404(15) 0.02084(15) 0.02380(15) 0.00270(11) -0.00190(11) 0.00095(11)
Cl1 0.0289(2) 0.02138(19) 0.0266(2) 0.00148(14) -0.00315(15) 0.00780(15)
Cl2 0.0254(2) 0.0263(2) 0.0300(2) 0.00453(15) 0.00337(15) 0.00069(15)
Cu2 0.02161(15) 0.01495(14) 0.03194(16) -0.00035(10) -0.00269(11) 0.00688(11)
Cl3 0.0283(2) 0.02016(19) 0.0324(2) 0.00104(15) -0.00179(15) 0.01148(15)
N1 0.0226(6) 0.0191(6) 0.0250(7) 0.0012(5) 0.0015(5) 0.0080(5)
N2 0.0220(6) 0.0174(6) 0.0293(7) 0.0012(5) 0.0016(5) 0.0080(5)
C3 0.0255(7) 0.0201(7) 0.0228(7) 0.0009(6) 0.0040(6) 0.0075(6)
N3 0.0262(7) 0.0235(7) 0.0437(9) -0.0016(6) -0.0054(6) 0.0073(6)
N4 0.0291(7) 0.0150(6) 0.0322(7) -0.0016(5) -0.0013(6) 0.0058(5)
C5 0.0285(8) 0.0197(8) 0.0295(8) 0.0013(6) -0.0012(6) 0.0095(6)
O1W 0.0312(7) 0.0436(8) 0.0376(7) 0.0091(6) 0.0056(6) 0.0109(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'
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'
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
Cl2 Cu1 Cl2 180.0 . 2_665 n
Cl2 Cu1 Cl1 89.901(15) . . y
Cl2 Cu1 Cl1 90.099(15) 2_665 . n
Cl2 Cu1 Cl1 90.099(15) . 2_665 n
Cl2 Cu1 Cl1 89.900(15) 2_665 2_665 n
Cl1 Cu1 Cl1 180.0 . 2_665 n
N1 Cu2 N1 180.0 2_666 . n
N1 Cu2 Cl3 89.47(4) 2_666 . n
N1 Cu2 Cl3 90.53(4) . . y
N1 Cu2 Cl3 90.53(4) 2_666 2_666 n
N1 Cu2 Cl3 89.47(4) . 2_666 n
Cl3 Cu2 Cl3 180.0 . 2_666 n
C5 N1 N2 104.80(13) . . y
C5 N1 Cu2 131.20(11) . . y
N2 N1 Cu2 124.00(10) . . y
C3 N2 N1 110.98(13) . . y
C3 N2 H2 124.5 . . n
N1 N2 H2 124.5 . . n
N3 C3 N2 127.60(15) . . y
N3 C3 N4 126.81(15) . . y
N2 C3 N4 105.58(13) . . y
C3 N3 H31 119.9 . . n
C3 N3 H32 120.1 . . n
H31 N3 H32 120.0 . . n
C3 N4 C5 107.61(13) . . y
C3 N4 H4 126.1 . . n
C5 N4 H4 126.2 . . n
N1 C5 N4 111.03(14) . . y
N1 C5 H5 124.4 . . n
N4 C5 H5 124.6 . . n
H1W O1W H2W 105(2) . . n
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 Cl2 2.2467(4) . y
Cu1 Cl2 2.2467(4) 2_665 n
Cu1 Cl1 2.3695(4) . y
Cu1 Cl1 2.3695(4) 2_665 n
Cu2 N1 2.0233(13) 2_666 n
Cu2 N1 2.0233(13) . y
Cu2 Cl3 2.2691(4) . y
Cu2 Cl3 2.2691(4) 2_666 n
N1 C5 1.295(2) . y
N1 N2 1.3749(18) . y
N2 C3 1.330(2) . y
N2 H2 0.8600 . n
C3 N3 1.312(2) . y
C3 N4 1.349(2) . y
N3 H31 0.8600 . n
N3 H32 0.8600 . n
N4 C5 1.355(2) . y
N4 H4 0.8600 . n
C5 H5 0.9300 . n
O1W H1W 0.828(16) . n
O1W H2W 0.806(16) . n
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
_geom_hbond_publ_flag
N2 H2 Cl1 0.86 2.46 3.2084(14) 146.4 1_455 y
N3 H32 O1W 0.86 2.05 2.892(2) 167.8 1_445 y
N4 H4 Cl1 0.86 2.34 3.1899(14) 170.3 1_445 y
O1W H1W Cl3 0.828(16) 2.529(18) 3.3078(15) 157(2) . y
O1W H2W Cl2 0.806(16) 2.475(17) 3.2728(15) 171(2) 1_455 y
|
1100155.cif | #------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100155.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_1100155
_chemical_formula_moiety 'C35 H46 Cl2 I N3 O2 Ni '
_chemical_formula_sum 'C35 H46 Cl2 I N3 Ni O2'
_chemical_formula_weight 797.28
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_cell_setting monoclinic
_symmetry_Int_Tables_number 14
_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 104.82(2)
_cell_angle_gamma 90
_cell_formula_units_Z 6
_cell_length_a 12.78(2)
_cell_length_b 17.04(3)
_cell_length_c 19.13(5)
_cell_measurement_reflns_used 155
_cell_measurement_temperature 173.1
_cell_measurement_theta_max 35.0
_cell_measurement_theta_min 1.6
_cell_volume 4027.5(14)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.9608
_diffrn_measured_fraction_theta_max 0.8587
_diffrn_measurement_device_type 'Rigaku Mercury'
_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 17
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_number 51956
_diffrn_reflns_theta_full 28.00
_diffrn_reflns_theta_max 34.82
_exptl_absorpt_coefficient_mu 2.117
_exptl_absorpt_correction_T_max 0.655
_exptl_absorpt_correction_T_min 0.363
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.972
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 2448.00
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.20
_refine_diff_density_max 3.44
_refine_diff_density_min -1.34
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.346
_refine_ls_hydrogen_treatment ?
_refine_ls_number_parameters 416
_refine_ls_number_reflns 9669
_refine_ls_R_factor_gt 0.1260
_refine_ls_shift/su_max 2.2830
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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_ref 0.3740
_reflns_number_gt 24769
_reflns_number_total 51956
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_cod_original_formula_sum 'C35 H46 Cl2 I N3 O2 Ni '
_cod_database_code 1100155
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
_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
I(1) I 0.23492(5) 0.22706(4) 0.33999(3) 0.0404(3) Uani 1.00 1 d . . .
Ni(2) Ni 0.09487(9) -0.04544(6) 0.56227(6) 0.0305(3) Uani 1.00 1 d . . .
Cl(1) Cl 0.4349(4) 0.6714(4) 0.0346(2) 0.105(2) Uani 1.00 1 d . . .
Cl(2) Cl 0.3512(6) 0.6736(9) 0.1561(4) 0.241(6) Uani 1.00 1 d . . .
Cl(3) Cl 0.3787(5) 0.4738(5) 0.2848(5) 0.163(3) Uani 1.00 1 d . . .
Cl(4) Cl 0.5452(9) 0.4416(7) 0.4173(6) 0.213(4) Uani 1.00 1 d . . .
N(1) N 0.0503(6) -0.0155(4) 0.6470(4) 0.033(2) Uani 1.00 1 d . . .
N(2) N 0.1688(5) 0.0501(4) 0.5799(4) 0.028(1) Uani 1.00 1 d . . .
N(3) N 0.1650(6) -0.0506(4) 0.4849(4) 0.038(2) Uani 1.00 1 d . . .
C(1) C 0.0298(8) -0.1488(6) 0.5474(6) 0.044(2) Uani 1.00 1 d . . .
C(2) C 0.1631(8) -0.1097(5) 0.4371(5) 0.038(2) Uani 1.00 1 d . . .
C(3) C 0.2218(8) -0.1091(5) 0.3876(6) 0.039(2) Uani 1.00 1 d . . .
C(4) C 0.2920(7) -0.0474(5) 0.3832(5) 0.035(2) Uani 1.00 1 d . . .
C(5) C 0.2907(8) 0.0167(5) 0.4318(5) 0.034(2) Uani 1.00 1 d . . .
C(6) C 0.2273(7) 0.0134(5) 0.4795(5) 0.033(2) Uani 1.00 1 d . . .
C(7) C 0.2260(7) 0.0754(5) 0.5334(4) 0.028(2) Uani 1.00 1 d . . .
C(8) C 0.2758(6) 0.1474(5) 0.5419(4) 0.029(2) Uani 1.00 1 d . . .
C(9) C 0.2663(7) 0.1958(5) 0.6003(5) 0.032(2) Uani 1.00 1 d . . .
C(10) C 0.2080(7) 0.1685(5) 0.6489(5) 0.035(2) Uani 1.00 1 d . . .
C(11) C 0.1590(7) 0.0947(5) 0.6349(5) 0.036(2) Uani 1.00 1 d . . .
C(12) C 0.0931(7) 0.0552(5) 0.6772(5) 0.034(2) Uani 1.00 1 d . . .
C(13) C 0.0814(7) 0.0795(5) 0.7427(5) 0.035(2) Uani 1.00 1 d . . .
C(14) C 0.0188(8) 0.0381(5) 0.7808(5) 0.037(2) Uani 1.00 1 d . . .
C(15) C -0.0309(8) -0.0328(6) 0.7464(6) 0.040(2) Uani 1.00 1 d . . .
C(16) C -0.0144(8) -0.0553(5) 0.6810(5) 0.037(2) Uani 1.00 1 d . . .
C(17) C 0.0096(9) 0.0621(6) 0.8556(5) 0.043(2) Uani 1.00 1 d . . .
C(18) C -0.0613(11) 0.0084(6) 0.8864(6) 0.059(3) Uani 1.00 1 d . . .
C(19) C 0.1293(10) 0.0557(7) 0.9075(6) 0.056(3) Uani 1.00 1 d . . .
C(20) C -0.0304(11) 0.1469(7) 0.8527(6) 0.054(3) Uani 1.00 1 d . . .
C(21) C 0.3171(8) 0.2785(4) 0.6107(5) 0.033(2) Uani 1.00 1 d . . .
C(22) C 0.3693(8) -0.0464(6) 0.3362(5) 0.040(2) Uani 1.00 1 d . . .
C(23) C 0.4876(11) -0.0486(11) 0.3831(8) 0.085(5) Uani 1.00 1 d . . .
C(24) C 0.355(2) -0.1182(8) 0.2859(11) 0.098(6) Uani 1.00 1 d . . .
C(25) C 0.3530(12) 0.0259(7) 0.2870(7) 0.064(3) Uani 1.00 1 d . . .
C(26) C 0.2273(8) 0.3390(6) 0.6129(7) 0.049(3) Uani 1.00 1 d . . .
C(27) C 0.4031(9) 0.2783(6) 0.6853(6) 0.046(2) Uani 1.00 1 d . . .
C(28) C 0.3705(10) 0.3017(6) 0.5514(6) 0.052(3) Uani 1.00 1 d . . .
C(29) C 0.829(2) 0.1955(9) 0.2215(10) 0.087(5) Uani 1.00 1 d . . .
C(30) C 0.733(2) 0.1696(9) 0.1767(10) 0.084(5) Uani 1.00 1 d . . .
C(31) C 0.7257(12) 0.1620(8) 0.1064(10) 0.073(4) Uani 1.00 1 d . . .
C(32) C 0.815(1) 0.1742(7) 0.0744(9) 0.076(4) Uani 1.00 1 d . . .
C(33) C 0.9173(12) 0.1964(7) 0.1246(12) 0.084(5) Uani 1.00 1 d . . .
C(34) C 0.922(2) 0.2083(8) 0.1974(9) 0.078(5) Uani 1.00 1 d . . .
C(35) C 0.450(1) 0.7088(12) 0.1241(10) 0.092(5) Uani 1.00 1 d . . .
C(37) C 0.413(3) 0.4422(13) 0.386(2) 0.177(13) Uani 1.00 1 d . . .
C(40) C 0.795(2) 0.160(1) -0.0056(12) 0.121(8) Uani 1.00 1 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 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
I I -0.474 1.812
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ni Ni 0.339 1.112
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
|
1100156.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100156.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_1100156
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C22 H22 N4 Ni O6'
_chemical_formula_weight 497.15
_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 106.910(7)
_cell_angle_beta 110.208(6)
_cell_angle_gamma 90.172(7)
_cell_formula_units_Z 2
_cell_length_a 9.170(3)
_cell_length_b 10.936(3)
_cell_length_c 12.717(4)
_cell_measurement_temperature 293(2)
_cell_volume 1137.4(6)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.800
_diffrn_measured_fraction_theta_max 0.800
_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 0.0628
_diffrn_reflns_av_sigmaI/netI 0.3102
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 6291
_diffrn_reflns_theta_full 28.03
_diffrn_reflns_theta_max 28.03
_diffrn_reflns_theta_min 1.80
_exptl_absorpt_coefficient_mu 0.899
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7469
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.452
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 516
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.07
_exptl_crystal_size_min 0.06
_refine_diff_density_max 0.286
_refine_diff_density_min -0.341
_refine_diff_density_rms 0.063
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.644
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 306
_refine_ls_number_reflns 4405
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 0.644
_refine_ls_R_factor_all 0.1784
_refine_ls_R_factor_gt 0.0541
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0629
_refine_ls_wR_factor_ref 0.0816
_reflns_number_gt 1452
_reflns_number_total 4405
_reflns_threshold_expression >2sigma(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.
'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-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
The following automatic conversions were performed:
'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^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^)+(0.0000P)^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-1
_cod_database_code 1100156
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
Ni Ni 0.24243(9) 0.24080(8) 0.49120(7) 0.0389(2) Uani 1 d . . .
O11 O 0.2049(4) 0.4045(3) 0.4461(3) 0.0397(10) Uani 1 d . . .
O12 O 0.0315(4) 0.5157(3) 0.3550(3) 0.0437(10) Uani 1 d . . .
O13 O 0.0133(4) 0.1985(4) 0.3616(3) 0.0392(10) Uani 1 d D . .
C11 C 0.0692(6) 0.4201(5) 0.3883(4) 0.0309(14) Uani 1 d . . .
C12 C -0.0612(5) 0.3098(5) 0.3567(4) 0.0316(14) Uani 1 d . . .
H12 H -0.1047 0.3312 0.4193 0.038 Uiso 1 calc R . .
C13 C -0.1945(6) 0.2945(5) 0.2417(5) 0.0359(14) Uani 1 d . . .
C14 C -0.2053(7) 0.2016(7) 0.1414(6) 0.071(2) Uani 1 d . . .
H14 H -0.1325 0.1425 0.1421 0.085 Uiso 1 calc R . .
C15 C -0.3274(8) 0.1955(8) 0.0368(6) 0.095(3) Uani 1 d . . .
H15 H -0.3336 0.1324 -0.0324 0.114 Uiso 1 calc R . .
C16 C -0.4360(9) 0.2774(8) 0.0326(6) 0.090(3) Uani 1 d . . .
H16 H -0.5164 0.2715 -0.0381 0.108 Uiso 1 calc R . .
C17 C -0.4262(7) 0.3686(7) 0.1332(8) 0.085(3) Uani 1 d . . .
H17 H -0.5015 0.4256 0.1317 0.102 Uiso 1 calc R . .
C18 C -0.3064(7) 0.3790(6) 0.2385(5) 0.0592(18) Uani 1 d . . .
H18 H -0.3012 0.4426 0.3071 0.071 Uiso 1 calc R . .
O21 O 0.2420(4) 0.0809(3) 0.5412(3) 0.0419(11) Uani 1 d . . .
O22 O 0.1827(4) -0.0106(3) 0.6587(3) 0.0453(11) Uani 1 d . . .
O23 O 0.1401(4) 0.2943(4) 0.6207(3) 0.0437(11) Uani 1 d D . .
C21 C 0.1770(5) 0.0777(5) 0.6120(5) 0.0334(15) Uani 1 d . . .
C22 C 0.0817(5) 0.1882(5) 0.6429(4) 0.0334(14) Uani 1 d . . .
H22 H -0.0263 0.1619 0.5873 0.040 Uiso 1 calc R . .
C23 C 0.0774(6) 0.2226(6) 0.7649(5) 0.0370(15) Uani 1 d . . .
C24 C -0.0007(7) 0.1388(6) 0.7953(6) 0.074(2) Uani 1 d . . .
H24 H -0.0502 0.0607 0.7391 0.089 Uiso 1 calc R . .
C25 C -0.0084(10) 0.1670(9) 0.9077(9) 0.104(3) Uani 1 d . . .
H25 H -0.0631 0.1096 0.9261 0.125 Uiso 1 calc R . .
C26 C 0.0653(11) 0.2791(10) 0.9881(8) 0.111(4) Uani 1 d . . .
H26 H 0.0640 0.2972 1.0639 0.133 Uiso 1 calc R . .
C27 C 0.1425(8) 0.3682(8) 0.9635(7) 0.096(3) Uani 1 d . . .
H27 H 0.1875 0.4476 1.0194 0.115 Uiso 1 calc R . .
C28 C 0.1512(6) 0.3349(7) 0.8498(6) 0.063(2) Uani 1 d . . .
H28 H 0.2090 0.3913 0.8327 0.076 Uiso 1 calc R . .
N1 N 0.3350(5) 0.1609(4) 0.3662(4) 0.0430(13) Uani 1 d . . .
N2 N 0.5156(6) 0.0886(5) 0.2955(5) 0.0640(16) Uani 1 d . . .
H20 H 0.5979 0.0542 0.2897 0.077 Uiso 1 calc R . .
C1 C 0.4677(7) 0.1082(6) 0.3846(6) 0.0576(19) Uani 1 d . . .
H1 H 0.5209 0.0875 0.4528 0.069 Uiso 1 calc R . .
C3 C 0.4101(8) 0.1331(7) 0.2142(6) 0.078(2) Uani 1 d . . .
H3 H 0.4138 0.1340 0.1422 0.093 Uiso 1 calc R . .
C2 C 0.2997(6) 0.1757(6) 0.2582(5) 0.0600(19) Uani 1 d . . .
H2 H 0.2119 0.2103 0.2202 0.072 Uiso 1 calc R . .
N3 N 0.4590(5) 0.3143(4) 0.6127(4) 0.0423(14) Uani 1 d . . .
N4 N 0.7074(5) 0.3904(4) 0.6804(5) 0.0563(15) Uani 1 d . . .
H40 H 0.7919 0.4287 0.6843 0.068 Uiso 1 calc R . .
C4 C 0.5678(7) 0.3752(6) 0.5969(5) 0.0594(19) Uani 1 d . . .
H4 H 0.5492 0.4055 0.5327 0.071 Uiso 1 calc R . .
C6 C 0.6927(7) 0.3346(6) 0.7584(5) 0.064(2) Uani 1 d . . .
H6 H 0.7707 0.3283 0.8259 0.076 Uiso 1 calc R . .
C5 C 0.5375(7) 0.2894(6) 0.7158(5) 0.0544(18) Uani 1 d . . .
H5 H 0.4913 0.2473 0.7522 0.065 Uiso 1 calc R . .
H23 H 0.076(5) 0.356(4) 0.630(5) 0.08(2) Uiso 1 d D . .
H13 H -0.037(5) 0.135(4) 0.369(5) 0.07(2) Uiso 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
Ni 0.0318(4) 0.0410(5) 0.0525(5) 0.0248(4) 0.0173(4) 0.0094(4)
O11 0.026(2) 0.043(3) 0.052(3) 0.027(2) 0.006(2) 0.0029(19)
O12 0.035(2) 0.033(2) 0.073(3) 0.033(2) 0.018(2) 0.010(2)
O13 0.037(2) 0.024(2) 0.063(3) 0.024(2) 0.017(2) 0.004(2)
C11 0.028(3) 0.040(4) 0.026(4) 0.010(3) 0.011(3) 0.001(3)
C12 0.026(3) 0.033(4) 0.037(4) 0.012(3) 0.011(3) 0.006(3)
C13 0.033(4) 0.037(4) 0.043(4) 0.011(3) 0.022(3) 0.001(3)
C14 0.051(4) 0.113(7) 0.041(5) 0.014(5) 0.013(4) 0.014(4)
C15 0.063(5) 0.148(9) 0.056(6) 0.008(5) 0.021(5) 0.014(5)
C16 0.078(6) 0.126(9) 0.050(6) 0.029(5) 0.003(5) -0.005(6)
C17 0.032(4) 0.095(7) 0.119(7) 0.059(6) -0.003(5) 0.009(4)
C18 0.038(4) 0.048(5) 0.074(5) 0.011(4) 0.005(4) -0.001(4)
O21 0.043(2) 0.040(3) 0.054(3) 0.020(2) 0.026(2) 0.015(2)
O22 0.043(2) 0.037(3) 0.072(3) 0.036(2) 0.025(2) 0.010(2)
O23 0.050(3) 0.035(3) 0.062(3) 0.028(2) 0.028(2) 0.011(2)
C21 0.014(3) 0.033(4) 0.042(4) 0.007(3) 0.001(3) -0.006(3)
C22 0.030(3) 0.038(4) 0.036(4) 0.017(3) 0.012(3) 0.008(3)
C23 0.038(4) 0.035(4) 0.045(4) 0.020(4) 0.017(3) 0.012(3)
C24 0.112(6) 0.059(5) 0.094(6) 0.042(5) 0.073(5) 0.028(4)
C25 0.135(9) 0.104(8) 0.144(10) 0.075(7) 0.106(8) 0.061(7)
C26 0.127(9) 0.164(12) 0.088(8) 0.086(8) 0.054(7) 0.075(8)
C27 0.075(6) 0.114(8) 0.059(6) -0.008(5) 0.005(5) 0.023(5)
C28 0.049(4) 0.087(6) 0.049(5) 0.017(4) 0.015(4) 0.011(4)
N1 0.033(3) 0.054(4) 0.053(4) 0.026(3) 0.022(3) 0.010(3)
N2 0.062(4) 0.054(4) 0.101(5) 0.029(4) 0.054(4) 0.027(3)
C1 0.054(4) 0.064(5) 0.067(5) 0.028(4) 0.030(4) 0.022(4)
C3 0.092(6) 0.093(6) 0.088(6) 0.058(5) 0.057(5) 0.037(5)
C2 0.051(4) 0.096(6) 0.055(5) 0.041(4) 0.030(4) 0.036(4)
N3 0.036(3) 0.038(3) 0.058(4) 0.023(3) 0.017(3) -0.004(3)
N4 0.031(3) 0.056(4) 0.078(4) 0.022(3) 0.016(3) -0.005(3)
C4 0.051(5) 0.058(5) 0.070(5) 0.035(4) 0.011(4) 0.003(4)
C6 0.052(5) 0.077(6) 0.059(5) 0.037(4) 0.003(4) 0.005(4)
C5 0.042(4) 0.074(5) 0.058(5) 0.045(4) 0.010(4) 0.002(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
C C 0.0033 0.0016 '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
O21 Ni O11 169.40(14) . . ?
O21 Ni N3 93.05(18) . . ?
O11 Ni N3 93.24(17) . . ?
O21 Ni N1 94.40(17) . . ?
O11 Ni N1 94.03(17) . . ?
N3 Ni N1 90.92(18) . . ?
O21 Ni O23 77.03(15) . . ?
O11 Ni O23 94.26(15) . . ?
N3 Ni O23 91.71(18) . . ?
N1 Ni O23 171.15(18) . . ?
O21 Ni O13 97.12(14) . . ?
O11 Ni O13 76.31(14) . . ?
N3 Ni O13 169.49(18) . . ?
N1 Ni O13 90.90(17) . . ?
O23 Ni O13 88.04(15) . . ?
C11 O11 Ni 119.3(3) . . ?
C12 O13 Ni 112.1(3) . . ?
O12 C11 O11 125.3(5) . . ?
O12 C11 C12 118.5(5) . . ?
O11 C11 C12 116.2(5) . . ?
O13 C12 C13 114.2(4) . . ?
O13 C12 C11 106.7(4) . . ?
C13 C12 C11 113.5(4) . . ?
C14 C13 C18 119.2(6) . . ?
C14 C13 C12 121.6(6) . . ?
C18 C13 C12 119.2(5) . . ?
C13 C14 C15 119.1(7) . . ?
C16 C15 C14 122.2(8) . . ?
C15 C16 C17 118.6(8) . . ?
C16 C17 C18 121.1(8) . . ?
C17 C18 C13 119.8(6) . . ?
C21 O21 Ni 119.1(3) . . ?
C22 O23 Ni 113.5(3) . . ?
O21 C21 O22 124.8(5) . . ?
O21 C21 C22 117.2(5) . . ?
O22 C21 C22 117.9(5) . . ?
O23 C22 C23 112.3(5) . . ?
O23 C22 C21 107.0(4) . . ?
C23 C22 C21 115.3(4) . . ?
C28 C23 C24 117.4(6) . . ?
C28 C23 C22 122.2(6) . . ?
C24 C23 C22 120.4(6) . . ?
C23 C24 C25 122.4(7) . . ?
C26 C25 C24 118.1(9) . . ?
C25 C26 C27 122.8(10) . . ?
C26 C27 C28 117.4(9) . . ?
C23 C28 C27 121.8(6) . . ?
C1 N1 C2 104.4(5) . . ?
C1 N1 Ni 125.4(4) . . ?
C2 N1 Ni 128.5(4) . . ?
C1 N2 C3 106.7(5) . . ?
N2 C1 N1 112.3(6) . . ?
C2 C3 N2 106.5(6) . . ?
C3 C2 N1 110.0(6) . . ?
C4 N3 C5 103.0(5) . . ?
C4 N3 Ni 126.0(5) . . ?
C5 N3 Ni 129.5(4) . . ?
C4 N4 C6 107.4(5) . . ?
N3 C4 N4 113.9(6) . . ?
N4 C6 C5 104.5(5) . . ?
N3 C5 C6 111.1(5) . . ?
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
Ni O21 2.027(4) . ?
Ni O11 2.029(3) . ?
Ni N3 2.031(4) . ?
Ni N1 2.034(4) . ?
Ni O23 2.109(4) . ?
Ni O13 2.122(4) . ?
O11 C11 1.249(5) . ?
O12 C11 1.245(6) . ?
O13 C12 1.404(6) . ?
C11 C12 1.557(6) . ?
C12 C13 1.511(6) . ?
C13 C14 1.351(7) . ?
C13 C18 1.381(7) . ?
C14 C15 1.395(8) . ?
C15 C16 1.339(9) . ?
C16 C17 1.348(8) . ?
C17 C18 1.381(8) . ?
O21 C21 1.247(5) . ?
O22 C21 1.265(6) . ?
O23 C22 1.415(5) . ?
C21 C22 1.531(6) . ?
C22 C23 1.502(6) . ?
C23 C28 1.361(7) . ?
C23 C24 1.377(7) . ?
C24 C25 1.398(9) . ?
C25 C26 1.339(10) . ?
C26 C27 1.369(10) . ?
C27 C28 1.416(8) . ?
N1 C1 1.324(6) . ?
N1 C2 1.357(6) . ?
N2 C1 1.315(6) . ?
N2 C3 1.359(7) . ?
C3 C2 1.340(7) . ?
N3 C4 1.300(6) . ?
N3 C5 1.367(6) . ?
N4 C4 1.324(6) . ?
N4 C6 1.347(6) . ?
C6 C5 1.368(6) . ?
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
C28 H28 O23 0.93 2.44 2.782(8) 101.8 .
O13 H13 O22 0.876(19) 1.77(2) 2.620(5) 162(5) 2_556
O23 H23 O12 0.906(19) 1.72(2) 2.621(5) 173(5) 2_566
N2 H20 O22 0.86 2.00 2.812(6) 158.2 2_656
N4 H40 O12 0.86 1.99 2.827(5) 163.3 2_666
|
1100157.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100157.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_1100157
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C37 H34 N6 Ni O6'
_chemical_formula_weight 717.41
_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 90.00
_cell_angle_beta 94.428(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.2191(11)
_cell_length_b 29.972(4)
_cell_length_c 12.5644(15)
_cell_measurement_reflns_used 684
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.88
_cell_measurement_theta_min 2.60
_cell_volume 3461.3(7)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_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 0.0885
_diffrn_reflns_av_sigmaI/netI 0.1784
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 39
_diffrn_reflns_limit_k_min -38
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 18394
_diffrn_reflns_theta_full 28.07
_diffrn_reflns_theta_max 28.07
_diffrn_reflns_theta_min 1.36
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.616
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8782
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.377
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 1496
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.16
_refine_diff_density_max 0.605
_refine_diff_density_min -0.491
_refine_diff_density_rms 0.068
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 468
_refine_ls_number_reflns 7653
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.072
_refine_ls_R_factor_all 0.2271
_refine_ls_R_factor_gt 0.1056
_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^)+(0.0672P)^2^+0.8395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1633
_refine_ls_wR_factor_ref 0.2022
_reflns_number_gt 3567
_reflns_number_total 7653
_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.
'_exptl_absorpt_correction_type' value 'MULTISCAN' changed to
'multi-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 P2(1)/n
_cod_database_code 1100157
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
Ni Ni 0.33844(8) 0.14851(2) 0.50942(6) 0.0372(2) Uani 1 1 d . . .
O11 O 0.5421(4) 0.15643(12) 0.4605(3) 0.0402(10) Uani 1 1 d . . .
O12 O 0.6853(4) 0.19225(13) 0.3574(3) 0.0494(12) Uani 1 1 d . . .
O13 O 0.2997(4) 0.19112(13) 0.3740(3) 0.0381(10) Uani 1 1 d . . .
C101 C 0.5641(6) 0.18459(19) 0.3894(5) 0.0373(15) Uani 1 1 d . . .
C102 C 0.4291(6) 0.21106(18) 0.3381(5) 0.0371(14) Uani 1 1 d . . .
C103 C 0.4327(6) 0.25950(18) 0.3773(5) 0.0396(15) Uani 1 1 d . . .
C104 C 0.5579(7) 0.2838(2) 0.3863(6) 0.064(2) Uani 1 1 d . . .
H104 H 0.6446 0.2700 0.3719 0.077 Uiso 1 1 calc R . .
C105 C 0.5606(9) 0.3283(2) 0.4161(7) 0.087(3) Uani 1 1 d . . .
H105 H 0.6475 0.3442 0.4202 0.105 Uiso 1 1 calc R . .
C106 C 0.4357(10) 0.3483(2) 0.4390(8) 0.093(3) Uani 1 1 d . . .
H106 H 0.4364 0.3779 0.4610 0.112 Uiso 1 1 calc R . .
C107 C 0.3099(9) 0.3251(3) 0.4301(10) 0.127(4) Uani 1 1 d . . .
H107 H 0.2236 0.3389 0.4454 0.152 Uiso 1 1 calc R . .
C108 C 0.3081(7) 0.2812(2) 0.3984(8) 0.088(3) Uani 1 1 d . . .
H108 H 0.2200 0.2659 0.3912 0.106 Uiso 1 1 calc R . .
C109 C 0.4293(6) 0.20746(19) 0.2174(5) 0.0376(14) Uani 1 1 d . . .
C110 C 0.3895(6) 0.2428(2) 0.1509(6) 0.0491(17) Uani 1 1 d . . .
H110 H 0.3627 0.2700 0.1793 0.059 Uiso 1 1 calc R . .
C111 C 0.3901(7) 0.2375(2) 0.0416(6) 0.060(2) Uani 1 1 d . . .
H111 H 0.3640 0.2614 -0.0028 0.072 Uiso 1 1 calc R . .
C112 C 0.4278(7) 0.1980(3) -0.0029(6) 0.064(2) Uani 1 1 d . . .
H112 H 0.4281 0.1951 -0.0765 0.077 Uiso 1 1 calc R . .
C113 C 0.4652(7) 0.1630(2) 0.0634(6) 0.061(2) Uani 1 1 d . . .
H113 H 0.4917 0.1359 0.0347 0.073 Uiso 1 1 calc R . .
C114 C 0.4637(7) 0.1677(2) 0.1722(5) 0.0530(18) Uani 1 1 d . . .
H114 H 0.4866 0.1433 0.2160 0.064 Uiso 1 1 calc R . .
O21 O 0.3046(4) 0.09236(12) 0.4032(3) 0.0477(11) Uani 1 1 d . . .
O22 O 0.1791(4) 0.12654(13) 0.2669(3) 0.0478(11) Uani 1 1 d . . .
O23 O 0.2272(5) 0.01446(13) 0.3532(3) 0.0563(12) Uani 1 1 d . . .
H23 H 0.2564 0.0265 0.4094 0.084 Uiso 1 1 calc R . .
C201 C 0.2194(6) 0.0925(2) 0.3189(5) 0.0399(15) Uani 1 1 d . . .
C202 C 0.1576(6) 0.04702(19) 0.2827(5) 0.0414(15) Uani 1 1 d . . .
C203 C -0.0066(7) 0.0465(2) 0.2940(5) 0.0459(16) Uani 1 1 d . . .
C204 C -0.0707(9) 0.0154(3) 0.3544(6) 0.079(2) Uani 1 1 d . . .
H204 H -0.0145 -0.0065 0.3902 0.095 Uiso 1 1 calc R . .
C205 C -0.2219(11) 0.0166(4) 0.3623(8) 0.122(4) Uani 1 1 d . . .
H205 H -0.2647 -0.0047 0.4036 0.147 Uiso 1 1 calc R . .
C206 C -0.3057(11) 0.0476(5) 0.3120(9) 0.128(5) Uani 1 1 d . . .
H206 H -0.4049 0.0486 0.3206 0.154 Uiso 1 1 calc R . .
C207 C -0.2439(9) 0.0775(3) 0.2481(9) 0.097(3) Uani 1 1 d . . .
H207 H -0.3022 0.0983 0.2100 0.117 Uiso 1 1 calc R . .
C208 C -0.0966(8) 0.0775(2) 0.2391(6) 0.067(2) Uani 1 1 d . . .
H208 H -0.0561 0.0985 0.1957 0.080 Uiso 1 1 calc R . .
C209 C 0.1908(7) 0.0345(2) 0.1695(5) 0.0499(17) Uani 1 1 d . . .
C210 C 0.1550(9) -0.0053(3) 0.1289(6) 0.075(2) Uani 1 1 d . . .
H210 H 0.1050 -0.0249 0.1701 0.090 Uiso 1 1 calc R . .
C211 C 0.1883(10) -0.0190(3) 0.0285(7) 0.080(2) Uani 1 1 d . . .
H211 H 0.1637 -0.0476 0.0050 0.096 Uiso 1 1 calc R . .
C212 C 0.2536(13) 0.0079(4) -0.0330(8) 0.129(4) Uani 1 1 d . . .
H212 H 0.2773 -0.0009 -0.1004 0.155 Uiso 1 1 calc R . .
C213 C 0.285(2) 0.0481(5) 0.0032(11) 0.271(12) Uani 1 1 d . . .
H213 H 0.3291 0.0682 -0.0404 0.325 Uiso 1 1 calc R . .
C214 C 0.2542(16) 0.0613(4) 0.1045(10) 0.216(9) Uani 1 1 d . . .
H214 H 0.2792 0.0900 0.1273 0.260 Uiso 1 1 calc R . .
N1 N 0.3685(5) 0.20248(16) 0.6095(4) 0.0429(13) Uani 1 1 d . . .
N2 N 0.3251(7) 0.26150(19) 0.7049(5) 0.0606(17) Uani 1 1 d . . .
C2 C 0.4956(7) 0.2226(3) 0.6435(6) 0.067(2) Uani 1 1 d . . .
H2 H 0.5877 0.2128 0.6288 0.080 Uiso 1 1 calc R . .
C3 C 0.4686(8) 0.2588(3) 0.7014(6) 0.074(2) Uani 1 1 d . . .
H3 H 0.5373 0.2784 0.7331 0.089 Uiso 1 1 calc R . .
C1 C 0.2689(7) 0.2268(2) 0.6500(6) 0.0555(18) Uani 1 1 d . . .
H1 H 0.1698 0.2206 0.6414 0.067 Uiso 1 1 calc R . .
N3 N 0.4241(5) 0.10459(16) 0.6235(4) 0.0421(13) Uani 1 1 d . . .
N4 N 0.5741(6) 0.0534(2) 0.6884(5) 0.0534(15) Uani 1 1 d . . .
C5 C 0.4241(8) 0.1038(2) 0.7315(6) 0.066(2) Uani 1 1 d . . .
H5 H 0.3675 0.1222 0.7713 0.079 Uiso 1 1 calc R . .
C6 C 0.5169(8) 0.0730(3) 0.7726(6) 0.075(2) Uani 1 1 d . . .
H6 H 0.5379 0.0663 0.8444 0.090 Uiso 1 1 calc R . .
C4 C 0.5158(6) 0.0732(2) 0.6005(5) 0.0484(17) Uani 1 1 d . . .
H4 H 0.5372 0.0657 0.5316 0.058 Uiso 1 1 calc R . .
N5 N 0.1198(5) 0.14080(16) 0.5347(4) 0.0436(13) Uani 1 1 d . . .
N6 N -0.1164(7) 0.1415(2) 0.5085(6) 0.066(2) Uani 1 1 d . . .
C8 C 0.0592(8) 0.1199(3) 0.6150(7) 0.107(4) Uani 1 1 d . . .
H8 H 0.1109 0.1069 0.6735 0.129 Uiso 1 1 calc R . .
C9 C -0.0863(8) 0.1203(3) 0.5985(9) 0.127(4) Uani 1 1 d . . .
H9 H -0.1526 0.1080 0.6424 0.153 Uiso 1 1 calc R . .
C7 C 0.0071(8) 0.1537(2) 0.4726(6) 0.0582(19) Uani 1 1 d . . .
H7 H 0.0140 0.1698 0.4099 0.070 Uiso 1 1 calc R . .
H60 H -0.190(7) 0.145(2) 0.470(6) 0.07(2) Uiso 1 1 d . . .
H13 H 0.270(7) 0.171(2) 0.326(6) 0.08(3) Uiso 1 1 d . . .
H20 H 0.272(8) 0.280(3) 0.755(6) 0.10(3) Uiso 1 1 d . . .
H40 H 0.639(6) 0.031(2) 0.686(5) 0.05(2) 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
Ni 0.0375(4) 0.0374(4) 0.0360(5) 0.0001(4) -0.0030(3) 0.0060(4)
O11 0.036(2) 0.041(2) 0.043(3) 0.008(2) 0.0015(19) 0.0087(18)
O12 0.023(2) 0.057(3) 0.067(3) 0.018(2) -0.001(2) 0.0044(19)
O13 0.033(2) 0.037(2) 0.044(3) -0.002(2) -0.001(2) -0.0003(18)
C101 0.039(4) 0.033(3) 0.038(4) -0.008(3) -0.009(3) 0.001(3)
C102 0.034(3) 0.032(3) 0.045(4) 0.005(3) -0.001(3) 0.004(3)
C103 0.039(4) 0.032(3) 0.046(4) 0.000(3) -0.007(3) 0.003(3)
C104 0.045(4) 0.045(4) 0.101(6) -0.018(4) -0.004(4) 0.004(3)
C105 0.060(5) 0.052(5) 0.149(9) -0.026(5) -0.007(5) -0.005(4)
C106 0.087(6) 0.041(4) 0.156(9) -0.028(5) 0.036(6) -0.008(5)
C107 0.069(6) 0.061(6) 0.258(14) -0.034(7) 0.066(8) 0.001(5)
C108 0.039(4) 0.045(4) 0.182(10) -0.021(5) 0.015(5) 0.006(3)
C109 0.026(3) 0.038(3) 0.049(4) 0.008(3) -0.002(3) -0.002(3)
C110 0.041(4) 0.049(4) 0.054(5) 0.008(3) -0.016(3) -0.001(3)
C111 0.059(5) 0.061(5) 0.056(5) 0.024(4) -0.022(4) -0.009(4)
C112 0.046(4) 0.107(7) 0.040(5) 0.007(5) -0.002(4) -0.019(4)
C113 0.057(5) 0.064(5) 0.061(5) -0.001(4) 0.005(4) 0.003(4)
C114 0.060(5) 0.059(4) 0.040(4) 0.011(3) 0.003(4) 0.012(3)
O21 0.053(3) 0.042(3) 0.046(3) -0.006(2) -0.012(2) 0.004(2)
O22 0.064(3) 0.036(2) 0.042(3) 0.002(2) -0.005(2) -0.003(2)
O23 0.072(3) 0.040(2) 0.054(3) 0.003(2) -0.013(3) 0.015(2)
C201 0.033(3) 0.048(4) 0.039(4) -0.002(3) 0.006(3) 0.000(3)
C202 0.050(4) 0.038(4) 0.036(4) 0.003(3) -0.002(3) 0.002(3)
C203 0.048(4) 0.048(4) 0.042(4) -0.009(3) 0.001(3) -0.008(3)
C204 0.074(6) 0.112(7) 0.050(5) 0.024(5) -0.001(4) -0.019(5)
C205 0.067(7) 0.220(14) 0.082(8) 0.023(8) 0.016(6) -0.062(8)
C206 0.053(7) 0.238(16) 0.098(10) -0.063(10) 0.031(6) -0.018(8)
C207 0.049(6) 0.107(8) 0.132(10) -0.042(7) -0.013(6) 0.020(5)
C208 0.055(5) 0.053(5) 0.090(6) -0.006(4) -0.009(4) 0.003(4)
C209 0.055(4) 0.044(4) 0.051(4) -0.018(4) 0.010(4) -0.006(3)
C210 0.109(7) 0.069(5) 0.049(5) -0.015(4) 0.012(5) -0.023(5)
C211 0.108(7) 0.067(6) 0.064(6) -0.031(5) 0.008(5) -0.007(5)
C212 0.190(12) 0.123(9) 0.082(7) -0.052(7) 0.064(8) -0.054(8)
C213 0.47(3) 0.188(13) 0.191(13) -0.139(11) 0.260(17) -0.215(16)
C214 0.35(2) 0.151(10) 0.175(12) -0.119(9) 0.215(13) -0.169(12)
N1 0.029(3) 0.049(3) 0.051(3) -0.004(3) 0.007(3) 0.007(2)
N2 0.057(4) 0.061(4) 0.063(4) -0.027(3) 0.007(3) 0.003(3)
C2 0.024(4) 0.099(6) 0.075(6) -0.041(5) -0.001(4) 0.001(4)
C3 0.041(5) 0.101(6) 0.080(6) -0.045(5) 0.002(4) -0.024(4)
C1 0.035(4) 0.064(5) 0.068(5) -0.016(4) 0.004(4) -0.002(3)
N3 0.039(3) 0.051(3) 0.036(3) 0.006(3) 0.003(3) 0.006(2)
N4 0.050(4) 0.056(4) 0.053(4) 0.007(3) 0.000(3) 0.016(3)
C5 0.071(5) 0.084(6) 0.042(5) 0.005(4) 0.003(4) 0.026(4)
C6 0.084(6) 0.101(6) 0.040(5) 0.014(5) 0.005(4) 0.032(5)
C4 0.042(4) 0.061(4) 0.042(4) 0.006(4) -0.001(3) 0.007(3)
N5 0.039(3) 0.043(3) 0.047(3) 0.002(3) -0.006(3) 0.003(2)
N6 0.038(4) 0.072(5) 0.083(5) -0.012(4) -0.023(4) 0.007(3)
C8 0.036(5) 0.172(9) 0.110(8) 0.089(7) -0.021(5) -0.016(5)
C9 0.036(5) 0.167(10) 0.178(11) 0.092(9) -0.003(6) -0.023(5)
C7 0.055(5) 0.066(5) 0.052(5) -0.001(4) -0.004(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'
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'
Ni Ni 0.3393 1.1124 '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
O11 Ni N1 90.52(17) . . ?
O11 Ni N3 88.37(17) . . ?
N1 Ni N3 92.91(19) . . ?
O11 Ni N5 171.23(18) . . ?
N1 Ni N5 94.61(19) . . ?
N3 Ni N5 98.45(19) . . ?
O11 Ni O13 77.94(15) . . ?
N1 Ni O13 91.35(18) . . ?
N3 Ni O13 165.70(17) . . ?
N5 Ni O13 94.80(18) . . ?
O11 Ni O21 89.84(15) . . ?
N1 Ni O21 179.23(17) . . ?
N3 Ni O21 87.79(17) . . ?
N5 Ni O21 84.95(17) . . ?
O13 Ni O21 88.06(16) . . ?
C101 O11 Ni 119.7(4) . . ?
C102 O13 Ni 114.0(3) . . ?
O12 C101 O11 123.6(5) . . ?
O12 C101 C102 118.6(5) . . ?
O11 C101 C102 117.7(5) . . ?
O13 C102 C109 110.4(4) . . ?
O13 C102 C103 106.9(5) . . ?
C109 C102 C103 112.7(5) . . ?
O13 C102 C101 108.1(5) . . ?
C109 C102 C101 108.1(5) . . ?
C103 C102 C101 110.5(4) . . ?
C108 C103 C104 116.8(6) . . ?
C108 C103 C102 121.1(5) . . ?
C104 C103 C102 122.0(5) . . ?
C103 C104 C105 122.4(6) . . ?
C106 C105 C104 119.2(7) . . ?
C105 C106 C107 119.7(7) . . ?
C106 C107 C108 120.5(7) . . ?
C103 C108 C107 121.4(7) . . ?
C114 C109 C110 118.5(6) . . ?
C114 C109 C102 119.6(5) . . ?
C110 C109 C102 121.8(6) . . ?
C109 C110 C111 119.3(6) . . ?
C112 C111 C110 121.9(7) . . ?
C111 C112 C113 118.4(7) . . ?
C112 C113 C114 120.4(7) . . ?
C109 C114 C113 121.4(6) . . ?
C201 O21 Ni 124.4(4) . . ?
O22 C201 O21 125.3(6) . . ?
O22 C201 C202 118.7(5) . . ?
O21 C201 C202 115.9(5) . . ?
O23 C202 C209 107.2(5) . . ?
O23 C202 C203 109.5(5) . . ?
C209 C202 C203 110.8(5) . . ?
O23 C202 C201 106.5(5) . . ?
C209 C202 C201 113.6(5) . . ?
C203 C202 C201 109.2(5) . . ?
C204 C203 C208 117.6(7) . . ?
C204 C203 C202 122.1(6) . . ?
C208 C203 C202 120.2(6) . . ?
C203 C204 C205 119.7(8) . . ?
C206 C205 C204 121.7(10) . . ?
C205 C206 C207 119.0(10) . . ?
C206 C207 C208 120.7(10) . . ?
C207 C208 C203 121.0(8) . . ?
C214 C209 C210 114.7(7) . . ?
C214 C209 C202 124.0(6) . . ?
C210 C209 C202 121.3(6) . . ?
C209 C210 C211 123.5(8) . . ?
C212 C211 C210 120.2(8) . . ?
C211 C212 C213 117.7(9) . . ?
C212 C213 C214 121.8(10) . . ?
C209 C214 C213 122.0(9) . . ?
C1 N1 C2 104.2(5) . . ?
C1 N1 Ni 127.8(4) . . ?
C2 N1 Ni 127.9(4) . . ?
C3 N2 C1 106.5(6) . . ?
C3 C2 N1 109.8(6) . . ?
N2 C3 C2 107.1(6) . . ?
N1 C1 N2 112.4(6) . . ?
C4 N3 C5 104.9(5) . . ?
C4 N3 Ni 121.6(4) . . ?
C5 N3 Ni 132.7(5) . . ?
C4 N4 C6 107.5(6) . . ?
C6 C5 N3 110.4(6) . . ?
C5 C6 N4 105.9(6) . . ?
N3 C4 N4 111.3(6) . . ?
C7 N5 C8 103.2(6) . . ?
C7 N5 Ni 127.7(5) . . ?
C8 N5 Ni 129.1(4) . . ?
C7 N6 C9 107.5(6) . . ?
C9 C8 N5 110.4(7) . . ?
N6 C9 C8 106.3(8) . . ?
N6 C7 N5 112.6(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
Ni O11 2.034(4) . ?
Ni N1 2.055(5) . ?
Ni N3 2.058(5) . ?
Ni N5 2.078(5) . ?
Ni O13 2.136(4) . ?
Ni O21 2.156(4) . ?
O11 C101 1.257(7) . ?
O12 C101 1.238(7) . ?
O13 C102 1.438(7) . ?
C101 C102 1.571(7) . ?
C102 C109 1.521(8) . ?
C102 C103 1.533(7) . ?
C103 C108 1.363(8) . ?
C103 C104 1.362(8) . ?
C104 C105 1.385(9) . ?
C105 C106 1.349(10) . ?
C106 C107 1.350(10) . ?
C107 C108 1.375(10) . ?
C109 C114 1.367(8) . ?
C109 C110 1.382(8) . ?
C110 C111 1.382(9) . ?
C111 C112 1.364(9) . ?
C112 C113 1.367(9) . ?
C113 C114 1.375(9) . ?
O21 C201 1.269(6) . ?
O22 C201 1.252(6) . ?
O23 C202 1.436(6) . ?
C201 C202 1.533(8) . ?
C202 C209 1.524(8) . ?
C202 C203 1.531(8) . ?
C203 C204 1.365(9) . ?
C203 C208 1.393(9) . ?
C204 C205 1.406(11) . ?
C205 C206 1.335(14) . ?
C206 C207 1.359(14) . ?
C207 C208 1.372(10) . ?
C209 C214 1.315(11) . ?
C209 C210 1.327(8) . ?
C210 C211 1.383(10) . ?
C211 C212 1.297(11) . ?
C212 C213 1.310(12) . ?
C213 C214 1.383(13) . ?
N1 C1 1.306(7) . ?
N1 C2 1.358(7) . ?
N2 C3 1.330(8) . ?
N2 C1 1.330(8) . ?
C2 C3 1.340(9) . ?
N3 C4 1.312(7) . ?
N3 C5 1.358(8) . ?
N4 C4 1.329(7) . ?
N4 C6 1.352(8) . ?
C5 C6 1.336(9) . ?
N5 C7 1.309(7) . ?
N5 C8 1.345(8) . ?
N6 C7 1.309(9) . ?
N6 C9 1.309(10) . ?
C8 C9 1.342(10) . ?
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
C214 H214 O22 0.93 2.32 2.947(10) 124.5 .
C208 H208 O22 0.93 2.43 2.933(8) 113.9 .
C204 H204 O23 0.93 2.40 2.748(9) 102.3 .
C108 H108 O13 0.93 2.37 2.716(8) 101.5 .
C104 H104 O12 0.93 2.37 3.018(7) 126.5 .
N4 H40 O23 0.89(6) 1.93(6) 2.814(7) 168(6) 3_656
N2 H20 O12 0.99(8) 1.78(8) 2.763(7) 172(7) 4_566
O13 H13 O21 0.87(7) 2.56(7) 2.982(5) 110(5) .
O13 H13 O22 0.87(7) 1.72(7) 2.562(5) 161(7) .
N6 H60 O11 0.81(7) 2.48(7) 3.191(7) 146(6) 1_455
N6 H60 O12 0.81(7) 2.25(7) 2.953(8) 145(6) 1_455
O23 H23 O21 0.82 2.03 2.507(5) 117.0 .
|
1100158.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100158.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_1100158
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C7 H10 Cu N2 O6'
_chemical_formula_weight 281.71
_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 75.045(5)
_cell_angle_beta 85.826(6)
_cell_angle_gamma 75.613(7)
_cell_formula_units_Z 2
_cell_length_a 5.528(2)
_cell_length_b 7.267(3)
_cell_length_c 13.626(5)
_cell_measurement_reflns_used 451
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 22.80
_cell_measurement_theta_min 2.99
_cell_volume 512.2(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.795
_diffrn_measured_fraction_theta_max 0.795
_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 0.0229
_diffrn_reflns_av_sigmaI/netI 0.0675
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -3
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 2335
_diffrn_reflns_theta_full 28.07
_diffrn_reflns_theta_max 28.07
_diffrn_reflns_theta_min 1.55
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 2.148
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6652
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.826
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 286
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.09
_refine_diff_density_max 0.666
_refine_diff_density_min -0.528
_refine_diff_density_rms 0.103
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.092
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 157
_refine_ls_number_reflns 1984
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.092
_refine_ls_R_factor_all 0.0965
_refine_ls_R_factor_gt 0.0675
_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^)+(0.0385P)^2^+1.3732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1157
_refine_ls_wR_factor_ref 0.1259
_reflns_number_gt 1472
_reflns_number_total 1984
_reflns_threshold_expression >2sigma(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.
'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-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 P-1
_cod_database_code 1100158
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
Cu Cu 0.85489(16) 0.17931(12) 0.24638(6) 0.0339(2) Uani 1 1 d . . .
O11 O 1.1010(8) 0.1569(6) 0.3482(3) 0.0355(10) Uani 1 1 d . . .
O12 O 1.2067(8) 0.2078(7) 0.4906(3) 0.0453(12) Uani 1 1 d . . .
O13 O 0.6099(8) 0.3058(7) 0.3762(4) 0.0441(12) Uani 1 1 d . . .
C11 C 1.0453(11) 0.2179(8) 0.4281(4) 0.0284(13) Uani 1 1 d . . .
C12 C 0.7774(12) 0.3070(11) 0.4509(5) 0.0438(16) Uani 1 1 d . . .
H12A H 0.7306 0.2345 0.5168 0.053 Uiso 1 1 calc R . .
H12B H 0.7620 0.4412 0.4543 0.053 Uiso 1 1 calc R . .
O21 O 0.6140(9) 0.1710(6) 0.1514(3) 0.0425(11) Uani 1 1 d . . .
O22 O 0.3233(9) 0.0174(7) 0.1353(3) 0.0513(13) Uani 1 1 d . . .
O23 O 0.8172(9) -0.0923(7) 0.3088(4) 0.0383(11) Uani 1 1 d . . .
C21 C 0.5043(12) 0.0325(9) 0.1778(4) 0.0348(14) Uani 1 1 d . . .
C22 C 0.6013(12) -0.1304(9) 0.2729(4) 0.0341(14) Uani 1 1 d . . .
H22A H 0.4727 -0.1330 0.3253 0.041 Uiso 1 1 calc R . .
H22B H 0.6450 -0.2568 0.2565 0.041 Uiso 1 1 calc R . .
N1 N 0.9023(9) 0.4332(7) 0.1657(3) 0.0304(11) Uani 1 1 d . . .
N2 N 0.8416(11) 0.7075(8) 0.0454(4) 0.0380(13) Uani 1 1 d . . .
C1 C 0.7598(12) 0.5469(8) 0.0879(4) 0.0324(13) Uani 1 1 d . . .
H1 H 0.6213 0.5180 0.0660 0.039 Uiso 1 1 calc R . .
C2 C 1.0842(12) 0.5292(9) 0.1720(5) 0.0364(15) Uani 1 1 d . . .
H2 H 1.2116 0.4843 0.2196 0.044 Uiso 1 1 calc R . .
C3 C 1.0492(13) 0.6997(9) 0.0981(5) 0.0393(15) Uani 1 1 d . . .
H3 H 1.1453 0.7919 0.0857 0.047 Uiso 1 1 calc R . .
H20 H 0.785(12) 0.801(9) -0.009(5) 0.035(17) Uiso 1 1 d . . .
H23 H 0.814(13) -0.112(10) 0.363(5) 0.04(2) Uiso 1 1 d . . .
H13 H 0.505(13) 0.252(9) 0.407(5) 0.04(2) 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
Cu 0.0388(4) 0.0377(4) 0.0255(4) -0.0017(3) -0.0103(3) -0.0131(3)
O11 0.031(2) 0.049(3) 0.028(2) -0.0096(19) -0.0045(18) -0.009(2)
O12 0.043(3) 0.075(3) 0.024(2) -0.009(2) -0.008(2) -0.026(3)
O13 0.028(2) 0.065(3) 0.042(3) -0.011(2) -0.003(2) -0.016(2)
C11 0.033(3) 0.030(3) 0.021(3) 0.001(2) 0.001(2) -0.013(3)
C12 0.039(4) 0.060(4) 0.037(3) -0.018(3) 0.002(3) -0.015(3)
O21 0.052(3) 0.044(3) 0.032(2) 0.0026(19) -0.017(2) -0.022(2)
O22 0.059(3) 0.044(3) 0.056(3) 0.002(2) -0.029(3) -0.027(2)
O23 0.046(3) 0.043(3) 0.026(2) -0.002(2) -0.011(2) -0.015(2)
C21 0.040(4) 0.038(3) 0.028(3) -0.007(3) -0.008(3) -0.011(3)
C22 0.035(3) 0.037(3) 0.030(3) -0.007(3) -0.001(3) -0.009(3)
N1 0.031(3) 0.034(3) 0.027(2) -0.004(2) -0.004(2) -0.010(2)
N2 0.042(3) 0.039(3) 0.030(3) -0.003(2) -0.004(2) -0.008(3)
C1 0.035(3) 0.033(3) 0.028(3) -0.005(2) -0.005(3) -0.009(3)
C2 0.035(4) 0.045(4) 0.033(3) -0.011(3) -0.008(3) -0.013(3)
C3 0.046(4) 0.036(4) 0.043(3) -0.010(3) -0.001(3) -0.021(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'
Cu Cu 0.3201 1.2651 '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'
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
O21 Cu N1 92.56(19) . . ?
O21 Cu O11 173.74(19) . . ?
N1 Cu O11 93.45(19) . . ?
O21 Cu O23 82.06(18) . . ?
N1 Cu O23 171.2(2) . . ?
O11 Cu O23 91.76(18) . . ?
O21 Cu O13 105.03(18) . . ?
N1 Cu O13 95.42(19) . . ?
O11 Cu O13 76.14(16) . . ?
O23 Cu O13 92.66(19) . . ?
C11 O11 Cu 123.5(4) . . ?
C12 O13 Cu 107.6(4) . . ?
O12 C11 O11 122.4(6) . . ?
O12 C11 C12 117.4(5) . . ?
O11 C11 C12 120.2(5) . . ?
O13 C12 C11 112.4(5) . . ?
C21 O21 Cu 116.6(4) . . ?
C22 O23 Cu 112.6(4) . . ?
O22 C21 O21 126.0(6) . . ?
O22 C21 C22 116.8(5) . . ?
O21 C21 C22 117.2(5) . . ?
O23 C22 C21 108.7(5) . . ?
C1 N1 C2 105.6(5) . . ?
C1 N1 Cu 124.6(4) . . ?
C2 N1 Cu 129.8(4) . . ?
C1 N2 C3 107.9(5) . . ?
N1 C1 N2 111.2(5) . . ?
C3 C2 N1 109.6(5) . . ?
C2 C3 N2 105.7(5) . . ?
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
Cu O21 1.945(4) . ?
Cu N1 1.958(5) . ?
Cu O11 1.962(4) . ?
Cu O23 1.993(5) . ?
Cu O13 2.383(5) . ?
O11 C11 1.268(6) . ?
O12 C11 1.254(7) . ?
O13 C12 1.429(7) . ?
C11 C12 1.507(9) . ?
O21 C21 1.263(7) . ?
O22 C21 1.233(7) . ?
O23 C22 1.435(7) . ?
C21 C22 1.536(8) . ?
N1 C1 1.332(7) . ?
N1 C2 1.378(7) . ?
N2 C1 1.333(7) . ?
N2 C3 1.379(8) . ?
C2 C3 1.362(9) . ?
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
N2 H20 O22 0.88(6) 1.91(6) 2.787(7) 174(6) 2_665
O23 H23 O12 0.71(6) 1.94(7) 2.648(6) 170(7) 2_756
O13 H13 O12 0.81(6) 1.98(7) 2.760(6) 161(6) 1_455
C1 H1 O21 0.93 2.50 2.938(7) 109.1 .
C3 H3 O22 0.93 2.36 3.215(7) 152.3 1_665
|
1100159.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100159.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_1100159
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C9 H14 Cu N2 O6'
_chemical_formula_weight 309.76
_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 mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 92.324(11)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 5.422(3)
_cell_length_b 13.436(7)
_cell_length_c 17.000(9)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1237.4(11)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_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 0.0864
_diffrn_reflns_av_sigmaI/netI 0.2921
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 6303
_diffrn_reflns_theta_full 27.98
_diffrn_reflns_theta_max 27.98
_diffrn_reflns_theta_min 1.93
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.786
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7576
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.663
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 636
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.516
_refine_diff_density_min -0.453
_refine_diff_density_rms 0.081
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.753
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 174
_refine_ls_number_reflns 2705
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 0.754
_refine_ls_R_factor_all 0.2235
_refine_ls_R_factor_gt 0.0495
_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^)+(0.0199P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0686
_refine_ls_wR_factor_ref 0.0926
_reflns_number_gt 902
_reflns_number_total 2705
_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.
'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-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
The following automatic conversions were performed:
'_atom_sites_solution_hydrogens' value 'geom & difmap' was changed to
'mixed'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M P2(1)/c
_cod_database_code 1100159
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
Cu Cu 0.34092(13) 0.24814(7) 0.02425(5) 0.0369(2) Uani 1 1 d . . .
O11 O 0.6121(7) 0.1625(3) -0.0060(3) 0.0345(12) Uani 1 1 d . . .
O12 O 0.7480(7) 0.0344(3) -0.0724(3) 0.0491(14) Uani 1 1 d . . .
O13 O 0.1610(8) 0.1502(3) -0.0718(3) 0.0476(13) Uani 1 1 d D . .
C11 C 0.5812(12) 0.0944(4) -0.0576(4) 0.0330(19) Uani 1 1 d . . .
C12 C 0.3363(12) 0.0829(5) -0.1015(5) 0.045(2) Uani 1 1 d . . .
H12 H 0.2768 0.0146 -0.0950 0.053 Uiso 1 1 calc R . .
C13 C 0.3702(14) 0.1024(6) -0.1871(4) 0.098(3) Uani 1 1 d . . .
H13A H 0.2164 0.0922 -0.2160 0.147 Uiso 1 1 calc R . .
H13B H 0.4920 0.0576 -0.2063 0.147 Uiso 1 1 calc R . .
H13C H 0.4239 0.1698 -0.1940 0.147 Uiso 1 1 calc R . .
O21 O 0.0853(8) 0.3252(3) 0.0701(3) 0.0450(13) Uani 1 1 d . . .
O22 O -0.2260(9) 0.3179(3) 0.1507(3) 0.0760(18) Uani 1 1 d . . .
O23 O 0.2597(8) 0.1564(3) 0.1098(3) 0.0423(13) Uani 1 1 d D . .
C21 C -0.0436(13) 0.2834(4) 0.1211(4) 0.041(2) Uani 1 1 d . . .
C22 C 0.0287(12) 0.1764(4) 0.1431(4) 0.041(2) Uani 1 1 d . . .
H22 H -0.0946 0.1313 0.1189 0.050 Uiso 1 1 calc R . .
C23 C 0.0388(15) 0.1589(5) 0.2283(4) 0.091(3) Uani 1 1 d . . .
H23A H 0.0740 0.0900 0.2386 0.137 Uiso 1 1 calc R . .
H23B H -0.1171 0.1759 0.2494 0.137 Uiso 1 1 calc R . .
H23C H 0.1663 0.1993 0.2527 0.137 Uiso 1 1 calc R . .
N1 N 0.4281(9) 0.3568(3) -0.0448(3) 0.0325(14) Uani 1 1 d . . .
N2 N 0.4027(10) 0.4991(4) -0.1093(3) 0.0352(14) Uani 1 1 d . . .
C1 C 0.2965(11) 0.4378(5) -0.0603(4) 0.037(2) Uani 1 1 d . . .
H1 H 0.1445 0.4503 -0.0389 0.045 Uiso 1 1 calc R . .
C2 C 0.6379(12) 0.3676(4) -0.0881(4) 0.041(2) Uani 1 1 d . . .
H2 H 0.7668 0.3221 -0.0903 0.049 Uiso 1 1 calc R . .
C3 C 0.6228(12) 0.4556(5) -0.1265(4) 0.045(2) Uani 1 1 d . . .
H3 H 0.7408 0.4820 -0.1588 0.054 Uiso 1 1 calc R . .
H13 H 0.034(7) 0.121(4) -0.060(4) 0.08(3) Uiso 1 1 d D . .
H23 H 0.294(9) 0.1013(18) 0.100(3) 0.026(19) Uiso 1 1 d D . .
H20 H 0.3002 0.5557 -0.1281 0.69(17) 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
Cu 0.0359(4) 0.0173(3) 0.0585(5) 0.0029(6) 0.0122(3) 0.0045(5)
O11 0.021(3) 0.024(2) 0.058(4) -0.002(2) 0.000(2) 0.003(2)
O12 0.026(3) 0.021(2) 0.101(4) -0.013(3) 0.020(3) 0.008(2)
O13 0.024(3) 0.035(3) 0.084(4) -0.010(3) 0.002(3) 0.004(3)
C11 0.032(5) 0.020(4) 0.047(6) 0.007(4) 0.006(4) -0.013(3)
C12 0.029(5) 0.035(4) 0.070(7) -0.016(4) 0.007(5) -0.003(4)
C13 0.083(7) 0.149(9) 0.061(7) -0.037(6) -0.015(6) 0.033(6)
O21 0.053(3) 0.021(2) 0.063(4) 0.009(2) 0.029(3) 0.013(2)
O22 0.083(4) 0.038(3) 0.112(5) 0.031(3) 0.062(4) 0.033(3)
O23 0.048(3) 0.013(3) 0.067(4) 0.002(3) 0.022(3) 0.013(2)
C21 0.045(5) 0.022(4) 0.057(6) 0.008(3) 0.016(4) 0.009(3)
C22 0.043(5) 0.022(4) 0.060(6) 0.007(4) 0.009(4) 0.015(4)
C23 0.150(8) 0.058(5) 0.068(7) 0.024(5) 0.041(6) 0.057(5)
N1 0.030(3) 0.026(3) 0.043(4) 0.005(3) 0.017(3) 0.003(3)
N2 0.040(4) 0.025(3) 0.042(4) 0.008(3) 0.015(3) -0.004(3)
C1 0.028(4) 0.033(4) 0.052(6) -0.002(4) 0.008(4) 0.018(3)
C2 0.043(5) 0.020(4) 0.060(6) 0.004(4) 0.005(4) 0.008(3)
C3 0.037(5) 0.043(5) 0.056(6) 0.006(4) 0.017(4) -0.011(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'
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
O21 Cu N1 92.14(19) . . ?
O21 Cu O11 171.22(19) . . ?
N1 Cu O11 94.56(18) . . ?
O21 Cu O23 81.44(18) . . ?
N1 Cu O23 169.4(2) . . ?
O11 Cu O23 91.08(17) . . ?
O21 Cu O13 107.83(18) . . ?
N1 Cu O13 96.2(2) . . ?
O11 Cu O13 77.09(17) . . ?
O23 Cu O13 93.8(2) . . ?
C11 O11 Cu 121.7(4) . . ?
C12 O13 Cu 110.4(4) . . ?
O12 C11 O11 121.8(6) . . ?
O12 C11 C12 117.9(6) . . ?
O11 C11 C12 120.3(6) . . ?
O13 C12 C13 110.2(6) . . ?
O13 C12 C11 110.4(6) . . ?
C13 C12 C11 108.9(6) . . ?
C21 O21 Cu 117.7(4) . . ?
C22 O23 Cu 113.8(4) . . ?
O22 C21 O21 126.3(6) . . ?
O22 C21 C22 117.4(6) . . ?
O21 C21 C22 116.1(6) . . ?
O23 C22 C23 111.4(6) . . ?
O23 C22 C21 107.5(5) . . ?
C23 C22 C21 112.9(6) . . ?
C1 N1 C2 104.8(5) . . ?
C1 N1 Cu 126.6(4) . . ?
C2 N1 Cu 128.6(4) . . ?
C1 N2 C3 106.0(5) . . ?
N2 C1 N1 113.1(6) . . ?
C3 C2 N1 108.2(6) . . ?
C2 C3 N2 107.8(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
Cu O21 1.920(4) . ?
Cu N1 1.944(5) . ?
Cu O11 1.952(4) . ?
Cu O23 1.969(4) . ?
Cu O13 2.284(5) . ?
O11 C11 1.274(7) . ?
O12 C11 1.244(7) . ?
O13 C12 1.420(7) . ?
C11 C12 1.505(8) . ?
C12 C13 1.498(9) . ?
O21 C21 1.268(7) . ?
O22 C21 1.220(7) . ?
O23 C22 1.421(7) . ?
C21 C22 1.532(7) . ?
C22 C23 1.466(8) . ?
N1 C1 1.322(6) . ?
N1 C2 1.387(7) . ?
N2 C1 1.320(6) . ?
N2 C3 1.370(7) . ?
C2 C3 1.352(8) . ?
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
O13 H13 O12 0.823(19) 1.94(3) 2.727(6) 159(7) 1_455
O13 H13 O11 0.823(19) 2.56(4) 3.226(6) 138(6) 1_455
O23 H23 O12 0.781(19) 1.90(3) 2.642(6) 160(5) 3_655
N2 H20 O22 0.988(5) 1.783(4) 2.721(7) 157.3(3) 3_565
C1 H1 O21 0.93 2.53 2.953(8) 107.9 .
|
1100160.cif | #------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100160.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_1100160
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C11 H18 Cu N2 O6'
_chemical_formula_weight 337.81
_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 mixed
_atom_sites_solution_primary patterson
_atom_sites_solution_secondary difmap
_cell_angle_alpha 90.00
_cell_angle_beta 118.748(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.6623(15)
_cell_length_b 17.630(3)
_cell_length_c 9.7978(16)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 1463.3(4)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_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 0.0736
_diffrn_reflns_av_sigmaI/netI 0.2177
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 8121
_diffrn_reflns_theta_full 28.00
_diffrn_reflns_theta_max 28.00
_diffrn_reflns_theta_min 2.43
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.518
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8787
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.533
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 700
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.08
_refine_diff_density_max 0.495
_refine_diff_density_min -0.404
_refine_diff_density_rms 0.068
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.694
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 197
_refine_ls_number_reflns 3293
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.694
_refine_ls_R_factor_all 0.1503
_refine_ls_R_factor_gt 0.0448
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0511
_refine_ls_wR_factor_ref 0.0634
_reflns_number_gt 1411
_reflns_number_total 3293
_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.
'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-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
The following automatic conversions were performed:
'_atom_sites_solution_hydrogens' value 'geom&difmap' was changed to
'mixed'.
Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius
;
_cod_original_sg_symbol_H-M P2(1)/n
_cod_database_code 1100160
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
Cu Cu 0.47359(6) 0.79480(3) 0.05160(7) 0.03203(15) Uani 1 1 d . . .
O11 O 0.3755(3) 0.70760(16) -0.0789(3) 0.0331(7) Uani 1 1 d . . .
O12 O 0.3248(3) 0.58449(14) -0.1005(3) 0.0369(8) Uani 1 1 d . . .
O13 O 0.5382(3) 0.69875(16) 0.2237(3) 0.0343(8) Uani 1 1 d . . .
C11 C 0.3992(5) 0.6407(3) -0.0238(5) 0.0280(11) Uani 1 1 d . . .
C12 C 0.5260(5) 0.6277(2) 0.1448(5) 0.0314(11) Uani 1 1 d . . .
C13 C 0.4812(5) 0.5637(2) 0.2207(5) 0.0516(14) Uani 1 1 d . . .
H13A H 0.5615 0.5584 0.3273 0.077 Uiso 1 1 calc R . .
H13B H 0.4717 0.5172 0.1660 0.077 Uiso 1 1 calc R . .
H13C H 0.3823 0.5753 0.2167 0.077 Uiso 1 1 calc R . .
C14 C 0.6823(4) 0.6107(2) 0.1476(5) 0.0491(13) Uani 1 1 d . . .
H14A H 0.7111 0.6529 0.1045 0.074 Uiso 1 1 calc R . .
H14B H 0.6711 0.5661 0.0869 0.074 Uiso 1 1 calc R . .
H14C H 0.7630 0.6024 0.2530 0.074 Uiso 1 1 calc R . .
O21 O 0.2704(3) 0.82048(14) 0.0381(3) 0.0348(8) Uani 1 1 d . . .
O22 O 0.1519(3) 0.89599(16) 0.1314(4) 0.0554(10) Uani 1 1 d . . .
O23 O 0.5391(3) 0.88380(15) 0.1866(3) 0.0395(8) Uani 1 1 d . . .
C21 C 0.2703(5) 0.8749(2) 0.1259(5) 0.0349(11) Uani 1 1 d . . .
C22 C 0.4257(5) 0.9136(2) 0.2306(5) 0.0343(11) Uani 1 1 d . . .
C23 C 0.4134(5) 0.9976(2) 0.2041(6) 0.0772(19) Uani 1 1 d . . .
H23A H 0.5125 1.0210 0.2732 0.116 Uiso 1 1 calc R . .
H23B H 0.3323 1.0176 0.2238 0.116 Uiso 1 1 calc R . .
H23C H 0.3876 1.0079 0.0983 0.116 Uiso 1 1 calc R . .
C24 C 0.4784(5) 0.8937(3) 0.3982(5) 0.0720(17) Uani 1 1 d . . .
H24A H 0.4970 0.8401 0.4130 0.108 Uiso 1 1 calc R . .
H24B H 0.3976 0.9079 0.4238 0.108 Uiso 1 1 calc R . .
H24C H 0.5739 0.9206 0.4645 0.108 Uiso 1 1 calc R . .
N1 N 0.6366(4) 0.80589(19) -0.0134(4) 0.0332(9) Uani 1 1 d . . .
N2 N 0.8517(5) 0.8356(2) -0.0221(5) 0.0439(11) Uani 1 1 d . . .
C1 C 0.7731(5) 0.8405(2) 0.0594(5) 0.0373(12) Uani 1 1 d . . .
H1 H 0.8106 0.8652 0.1546 0.045 Uiso 1 1 calc R . .
C2 C 0.6273(5) 0.7781(3) -0.1473(6) 0.0533(15) Uani 1 1 d . . .
H2 H 0.5427 0.7509 -0.2229 0.064 Uiso 1 1 calc R . .
C3 C 0.7609(5) 0.7965(3) -0.1529(6) 0.0526(13) Uani 1 1 d . . .
H3 H 0.7848 0.7845 -0.2316 0.063 Uiso 1 1 calc R . .
H23 H 0.648(4) 0.889(2) 0.258(5) 0.055(14) Uiso 1 1 d . . .
H13 H 0.623(4) 0.699(2) 0.325(4) 0.049(13) Uiso 1 1 d . . .
H20 H 0.956(5) 0.856(2) 0.016(6) 0.088(18) 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
Cu 0.0277(3) 0.0372(3) 0.0309(3) -0.0053(3) 0.0138(2) -0.0044(3)
O11 0.0350(16) 0.0299(16) 0.0313(19) 0.0031(16) 0.0133(14) -0.0044(15)
O12 0.0324(17) 0.0298(18) 0.033(2) -0.0067(15) 0.0034(15) -0.0022(14)
O13 0.0314(17) 0.0348(18) 0.0263(19) -0.0072(18) 0.0056(15) 0.0027(16)
C11 0.024(2) 0.040(3) 0.027(3) -0.005(2) 0.018(2) -0.003(2)
C12 0.032(3) 0.026(3) 0.040(3) -0.003(2) 0.020(3) 0.000(2)
C13 0.066(3) 0.041(3) 0.040(3) -0.001(3) 0.020(3) -0.006(2)
C14 0.034(3) 0.053(3) 0.052(4) -0.005(3) 0.014(3) 0.010(2)
O21 0.0254(16) 0.043(2) 0.032(2) -0.0066(15) 0.0112(15) -0.0041(13)
O22 0.0316(19) 0.082(2) 0.056(2) -0.0179(19) 0.0236(18) 0.0007(17)
O23 0.0197(17) 0.0484(19) 0.045(2) -0.0160(17) 0.0107(17) -0.0021(15)
C21 0.031(3) 0.042(3) 0.031(3) 0.004(2) 0.014(2) 0.004(2)
C22 0.027(3) 0.042(3) 0.037(3) -0.011(2) 0.018(2) -0.004(2)
C23 0.060(4) 0.040(3) 0.140(6) -0.019(4) 0.055(4) -0.006(3)
C24 0.051(3) 0.122(5) 0.041(4) -0.026(3) 0.020(3) -0.016(3)
N1 0.029(2) 0.043(2) 0.032(3) -0.007(2) 0.0183(19) -0.0063(18)
N2 0.033(3) 0.056(3) 0.045(3) 0.007(2) 0.021(2) 0.002(2)
C1 0.033(3) 0.047(3) 0.030(3) 0.000(2) 0.014(3) 0.000(2)
C2 0.054(3) 0.065(4) 0.051(4) -0.028(3) 0.034(3) -0.027(3)
C3 0.062(3) 0.059(3) 0.057(4) -0.015(3) 0.044(3) -0.009(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'
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
O11 Cu O23 169.96(11) . . ?
O11 Cu O21 88.99(11) . . ?
O23 Cu O21 81.22(11) . . ?
O11 Cu N1 94.54(12) . . ?
O23 Cu N1 95.18(13) . . ?
O21 Cu N1 152.45(12) . . ?
O11 Cu O13 76.64(10) . . ?
O23 Cu O13 102.35(11) . . ?
O21 Cu O13 97.60(10) . . ?
N1 Cu O13 109.81(12) . . ?
C11 O11 Cu 121.8(3) . . ?
C12 O13 Cu 109.2(2) . . ?
O12 C11 O11 123.3(4) . . ?
O12 C11 C12 117.6(4) . . ?
O11 C11 C12 119.1(4) . . ?
O13 C12 C13 110.5(3) . . ?
O13 C12 C14 109.5(3) . . ?
C13 C12 C14 110.9(3) . . ?
O13 C12 C11 105.3(3) . . ?
C13 C12 C11 111.7(3) . . ?
C14 C12 C11 108.7(3) . . ?
C21 O21 Cu 116.8(3) . . ?
C22 O23 Cu 116.5(2) . . ?
O22 C21 O21 123.7(4) . . ?
O22 C21 C22 118.4(4) . . ?
O21 C21 C22 117.9(4) . . ?
O23 C22 C23 108.3(3) . . ?
O23 C22 C24 109.3(3) . . ?
C23 C22 C24 112.0(4) . . ?
O23 C22 C21 106.2(3) . . ?
C23 C22 C21 111.0(3) . . ?
C24 C22 C21 109.8(4) . . ?
C1 N1 C2 106.0(3) . . ?
C1 N1 Cu 128.4(3) . . ?
C2 N1 Cu 125.6(3) . . ?
C3 N2 C1 107.7(4) . . ?
N1 C1 N2 110.8(4) . . ?
C3 C2 N1 109.2(4) . . ?
N2 C3 C2 106.4(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
Cu O11 1.932(3) . ?
Cu O23 1.951(3) . ?
Cu O21 1.956(3) . ?
Cu N1 1.973(3) . ?
Cu O13 2.256(3) . ?
O11 C11 1.271(4) . ?
O12 C11 1.242(4) . ?
O13 C12 1.447(4) . ?
C11 C12 1.529(5) . ?
C12 C13 1.523(5) . ?
C12 C14 1.527(5) . ?
O21 C21 1.289(4) . ?
O22 C21 1.228(4) . ?
O23 C22 1.454(4) . ?
C21 C22 1.514(5) . ?
C22 C23 1.498(5) . ?
C22 C24 1.509(6) . ?
N1 C1 1.310(4) . ?
N1 C2 1.362(5) . ?
N2 C3 1.344(5) . ?
N2 C1 1.344(5) . ?
C2 C3 1.358(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
O23 H23 O12 0.94(4) 1.67(4) 2.597(4) 166(3) 4_676
O13 H13 O21 0.93(4) 1.91(4) 2.827(4) 167(3) 4_676
N2 H20 O22 0.96(4) 1.82(4) 2.759(5) 166(4) 1_655
C1 H1 O12 0.93 2.50 3.391(5) 160.7 4_676
|
1100161.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100161.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_1100161
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C12 H19 N4 O6.5 Zn'
_chemical_formula_weight 388.68
_space_group_IT_number 60
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2n 2ab'
_symmetry_space_group_name_H-M 'P b 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 20.4557(18)
_cell_length_b 10.4408(9)
_cell_length_c 15.0918(13)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 3223.2(5)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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 0.0610
_diffrn_reflns_av_sigmaI/netI 0.0790
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 17452
_diffrn_reflns_theta_full 28.05
_diffrn_reflns_theta_max 28.05
_diffrn_reflns_theta_min 1.99
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.564
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.7299
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.602
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description irregular
_exptl_crystal_F_000 1608
_exptl_crystal_size_max .35
_exptl_crystal_size_mid .30
_exptl_crystal_size_min .20
_refine_diff_density_max 0.820
_refine_diff_density_min -0.435
_refine_diff_density_rms 0.074
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.924
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 231
_refine_ls_number_reflns 3852
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.924
_refine_ls_R_factor_all 0.1021
_refine_ls_R_factor_gt 0.0401
_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^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0869
_refine_ls_wR_factor_ref 0.0986
_reflns_number_gt 2192
_reflns_number_total 3852
_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.
'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-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 Pbcn
_cod_original_formula_sum 'C12 H19 N4 O6.50 Zn'
_cod_database_code 1100161
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.675359(17) 0.25899(3) 0.02269(2) 0.02716(12) Uani 1 1 d . . .
O11 O 0.64856(12) 0.2044(2) -0.10604(13) 0.0328(5) Uani 1 1 d . . .
O12 O 0.59094(15) 0.2516(3) -0.22429(16) 0.0707(10) Uani 1 1 d . . .
O13 O 0.60352(12) 0.3947(2) -0.01164(14) 0.0306(6) Uani 1 1 d . . .
C11 C 0.60685(17) 0.2694(3) -0.1461(2) 0.0347(8) Uani 1 1 d . . .
C12 C 0.57569(19) 0.3814(4) -0.0985(2) 0.0455(10) Uani 1 1 d . . .
H12 H 0.5882 0.4584 -0.1316 0.055 Uiso 1 1 calc R . .
C13 C 0.5056(2) 0.3776(5) -0.0986(3) 0.0943(19) Uani 1 1 d . . .
H13A H 0.4908 0.3135 -0.0576 0.142 Uiso 1 1 calc R . .
H13B H 0.4903 0.3570 -0.1570 0.142 Uiso 1 1 calc R . .
H13C H 0.4888 0.4597 -0.0812 0.142 Uiso 1 1 calc R . .
O21 O 0.75764(11) 0.14416(19) 0.00791(14) 0.0323(5) Uani 1 1 d . . .
O22 O 0.86440(13) 0.1343(2) -0.01276(18) 0.0522(7) Uani 1 1 d . . .
O23 O 0.75153(11) 0.3870(2) -0.03947(15) 0.0323(6) Uani 1 1 d . . .
C21 C 0.81239(18) 0.1925(3) -0.0114(2) 0.0291(8) Uani 1 1 d . . .
C22 C 0.81607(17) 0.3355(3) -0.0325(2) 0.0328(8) Uani 1 1 d . . .
H22 H 0.8379 0.3781 0.0172 0.039 Uiso 1 1 calc R . .
C23 C 0.8558(2) 0.3604(4) -0.1147(2) 0.0521(11) Uani 1 1 d . . .
H23A H 0.8326 0.3291 -0.1655 0.078 Uiso 1 1 calc R . .
H23B H 0.8971 0.3171 -0.1100 0.078 Uiso 1 1 calc R . .
H23C H 0.8631 0.4508 -0.1209 0.078 Uiso 1 1 calc R . .
N1 N 0.70376(14) 0.3442(3) 0.14391(17) 0.0317(7) Uani 1 1 d . . .
N2 N 0.75677(15) 0.3670(3) 0.26949(18) 0.0352(7) Uani 1 1 d . . .
C1 C 0.75114(18) 0.2999(3) 0.1942(2) 0.0347(8) Uani 1 1 d . . .
H1 H 0.7775 0.2306 0.1793 0.042 Uiso 1 1 calc R . .
C2 C 0.67814(17) 0.4447(3) 0.1899(2) 0.0382(9) Uani 1 1 d . . .
H2 H 0.6435 0.4953 0.1709 0.046 Uiso 1 1 calc R . .
C3 C 0.71045(19) 0.4599(3) 0.2669(2) 0.0408(9) Uani 1 1 d . . .
H3 H 0.7026 0.5219 0.3098 0.049 Uiso 1 1 calc R . .
N3 N 0.61780(14) 0.1223(3) 0.08526(17) 0.0331(7) Uani 1 1 d . . .
N4 N 0.59152(18) -0.0367(3) 0.1728(2) 0.0454(9) Uani 1 1 d . . .
C4 C 0.6382(2) 0.0406(3) 0.1448(2) 0.0389(9) Uani 1 1 d . . .
H4 H 0.6811 0.0373 0.1653 0.047 Uiso 1 1 calc R . .
C5 C 0.5541(2) 0.0934(5) 0.0752(3) 0.0787(16) Uani 1 1 d . . .
H5 H 0.5257 0.1358 0.0371 0.094 Uiso 1 1 calc R . .
C6 C 0.5372(2) -0.0052(5) 0.1280(3) 0.0846(17) Uani 1 1 d . . .
H6 H 0.4963 -0.0436 0.1324 0.101 Uiso 1 1 calc R . .
H23 H 0.7519(17) 0.462(3) -0.016(2) 0.046(11) Uiso 1 1 d . . .
H40 H 0.5996(16) -0.096(3) 0.210(2) 0.038(11) Uiso 1 1 d . . .
H13 H 0.616(2) 0.465(4) -0.005(3) 0.070(15) Uiso 1 1 d . . .
H20 H 0.785(2) 0.348(4) 0.319(3) 0.082(15) Uiso 1 1 d . . .
O1W O 0.5000 0.324(2) 0.2500 0.607(19) 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
Zn 0.0311(2) 0.02526(19) 0.02511(19) 0.00038(17) -0.00047(17) 0.00110(19)
O11 0.0392(14) 0.0316(12) 0.0277(12) -0.0046(10) -0.0015(11) 0.0089(11)
O12 0.098(2) 0.073(2) 0.0411(15) -0.0311(14) -0.0331(16) 0.0458(18)
O13 0.0381(15) 0.0257(13) 0.0281(12) -0.0068(10) -0.0075(11) 0.0039(11)
C11 0.041(2) 0.0308(19) 0.0321(17) -0.0081(15) -0.0057(16) 0.0031(17)
C12 0.051(3) 0.047(2) 0.038(2) -0.0175(17) -0.021(2) 0.019(2)
C13 0.057(3) 0.140(5) 0.086(4) -0.064(3) -0.026(3) 0.040(3)
O21 0.0323(14) 0.0206(11) 0.0438(14) 0.0031(9) -0.0001(11) 0.0019(10)
O22 0.0347(16) 0.0334(14) 0.089(2) 0.0079(13) 0.0078(15) 0.0092(12)
O23 0.0339(15) 0.0217(12) 0.0412(14) -0.0007(10) 0.0013(11) 0.0022(11)
C21 0.034(2) 0.0250(15) 0.0288(18) -0.0009(14) -0.0026(16) -0.0007(15)
C22 0.036(2) 0.0230(16) 0.040(2) -0.0008(15) -0.0014(17) -0.0013(16)
C23 0.047(3) 0.042(2) 0.068(3) 0.016(2) 0.017(2) -0.002(2)
N1 0.0354(17) 0.0340(16) 0.0256(14) 0.0001(12) -0.0043(13) -0.0017(14)
N2 0.0392(19) 0.0394(18) 0.0270(15) 0.0051(13) -0.0059(15) -0.0006(15)
C1 0.040(2) 0.0325(19) 0.0315(18) -0.0003(15) 0.0007(17) -0.0009(17)
C2 0.038(2) 0.044(2) 0.0327(19) -0.0007(16) -0.0025(18) 0.0082(19)
C3 0.046(3) 0.045(2) 0.032(2) -0.0089(17) 0.0034(18) 0.0025(19)
N3 0.0352(19) 0.0334(16) 0.0306(15) 0.0065(12) -0.0029(13) -0.0040(14)
N4 0.059(2) 0.045(2) 0.0321(18) 0.0153(15) 0.0004(17) -0.0063(18)
C4 0.047(3) 0.037(2) 0.0327(19) 0.0066(16) -0.0050(18) -0.0052(19)
C5 0.052(3) 0.094(4) 0.089(4) 0.062(3) -0.023(3) -0.014(3)
C6 0.044(3) 0.099(4) 0.110(4) 0.056(3) -0.006(3) -0.025(3)
O1W 0.48(3) 0.42(2) 0.92(6) 0.000 0.02(3) 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N3 Zn O21 96.40(10) . . ?
N3 Zn O11 94.95(10) . . ?
O21 Zn O11 87.45(9) . . ?
N3 Zn O13 100.28(11) . . ?
O21 Zn O13 157.93(9) . . ?
O11 Zn O13 76.85(8) . . ?
N3 Zn N1 92.94(10) . . ?
O21 Zn N1 96.48(10) . . ?
O11 Zn N1 170.74(10) . . ?
O13 Zn N1 96.99(10) . . ?
N3 Zn O23 170.79(10) . . ?
O21 Zn O23 74.81(8) . . ?
O11 Zn O23 87.50(9) . . ?
O13 Zn O23 88.92(9) . . ?
N1 Zn O23 85.47(10) . . ?
C11 O11 Zn 118.7(2) . . ?
C12 O13 Zn 115.87(19) . . ?
O12 C11 O11 124.1(3) . . ?
O12 C11 C12 117.2(3) . . ?
O11 C11 C12 118.6(3) . . ?
C13 C12 O13 113.5(3) . . ?
C13 C12 C11 113.5(3) . . ?
O13 C12 C11 109.9(3) . . ?
C21 O21 Zn 120.8(2) . . ?
C22 O23 Zn 112.59(18) . . ?
O22 C21 O21 125.2(3) . . ?
O22 C21 C22 116.0(3) . . ?
O21 C21 C22 118.8(3) . . ?
O23 C22 C23 111.9(3) . . ?
O23 C22 C21 109.7(3) . . ?
C23 C22 C21 111.5(3) . . ?
C1 N1 C2 105.1(3) . . ?
C1 N1 Zn 123.6(2) . . ?
C2 N1 Zn 131.2(2) . . ?
C1 N2 C3 106.8(3) . . ?
N1 C1 N2 111.7(3) . . ?
C3 C2 N1 110.0(3) . . ?
C2 C3 N2 106.5(3) . . ?
C4 N3 C5 103.9(3) . . ?
C4 N3 Zn 125.4(3) . . ?
C5 N3 Zn 130.6(2) . . ?
C4 N4 C6 106.7(3) . . ?
N3 C4 N4 112.8(4) . . ?
N3 C5 C6 110.6(4) . . ?
N4 C6 C5 105.9(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
Zn N3 2.077(3) . ?
Zn O21 2.079(2) . ?
Zn O11 2.098(2) . ?
Zn O13 2.106(2) . ?
Zn N1 2.115(3) . ?
Zn O23 2.257(2) . ?
O11 C11 1.246(4) . ?
O12 C11 1.238(4) . ?
O13 C12 1.436(4) . ?
C11 C12 1.513(4) . ?
C12 C13 1.434(5) . ?
O21 C21 1.263(4) . ?
O22 C21 1.225(4) . ?
O23 C22 1.429(4) . ?
C21 C22 1.528(4) . ?
C22 C23 1.505(5) . ?
N1 C1 1.315(4) . ?
N1 C2 1.363(4) . ?
N2 C1 1.340(4) . ?
N2 C3 1.356(4) . ?
C2 C3 1.346(5) . ?
N3 C4 1.308(4) . ?
N3 C5 1.346(5) . ?
N4 C4 1.320(4) . ?
N4 C6 1.342(5) . ?
C5 C6 1.347(6) . ?
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
N2 H20 O11 0.96(4) 1.86(4) 2.799(4) 167(4) 2_655
O13 H13 O22 0.79(4) 1.81(4) 2.587(3) 168(4) 8_765
N4 H40 O12 0.85(3) 1.92(3) 2.729(4) 160(3) 7_556
O23 H23 O21 0.86(4) 1.94(4) 2.785(3) 165(3) 8_765
|
1100162.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100162.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_1100162
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C14 H22 N4 O6 Zn'
_chemical_formula_weight 407.73
_space_group_IT_number 96
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_Hall 'P 4nw 2abw'
_symmetry_space_group_name_H-M 'P 43 21 2'
_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 10.7634(9)
_cell_length_b 10.7634(9)
_cell_length_c 16.442(3)
_cell_measurement_reflns_used 991
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.11
_cell_measurement_theta_min 2.26
_cell_volume 1904.8(4)
_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 '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 0.0231
_diffrn_reflns_av_sigmaI/netI 0.0161
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 8295
_diffrn_reflns_theta_full 23.25
_diffrn_reflns_theta_max 23.25
_diffrn_reflns_theta_min 2.26
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 1.325
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9429
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.422
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description octahedral
_exptl_crystal_F_000 848
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.32
_refine_diff_density_max 0.662
_refine_diff_density_min -0.134
_refine_diff_density_rms 0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.47(3)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.157
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 125
_refine_ls_number_reflns 1366
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.157
_refine_ls_R_factor_all 0.0369
_refine_ls_R_factor_gt 0.0326
_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^)+(0.0477P)^2^+0.5646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0809
_refine_ls_wR_factor_ref 0.0828
_reflns_number_gt 1276
_reflns_number_total 1366
_reflns_threshold_expression >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.
'_exptl_absorpt_correction_type' value 'MULTISCAN' changed to
'multi-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 P4(3)2(1)2
_cod_database_code 1100162
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x+1/2, z+3/4'
'-x, -y, z+1/2'
'y+1/2, -x+1/2, z+1/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-x+1/2, y+1/2, -z+3/4'
'-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
_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
Zn Zn 0.25021(3) 0.74979(3) 0.2500 0.0288(2) Uani 1 2 d S . .
O11 O 0.2538(2) 0.5604(2) 0.28451(13) 0.0410(6) Uani 1 1 d . . .
O12 O 0.2248(2) 0.3656(2) 0.24867(14) 0.0437(6) Uani 1 1 d . . .
O13 O 0.1980(3) 0.6502(2) 0.14469(15) 0.0461(7) Uani 1 1 d . . .
C11 C 0.2317(3) 0.4799(3) 0.23344(19) 0.0304(8) Uani 1 1 d . . .
C12 C 0.2078(4) 0.5175(3) 0.1450(2) 0.0426(10) Uani 1 1 d . . .
C13 C 0.3161(5) 0.4769(5) 0.0941(3) 0.0815(17) Uani 1 1 d . . .
H13A H 0.3045 0.5048 0.0391 0.122 Uiso 1 1 calc R . .
H13B H 0.3218 0.3879 0.0949 0.122 Uiso 1 1 calc R . .
H13C H 0.3912 0.5120 0.1156 0.122 Uiso 1 1 calc R . .
C14 C 0.0862(5) 0.4616(4) 0.1159(3) 0.0783(16) Uani 1 1 d . . .
H14A H 0.0203 0.4865 0.1517 0.117 Uiso 1 1 calc R . .
H14B H 0.0927 0.3727 0.1157 0.117 Uiso 1 1 calc R . .
H14C H 0.0688 0.4904 0.0618 0.117 Uiso 1 1 calc R . .
N1 N 0.0739(2) 0.7635(3) 0.30306(17) 0.0418(7) Uani 1 1 d . . .
N2 N -0.1284(3) 0.7657(4) 0.3111(2) 0.0582(10) Uani 1 1 d . . .
C1 C -0.0305(3) 0.7539(4) 0.2636(2) 0.0462(9) Uani 1 1 d . . .
H1 H -0.0355 0.7402 0.2078 0.055 Uiso 1 1 calc R . .
C2 C 0.0388(4) 0.7857(6) 0.3799(3) 0.087(2) Uani 1 1 d . . .
H2 H 0.0930 0.7988 0.4231 0.104 Uiso 1 1 calc R . .
C3 C -0.0855(4) 0.7864(6) 0.3858(3) 0.095(2) Uani 1 1 d . . .
H3 H -0.1322 0.7989 0.4327 0.114 Uiso 1 1 calc R . .
H13 H 0.181(5) 0.680(5) 0.090(4) 0.105(18) Uiso 1 1 d . . .
H20 H -0.194(4) 0.782(4) 0.286(3) 0.065(13) 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
Zn 0.0282(2) 0.0282(2) 0.0302(3) -0.00220(15) -0.00220(15) 0.0000(3)
O11 0.0603(16) 0.0320(13) 0.0307(12) 0.0011(10) -0.0066(12) -0.0004(13)
O12 0.0653(18) 0.0294(13) 0.0363(12) 0.0018(10) 0.0007(14) -0.0008(12)
O13 0.0758(19) 0.0285(14) 0.0341(13) 0.0020(12) -0.0154(12) -0.0021(12)
C11 0.038(2) 0.0239(17) 0.0296(16) 0.0003(14) 0.0007(17) 0.0017(15)
C12 0.065(3) 0.027(2) 0.0364(19) -0.0006(16) -0.0056(17) -0.0016(16)
C13 0.131(5) 0.058(3) 0.056(3) 0.004(2) 0.035(3) 0.019(3)
C14 0.102(4) 0.052(3) 0.080(3) 0.013(3) -0.045(3) -0.024(3)
N1 0.0310(16) 0.0494(19) 0.0449(18) 0.0011(16) 0.0000(13) 0.0006(15)
N2 0.0265(17) 0.091(3) 0.058(2) -0.003(2) -0.0049(16) 0.005(2)
C1 0.0315(19) 0.063(3) 0.0438(19) 0.001(2) -0.0057(16) 0.0058(19)
C2 0.036(3) 0.176(7) 0.047(3) -0.027(3) -0.002(2) -0.008(3)
C3 0.047(3) 0.185(7) 0.054(3) -0.019(3) 0.006(2) 0.003(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 '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'
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'
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 Zn N1 92.63(16) 8_665 . ?
N1 Zn O13 97.83(11) 8_665 8_665 ?
N1 Zn O13 95.73(10) . 8_665 ?
N1 Zn O13 95.73(10) 8_665 . ?
N1 Zn O13 97.83(11) . . ?
O13 Zn O13 160.32(14) 8_665 . ?
N1 Zn O11 170.40(10) 8_665 . ?
N1 Zn O11 88.44(10) . . ?
O13 Zn O11 91.55(9) 8_665 . ?
O13 Zn O11 74.68(9) . . ?
N1 Zn O11 88.44(10) 8_665 8_665 ?
N1 Zn O11 170.40(10) . 8_665 ?
O13 Zn O11 74.68(9) 8_665 8_665 ?
O13 Zn O11 91.55(9) . 8_665 ?
O11 Zn O11 92.09(14) . 8_665 ?
C11 O11 Zn 119.46(19) . . ?
C12 O13 Zn 118.9(2) . . ?
O11 C11 O12 124.4(3) . . ?
O11 C11 C12 119.7(3) . . ?
O12 C11 C12 116.0(3) . . ?
O13 C12 C13 110.2(4) . . ?
O13 C12 C14 109.3(3) . . ?
C13 C12 C14 112.2(4) . . ?
O13 C12 C11 106.2(3) . . ?
C13 C12 C11 108.8(3) . . ?
C14 C12 C11 109.9(3) . . ?
C1 N1 C2 103.9(3) . . ?
C1 N1 Zn 124.7(2) . . ?
C2 N1 Zn 131.4(3) . . ?
C1 N2 C3 106.6(3) . . ?
N1 C1 N2 112.8(3) . . ?
N1 C2 C3 110.5(4) . . ?
N2 C3 C2 106.2(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
Zn N1 2.094(3) 8_665 ?
Zn N1 2.094(3) . ?
Zn O13 2.113(2) 8_665 ?
Zn O13 2.113(2) . ?
Zn O11 2.117(2) . ?
Zn O11 2.117(2) 8_665 ?
O11 C11 1.230(4) . ?
O12 C11 1.258(4) . ?
O13 C12 1.432(4) . ?
C11 C12 1.531(5) . ?
C12 C13 1.500(6) . ?
C12 C14 1.518(6) . ?
N1 C1 1.302(4) . ?
N1 C2 1.341(5) . ?
N2 C1 1.318(5) . ?
N2 C3 1.331(6) . ?
C2 C3 1.341(6) . ?
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
C2 H2 O12 0.93 2.45 3.346(5) 161.2 7
O13 H13 O12 0.98(6) 1.65(6) 2.623(3) 173(5) 2_554
N2 H20 O12 0.84(5) 1.93(5) 2.737(4) 160(4) 8_565
|
1100163.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100163.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_1100163
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C46 H46 N12 O6 Zn'
_chemical_formula_weight 928.32
_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 119.763(6)
_cell_angle_gamma 90.00
_cell_formula_units_Z 2
_cell_length_a 12.9507(17)
_cell_length_b 9.0191(11)
_cell_length_c 22.209(3)
_cell_measurement_reflns_used 1011
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 20.53
_cell_measurement_theta_min 2.49
_cell_volume 2251.9(5)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_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 0.0446
_diffrn_reflns_av_sigmaI/netI 0.0748
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 12535
_diffrn_reflns_theta_full 28.03
_diffrn_reflns_theta_max 28.03
_diffrn_reflns_theta_min 1.81
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.608
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.9374
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.369
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 968
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.23
_refine_diff_density_max 0.220
_refine_diff_density_min -0.286
_refine_diff_density_rms 0.052
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.048
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 308
_refine_ls_number_reflns 5094
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.048
_refine_ls_R_factor_all 0.1162
_refine_ls_R_factor_gt 0.0621
_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^)+(0.0371P)^2^+0.8501P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1005
_refine_ls_wR_factor_ref 0.1152
_reflns_number_gt 3207
_reflns_number_total 5094
_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.
'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-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 P2(1)/c
_cod_database_code 1100163
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
Zn Zn 0.5000 0.5000 0.0000 0.03725(15) Uani 1 2 d S . .
N1 N 0.6128(2) 0.4223(3) 0.10618(12) 0.0407(6) Uani 1 1 d . . .
N2 N 0.7507(3) 0.4149(4) 0.21557(16) 0.0559(8) Uani 1 1 d . . .
C1 C 0.7013(3) 0.4931(4) 0.15769(16) 0.0538(8) Uani 1 1 d . . .
H1 H 0.7262 0.5875 0.1538 0.065 Uiso 1 1 calc R . .
C2 C 0.6065(3) 0.2922(4) 0.13474(18) 0.0630(10) Uani 1 1 d . . .
H2 H 0.5514 0.2175 0.1114 0.076 Uiso 1 1 calc R . .
C3 C 0.6921(3) 0.2870(4) 0.20210(19) 0.0706(11) Uani 1 1 d . . .
H3 H 0.7071 0.2094 0.2330 0.085 Uiso 1 1 calc R . .
N3 N 0.37383(19) 0.5927(3) 0.02845(12) 0.0400(6) Uani 1 1 d . . .
N4 N 0.2203(3) 0.7046(4) 0.02270(17) 0.0682(10) Uani 1 1 d . . .
C4 C 0.2804(3) 0.6746(4) -0.00977(17) 0.0555(9) Uani 1 1 d . . .
H4 H 0.2589 0.7077 -0.0541 0.067 Uiso 1 1 calc R . .
C5 C 0.3709(3) 0.5701(4) 0.08801(18) 0.0559(9) Uani 1 1 d . . .
H5 H 0.4266 0.5155 0.1257 0.067 Uiso 1 1 calc R . .
C6 C 0.2756(3) 0.6383(4) 0.0845(2) 0.0689(11) Uani 1 1 d . . .
H6 H 0.2531 0.6391 0.1182 0.083 Uiso 1 1 calc R . .
N5 N 0.6029(2) 0.7078(3) 0.02842(12) 0.0409(6) Uani 1 1 d . . .
N6 N 0.7492(3) 0.8647(3) 0.05575(15) 0.0556(8) Uani 1 1 d . . .
C7 C 0.6984(3) 0.7386(4) 0.02441(17) 0.0512(8) Uani 1 1 d . . .
H7 H 0.7273 0.6785 0.0020 0.061 Uiso 1 1 calc R . .
C9 C 0.6844(4) 0.9189(4) 0.0824(2) 0.0781(12) Uani 1 1 d . . .
H9 H 0.6987 1.0059 0.1078 0.094 Uiso 1 1 calc R . .
C8 C 0.5943(3) 0.8231(4) 0.0652(2) 0.0675(11) Uani 1 1 d . . .
H8 H 0.5349 0.8340 0.0768 0.081 Uiso 1 1 calc R . .
O11 O 0.05247(18) -0.0084(2) 0.15984(10) 0.0518(5) Uani 1 1 d . . .
O12 O -0.07190(17) 0.0218(2) 0.04798(10) 0.0460(5) Uani 1 1 d . . .
O13 O 0.05581(18) 0.2265(2) 0.03114(9) 0.0415(5) Uani 1 1 d . . .
H13 H 0.0565 0.1505 0.0111 0.062 Uiso 1 1 calc R . .
C11 C 0.0190(2) 0.0565(3) 0.10437(15) 0.0343(6) Uani 1 1 d . . .
C12 C 0.0906(2) 0.1927(3) 0.10160(13) 0.0314(6) Uani 1 1 d . . .
C13 C 0.0606(2) 0.3294(3) 0.13070(14) 0.0331(6) Uani 1 1 d . . .
C14 C 0.0444(3) 0.4649(3) 0.09876(17) 0.0484(8) Uani 1 1 d . . .
H14 H 0.0484 0.4715 0.0582 0.058 Uiso 1 1 calc R . .
C15 C 0.0224(3) 0.5909(4) 0.1257(2) 0.0603(9) Uani 1 1 d . . .
H15 H 0.0112 0.6812 0.1030 0.072 Uiso 1 1 calc R . .
C16 C 0.0170(3) 0.5837(4) 0.1852(2) 0.0633(10) Uani 1 1 d . . .
H16 H 0.0034 0.6692 0.2037 0.076 Uiso 1 1 calc R . .
C17 C 0.0314(4) 0.4515(4) 0.2174(2) 0.0680(11) Uani 1 1 d . . .
H17 H 0.0264 0.4459 0.2577 0.082 Uiso 1 1 calc R . .
C18 C 0.0534(3) 0.3251(4) 0.19049(17) 0.0582(9) Uani 1 1 d . . .
H18 H 0.0635 0.2352 0.2132 0.070 Uiso 1 1 calc R . .
C19 C 0.2236(2) 0.1551(3) 0.14163(14) 0.0353(7) Uani 1 1 d . . .
C20 C 0.3052(3) 0.2300(4) 0.1983(2) 0.0784(12) Uani 1 1 d . . .
H20 H 0.2811 0.3096 0.2149 0.094 Uiso 1 1 calc R . .
C21 C 0.4246(3) 0.1894(5) 0.2319(3) 0.1077(18) Uani 1 1 d . . .
H21 H 0.4791 0.2425 0.2706 0.129 Uiso 1 1 calc R . .
C22 C 0.4622(3) 0.0752(5) 0.2093(2) 0.0788(12) Uani 1 1 d . . .
H22 H 0.5418 0.0469 0.2326 0.095 Uiso 1 1 calc R . .
C23 C 0.3824(3) 0.0023(5) 0.1523(2) 0.0841(13) Uani 1 1 d . . .
H23 H 0.4076 -0.0756 0.1354 0.101 Uiso 1 1 calc R . .
C24 C 0.2645(3) 0.0408(4) 0.11877(18) 0.0712(11) Uani 1 1 d . . .
H24 H 0.2112 -0.0120 0.0796 0.085 Uiso 1 1 calc R . .
H60 H 0.812(3) 0.911(4) 0.0571(18) 0.077(12) Uiso 1 1 d . . .
H20 H 0.801(3) 0.442(4) 0.251(2) 0.082(14) Uiso 1 1 d . . .
H40 H 0.164(4) 0.751(4) 0.008(2) 0.088(15) 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
Zn 0.0281(2) 0.0407(3) 0.0370(3) 0.0006(2) 0.0117(2) -0.0026(2)
N1 0.0308(13) 0.0454(14) 0.0374(14) -0.0006(12) 0.0105(11) -0.0020(12)
N2 0.0463(17) 0.069(2) 0.0360(18) 0.0007(17) 0.0079(14) -0.0009(16)
C1 0.0462(18) 0.0535(19) 0.0437(19) 0.0054(19) 0.0086(15) -0.0078(18)
C2 0.061(2) 0.053(2) 0.053(2) 0.0102(18) 0.0114(18) -0.0125(18)
C3 0.069(3) 0.068(3) 0.048(2) 0.0199(19) 0.0086(19) -0.009(2)
N3 0.0318(13) 0.0417(14) 0.0424(15) 0.0019(12) 0.0153(12) 0.0016(11)
N4 0.0375(18) 0.093(3) 0.057(2) -0.0178(19) 0.0106(16) 0.0229(18)
C4 0.048(2) 0.066(2) 0.042(2) 0.0006(17) 0.0139(16) 0.0159(18)
C5 0.050(2) 0.067(2) 0.051(2) 0.0150(18) 0.0249(17) 0.0154(18)
C6 0.053(2) 0.100(3) 0.061(3) 0.001(2) 0.034(2) 0.016(2)
N5 0.0333(14) 0.0422(14) 0.0438(15) -0.0023(12) 0.0166(12) -0.0048(11)
N6 0.0485(17) 0.0500(17) 0.069(2) -0.0084(15) 0.0297(16) -0.0185(15)
C7 0.047(2) 0.0490(19) 0.058(2) -0.0105(17) 0.0265(17) -0.0134(16)
C9 0.085(3) 0.051(2) 0.113(4) -0.032(2) 0.060(3) -0.024(2)
C8 0.065(2) 0.057(2) 0.098(3) -0.021(2) 0.055(2) -0.016(2)
O11 0.0513(12) 0.0509(12) 0.0387(12) 0.0112(11) 0.0114(10) -0.0120(11)
O12 0.0399(11) 0.0548(13) 0.0330(11) -0.0079(10) 0.0103(9) -0.0150(10)
O13 0.0552(13) 0.0423(11) 0.0247(11) 0.0026(9) 0.0180(10) 0.0026(10)
C11 0.0315(15) 0.0368(15) 0.0347(17) -0.0053(14) 0.0164(13) -0.0002(13)
C12 0.0339(15) 0.0333(15) 0.0238(14) 0.0000(12) 0.0119(12) -0.0018(12)
C13 0.0309(15) 0.0360(16) 0.0300(16) -0.0010(13) 0.0133(12) -0.0052(12)
C14 0.062(2) 0.0424(19) 0.0436(19) 0.0021(15) 0.0282(16) -0.0028(15)
C15 0.074(2) 0.0364(18) 0.069(3) 0.0040(18) 0.034(2) 0.0079(18)
C16 0.080(3) 0.047(2) 0.081(3) -0.017(2) 0.053(2) 0.0001(19)
C17 0.106(3) 0.058(2) 0.071(3) -0.011(2) 0.068(3) -0.005(2)
C18 0.091(3) 0.0444(19) 0.055(2) -0.0011(17) 0.048(2) -0.0021(18)
C19 0.0335(16) 0.0364(15) 0.0324(16) 0.0028(13) 0.0137(13) -0.0043(13)
C20 0.046(2) 0.060(2) 0.088(3) -0.027(2) 0.002(2) 0.0007(18)
C21 0.043(2) 0.069(3) 0.136(4) -0.031(3) -0.012(2) -0.007(2)
C22 0.034(2) 0.071(3) 0.111(4) 0.015(3) 0.021(2) 0.005(2)
C23 0.058(2) 0.112(3) 0.075(3) -0.007(3) 0.027(2) 0.034(3)
C24 0.051(2) 0.094(3) 0.049(2) -0.020(2) 0.0100(17) 0.021(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Zn Zn 0.2839 1.4301 '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'
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'
O O 0.0106 0.0060 '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 Zn N1 180.00(12) . 3_665 ?
N1 Zn N3 90.35(9) . . ?
N1 Zn N3 89.65(9) 3_665 . ?
N1 Zn N3 89.65(9) . 3_665 ?
N1 Zn N3 90.35(9) 3_665 3_665 ?
N3 Zn N3 180.00(11) . 3_665 ?
N1 Zn N5 88.76(9) . . ?
N1 Zn N5 91.24(9) 3_665 . ?
N3 Zn N5 91.38(9) . . ?
N3 Zn N5 88.62(9) 3_665 . ?
N1 Zn N5 91.24(9) . 3_665 ?
N1 Zn N5 88.76(9) 3_665 3_665 ?
N3 Zn N5 88.62(9) . 3_665 ?
N3 Zn N5 91.38(9) 3_665 3_665 ?
N5 Zn N5 180.0 . 3_665 ?
C1 N1 C2 104.0(3) . . ?
C1 N1 Zn 127.7(2) . . ?
C2 N1 Zn 128.3(2) . . ?
C1 N2 C3 107.3(3) . . ?
N1 C1 N2 112.3(3) . . ?
C3 C2 N1 110.0(3) . . ?
N2 C3 C2 106.4(3) . . ?
C4 N3 C5 104.7(3) . . ?
C4 N3 Zn 127.7(2) . . ?
C5 N3 Zn 127.6(2) . . ?
C4 N4 C6 107.9(3) . . ?
N3 C4 N4 111.5(3) . . ?
C6 C5 N3 110.1(3) . . ?
N4 C6 C5 105.9(3) . . ?
C7 N5 C8 103.9(3) . . ?
C7 N5 Zn 128.1(2) . . ?
C8 N5 Zn 127.2(2) . . ?
C7 N6 C9 106.8(3) . . ?
N5 C7 N6 112.6(3) . . ?
N6 C9 C8 106.6(3) . . ?
C9 C8 N5 110.1(3) . . ?
O11 C11 O12 124.6(3) . . ?
O11 C11 C12 119.5(2) . . ?
O12 C11 C12 115.9(2) . . ?
O13 C12 C13 106.4(2) . . ?
O13 C12 C19 109.6(2) . . ?
C13 C12 C19 112.4(2) . . ?
O13 C12 C11 109.9(2) . . ?
C13 C12 C11 109.7(2) . . ?
C19 C12 C11 108.8(2) . . ?
C14 C13 C18 117.1(3) . . ?
C14 C13 C12 120.2(2) . . ?
C18 C13 C12 122.6(3) . . ?
C13 C14 C15 121.4(3) . . ?
C16 C15 C14 120.3(3) . . ?
C17 C16 C15 119.7(3) . . ?
C16 C17 C18 120.1(3) . . ?
C13 C18 C17 121.4(3) . . ?
C20 C19 C24 116.9(3) . . ?
C20 C19 C12 124.2(3) . . ?
C24 C19 C12 118.8(3) . . ?
C19 C20 C21 120.9(4) . . ?
C22 C21 C20 121.0(4) . . ?
C21 C22 C23 118.5(4) . . ?
C22 C23 C24 121.1(4) . . ?
C19 C24 C23 121.5(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
Zn N1 2.183(2) . ?
Zn N1 2.183(2) 3_665 ?
Zn N3 2.189(2) . ?
Zn N3 2.189(2) 3_665 ?
Zn N5 2.203(2) . ?
Zn N5 2.203(2) 3_665 ?
N1 C1 1.315(4) . ?
N1 C2 1.355(4) . ?
N2 C1 1.320(4) . ?
N2 C3 1.331(4) . ?
C2 C3 1.350(5) . ?
N3 C4 1.308(4) . ?
N3 C5 1.357(4) . ?
N4 C4 1.326(4) . ?
N4 C6 1.333(5) . ?
C5 C6 1.346(4) . ?
N5 C7 1.314(3) . ?
N5 C8 1.360(4) . ?
N6 C7 1.325(4) . ?
N6 C9 1.337(4) . ?
C9 C8 1.346(5) . ?
O11 C11 1.232(3) . ?
O12 C11 1.260(3) . ?
O13 C12 1.430(3) . ?
C11 C12 1.559(4) . ?
C12 C13 1.529(4) . ?
C12 C19 1.534(4) . ?
C13 C14 1.376(4) . ?
C13 C18 1.377(4) . ?
C14 C15 1.379(4) . ?
C15 C16 1.359(5) . ?
C16 C17 1.355(5) . ?
C17 C18 1.381(4) . ?
C19 C20 1.355(4) . ?
C19 C24 1.367(4) . ?
C20 C21 1.391(5) . ?
C21 C22 1.339(6) . ?
C22 C23 1.342(5) . ?
C23 C24 1.370(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
C24 H24 O12 0.93 2.49 3.329(4) 149.8 3
C18 H18 O11 0.93 2.47 3.083(4) 123.8 .
C17 H17 O11 0.93 2.53 3.418(4) 158.7 2
C14 H14 O13 0.93 2.30 2.668(3) 102.7 .
N4 H40 O13 0.76(4) 2.54(4) 3.218(4) 150(4) 3_565
N4 H40 O12 0.76(4) 2.38(4) 3.041(4) 145(4) 3_565
N2 H20 O11 0.78(4) 1.99(4) 2.762(4) 171(4) 2_655
N6 H60 O12 0.90(3) 1.90(4) 2.793(3) 172(3) 1_665
O13 H13 O12 0.82 2.11 2.918(3) 170.1 3
|
1100164.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100164.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_1100164
loop_
_publ_author_name
'Carballo, Rosa'
'Vazquez-Lopez, Ezequiel M.'
'Covelo, Berta'
'Garcia-Martinez, Emilia'
'Castineiras, Alfonso'
'Niclos, Juan'
_publ_section_title
;
'Solid state coordination chemistry of mononuclear
mixed-ligand complexes of Ni(II), Cu(II) and Zn(II)
with \a-hydroxycarboxylic acids and imidazole'
;
_journal_name_full Polyhedron
_journal_page_first 1505
_journal_page_last 1518
_journal_paper_doi 10.1016/j.poly.2004.02.028
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C14 H22 N4 Ni O6'
_chemical_formula_weight 401.07
_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 111.795(7)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 19.392(7)
_cell_length_b 8.477(3)
_cell_length_c 11.412(4)
_cell_measurement_reflns_used 793
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 24.14
_cell_measurement_theta_min 2.26
_cell_volume 1741.9(11)
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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 0.0308
_diffrn_reflns_av_sigmaI/netI 0.0380
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -8
_diffrn_reflns_number 4760
_diffrn_reflns_theta_full 26.37
_diffrn_reflns_theta_max 26.37
_diffrn_reflns_theta_min 2.26
_exptl_absorpt_coefficient_mu 1.152
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8297
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour blue
_exptl_crystal_density_diffrn 1.529
_exptl_crystal_density_meas 0
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description prism
_exptl_crystal_F_000 840
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.19
_refine_diff_density_max 0.262
_refine_diff_density_min -0.274
_refine_diff_density_rms 0.050
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 124
_refine_ls_number_reflns 1763
_refine_ls_number_restraints 2
_refine_ls_restrained_S_all 1.063
_refine_ls_R_factor_all 0.0409
_refine_ls_R_factor_gt 0.0317
_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^)+(0.0296P)^2^+0.5632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0663
_refine_ls_wR_factor_ref 0.0691
_reflns_number_gt 1532
_reflns_number_total 1763
_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.
'_exptl_absorpt_correction_type' value 'MULTISCAN' changed to
'multi-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 C2/c
_cod_database_code 1100164
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
Ni Ni 0.0000 0.79895(4) 0.2500 0.02665(13) Uani 1 2 d S . .
O11 O 0.05320(8) 0.81401(16) 0.44164(12) 0.0340(3) Uani 1 1 d . . .
O12 O 0.13975(8) 0.9299(2) 0.60449(13) 0.0431(4) Uani 1 1 d . . .
O13 O 0.07923(8) 0.97856(17) 0.27340(13) 0.0342(4) Uani 1 1 d D . .
C11 C 0.10259(11) 0.9170(2) 0.48868(18) 0.0294(4) Uani 1 1 d . . .
C12 C 0.11769(11) 1.0365(2) 0.39974(18) 0.0295(4) Uani 1 1 d . . .
C13 C 0.08497(15) 1.1936(2) 0.4162(2) 0.0463(6) Uani 1 1 d . . .
H13A H 0.0912 1.2690 0.3581 0.069 Uiso 1 1 calc R . .
H13B H 0.1099 1.2305 0.5010 0.069 Uiso 1 1 calc R . .
H13C H 0.0330 1.1808 0.3998 0.069 Uiso 1 1 calc R . .
C14 C 0.20018(12) 1.0497(3) 0.4267(2) 0.0454(6) Uani 1 1 d . . .
H14A H 0.2194 0.9478 0.4183 0.068 Uiso 1 1 calc R . .
H14B H 0.2253 1.0881 0.5110 0.068 Uiso 1 1 calc R . .
H14C H 0.2080 1.1216 0.3678 0.068 Uiso 1 1 calc R . .
N1 N 0.07141(9) 0.6296(2) 0.23057(15) 0.0333(4) Uani 1 1 d . . .
N2 N 0.10586(15) 0.4211(2) 0.1534(2) 0.0545(6) Uani 1 1 d D . .
C1 C 0.04898(14) 0.5073(3) 0.1555(2) 0.0406(5) Uani 1 1 d . . .
H1 H -0.0006 0.4838 0.1093 0.049 Uiso 1 1 calc R . .
C2 C 0.14728(13) 0.6183(3) 0.2790(2) 0.0469(6) Uani 1 1 d . . .
H2 H 0.1791 0.6891 0.3359 0.056 Uiso 1 1 calc R . .
C3 C 0.16916(16) 0.4903(3) 0.2327(3) 0.0553(7) Uani 1 1 d . . .
H3 H 0.2176 0.4561 0.2511 0.066 Uiso 1 1 calc R . .
H13 H 0.0978(13) 1.013(3) 0.223(2) 0.057(8) Uiso 1 1 d D . .
H20 H 0.100(2) 0.336(3) 0.107(3) 0.113(13) 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
Ni 0.0329(2) 0.02337(19) 0.0246(2) 0.000 0.01184(15) 0.000
O11 0.0448(8) 0.0329(8) 0.0259(7) 0.0051(6) 0.0149(6) -0.0043(7)
O12 0.0439(9) 0.0654(11) 0.0207(8) 0.0020(7) 0.0129(7) -0.0014(8)
O13 0.0463(9) 0.0382(8) 0.0203(7) -0.0030(6) 0.0150(7) -0.0148(7)
C11 0.0344(11) 0.0340(11) 0.0236(10) 0.0012(9) 0.0152(9) 0.0072(9)
C12 0.0397(12) 0.0295(10) 0.0200(10) -0.0026(8) 0.0119(9) -0.0053(9)
C13 0.0683(16) 0.0302(11) 0.0435(13) -0.0015(10) 0.0243(12) 0.0002(11)
C14 0.0442(13) 0.0554(15) 0.0384(13) -0.0017(11) 0.0176(11) -0.0135(11)
N1 0.0386(11) 0.0282(9) 0.0321(10) -0.0027(8) 0.0120(8) 0.0027(7)
N2 0.0922(18) 0.0333(11) 0.0585(14) -0.0047(10) 0.0516(14) 0.0062(12)
C1 0.0554(14) 0.0347(12) 0.0345(12) -0.0050(10) 0.0201(11) -0.0031(11)
C2 0.0410(14) 0.0478(14) 0.0493(14) -0.0066(12) 0.0135(11) 0.0025(11)
C3 0.0581(17) 0.0554(16) 0.0658(18) 0.0123(14) 0.0384(15) 0.0212(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
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'
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
O11 Ni O11 172.85(8) . 2 ?
O11 Ni N1 91.19(6) . 2 ?
O11 Ni N1 93.79(6) 2 2 ?
O11 Ni N1 93.79(6) . . ?
O11 Ni N1 91.19(6) 2 . ?
N1 Ni N1 91.79(10) 2 . ?
O11 Ni O13 76.41(5) . . ?
O11 Ni O13 98.33(6) 2 . ?
N1 Ni O13 167.32(6) 2 . ?
N1 Ni O13 91.70(7) . . ?
O11 Ni O13 98.33(6) . 2 ?
O11 Ni O13 76.41(5) 2 2 ?
N1 Ni O13 91.70(7) 2 2 ?
N1 Ni O13 167.32(6) . 2 ?
O13 Ni O13 87.54(9) . 2 ?
C11 O11 Ni 120.04(12) . . ?
C12 O13 Ni 117.05(11) . . ?
O12 C11 O11 123.95(18) . . ?
O12 C11 C12 117.58(18) . . ?
O11 C11 C12 118.46(17) . . ?
O13 C12 C14 110.06(16) . . ?
O13 C12 C13 109.76(17) . . ?
C14 C12 C13 111.60(18) . . ?
O13 C12 C11 106.34(15) . . ?
C14 C12 C11 111.11(17) . . ?
C13 C12 C11 107.81(17) . . ?
C1 N1 C2 104.75(19) . . ?
C1 N1 Ni 123.16(15) . . ?
C2 N1 Ni 131.96(15) . . ?
C1 N2 C3 107.5(2) . . ?
N1 C1 N2 111.7(2) . . ?
C3 C2 N1 110.3(2) . . ?
C2 C3 N2 105.8(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
Ni O11 2.0465(15) . ?
Ni O11 2.0465(15) 2 ?
Ni N1 2.0632(17) 2 ?
Ni N1 2.0632(17) . ?
Ni O13 2.1084(15) . ?
Ni O13 2.1084(15) 2 ?
O11 C11 1.259(2) . ?
O12 C11 1.253(2) . ?
O13 C12 1.441(2) . ?
C11 C12 1.537(3) . ?
C12 C14 1.517(3) . ?
C12 C13 1.517(3) . ?
N1 C1 1.312(3) . ?
N1 C2 1.369(3) . ?
N2 C1 1.331(3) . ?
N2 C3 1.358(4) . ?
C2 C3 1.343(3) . ?
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
N2 H20 O12 0.874(18) 2.39(3) 3.141(3) 145(3) 6_565
N2 H20 O11 0.874(18) 2.18(2) 3.004(3) 158(3) 6_565
O13 H13 O12 0.832(17) 1.886(17) 2.716(2) 175(3) 6_575
|
1100165.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100165.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_1100165
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_journal_name_full Polyhedron
_journal_page_first 743
_journal_page_last 747
_journal_paper_doi 10.1016/j.poly.2003.11.052
_journal_volume 23
_journal_year 2004
_chemical_formula_moiety ?
_chemical_formula_sum 'C10 H18 N8 O8 Zn'
_chemical_formula_weight 443.69
_chemical_melting_point ?
_chemical_name_common ?
_chemical_name_systematic
;
Diaqua bis(4,7-dihydro-1,2,4-triazolo[1,5-a]pyrimidine-7-one-N3)zinc(II) tetrah
;
_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'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary heavy
_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 7.5430(8)
_cell_length_b 13.1384(12)
_cell_length_c 17.2599(10)
_cell_measurement_reflns_used 24
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 19.5
_cell_measurement_theta_min 12.5
_cell_volume 1710.5(3)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 0.26 - 2.16, scan ratio 2theta:omega = 1.00
I(Net) and sigma(I) from profile fitting (Clegg, 1981)
;
_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 0.0449
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_number 2487
_diffrn_reflns_theta_full 29.97
_diffrn_reflns_theta_max 29.97
_diffrn_reflns_theta_min 2.36
_diffrn_standards_decay_% 5.3
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 60
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.497
_exptl_absorpt_correction_T_max 0.7119
_exptl_absorpt_correction_T_min 0.6309
_exptl_absorpt_correction_type psi-scan
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.723
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'brick shaped'
_exptl_crystal_F_000 912
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.32
_refine_diff_density_max 1.497
_refine_diff_density_min -1.329
_refine_diff_density_rms 0.175
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.025
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 142
_refine_ls_number_reflns 2487
_refine_ls_number_restraints 9
_refine_ls_restrained_S_all 1.023
_refine_ls_R_factor_all 0.1402
_refine_ls_R_factor_gt 0.0872
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1400P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2186
_refine_ls_wR_factor_ref 0.2760
_reflns_number_gt 1389
_reflns_number_total 2487
_reflns_threshold_expression >2sigma(I)
_cod_database_code 1100165
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.5000 0.5000 0.5000 0.0289(3) Uani 1 2 d S . .
N1 N 0.5663(8) 0.6072(4) 0.7330(3) 0.0380(12) Uani 1 1 d . . .
C2 C 0.5665(10) 0.6056(4) 0.6561(3) 0.0381(13) Uani 1 1 d . . .
H2 H 0.6153 0.6585 0.6273 0.080 Uiso 1 1 d R . .
N3 N 0.4916(6) 0.5241(4) 0.6217(3) 0.0312(11) Uani 1 1 d . . .
C3A C 0.4325(8) 0.4677(4) 0.6814(3) 0.0287(11) Uani 1 1 d . . .
N4 N 0.3473(7) 0.3804(4) 0.6811(3) 0.0349(11) Uani 1 1 d . . .
C5 C 0.3027(9) 0.3442(4) 0.7521(3) 0.0399(13) Uani 1 1 d . . .
H5 H 0.2359 0.2847 0.7537 0.080 Uiso 1 1 d R . .
C6 C 0.3468(9) 0.3887(5) 0.8212(3) 0.0379(14) Uani 1 1 d . . .
H6 H 0.3143 0.3575 0.8675 0.080 Uiso 1 1 d R . .
C7 C 0.4414(9) 0.4793(5) 0.8234(3) 0.0354(13) Uani 1 1 d . . .
O7 O 0.4936(5) 0.5290(4) 0.8816(2) 0.0383(10) Uani 1 1 d . . .
N8 N 0.4802(6) 0.5171(3) 0.7488(3) 0.0283(10) Uani 1 1 d . . .
O1W O 0.5919(7) 0.3492(3) 0.5142(3) 0.0423(11) Uani 1 1 d D . .
H11W H 0.656(10) 0.339(6) 0.474(3) 0.080 Uiso 1 1 d D . .
H12W H 0.578(12) 0.291(3) 0.536(4) 0.080 Uiso 1 1 d D . .
O2W O 0.2328(6) 0.4447(4) 0.5042(2) 0.0396(10) Uani 1 1 d D . .
H21W H 0.181(10) 0.474(6) 0.543(2) 0.080 Uiso 1 1 d D . .
H22W H 0.188(10) 0.468(6) 0.463(2) 0.080 Uiso 1 1 d D . .
O3W O 0.8544(7) 0.2856(3) 0.4198(2) 0.0461(12) Uani 1 1 d D . .
H31W H 0.846(11) 0.239(4) 0.386(3) 0.080 Uiso 1 1 d D . .
H32W H 0.872(12) 0.344(3) 0.399(4) 0.080 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
Zn 0.0385(6) 0.0355(5) 0.0128(4) -0.0012(3) 0.0008(3) 0.0023(4)
N1 0.051(3) 0.044(3) 0.019(2) -0.0026(19) -0.002(2) -0.007(2)
C2 0.057(4) 0.036(3) 0.021(3) 0.000(2) 0.002(3) -0.005(3)
N3 0.038(3) 0.038(2) 0.018(2) -0.0016(17) -0.0012(17) -0.001(2)
C3A 0.036(3) 0.037(3) 0.013(2) -0.004(2) 0.003(2) 0.005(2)
N4 0.048(3) 0.038(2) 0.019(2) -0.0043(18) -0.001(2) 0.000(2)
C5 0.053(4) 0.035(3) 0.031(3) 0.001(3) 0.009(3) 0.001(3)
C6 0.047(4) 0.040(3) 0.027(3) -0.002(2) 0.009(2) 0.000(3)
C7 0.042(3) 0.050(3) 0.014(2) -0.003(2) 0.000(2) 0.010(3)
O7 0.050(3) 0.053(2) 0.0123(19) -0.0069(17) 0.0051(15) 0.0007(19)
N8 0.033(2) 0.037(2) 0.016(2) -0.0026(17) -0.0010(16) -0.0016(18)
O1W 0.056(3) 0.036(2) 0.035(2) 0.0035(18) 0.012(2) 0.007(2)
O2W 0.043(2) 0.059(3) 0.0168(18) 0.0018(17) 0.0030(16) 0.000(2)
O3W 0.070(3) 0.041(2) 0.027(2) -0.0061(18) 0.006(2) 0.008(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'
Zn Zn 0.2839 1.4301 '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 Zn N3 92.00(19) . . ?
O1W Zn O2W 89.25(19) . . ?
N3 Zn O2W 89.37(16) . . ?
C2 N1 N8 100.6(5) . . ?
N1 C2 N3 116.9(5) . . ?
C3A N3 C2 103.8(5) . . ?
C3A N3 Zn 133.3(4) . . ?
C2 N3 Zn 122.8(4) . . ?
N4 C3A N3 129.7(5) . . ?
N4 C3A N8 122.9(5) . . ?
N3 C3A N8 107.4(5) . . ?
C3A N4 C5 115.0(5) . . ?
N4 C5 C6 125.2(6) . . ?
C5 C6 C7 120.9(6) . . ?
O7 C7 C6 128.7(6) . . ?
O7 C7 N8 118.7(6) . . ?
C6 C7 N8 112.6(5) . . ?
N1 N8 C3A 111.2(5) . . ?
N1 N8 C7 125.5(5) . . ?
C3A N8 C7 123.3(5) . . ?
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
Zn O1W 2.113(4) . ?
Zn N3 2.125(5) . ?
Zn O2W 2.143(5) . ?
N1 C2 1.327(7) . ?
N1 N8 1.377(7) . ?
C2 N3 1.348(8) . ?
N3 C3A 1.346(7) . ?
C3A N4 1.315(8) . ?
C3A N8 1.379(7) . ?
N4 C5 1.356(7) . ?
C5 C6 1.370(8) . ?
C6 C7 1.389(9) . ?
C7 O7 1.262(7) . ?
C7 N8 1.411(7) . ?
|
1100166.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100166.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_1100166
loop_
_publ_author_name
'Norie Momiyama'
'Hisashi Yamamoto'
_publ_section_title
;
Enantioselective O- and N-Nitroso Aldol Synthesis of Tin Enolates. Isolation
of Three BINAP-Silver Complexes and Their Role in Regio- and
Enantioselectivity
;
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 5360
_journal_page_last 5361
_journal_paper_doi 10.1021/ja039103i
_journal_volume 126
_journal_year 2004
_chemical_formula_sum 'C44.75 H32 Ag O2 P2'
_chemical_formula_weight 771.51
_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 117.15(3)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 17.417(3)
_cell_length_b 21.402(4)
_cell_length_c 11.298(2)
_cell_measurement_reflns_used ?
_cell_measurement_temperature 546(2)
_cell_measurement_theta_max ?
_cell_measurement_theta_min ?
_cell_volume 3747.4(12)
_diffrn_ambient_temperature 546(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 0.71073
_diffrn_reflns_av_R_equivalents 0.0276
_diffrn_reflns_av_sigmaI/netI 0.0202
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 18018
_diffrn_reflns_theta_full 25.03
_diffrn_reflns_theta_max 25.03
_diffrn_reflns_theta_min 1.62
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number ?
_exptl_absorpt_coefficient_mu 0.660
_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 1.367
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 1574
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 3.332
_refine_diff_density_min -0.590
_refine_diff_density_rms 0.265
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.587
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 230
_refine_ls_number_reflns 3315
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.587
_refine_ls_R_factor_all 0.0963
_refine_ls_R_factor_gt 0.0940
_refine_ls_shift/su_max 1.399
_refine_ls_shift/su_mean 0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3306
_refine_ls_wR_factor_ref 0.3336
_reflns_number_gt 3161
_reflns_number_total 3315
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M C2/c
_cod_database_code 1100166
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
Ag1 Ag 0.0000 0.29309(3) 0.2500 0.0525(5) Uani 1 2 d S . .
C1 C 0.0676(4) 0.2479(3) 0.0036(6) 0.0392(13) Uani 1 1 d . . .
C2 C 0.0674(5) 0.3111(4) -0.0075(9) 0.063(2) Uani 1 1 d . . .
H2 H 0.0424 0.3355 0.0338 0.075 Uiso 1 1 calc R . .
C3 C 0.1046(8) 0.3400(4) -0.0812(12) 0.092(3) Uani 1 1 d . . .
H3 H 0.1049 0.3833 -0.0875 0.110 Uiso 1 1 calc R . .
C4 C 0.1401(6) 0.3044(5) -0.1428(10) 0.070(2) Uani 1 1 d . . .
H4 H 0.1644 0.3233 -0.1919 0.084 Uiso 1 1 calc R . .
C5 C 0.1402(6) 0.2405(5) -0.1329(9) 0.070(2) Uani 1 1 d . . .
H5 H 0.1640 0.2161 -0.1760 0.084 Uiso 1 1 calc R . .
C6 C 0.1049(7) 0.2124(3) -0.0587(9) 0.061(2) Uani 1 1 d . . .
H6 H 0.1062 0.1691 -0.0506 0.073 Uiso 1 1 calc R . .
C7 C 0.0788(3) 0.1547(3) 0.2046(5) 0.0311(11) Uani 1 1 d . . .
C8 C 0.1677(3) 0.1561(3) 0.2424(6) 0.0393(13) Uani 1 1 d . . .
H8 H 0.1891 0.1859 0.2055 0.047 Uiso 1 1 calc R . .
C9 C 0.2228(4) 0.1147(3) 0.3316(6) 0.0416(13) Uani 1 1 d . . .
H9 H 0.2816 0.1175 0.3574 0.050 Uiso 1 1 calc R . .
C10 C 0.1916(3) 0.0672(3) 0.3859(6) 0.0394(13) Uani 1 1 d . . .
C11 C 0.2475(4) 0.0219(3) 0.4775(7) 0.0496(16) Uani 1 1 d . . .
H11 H 0.3061 0.0227 0.5006 0.059 Uiso 1 1 calc R . .
C12 C 0.2176(4) -0.0217(3) 0.5309(7) 0.0532(17) Uani 1 1 d . . .
H12 H 0.2555 -0.0501 0.5920 0.064 Uiso 1 1 calc R . .
C13 C 0.1307(4) -0.0248(3) 0.4959(6) 0.0462(14) Uani 1 1 d . . .
H13 H 0.1104 -0.0562 0.5310 0.055 Uiso 1 1 calc R . .
C14 C 0.0737(3) 0.0182(3) 0.4095(6) 0.0387(13) Uani 1 1 d . . .
H14 H 0.0156 0.0163 0.3889 0.046 Uiso 1 1 calc R . .
C15 C 0.1031(3) 0.0649(3) 0.3525(5) 0.0331(12) Uani 1 1 d . . .
C16 C 0.0454(3) 0.1117(2) 0.2617(5) 0.0271(11) Uani 1 1 d . . .
C17 C -0.0841(4) 0.1808(3) -0.0312(5) 0.0379(12) Uani 1 1 d . . .
C18 C -0.0811(4) 0.1298(3) -0.1041(6) 0.0484(15) Uani 1 1 d . . .
H18 H -0.0282 0.1141 -0.0921 0.058 Uiso 1 1 calc R . .
C19 C -0.1567(5) 0.1025(4) -0.1947(7) 0.0568(18) Uani 1 1 d . . .
H19 H -0.1544 0.0675 -0.2419 0.068 Uiso 1 1 calc R . .
C20 C -0.2343(5) 0.1256(4) -0.2163(7) 0.069(2) Uani 1 1 d . . .
H20 H -0.2845 0.1070 -0.2796 0.082 Uiso 1 1 calc R . .
C21 C -0.2399(5) 0.1760(5) -0.1461(8) 0.068(2) Uani 1 1 d . . .
H21 H -0.2936 0.1908 -0.1600 0.081 Uiso 1 1 calc R . .
C22 C -0.1640(4) 0.2055(3) -0.0528(7) 0.0500(18) Uani 1 1 d . . .
H22 H -0.1669 0.2407 -0.0065 0.060 Uiso 1 1 calc R . .
C23 C 0.0000 0.4162(8) 0.2500 0.21(3) Uani 0.82(6) 2 d SP . .
O1 O 0.0649(5) 0.3922(4) 0.3139(15) 0.167(8) Uani 1.00(3) 1 d . . .
P1 P 0.01206(10) 0.21793(7) 0.09591(15) 0.0338(5) 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
Ag1 0.0845(7) 0.0325(6) 0.0607(7) 0.000 0.0505(5) 0.000
C1 0.043(3) 0.040(3) 0.036(3) 0.001(2) 0.020(2) -0.008(2)
C2 0.086(5) 0.037(4) 0.093(6) 0.002(4) 0.065(5) -0.004(4)
C3 0.134(8) 0.054(5) 0.145(9) 0.027(6) 0.113(8) 0.003(5)
C4 0.070(5) 0.083(6) 0.072(5) 0.024(5) 0.044(4) -0.010(4)
C5 0.091(6) 0.081(6) 0.068(5) -0.017(4) 0.061(5) -0.020(5)
C6 0.104(6) 0.039(4) 0.068(5) -0.004(3) 0.064(5) -0.007(3)
C7 0.036(3) 0.029(3) 0.032(2) -0.003(2) 0.019(2) -0.003(2)
C8 0.039(3) 0.046(3) 0.039(3) -0.003(2) 0.024(2) -0.008(2)
C9 0.032(3) 0.045(3) 0.049(3) -0.002(3) 0.019(2) 0.001(2)
C10 0.036(3) 0.035(3) 0.046(3) -0.004(2) 0.018(2) -0.004(2)
C11 0.032(3) 0.048(4) 0.060(4) 0.005(3) 0.014(3) 0.009(2)
C12 0.043(3) 0.051(4) 0.051(3) 0.011(3) 0.008(3) 0.012(3)
C13 0.050(3) 0.041(3) 0.043(3) 0.004(3) 0.017(3) 0.002(2)
C14 0.038(3) 0.032(3) 0.045(3) 0.000(2) 0.018(2) 0.000(2)
C15 0.028(2) 0.035(3) 0.032(2) -0.001(2) 0.010(2) 0.005(2)
C16 0.032(3) 0.023(3) 0.029(2) -0.0043(18) 0.0155(19) -0.0007(18)
C17 0.043(3) 0.034(3) 0.036(3) 0.004(2) 0.017(2) -0.002(2)
C18 0.051(3) 0.045(4) 0.042(3) 0.006(3) 0.016(3) 0.010(3)
C19 0.060(4) 0.049(4) 0.047(3) 0.000(3) 0.012(3) -0.002(3)
C20 0.055(4) 0.083(6) 0.051(4) 0.003(4) 0.010(3) -0.018(4)
C21 0.041(3) 0.091(7) 0.065(4) 0.018(4) 0.018(3) 0.004(4)
C22 0.048(4) 0.059(5) 0.045(4) 0.009(3) 0.023(3) 0.006(3)
C23 0.053(12) 0.040(10) 0.37(5) 0.000 -0.053(17) 0.000
O1 0.062(5) 0.056(5) 0.306(17) 0.034(7) 0.018(6) 0.003(3)
P1 0.0431(9) 0.0288(8) 0.0342(8) 0.0017(5) 0.0217(7) 0.0004(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'
Ag Ag -0.8971 1.1015 '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'
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
O1 Ag1 O1 51.7(4) 2 . ?
O1 Ag1 P1 123.9(4) 2 . ?
O1 Ag1 P1 128.6(4) . . ?
O1 Ag1 P1 128.6(4) 2 2 ?
O1 Ag1 P1 123.9(4) . 2 ?
P1 Ag1 P1 97.87(7) . 2 ?
C2 C1 C6 118.9(6) . . ?
C2 C1 P1 114.9(5) . . ?
C6 C1 P1 126.2(5) . . ?
C1 C2 C3 120.6(8) . . ?
C4 C3 C2 119.7(8) . . ?
C3 C4 C5 120.1(8) . . ?
C4 C5 C6 119.9(8) . . ?
C1 C6 C5 120.7(7) . . ?
C16 C7 C8 120.5(5) . . ?
C16 C7 P1 121.6(4) . . ?
C8 C7 P1 117.4(4) . . ?
C9 C8 C7 121.4(6) . . ?
C8 C9 C10 120.6(5) . . ?
C15 C10 C9 119.7(5) . . ?
C15 C10 C11 118.1(5) . . ?
C9 C10 C11 122.1(5) . . ?
C12 C11 C10 121.5(6) . . ?
C11 C12 C13 120.4(6) . . ?
C14 C13 C12 120.9(6) . . ?
C13 C14 C15 120.2(5) . . ?
C14 C15 C10 118.9(5) . . ?
C14 C15 C16 122.1(5) . . ?
C10 C15 C16 118.9(5) . . ?
C7 C16 C15 118.7(5) . . ?
C7 C16 C16 123.7(4) . 2 ?
C15 C16 C16 117.6(4) . 2 ?
C18 C17 C22 119.9(6) . . ?
C18 C17 P1 123.0(5) . . ?
C22 C17 P1 117.1(5) . . ?
C19 C18 C17 119.7(6) . . ?
C20 C19 C18 121.1(7) . . ?
C19 C20 C21 120.8(7) . . ?
C20 C21 C22 119.8(7) . . ?
C17 C22 C21 118.5(7) . . ?
O1 C23 O1 126.7(19) 2 . ?
C23 O1 Ag1 90.8(10) . . ?
C17 P1 C1 103.8(3) . . ?
C17 P1 C7 106.2(3) . . ?
C1 P1 C7 107.5(3) . . ?
C17 P1 Ag1 120.1(2) . . ?
C1 P1 Ag1 114.4(2) . . ?
C7 P1 Ag1 103.97(17) . . ?
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
Ag1 O1 2.356(8) 2 ?
Ag1 O1 2.356(8) . ?
Ag1 P1 2.4486(16) . ?
Ag1 P1 2.4486(16) 2 ?
C1 C2 1.358(10) . ?
C1 C6 1.382(10) . ?
C1 P1 1.832(6) . ?
C2 C3 1.411(11) . ?
C3 C4 1.356(14) . ?
C4 C5 1.372(13) . ?
C5 C6 1.384(11) . ?
C7 C16 1.393(7) . ?
C7 C8 1.406(7) . ?
C7 P1 1.840(5) . ?
C8 C9 1.356(9) . ?
C9 C10 1.417(9) . ?
C10 C15 1.410(7) . ?
C10 C11 1.427(8) . ?
C11 C12 1.340(10) . ?
C12 C13 1.379(9) . ?
C13 C14 1.379(8) . ?
C14 C15 1.407(8) . ?
C15 C16 1.458(7) . ?
C16 C16 1.480(9) 2 ?
C17 C18 1.382(9) . ?
C17 C22 1.404(9) . ?
C17 P1 1.818(6) . ?
C18 C19 1.376(10) . ?
C19 C20 1.353(11) . ?
C20 C21 1.369(14) . ?
C21 C22 1.408(11) . ?
C23 O1 1.149(11) 2 ?
C23 O1 1.149(11) . ?
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
C6 C1 C2 C3 -0.1(13) . . . . ?
P1 C1 C2 C3 -177.2(8) . . . . ?
C1 C2 C3 C4 0.8(16) . . . . ?
C2 C3 C4 C5 -0.4(17) . . . . ?
C3 C4 C5 C6 -0.7(15) . . . . ?
C2 C1 C6 C5 -1.0(13) . . . . ?
P1 C1 C6 C5 175.8(7) . . . . ?
C4 C5 C6 C1 1.4(14) . . . . ?
C16 C7 C8 C9 2.1(8) . . . . ?
P1 C7 C8 C9 174.0(5) . . . . ?
C7 C8 C9 C10 2.4(9) . . . . ?
C8 C9 C10 C15 -3.5(9) . . . . ?
C8 C9 C10 C11 178.4(6) . . . . ?
C15 C10 C11 C12 0.0(10) . . . . ?
C9 C10 C11 C12 178.1(7) . . . . ?
C10 C11 C12 C13 1.5(11) . . . . ?
C11 C12 C13 C14 -2.5(11) . . . . ?
C12 C13 C14 C15 1.9(10) . . . . ?
C13 C14 C15 C10 -0.4(9) . . . . ?
C13 C14 C15 C16 -179.3(5) . . . . ?
C9 C10 C15 C14 -178.7(5) . . . . ?
C11 C10 C15 C14 -0.5(8) . . . . ?
C9 C10 C15 C16 0.3(8) . . . . ?
C11 C10 C15 C16 178.4(5) . . . . ?
C8 C7 C16 C15 -5.2(7) . . . . ?
P1 C7 C16 C15 -176.8(4) . . . . ?
C8 C7 C16 C16 173.2(5) . . . 2 ?
P1 C7 C16 C16 1.6(7) . . . 2 ?
C14 C15 C16 C7 -177.1(5) . . . . ?
C10 C15 C16 C7 4.0(7) . . . . ?
C14 C15 C16 C16 4.4(7) . . . 2 ?
C10 C15 C16 C16 -174.5(5) . . . 2 ?
C22 C17 C18 C19 -2.0(10) . . . . ?
P1 C17 C18 C19 177.2(5) . . . . ?
C17 C18 C19 C20 1.7(11) . . . . ?
C18 C19 C20 C21 -1.6(12) . . . . ?
C19 C20 C21 C22 1.8(12) . . . . ?
C18 C17 C22 C21 2.2(10) . . . . ?
P1 C17 C22 C21 -177.1(6) . . . . ?
C20 C21 C22 C17 -2.1(11) . . . . ?
O1 C23 O1 Ag1 0.000(2) 2 . . . ?
O1 Ag1 O1 C23 0.000(1) 2 . . . ?
P1 Ag1 O1 C23 106.2(7) . . . . ?
P1 Ag1 O1 C23 -115.3(7) 2 . . . ?
C18 C17 P1 C1 63.2(6) . . . . ?
C22 C17 P1 C1 -117.5(5) . . . . ?
C18 C17 P1 C7 -50.0(6) . . . . ?
C22 C17 P1 C7 129.3(5) . . . . ?
C18 C17 P1 Ag1 -167.3(5) . . . . ?
C22 C17 P1 Ag1 11.9(6) . . . . ?
C2 C1 P1 C17 109.9(6) . . . . ?
C6 C1 P1 C17 -67.0(7) . . . . ?
C2 C1 P1 C7 -137.9(5) . . . . ?
C6 C1 P1 C7 45.2(7) . . . . ?
C2 C1 P1 Ag1 -22.9(6) . . . . ?
C6 C1 P1 Ag1 160.2(6) . . . . ?
C16 C7 P1 C17 -52.5(5) . . . . ?
C8 C7 P1 C17 135.7(4) . . . . ?
C16 C7 P1 C1 -163.1(4) . . . . ?
C8 C7 P1 C1 25.1(5) . . . . ?
C16 C7 P1 Ag1 75.2(4) . . . . ?
C8 C7 P1 Ag1 -96.6(4) . . . . ?
O1 Ag1 P1 C17 -68.0(3) 2 . . . ?
O1 Ag1 P1 C17 -133.2(4) . . . . ?
P1 Ag1 P1 C17 80.5(2) 2 . . . ?
O1 Ag1 P1 C1 56.6(3) 2 . . . ?
O1 Ag1 P1 C1 -8.7(4) . . . . ?
P1 Ag1 P1 C1 -155.0(2) 2 . . . ?
O1 Ag1 P1 C7 173.5(3) 2 . . . ?
O1 Ag1 P1 C7 108.3(3) . . . . ?
P1 Ag1 P1 C7 -37.99(17) 2 . . . ?
|
1100167.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100167.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_1100167
_chemical_formula_sum 'La Mn O3'
_space_group_IT_number 62
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall '-P 2c 2ab'
_symmetry_space_group_name_H-M 'P b n m'
_cell_angle_alpha 90.00000
_cell_angle_beta 90.00000
_cell_angle_gamma 90.00000
_cell_formula_units_Z ?
_cell_length_a 5.53649(5)
_cell_length_b 5.74713(5)
_cell_length_c 7.69259(7)
_cell_volume 244.770(4)
_diffrn_radiation_probe neutron
_diffrn_radiation_type 'Constant Wavelength Neutron Diffraction'
_diffrn_radiation_wavelength 1.22720
_diffrn_source 'nuclear reactor'
_pd_meas_2theta_range_inc 0.050000
_pd_meas_2theta_range_max 125.45000
_pd_meas_2theta_range_min 0.00000
_pd_meas_number_of_points 2510
_pd_proc_2theta_range_inc 0.050000
_pd_proc_2theta_range_max 125.4496
_pd_proc_2theta_range_min -0.0005
_pd_proc_ls_prof_R_factor 5.0739
_pd_proc_ls_prof_wR_expected 3.9633
_pd_proc_ls_prof_wR_factor 5.9063
_pd_proc_wavelength 1.227200
_refine_ls_number_parameters 28
_refine_ls_number_reflns 438
_refine_ls_number_restraints 3
_refine_ls_R_I_factor 4.9552
_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_original_sg_symbol_H-M 'P B N M'
_cod_database_code 1100167
#BEGIN Tags that were not found in dictionaries:
_pd_proc_ls_prof_cr_factor 9.2733
_pd_proc_ls_prof_cwr_factor 9.0514
_pd_proc_ls_prof_cwr_expected 6.0738
_pd_proc_ls_prof_chi2 2.2208
_pd_proc_ls_prof_echi2 2.2437
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,-z+1/2
-x,-y,z+1/2
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,z+1/2
x,y,-z+1/2
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_type_symbol
La -0.00768(11) 0.04908(12) 0.25000 0.0043(2) 1.00000 Uiso LA
Mn 0.50000 0.00000 0.00000 0.0026(4) 1.00000 Uiso MN
O1 0.0743(2) 0.4873(2) 0.25000 0.0062(3) 1.00000 Uiso O
O2 0.72563(17) 0.30660(17) 0.03842(12) 0.0053(2) 1.00000 Uiso O
loop_
_atom_type_symbol
_atom_type_scat_length_neutron
_atom_type_scat_source
LA 0.82400 V.F._Sears_Neutron_News_3_26_(1992)
MN -0.37300 V.F._Sears_Neutron_News_3_26_(1992)
O 0.58030 V.F._Sears_Neutron_News_3_26_(1992)
|
1100168.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100168.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_1100168
loop_
_publ_author_name
'Esther R. Acuna-Cueva'
'Rene Faure'
'Nuria A. Illan-Cabeza'
'Sonia B. Jimenez-Pulido'
'Miguel N. Moreno-Carretero'
'Miguel Quiros'
_journal_name_full Polyhedron
_journal_page_first 483
_journal_page_last 488
_journal_paper_doi 10.1016/S0277-5387(02)01374-8
_journal_volume 22
_journal_year 2003
_chemical_formula_sum 'C14 H12 Br2 N8 O4 Pd'
_chemical_formula_weight 622.54
_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 94.351(10)
_cell_angle_beta 106.036(8)
_cell_angle_gamma 109.334(14)
_cell_formula_units_Z 1
_cell_length_a 6.5185(9)
_cell_length_b 7.5119(11)
_cell_length_c 10.7736(9)
_cell_measurement_reflns_used 33
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 14.63
_cell_measurement_theta_min 5.06
_cell_volume 470.21(10)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0273
_diffrn_reflns_av_sigmaI/netI 0.0475
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 3372
_diffrn_reflns_theta_full 29.99
_diffrn_reflns_theta_max 29.99
_diffrn_reflns_theta_min 2.00
_diffrn_standards_decay_% 12.21
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 5.278
_exptl_absorpt_correction_T_max 0.9040
_exptl_absorpt_correction_T_min 0.5196
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 2.198
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description 'flat needles'
_exptl_crystal_F_000 300
_exptl_crystal_size_max 0.5
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.02
_refine_diff_density_max 2.915
_refine_diff_density_min -2.364
_refine_diff_density_rms 0.279
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.074
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 134
_refine_ls_number_reflns 2716
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.074
_refine_ls_R_factor_all 0.0953
_refine_ls_R_factor_gt 0.0720
_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^)+(0.1500P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1998
_refine_ls_wR_factor_ref 0.2209
_reflns_number_gt 2025
_reflns_number_total 2716
_reflns_threshold_expression >2sigma(I)
_cod_database_code 1100168
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
Pd Pd 0.5000 0.5000 0.5000 0.0323(2) Uani 1 2 d S . .
Br Br 0.67601(14) 0.29558(12) 0.61895(9) 0.0520(3) Uani 1 1 d . . .
N1 N 0.0461(12) -0.1330(9) 0.1222(6) 0.0439(14) Uani 1 1 d . . .
C1 C -0.1430(18) -0.3256(13) 0.0720(10) 0.062(2) Uani 1 1 d . . .
H11 H -0.1343 -0.3836 -0.0080 0.075 Uiso 1 1 d R . .
H12 H -0.2885 -0.3109 0.0552 0.075 Uiso 1 1 d R . .
H13 H -0.1276 -0.4059 0.1364 0.075 Uiso 1 1 d R . .
C1A C 0.0420(13) -0.0108(10) 0.2273(7) 0.0396(14) Uani 1 1 d . . .
C2 C 0.2293(16) -0.0880(12) 0.0742(8) 0.0501(18) Uani 1 1 d . . .
O2 O 0.2318(14) -0.1898(10) -0.0162(7) 0.0667(19) Uani 1 1 d . . .
N3 N 0.4057(13) 0.0836(10) 0.1341(7) 0.0502(16) Uani 1 1 d . . .
H3 H 0.5163 0.1131 0.1015 0.060 Uiso 1 1 d R . .
C4 C 0.4324(13) 0.2146(11) 0.2389(7) 0.0409(14) Uani 1 1 d . . .
O4 O 0.6003(11) 0.3587(9) 0.2816(6) 0.0586(16) Uani 1 1 d . . .
C4A C 0.2313(12) 0.1556(10) 0.2863(7) 0.0378(13) Uani 1 1 d . . .
N5 N 0.2313(10) 0.2668(8) 0.3903(6) 0.0358(11) Uani 1 1 d . . .
C6 C 0.0416(13) 0.2202(10) 0.4263(8) 0.0420(15) Uani 1 1 d . . .
H6 H 0.0340 0.2995 0.4942 0.050 Uiso 1 1 d R . .
C7 C -0.1439(13) 0.0518(12) 0.3608(9) 0.0482(17) Uani 1 1 d . . .
H7 H -0.2746 0.0204 0.3864 0.058 Uiso 1 1 d R . .
N8 N -0.1424(12) -0.0660(10) 0.2631(7) 0.0488(15) 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
Pd 0.0308(4) 0.0313(4) 0.0344(4) 0.0064(2) 0.0135(3) 0.0083(3)
Br 0.0436(5) 0.0474(5) 0.0657(6) 0.0252(4) 0.0147(4) 0.0164(4)
N1 0.048(4) 0.037(3) 0.043(3) 0.008(2) 0.011(3) 0.013(3)
C1 0.059(6) 0.040(4) 0.065(5) -0.001(4) 0.005(4) 0.004(4)
C1A 0.040(4) 0.031(3) 0.045(3) 0.008(3) 0.010(3) 0.012(3)
C2 0.059(5) 0.043(4) 0.041(4) 0.006(3) 0.013(3) 0.012(4)
O2 0.087(5) 0.054(4) 0.055(4) -0.004(3) 0.032(4) 0.016(3)
N3 0.051(4) 0.050(4) 0.045(3) -0.002(3) 0.021(3) 0.010(3)
C4 0.039(3) 0.043(4) 0.039(3) 0.006(3) 0.016(3) 0.011(3)
O4 0.045(3) 0.054(3) 0.064(4) -0.006(3) 0.029(3) -0.004(3)
C4A 0.037(3) 0.039(3) 0.037(3) 0.011(2) 0.012(3) 0.012(3)
N5 0.035(3) 0.033(3) 0.040(3) 0.008(2) 0.016(2) 0.009(2)
C6 0.040(4) 0.037(3) 0.052(4) 0.012(3) 0.021(3) 0.013(3)
C7 0.032(3) 0.052(4) 0.061(5) 0.020(4) 0.019(3) 0.011(3)
N8 0.038(3) 0.046(3) 0.057(4) 0.016(3) 0.014(3) 0.007(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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0100
0.00 0.00 -1.00 0.0100
1.00 -1.00 0.00 0.2500
-1.00 1.00 0.00 0.2500
1.00 2.00 2.00 0.0500
-1.00 -2.00 -2.00 0.0500
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
N5 Pd N5 180.0 2_666 . ?
N5 Pd Br 90.37(17) 2_666 2_666 ?
N5 Pd Br 89.63(17) . 2_666 ?
N5 Pd Br 89.63(17) 2_666 . ?
N5 Pd Br 90.37(17) . . ?
Br Pd Br 180.0 2_666 . ?
N5 Pd O4 109.8(2) 2_666 . ?
N5 Pd O4 70.2(2) . . ?
Br Pd O4 93.67(16) 2_666 . ?
Br Pd O4 86.33(16) . . ?
C2 N1 C1A 122.1(6) . . ?
C2 N1 C1 119.3(7) . . ?
C1A N1 C1 118.3(7) . . ?
N8 C1A C4A 124.5(7) . . ?
N8 C1A N1 116.9(7) . . ?
C4A C1A N1 118.6(7) . . ?
O2 C2 N3 122.0(9) . . ?
O2 C2 N1 122.3(8) . . ?
N3 C2 N1 115.7(7) . . ?
C2 N3 C4 129.6(7) . . ?
O4 C4 N3 121.7(7) . . ?
O4 C4 C4A 126.7(7) . . ?
N3 C4 C4A 111.6(6) . . ?
C4 O4 Pd 98.6(5) . . ?
N5 C4A C1A 118.4(7) . . ?
N5 C4A C4 119.3(6) . . ?
C1A C4A C4 122.3(7) . . ?
C6 N5 C4A 118.9(6) . . ?
C6 N5 Pd 116.5(5) . . ?
C4A N5 Pd 124.6(5) . . ?
N5 C6 C7 119.2(7) . . ?
N8 C7 C6 122.9(7) . . ?
C1A N8 C7 115.9(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
Pd N5 2.011(6) 2_666 ?
Pd N5 2.011(6) . ?
Pd Br 2.4432(8) 2_666 ?
Pd Br 2.4432(8) . ?
Pd O4 2.832(6) . ?
N1 C2 1.382(11) . ?
N1 C1A 1.414(9) . ?
N1 C1 1.496(10) . ?
C1A N8 1.310(10) . ?
C1A C4A 1.384(10) . ?
C2 O2 1.199(10) . ?
C2 N3 1.372(10) . ?
N3 C4 1.372(9) . ?
C4 O4 1.202(9) . ?
C4 C4A 1.481(10) . ?
C4A N5 1.346(9) . ?
N5 C6 1.342(9) . ?
C6 C7 1.393(11) . ?
C7 N8 1.326(11) . ?
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
N3 H3 O2 0.86 2.04 2.898(10) 176.6 2_655
|
1100169.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100169.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_1100169
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_journal_name_full Polyhedron
_journal_page_first 2373
_journal_page_last 2379
_journal_paper_doi 10.1016/j.poly.2004.07.024
_journal_volume 23
_journal_year 2004
_chemical_absolute_configuration ad
_chemical_formula_sum 'C20 H20 N16 O8 Pd2'
_chemical_formula_weight 825.32
_chemical_name_systematic
;
Tetrakis(4,5-dihydro-1,2,4-triazolo[1,5-a]pyrimidinate-5-one-mu-N3,N4)
dipalladium(II) tetrahydrate
;
_space_group_IT_number 20
_symmetry_cell_setting orthorhombic
_symmetry_space_group_name_Hall 'C 2c 2'
_symmetry_space_group_name_H-M 'C 2 2 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 12.864(2)
_cell_length_b 14.634(2)
_cell_length_c 30.703(3)
_cell_measurement_reflns_used 39
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.51
_cell_measurement_theta_min 5.14
_cell_volume 5779.7(14)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0649
_diffrn_reflns_av_sigmaI/netI 0.0428
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 43
_diffrn_reflns_limit_l_min -1
_diffrn_reflns_number 5360
_diffrn_reflns_theta_full 30.01
_diffrn_reflns_theta_max 30.01
_diffrn_reflns_theta_min 2.11
_diffrn_standards_decay_% ?
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.320
_exptl_absorpt_correction_T_max 0.6778
_exptl_absorpt_correction_T_min 0.4251
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.897
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 3264
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.688
_refine_diff_density_min -1.642
_refine_diff_density_rms 0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.12(10)
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.256
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 414
_refine_ls_number_reflns 5222
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.256
_refine_ls_R_factor_all 0.0857
_refine_ls_R_factor_gt 0.0765
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1864
_refine_ls_wR_factor_ref 0.1972
_reflns_number_gt 4875
_reflns_number_total 5222
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'C 2 2 2(1) '
_cod_database_code 1100169
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.09834(7) 0.34416(6) 0.26717(3) 0.02683(19) Uani 1 1 d . . .
Pd2 Pd 0.28696(9) 0.0000 0.5000 0.0262(3) Uani 1 2 d S . .
Pd3 Pd 0.07363(10) 0.0000 0.5000 0.0335(3) Uani 1 2 d S . .
N1A N -0.0247(12) 0.1278(9) 0.1455(5) 0.046(3) Uani 1 1 d . . .
C2A C -0.0859(12) 0.1844(10) 0.1646(5) 0.041(3) Uani 1 1 d . . .
H2A H -0.1563 0.1861 0.1578 0.049 Uiso 1 1 d R . .
N3A N -0.0451(9) 0.2415(8) 0.1954(4) 0.030(2) Uani 1 1 d . . .
C3AA C 0.0531(11) 0.2187(9) 0.1950(4) 0.031(3) Uani 1 1 d . . .
N4A N 0.1332(9) 0.2500(7) 0.2201(4) 0.031(2) Uani 1 1 d . . .
C5A C 0.2303(14) 0.2159(10) 0.2148(6) 0.046(4) Uani 1 1 d . . .
O5A O 0.3047(10) 0.2469(8) 0.2354(5) 0.058(3) Uani 1 1 d . . .
C6A C 0.2428(15) 0.1462(13) 0.1818(6) 0.056(5) Uani 1 1 d . . .
H6A H 0.3098 0.1254 0.1762 0.067 Uiso 1 1 d R . .
C7A C 0.1641(14) 0.1111(11) 0.1582(6) 0.052(4) Uani 1 1 d . . .
H7A H 0.1742 0.0628 0.1389 0.062 Uiso 1 1 d R . .
N8A N 0.0679(9) 0.1507(10) 0.1648(4) 0.040(3) Uani 1 1 d . . .
N1B N -0.1931(14) 0.5588(10) 0.3178(6) 0.064(5) Uani 1 1 d . . .
C2B C -0.2101(15) 0.5021(12) 0.2842(5) 0.052(4) Uani 1 1 d . . .
H2B H -0.2711 0.5008 0.2679 0.063 Uiso 1 1 d R . .
N3B N -0.1253(11) 0.4470(7) 0.2761(4) 0.039(3) Uani 1 1 d . . .
C3AB C -0.0548(11) 0.4704(9) 0.3050(4) 0.032(3) Uani 1 1 d . . .
N4B N 0.0406(12) 0.4369(8) 0.3115(4) 0.039(3) Uani 1 1 d . . .
C5B C 0.1011(14) 0.4662(11) 0.3453(5) 0.042(3) Uani 1 1 d . . .
O5B O 0.1862(11) 0.4337(9) 0.3532(4) 0.053(3) Uani 1 1 d . . .
C6B C 0.0510(17) 0.5357(14) 0.3726(5) 0.059(5) Uani 1 1 d . . .
H6B H 0.0843 0.5532 0.3982 0.071 Uiso 1 1 d R . .
C7B C -0.0411(18) 0.5735(13) 0.3630(5) 0.059(5) Uani 1 1 d . . .
H7B H -0.0664 0.6239 0.3782 0.071 Uiso 1 1 d R . .
N8B N -0.0959(14) 0.5358(9) 0.3300(4) 0.050(4) Uani 1 1 d . . .
N1C N 0.062(2) 0.2640(13) 0.4441(7) 0.092(8) Uani 1 1 d . . .
C2C C 0.013(2) 0.1951(15) 0.4623(6) 0.075(8) Uani 1 1 d . . .
H2C H -0.0582 0.1924 0.4675 0.090 Uiso 1 1 d R . .
N3C N 0.0866(14) 0.1281(9) 0.4743(4) 0.053(4) Uani 1 1 d . . .
C3AC C 0.1769(14) 0.1639(10) 0.4643(4) 0.040(4) Uani 1 1 d . . .
N4C N 0.2723(10) 0.1242(8) 0.4692(4) 0.035(2) Uani 1 1 d . . .
C5C C 0.3638(16) 0.1703(10) 0.4592(5) 0.046(4) Uani 1 1 d . . .
O5C O 0.4502(14) 0.1428(11) 0.4644(5) 0.075(4) Uani 1 1 d . . .
C6C C 0.340(2) 0.2615(14) 0.4375(8) 0.079(8) Uani 1 1 d . . .
H6C H 0.3949 0.2938 0.4254 0.094 Uiso 1 1 d R . .
C7C C 0.248(3) 0.2940(14) 0.4327(9) 0.088(9) Uani 1 1 d . . .
H7C H 0.2378 0.3524 0.4215 0.106 Uiso 1 1 d R . .
N8C N 0.1677(19) 0.2455(9) 0.4455(5) 0.068(6) Uani 1 1 d . . .
N1D N 0.2996(9) 0.1392(9) 0.6206(4) 0.043(3) Uani 1 1 d . . .
C2D C 0.3406(12) 0.1077(10) 0.5858(5) 0.040(3) Uani 1 1 d . . .
H2D H 0.4116 0.1118 0.5804 0.049 Uiso 1 1 d R . .
N3D N 0.2735(9) 0.0670(8) 0.5571(4) 0.030(2) Uani 1 1 d . . .
C3AD C 0.1821(12) 0.0747(9) 0.5765(4) 0.033(3) Uani 1 1 d . . .
N4D N 0.0880(11) 0.0487(8) 0.5620(4) 0.038(3) Uani 1 1 d . . .
C5D C 0.0014(12) 0.0577(10) 0.5893(6) 0.040(3) Uani 1 1 d . . .
O5D O -0.0838(9) 0.0319(8) 0.5777(4) 0.056(3) Uani 1 1 d . . .
C6D C 0.0229(16) 0.1028(12) 0.6306(6) 0.052(4) Uani 1 1 d . . .
H6D H -0.0327 0.1117 0.6495 0.063 Uiso 1 1 d R . .
C7D C 0.1150(16) 0.1324(13) 0.6437(5) 0.054(5) Uani 1 1 d . . .
H7D H 0.1247 0.1610 0.6705 0.065 Uiso 1 1 d R . .
N8D N 0.1985(11) 0.1169(10) 0.6149(4) 0.044(3) Uani 1 1 d . . .
O1W O 0.657(2) 0.2174(17) 0.4478(8) 0.129(9) Uani 1 1 d . . .
O2W O 0.3438(16) 0.3923(14) 0.2915(9) 0.125(8) Uani 1 1 d . . .
O3W O 0.499(2) 0.1414(12) 0.2406(6) 0.040(5) Uiso 0.50 1 d P . .
O4W O 0.482(4) 0.518(2) 0.250(2) 0.099(13) Uiso 0.50 1 d P . .
O5W O 0.783(4) 0.084(3) 0.4668(15) 0.178(18) Uiso 0.67 1 d P . .
O6W O 0.569(5) -0.008(8) 0.488(3) 0.15(3) Uiso 0.33 1 d P . .
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
Pd1 0.0296(4) 0.0214(3) 0.0295(4) -0.0001(4) -0.0008(4) -0.0021(4)
Pd2 0.0253(5) 0.0224(5) 0.0308(6) 0.0008(5) 0.000 0.000
Pd3 0.0243(6) 0.0354(7) 0.0409(7) -0.0065(7) 0.000 0.000
N1A 0.052(8) 0.039(7) 0.048(7) -0.009(6) -0.006(7) 0.002(6)
C2A 0.037(7) 0.032(6) 0.055(8) -0.011(6) -0.011(7) 0.001(6)
N3A 0.034(6) 0.031(5) 0.025(5) -0.004(4) -0.001(4) 0.004(5)
C3AA 0.038(7) 0.023(5) 0.032(6) 0.001(5) -0.004(6) 0.004(5)
N4A 0.030(5) 0.021(5) 0.041(6) -0.005(4) 0.005(5) 0.006(4)
C5A 0.049(9) 0.027(6) 0.063(10) 0.000(6) 0.029(8) 0.010(6)
O5A 0.052(7) 0.053(7) 0.070(8) -0.016(6) -0.002(7) 0.014(6)
C6A 0.054(10) 0.052(10) 0.062(10) -0.002(9) 0.024(8) 0.022(9)
C7A 0.051(10) 0.041(8) 0.063(10) -0.007(8) 0.021(8) 0.025(8)
N8A 0.036(6) 0.037(6) 0.046(6) -0.009(6) 0.002(5) 0.010(6)
N1B 0.070(11) 0.047(8) 0.077(11) -0.025(8) 0.037(9) 0.003(8)
C2B 0.074(11) 0.035(7) 0.048(8) 0.001(7) 0.015(8) 0.018(9)
N3B 0.064(9) 0.022(5) 0.032(6) 0.001(4) 0.005(5) 0.004(5)
C3AB 0.035(7) 0.028(6) 0.032(6) -0.004(5) 0.009(5) -0.005(5)
N4B 0.068(9) 0.024(5) 0.024(5) -0.004(4) 0.005(5) -0.007(6)
C5B 0.051(9) 0.041(7) 0.034(6) 0.006(6) -0.004(7) -0.021(8)
O5B 0.055(7) 0.056(7) 0.049(6) 0.004(5) -0.009(6) -0.019(7)
C6B 0.077(13) 0.067(11) 0.033(7) -0.017(8) 0.008(8) -0.029(11)
C7B 0.090(15) 0.058(10) 0.029(7) -0.017(7) 0.020(9) -0.006(11)
N8B 0.075(10) 0.033(6) 0.041(6) -0.010(5) 0.026(7) -0.005(7)
N1C 0.16(2) 0.057(11) 0.057(10) 0.003(9) -0.027(13) 0.060(14)
C2C 0.104(17) 0.075(13) 0.048(9) -0.005(10) -0.029(11) 0.073(14)
N3C 0.083(11) 0.033(6) 0.043(7) -0.013(5) -0.027(8) 0.029(7)
C3AC 0.068(9) 0.031(6) 0.021(5) 0.000(5) -0.009(6) -0.037(7)
N4C 0.046(7) 0.025(5) 0.033(5) 0.003(4) 0.005(5) -0.006(5)
C5C 0.076(11) 0.029(7) 0.034(7) -0.003(5) 0.011(7) -0.023(8)
O5C 0.087(11) 0.066(10) 0.070(9) -0.013(8) 0.011(9) -0.028(9)
C6C 0.12(2) 0.040(10) 0.074(14) 0.014(10) 0.020(15) -0.035(13)
C7C 0.14(3) 0.036(10) 0.088(17) 0.023(10) 0.012(18) 0.007(14)
N8C 0.132(17) 0.026(6) 0.046(8) 0.015(6) -0.010(11) -0.001(10)
N1D 0.028(6) 0.054(8) 0.047(7) -0.017(6) -0.014(5) 0.003(5)
C2D 0.038(8) 0.031(6) 0.053(8) -0.003(6) -0.012(7) -0.001(6)
N3D 0.031(5) 0.029(5) 0.031(5) 0.002(4) 0.001(4) 0.004(5)
C3AD 0.043(7) 0.026(5) 0.031(6) -0.001(5) -0.014(6) 0.003(6)
N4D 0.041(6) 0.028(5) 0.045(6) 0.003(5) 0.008(6) 0.007(5)
C5D 0.033(7) 0.031(7) 0.055(8) 0.007(7) 0.011(6) 0.002(6)
O5D 0.045(6) 0.047(6) 0.076(8) 0.001(6) 0.024(6) 0.007(5)
C6D 0.055(10) 0.047(9) 0.055(10) -0.004(8) 0.017(9) 0.013(8)
C7D 0.069(12) 0.059(11) 0.033(7) -0.001(7) -0.005(8) 0.005(9)
N8D 0.047(8) 0.051(7) 0.032(6) -0.007(5) -0.005(5) 0.007(6)
O1W 0.129(19) 0.132(19) 0.127(19) -0.022(16) 0.028(16) -0.053(17)
O2W 0.088(14) 0.104(14) 0.18(2) -0.022(15) -0.046(15) -0.026(13)
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'
Pd Pd -0.9988 1.0072 '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
N3A Pd1 N3B 169.2(5) 3 3 ?
N3A Pd1 N4A 88.6(5) 3 . ?
N3B Pd1 N4A 90.0(4) 3 . ?
N3A Pd1 N4B 89.5(4) 3 . ?
N3B Pd1 N4B 90.3(5) 3 . ?
N4A Pd1 N4B 171.4(5) . . ?
N3A Pd1 Pd1 84.6(3) 3 3 ?
N3B Pd1 Pd1 84.6(4) 3 3 ?
N4A Pd1 Pd1 86.0(3) . 3 ?
N4B Pd1 Pd1 85.5(4) . 3 ?
N3D Pd2 N3D 170.2(7) . 4_556 ?
N3D Pd2 N4C 91.2(5) . 4_556 ?
N3D Pd2 N4C 87.9(5) 4_556 4_556 ?
N3D Pd2 N4C 87.9(5) . . ?
N3D Pd2 N4C 91.2(5) 4_556 . ?
N4C Pd2 N4C 169.5(7) 4_556 . ?
N3D Pd2 Pd3 85.1(3) . . ?
N3D Pd2 Pd3 85.1(3) 4_556 . ?
N4C Pd2 Pd3 84.8(4) 4_556 . ?
N4C Pd2 Pd3 84.8(4) . . ?
N4D Pd3 N4D 169.6(8) . 4_556 ?
N4D Pd3 N3C 91.9(5) . . ?
N4D Pd3 N3C 87.3(5) 4_556 . ?
N4D Pd3 N3C 87.3(5) . 4_556 ?
N4D Pd3 N3C 91.9(5) 4_556 4_556 ?
N3C Pd3 N3C 170.6(10) . 4_556 ?
N4D Pd3 Pd2 84.8(4) . . ?
N4D Pd3 Pd2 84.8(4) 4_556 . ?
N3C Pd3 Pd2 85.3(5) . . ?
N3C Pd3 Pd2 85.3(5) 4_556 . ?
C2A N1A N8A 100.1(12) . . ?
N1A C2A N3A 118.4(14) . . ?
C3AA N3A C2A 102.1(12) . . ?
C3AA N3A Pd1 121.6(9) . 3 ?
C2A N3A Pd1 136.2(10) . 3 ?
N3A C3AA N4A 129.7(13) . . ?
N3A C3AA N8A 108.9(12) . . ?
N4A C3AA N8A 121.3(12) . . ?
C5A N4A C3AA 120.2(13) . . ?
C5A N4A Pd1 122.4(11) . . ?
C3AA N4A Pd1 117.4(9) . . ?
O5A C5A N4A 121.2(14) . . ?
O5A C5A C6A 122.1(15) . . ?
N4A C5A C6A 116.5(17) . . ?
C5A O5A O2W 137.6(11) . . ?
C5A O5A O3W 119.6(10) . . ?
O2W O5A O3W 102.4(7) . . ?
C7A C6A C5A 124.2(16) . . ?
C6A C7A N8A 115.7(14) . . ?
N1A N8A C3AA 110.5(12) . . ?
N1A N8A C7A 127.6(13) . . ?
C3AA N8A C7A 121.9(14) . . ?
C2B N1B N8B 102.1(14) . . ?
N1B C2B N3B 111.8(17) . . ?
C3AB N3B C2B 105.8(12) . . ?
C3AB N3B Pd1 121.0(11) . 3 ?
C2B N3B Pd1 133.1(12) . 3 ?
N3B C3AB N8B 107.6(14) . . ?
N3B C3AB N4B 129.7(13) . . ?
N8B C3AB N4B 122.6(14) . . ?
C3AB N4B C5B 121.5(13) . . ?
C3AB N4B Pd1 118.2(9) . . ?
C5B N4B Pd1 120.2(12) . . ?
O5B C5B N4B 122.8(16) . . ?
O5B C5B C6B 123.5(15) . . ?
N4B C5B C6B 113.6(16) . . ?
C5B O5B O2W 126.4(11) . . ?
C7B C6B C5B 123.3(16) . . ?
C6B C7B N8B 117.1(17) . . ?
C3AB N8B N1B 112.7(14) . . ?
C3AB N8B C7B 121.2(18) . . ?
N1B N8B C7B 126.1(15) . . ?
C2C N1C N8C 107.8(16) . . ?
N1C C2C N3C 109(2) . . ?
C3AC N3C C2C 104.8(18) . . ?
C3AC N3C Pd3 122.0(11) . . ?
C2C N3C Pd3 133.2(17) . . ?
N3C C3AC N8C 112.4(18) . . ?
N3C C3AC N4C 127.0(12) . . ?
N8C C3AC N4C 120.5(16) . . ?
C3AC N4C C5C 122.1(13) . . ?
C3AC N4C Pd2 120.5(9) . . ?
C5C N4C Pd2 116.9(11) . . ?
O5C C5C N4C 126.6(16) . . ?
O5C C5C C6C 122.9(18) . . ?
N4C C5C C6C 110.4(19) . . ?
C5C O5C O6W 145(2) . . ?
C5C O5C O1W 134.4(14) . . ?
O6W O5C O1W 80.8(19) . . ?
C7C C6C C5C 124(2) . . ?
C6C C7C N8C 119.3(19) . . ?
C7C N8C C3AC 123(2) . . ?
C7C N8C N1C 130.9(19) . . ?
C3AC N8C N1C 106.0(19) . . ?
C2D N1D N8D 101.5(12) . . ?
N1D C2D N3D 115.7(14) . . ?
C3AD N3D C2D 103.6(12) . . ?
C3AD N3D Pd2 120.5(9) . . ?
C2D N3D Pd2 135.8(10) . . ?
N3D C3AD N4D 128.9(12) . . ?
N3D C3AD N8D 107.0(13) . . ?
N4D C3AD N8D 124.0(14) . . ?
C3AD N4D C5D 119.4(13) . . ?
C3AD N4D Pd3 119.3(10) . . ?
C5D N4D Pd3 121.3(11) . . ?
O5D C5D N4D 120.9(16) . . ?
O5D C5D C6D 124.6(15) . . ?
N4D C5D C6D 114.4(14) . . ?
C7D C6D C5D 125.7(16) . . ?
C6D C7D N8D 115.9(15) . . ?
C3AD N8D N1D 112.1(13) . . ?
C3AD N8D C7D 120.3(14) . . ?
N1D N8D C7D 127.6(13) . . ?
O5W O1W O5C 104.3(14) . . ?
O5A O2W O5B 116.5(8) . . ?
O5A O2W O4W 109.0(15) . . ?
O5B O2W O4W 127.2(12) . . ?
O3W O3W N8B 136(4) 3_655 7_545 ?
O3W O3W O5A 95(4) 3_655 . ?
N8B O3W O5A 126.6(8) 7_545 . ?
O1W O5W O5D 137.1(19) . 4_656 ?
O6W O6W O5C 91(10) 4_556 . ?
O6W O6W O5C 73(10) 4_556 4_556 ?
O5C O6W O5C 112(2) . 4_556 ?
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
Pd1 N3A 2.012(11) 3 ?
Pd1 N3B 2.037(11) 3 ?
Pd1 N4A 2.045(11) . ?
Pd1 N4B 2.062(12) . ?
Pd1 Pd1 2.7409(19) 3 ?
Pd2 N3D 2.016(11) . ?
Pd2 N3D 2.016(11) 4_556 ?
Pd2 N4C 2.059(11) 4_556 ?
Pd2 N4C 2.059(11) . ?
Pd2 Pd3 2.7441(18) . ?
Pd3 N4D 2.040(13) . ?
Pd3 N4D 2.040(13) 4_556 ?
Pd3 N3C 2.040(14) . ?
Pd3 N3C 2.040(14) 4_556 ?
N1A C2A 1.29(2) . ?
N1A N8A 1.372(19) . ?
C2A N3A 1.366(17) . ?
N3A C3AA 1.307(18) . ?
N3A Pd1 2.012(11) 3 ?
C3AA N4A 1.367(18) . ?
C3AA N8A 1.373(18) . ?
N4A C5A 1.355(19) . ?
C5A O5A 1.23(2) . ?
C5A C6A 1.45(2) . ?
O5A O2W 2.78(2) . ?
O5A O3W 2.94(3) . ?
C6A C7A 1.35(3) . ?
C7A N8A 1.383(18) . ?
N1B C2B 1.34(2) . ?
N1B N8B 1.35(3) . ?
C2B N3B 1.38(2) . ?
N3B C3AB 1.314(19) . ?
N3B Pd1 2.037(11) 3 ?
C3AB N8B 1.336(17) . ?
C3AB N4B 1.34(2) . ?
N4B C5B 1.366(19) . ?
C5B O5B 1.22(2) . ?
C5B C6B 1.47(2) . ?
O5B O2W 2.84(3) . ?
C6B C7B 1.34(3) . ?
C7B N8B 1.35(2) . ?
N1C C2C 1.31(4) . ?
N1C N8C 1.39(3) . ?
C2C N3C 1.413(19) . ?
N3C C3AC 1.31(2) . ?
C3AC N8C 1.332(19) . ?
C3AC N4C 1.37(2) . ?
N4C C5C 1.39(2) . ?
C5C O5C 1.19(2) . ?
C5C C6C 1.52(3) . ?
O5C O6W 2.78(11) . ?
O5C O1W 2.92(3) . ?
C6C C7C 1.28(4) . ?
C7C N8C 1.31(3) . ?
N1D C2D 1.28(2) . ?
N1D N8D 1.353(17) . ?
C2D N3D 1.369(18) . ?
N3D C3AD 1.322(19) . ?
C3AD N4D 1.344(19) . ?
C3AD N8D 1.348(17) . ?
N4D C5D 1.402(19) . ?
C5D O5D 1.21(2) . ?
C5D C6D 1.46(3) . ?
C6D C7D 1.32(3) . ?
C7D N8D 1.41(2) . ?
O1W O5W 2.61(6) . ?
O2W O4W 2.86(6) . ?
O3W O3W 0.58(4) 3_655 ?
O3W N8B 2.94(2) 7_545 ?
O5W O5D 2.76(5) 4_656 ?
O6W O6W 0.80(16) 4_556 ?
O6W O5C 2.90(10) 4_556 ?
|
1100170.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100170.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_1100170
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_journal_name_full Polyhedron
_journal_page_first 2373
_journal_page_last 2379
_journal_paper_doi 10.1016/j.poly.2004.07.024
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C34 H30 N14 O12 Pd2'
_chemical_formula_weight 1039.52
_chemical_name_systematic
;
Bis(4,5-dihydro-1,2,4-triazolo[1,5-a]pyrimidinate-5-one-mu-N3-N4)
bis(phenanthroline)dipalladium(II) nitrate tetrahydrate
;
_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 110.02(4)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 19.688(12)
_cell_length_b 14.219(12)
_cell_length_c 14.448(6)
_cell_measurement_reflns_used 43
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.08
_cell_measurement_theta_min 5.04
_cell_volume 3800(4)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0541
_diffrn_reflns_av_sigmaI/netI 0.0762
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 6442
_diffrn_reflns_theta_full 30.07
_diffrn_reflns_theta_max 30.07
_diffrn_reflns_theta_min 1.81
_diffrn_standards_decay_% 40.24
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.031
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.817
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 2080
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 1.733
_refine_diff_density_min -1.256
_refine_diff_density_rms 0.194
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.049
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 272
_refine_ls_number_reflns 5547
_refine_ls_number_restraints 12
_refine_ls_restrained_S_all 1.049
_refine_ls_R_factor_all 0.1484
_refine_ls_R_factor_gt 0.0793
_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^)+(0.1200P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1920
_refine_ls_wR_factor_ref 0.2325
_reflns_number_gt 2956
_reflns_number_total 5547
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100170
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
Pd Pd 0.51944(3) 0.28682(4) 0.35998(4) 0.0478(2) Uani 1 1 d . . .
N1 N 0.6725(4) 0.0714(7) 0.3822(7) 0.086(2) Uani 1 1 d . . .
C2 C 0.6451(5) 0.1433(8) 0.4165(7) 0.083(3) Uani 1 1 d . . .
H2 H 0.6591 0.1574 0.4833 0.100 Uiso 1 1 d R . .
N3 N 0.5942(3) 0.1954(5) 0.3456(5) 0.0591(17) Uani 1 1 d . . .
C3A C 0.5909(4) 0.1535(6) 0.2605(6) 0.0554(18) Uani 1 1 d . . .
N4 N 0.5498(3) 0.1772(5) 0.1682(5) 0.0558(15) Uani 1 1 d . . .
C5 C 0.5533(5) 0.1210(6) 0.0921(7) 0.064(2) Uani 1 1 d . . .
O5 O 0.5137(4) 0.1400(5) 0.0081(5) 0.092(2) Uani 1 1 d . . .
C6 C 0.6019(6) 0.0423(7) 0.1187(8) 0.081(3) Uani 1 1 d . . .
H6 H 0.6051 0.0032 0.0688 0.098 Uiso 1 1 d R . .
C7 C 0.6427(6) 0.0227(8) 0.2114(9) 0.088(3) Uani 1 1 d . . .
H7 H 0.6741 -0.0284 0.2265 0.105 Uiso 1 1 d R . .
N8 N 0.6364(4) 0.0804(5) 0.2821(6) 0.0686(19) Uani 1 1 d . . .
N1P N 0.4453(3) 0.3817(5) 0.3699(4) 0.0520(15) Uani 1 1 d . . .
C1AP C 0.4687(4) 0.4707(6) 0.3722(5) 0.0506(17) Uani 1 1 d . . .
C2P C 0.3784(4) 0.3659(7) 0.3714(5) 0.062(2) Uani 1 1 d . . .
H2P H 0.3617 0.3044 0.3695 0.074 Uiso 1 1 d R . .
C3P C 0.3334(5) 0.4416(8) 0.3759(6) 0.069(2) Uani 1 1 d . . .
H3P H 0.2876 0.4294 0.3784 0.082 Uiso 1 1 d R . .
C4P C 0.3553(5) 0.5297(8) 0.3765(6) 0.069(2) Uani 1 1 d . . .
H4P H 0.3245 0.5789 0.3777 0.083 Uiso 1 1 d R . .
C4AP C 0.4260(5) 0.5494(6) 0.3755(5) 0.064(2) Uani 1 1 d . . .
C5P C 0.4573(6) 0.6427(7) 0.3773(6) 0.076(3) Uani 1 1 d . . .
H5P H 0.4297 0.6955 0.3784 0.091 Uiso 1 1 d R . .
C6P C 0.5255(6) 0.6542(7) 0.3777(6) 0.075(3) Uani 1 1 d . . .
H6P H 0.5439 0.7145 0.3778 0.090 Uiso 1 1 d R . .
C6AP C 0.5696(5) 0.5741(6) 0.3779(5) 0.064(2) Uani 1 1 d . . .
C7P C 0.6429(6) 0.5802(8) 0.3817(6) 0.080(3) Uani 1 1 d . . .
H7P H 0.6642 0.6385 0.3812 0.096 Uiso 1 1 d R . .
C8P C 0.6808(5) 0.4998(8) 0.3862(6) 0.074(3) Uani 1 1 d . . .
H8P H 0.7292 0.5039 0.3915 0.089 Uiso 1 1 d R . .
C9P C 0.6500(4) 0.4125(7) 0.3827(6) 0.065(2) Uani 1 1 d . . .
H9P H 0.6772 0.3589 0.3834 0.078 Uiso 1 1 d R . .
N10P N 0.5804(3) 0.4039(5) 0.3786(4) 0.0512(14) Uani 1 1 d . . .
C0AP C 0.5413(4) 0.4834(6) 0.3757(4) 0.0522(18) Uani 1 1 d . . .
N1N N 0.7711(13) 0.2618(11) 0.3177(12) 0.100(5) Uiso 0.50 1 d PD . .
O1N O 0.7783(12) 0.2267(12) 0.4003(11) 0.130(7) Uiso 0.50 1 d PD . .
O2N O 0.7632(15) 0.2094(13) 0.2457(12) 0.139(5) Uiso 0.50 1 d PD . .
O3N O 0.7916(14) 0.3454(10) 0.3168(15) 0.164(7) Uiso 0.50 1 d PD . .
N1N' N 0.7836(11) 0.2659(13) 0.2589(13) 0.100(5) Uiso 0.50 1 d PD . .
O1N' O 0.8207(16) 0.308(2) 0.216(2) 0.225(14) Uiso 0.50 1 d PD . .
O2N' O 0.7394(12) 0.2051(15) 0.2126(17) 0.139(5) Uiso 0.50 1 d PD . .
O3N' O 0.7896(17) 0.2873(17) 0.3444(14) 0.164(7) Uiso 0.50 1 d PD . .
O1W O 0.5458(7) 0.0853(10) -0.1558(8) 0.181(5) Uani 1 1 d . . .
O2W O 0.8217(15) 0.325(2) 0.106(2) 0.177(9) Uiso 0.50 1 d P . .
O2W' O 0.7987(18) 0.302(2) 0.013(3) 0.211(14) Uiso 0.50 1 d P . .
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
Pd 0.0439(3) 0.0606(4) 0.0383(3) -0.0003(3) 0.0134(2) -0.0044(3)
N1 0.070(5) 0.094(6) 0.078(5) 0.011(5) 0.003(4) 0.022(5)
C2 0.057(5) 0.109(8) 0.065(5) 0.006(6) -0.003(4) 0.010(6)
N3 0.049(3) 0.075(5) 0.048(3) -0.001(3) 0.010(3) 0.004(3)
C3A 0.044(4) 0.058(5) 0.061(4) -0.001(4) 0.014(3) -0.002(3)
N4 0.051(3) 0.056(4) 0.058(4) -0.006(3) 0.016(3) 0.002(3)
C5 0.066(5) 0.060(5) 0.064(5) -0.014(4) 0.021(4) 0.005(4)
O5 0.112(5) 0.095(5) 0.060(4) -0.006(4) 0.017(4) 0.023(4)
C6 0.084(7) 0.075(6) 0.086(7) -0.013(5) 0.031(6) 0.018(5)
C7 0.075(6) 0.081(7) 0.108(8) 0.002(6) 0.033(6) 0.027(5)
N8 0.056(4) 0.065(4) 0.084(5) 0.003(4) 0.022(4) 0.013(3)
N1P 0.049(3) 0.070(4) 0.037(3) -0.004(3) 0.016(2) 0.001(3)
C1AP 0.056(4) 0.060(5) 0.032(3) 0.003(3) 0.010(3) 0.004(4)
C2P 0.055(4) 0.085(6) 0.048(4) 0.001(4) 0.020(3) -0.005(4)
C3P 0.063(5) 0.103(7) 0.042(4) 0.010(5) 0.020(4) 0.012(5)
C4P 0.073(5) 0.092(7) 0.041(4) 0.003(4) 0.018(4) 0.028(5)
C4AP 0.080(6) 0.072(6) 0.033(3) -0.001(4) 0.012(4) 0.001(5)
C5P 0.097(7) 0.079(6) 0.043(4) -0.002(4) 0.012(4) 0.016(6)
C6P 0.106(8) 0.052(5) 0.056(5) -0.001(4) 0.012(5) -0.009(5)
C6AP 0.088(6) 0.068(5) 0.037(3) 0.000(4) 0.021(4) -0.021(5)
C7P 0.095(7) 0.094(7) 0.048(4) -0.007(5) 0.020(5) -0.050(6)
C8P 0.076(6) 0.098(7) 0.056(5) -0.018(5) 0.034(4) -0.036(6)
C9P 0.054(4) 0.095(7) 0.049(4) -0.014(4) 0.021(4) -0.017(4)
N10P 0.053(3) 0.066(4) 0.036(3) -0.005(3) 0.016(2) -0.013(3)
C0AP 0.063(4) 0.069(5) 0.026(3) -0.002(3) 0.017(3) -0.005(4)
O1W 0.197(11) 0.264(15) 0.107(7) 0.013(8) 0.083(8) 0.075(11)
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'
Pd Pd -0.9988 1.0072 '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
N10P Pd N4 174.2(2) . 2_655 ?
N10P Pd N3 97.1(3) . . ?
N4 Pd N3 87.0(3) 2_655 . ?
N10P Pd N1P 81.5(3) . . ?
N4 Pd N1P 94.3(3) 2_655 . ?
N3 Pd N1P 177.6(3) . . ?
C2 N1 N8 101.0(7) . . ?
N1 C2 N3 114.9(9) . . ?
C3A N3 C2 103.6(7) . . ?
C3A N3 Pd 124.6(5) . . ?
C2 N3 Pd 129.6(6) . . ?
N8 C3A N4 123.6(8) . . ?
N8 C3A N3 108.2(7) . . ?
N4 C3A N3 128.1(7) . . ?
C3A N4 C5 117.9(7) . . ?
C3A N4 Pd 122.0(5) . 2_655 ?
C5 N4 Pd 120.1(6) . 2_655 ?
O5 C5 N4 118.1(8) . . ?
O5 C5 C6 125.2(8) . . ?
N4 C5 C6 116.6(8) . . ?
C7 C6 C5 123.2(9) . . ?
C6 C7 N8 117.0(9) . . ?
C3A N8 C7 121.6(8) . . ?
C3A N8 N1 112.3(8) . . ?
C7 N8 N1 126.1(8) . . ?
C2P N1P C1AP 119.2(7) . . ?
C2P N1P Pd 128.5(6) . . ?
C1AP N1P Pd 112.3(5) . . ?
N1P C1AP C4AP 123.0(7) . . ?
N1P C1AP C0AP 116.9(7) . . ?
C4AP C1AP C0AP 120.1(8) . . ?
N1P C2P C3P 120.5(9) . . ?
C4P C3P C2P 120.9(9) . . ?
C3P C4P C4AP 120.3(9) . . ?
C1AP C4AP C4P 116.2(8) . . ?
C1AP C4AP C5P 117.9(8) . . ?
C4P C4AP C5P 125.9(9) . . ?
C6P C5P C4AP 121.6(9) . . ?
C5P C6P C6AP 120.3(9) . . ?
C0AP C6AP C7P 116.5(9) . . ?
C0AP C6AP C6P 119.8(8) . . ?
C7P C6AP C6P 123.8(9) . . ?
C8P C7P C6AP 118.9(9) . . ?
C7P C8P C9P 122.1(9) . . ?
N10P C9P C8P 120.6(9) . . ?
C9P N10P C0AP 118.6(7) . . ?
C9P N10P Pd 128.8(6) . . ?
C0AP N10P Pd 112.1(5) . . ?
N10P C0AP C6AP 123.2(7) . . ?
N10P C0AP C1AP 116.5(7) . . ?
C6AP C0AP C1AP 120.3(8) . . ?
O2N N1N O1N 119.8(10) . . ?
O2N N1N O3N 120.3(10) . . ?
O1N N1N O3N 117.0(10) . . ?
O3N' N1N' O2N' 121.1(10) . . ?
O3N' N1N' O1N' 120.0(10) . . ?
O2N' N1N' O1N' 118.9(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
Pd N10P 2.016(6) . ?
Pd N4 2.018(7) 2_655 ?
Pd N3 2.026(7) . ?
Pd N1P 2.029(6) . ?
Pd Pd 3.0031(18) 2_655 ?
N1 C2 1.329(13) . ?
N1 N8 1.381(11) . ?
C2 N3 1.379(11) . ?
N3 C3A 1.347(10) . ?
C3A N8 1.337(10) . ?
C3A N4 1.345(10) . ?
N4 C5 1.381(10) . ?
N4 Pd 2.018(7) 2_655 ?
C5 O5 1.227(10) . ?
C5 C6 1.436(12) . ?
O5 O1W 2.764(12) . ?
C6 C7 1.334(14) . ?
C7 N8 1.349(12) . ?
N1P C2P 1.343(10) . ?
N1P C1AP 1.343(10) . ?
C1AP C4AP 1.411(11) . ?
C1AP C0AP 1.424(11) . ?
C2P C3P 1.411(12) . ?
C3P C4P 1.325(13) . ?
C4P C4AP 1.423(13) . ?
C4AP C5P 1.460(14) . ?
C5P C6P 1.351(13) . ?
C6P C6AP 1.431(13) . ?
C6AP C0AP 1.401(11) . ?
C6AP C7P 1.427(14) . ?
C7P C8P 1.356(15) . ?
C8P C9P 1.374(13) . ?
C9P N10P 1.357(9) . ?
N10P C0AP 1.361(10) . ?
N1N O2N 1.246(9) . ?
N1N O1N 1.256(9) . ?
N1N O3N 1.258(9) . ?
N1N' O3N' 1.238(9) . ?
N1N' O2N' 1.246(9) . ?
N1N' O1N' 1.258(9) . ?
O1N' O2W' 2.82(4) . ?
O1W O1W 2.70(2) 2_654 ?
O1W O2W 2.77(3) 7_655 ?
|
1100171.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100171.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_1100171
loop_
_publ_author_name
'Mohammad Abul-Haj'
'Miguel Quiros'
'Juan M. Salas'
_journal_name_full Polyhedron
_journal_page_first 2373
_journal_page_last 2379
_journal_paper_doi 10.1016/j.poly.2004.07.024
_journal_volume 23
_journal_year 2004
_chemical_formula_sum 'C22 H40 N14 O11 Pd2'
_chemical_formula_weight 889.48
_chemical_name_systematic
;
Bis(4,5-dihydro-1,2,4-triazolo[1,5-a]pyrimidinate-5-one-mu-N3,N4)
bis(trans-diaminociclohexane) dipalladium(II) nitrate tetrahydrate
;
_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 104.117(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 10.2842(15)
_cell_length_b 18.920(3)
_cell_length_c 18.450(3)
_cell_measurement_reflns_used 40
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 12.38
_cell_measurement_theta_min 4.68
_cell_volume 3481.5(9)
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type 'Siemens P4'
_diffrn_measurement_method '2\q/\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 0.0243
_diffrn_reflns_av_sigmaI/netI 0.0373
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -1
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -1
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 5841
_diffrn_reflns_theta_full 22.50
_diffrn_reflns_theta_max 22.50
_diffrn_reflns_theta_min 1.57
_diffrn_standards_decay_% 18.45
_diffrn_standards_interval_count 97
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 1.106
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_type none
_exptl_absorpt_process_details ?
_exptl_crystal_colour ?
_exptl_crystal_density_diffrn 1.697
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description ?
_exptl_crystal_F_000 1800
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.10
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 1.089
_refine_diff_density_min -0.611
_refine_diff_density_rms 0.101
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.136
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 425
_refine_ls_number_reflns 4542
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.136
_refine_ls_R_factor_all 0.0604
_refine_ls_R_factor_gt 0.0487
_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^)+(0.0450P)^2^+16.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1171
_refine_ls_wR_factor_ref 0.1238
_reflns_number_gt 3834
_reflns_number_total 4542
_reflns_threshold_expression >2sigma(I)
_cod_original_sg_symbol_H-M 'P 2(1)/c'
_cod_database_code 1100171
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
Pd1 Pd 0.49372(6) 0.60688(3) 0.21038(3) 0.03507(19) Uani 1 1 d . A .
Pd2 Pd 0.51742(6) 0.45859(3) 0.30024(3) 0.03513(19) Uani 1 1 d . A .
N1A N 0.1577(8) 0.5243(4) 0.0572(4) 0.066(2) Uani 1 1 d . . .
C2A C 0.2453(9) 0.5709(5) 0.0892(5) 0.061(2) Uani 1 1 d . . .
H2A H 0.2472 0.6163 0.0702 0.073 Uiso 1 1 d R . .
N3A N 0.3331(6) 0.5497(3) 0.1540(3) 0.0450(16) Uani 1 1 d . . .
C3AA C 0.2995(7) 0.4830(4) 0.1623(4) 0.0421(19) Uani 1 1 d . . .
N4A N 0.3526(6) 0.4360(3) 0.2154(3) 0.0415(15) Uani 1 1 d . . .
C5A C 0.2990(9) 0.3689(4) 0.2102(5) 0.052(2) Uani 1 1 d . . .
O5A O 0.3462(7) 0.3242(3) 0.2597(4) 0.0664(17) Uani 1 1 d . . .
C6A C 0.1854(10) 0.3548(5) 0.1490(5) 0.069(3) Uani 1 1 d . . .
H6A H 0.1470 0.3101 0.1445 0.082 Uiso 1 1 d R . .
C7A C 0.1333(10) 0.4033(5) 0.0980(5) 0.067(3) Uani 1 1 d . . .
H7A H 0.0586 0.3937 0.0593 0.080 Uiso 1 1 d R . .
N8A N 0.1927(7) 0.4676(4) 0.1050(4) 0.0533(18) Uani 1 1 d . . .
N1B N 0.3199(8) 0.5528(4) 0.4496(4) 0.0586(19) Uani 1 1 d . . .
C2B C 0.3704(8) 0.5012(4) 0.4181(4) 0.050(2) Uani 1 1 d . . .
H2B H 0.3792 0.4555 0.4372 0.060 Uiso 1 1 d R . .
N3B N 0.4099(6) 0.5200(3) 0.3547(3) 0.0411(15) Uani 1 1 d . . .
C3AB C 0.3835(7) 0.5884(4) 0.3463(4) 0.0376(17) Uani 1 1 d . . .
N4B N 0.4029(6) 0.6339(3) 0.2939(3) 0.0376(14) Uani 1 1 d . . .
C5B C 0.3666(8) 0.7031(4) 0.2988(5) 0.049(2) Uani 1 1 d . . .
O5B O 0.3822(7) 0.7457(3) 0.2504(3) 0.0673(18) Uani 1 1 d . B .
C6B C 0.3103(10) 0.7236(4) 0.3611(5) 0.061(3) Uani 1 1 d . . .
H6B H 0.2855 0.7704 0.3653 0.073 Uiso 1 1 d R . .
C7B C 0.2904(10) 0.6775(5) 0.4109(5) 0.062(2) Uani 1 1 d . . .
H7B H 0.2546 0.6908 0.4505 0.074 Uiso 1 1 d R . .
N8B N 0.3268(7) 0.6093(3) 0.4029(3) 0.0483(17) Uani 1 1 d . . .
C1P C 0.7766(18) 0.6391(10) 0.2251(10) 0.051(3) Uiso 0.50 1 d P A 1
H1P H 0.8021 0.5918 0.2414 0.062 Uiso 0.50 1 d PR A 1
C1P' C 0.7520(18) 0.6597(10) 0.2053(10) 0.051(3) Uiso 0.50 1 d P A 2
H1P' H 0.7177 0.6971 0.1708 0.062 Uiso 0.50 1 d PR A 2
N1P N 0.6602(6) 0.6653(3) 0.2550(3) 0.0427(15) Uani 1 1 d . . .
H11P H 0.6814 0.6611 0.3051 0.051 Uiso 0.50 1 d PR A 1
H12P H 0.6445 0.7112 0.2432 0.051 Uiso 0.50 1 d PR A 1
H13P H 0.7021 0.6479 0.3000 0.051 Uiso 0.50 1 d PR A 2
H14P H 0.6373 0.7105 0.2608 0.051 Uiso 0.50 1 d PR A 2
C2P C 0.8928(9) 0.6876(6) 0.2377(6) 0.070(3) Uani 1 1 d . . .
H21P H 0.9289 0.6920 0.2907 0.084 Uiso 0.50 1 d PR A 1
H22P H 0.8642 0.7337 0.2183 0.084 Uiso 0.50 1 d PR A 1
H23P H 0.9330 0.6596 0.2808 0.084 Uiso 0.50 1 d PR A 2
H24P H 0.8922 0.7361 0.2529 0.084 Uiso 0.50 1 d PR A 2
C3P C 0.999(2) 0.6607(12) 0.2034(11) 0.067(4) Uiso 0.50 1 d P A 1
H31P H 1.0244 0.6131 0.2186 0.081 Uiso 0.50 1 d PR A 1
H32P H 1.0774 0.6903 0.2161 0.081 Uiso 0.50 1 d PR A 1
C4P C 0.926(2) 0.6650(13) 0.1083(12) 0.077(4) Uiso 0.50 1 d P A 1
H41P H 0.9894 0.6541 0.0795 0.092 Uiso 0.50 1 d PR A 1
H42P H 0.8898 0.7113 0.0947 0.092 Uiso 0.50 1 d PR A 1
C3P' C 0.977(2) 0.6782(12) 0.1758(12) 0.067(4) Uiso 0.50 1 d P A 2
H33P H 1.0707 0.6828 0.1994 0.081 Uiso 0.50 1 d PR A 2
H34P H 0.9531 0.7166 0.1411 0.081 Uiso 0.50 1 d PR A 2
C4P' C 0.957(2) 0.6192(12) 0.1349(12) 0.077(4) Uiso 0.50 1 d P A 2
H43P H 0.9842 0.5802 0.1685 0.092 Uiso 0.50 1 d PR A 2
H44P H 1.0107 0.6189 0.0992 0.092 Uiso 0.50 1 d PR A 2
C5P C 0.8095(10) 0.6072(7) 0.0955(6) 0.086(3) Uani 1 1 d . . .
H51P H 0.8416 0.5625 0.1173 0.103 Uiso 0.50 1 d PR A 1
H52P H 0.7698 0.6009 0.0432 0.103 Uiso 0.50 1 d PR A 1
H53P H 0.7965 0.5656 0.0649 0.103 Uiso 0.50 1 d PR A 2
H54P H 0.7791 0.6475 0.0643 0.103 Uiso 0.50 1 d PR A 2
C6P C 0.7056(16) 0.6416(10) 0.1364(9) 0.048(3) Uiso 0.50 1 d P A 1
H6P H 0.6757 0.6879 0.1185 0.057 Uiso 0.50 1 d PR A 1
C6P' C 0.7292(16) 0.6034(10) 0.1558(9) 0.048(3) Uiso 0.50 1 d P A 2
H6P' H 0.7665 0.5637 0.1862 0.057 Uiso 0.50 1 d PR A 2
N6P N 0.5900(6) 0.5874(4) 0.1292(3) 0.0475(16) Uani 1 1 d . . .
H61P H 0.5324 0.5913 0.0841 0.057 Uiso 0.50 1 d PR A 1
H62P H 0.6237 0.5433 0.1340 0.057 Uiso 0.50 1 d PR A 1
H63P H 0.5560 0.6151 0.0894 0.057 Uiso 0.50 1 d PR A 2
H64P H 0.5778 0.5420 0.1147 0.057 Uiso 0.50 1 d PR A 2
C1Q C 0.7855(16) 0.4225(9) 0.2869(9) 0.042(3) Uiso 0.50 1 d P A 1
H1Q H 0.7989 0.4694 0.2703 0.051 Uiso 0.50 1 d PR A 1
C1Q' C 0.7739(15) 0.3955(9) 0.3083(9) 0.042(3) Uiso 0.50 1 d P A 2
H1Q' H 0.7681 0.3589 0.3434 0.051 Uiso 0.50 1 d PR A 2
N1Q N 0.6410(6) 0.3996(3) 0.2541(3) 0.0402(15) Uani 1 1 d . . .
H11Q H 0.6200 0.4057 0.2042 0.048 Uiso 0.50 1 d PR A 1
H12Q H 0.6316 0.3535 0.2637 0.048 Uiso 0.50 1 d PR A 1
H13Q H 0.6512 0.4202 0.2118 0.048 Uiso 0.50 1 d PR A 2
H14Q H 0.6062 0.3562 0.2427 0.048 Uiso 0.50 1 d PR A 2
C2Q C 0.8878(9) 0.3742(6) 0.2704(5) 0.065(3) Uani 1 1 d . . .
H21Q H 0.8794 0.3728 0.2175 0.078 Uiso 0.50 1 d PR A 1
H22Q H 0.8751 0.3273 0.2872 0.078 Uiso 0.50 1 d PR A 1
H23Q H 0.8918 0.4085 0.2326 0.078 Uiso 0.50 1 d PR A 2
H24Q H 0.8697 0.3288 0.2470 0.078 Uiso 0.50 1 d PR A 2
C3Q C 1.028(2) 0.4018(12) 0.3106(11) 0.065(4) Uiso 0.50 1 d P A 1
H31Q H 1.0375 0.4502 0.2972 0.079 Uiso 0.50 1 d PR A 1
H32Q H 1.0962 0.3744 0.2965 0.079 Uiso 0.50 1 d PR A 1
C4Q C 1.040(2) 0.3947(13) 0.3965(12) 0.081(5) Uiso 0.50 1 d P A 1
H41Q H 1.1291 0.4059 0.4243 0.097 Uiso 0.50 1 d PR A 1
H42Q H 1.0175 0.3479 0.4095 0.097 Uiso 0.50 1 d PR A 1
C3Q' C 1.025(2) 0.3734(11) 0.3301(12) 0.065(4) Uiso 0.50 1 d P A 2
H33Q H 1.0972 0.3654 0.3065 0.079 Uiso 0.50 1 d PR A 2
H34Q H 1.0244 0.3354 0.3646 0.079 Uiso 0.50 1 d PR A 2
C4Q' C 1.046(2) 0.4389(13) 0.3739(13) 0.081(5) Uiso 0.50 1 d P A 2
H43Q H 1.0444 0.4771 0.3394 0.097 Uiso 0.50 1 d PR A 2
H44Q H 1.1308 0.4391 0.4097 0.097 Uiso 0.50 1 d PR A 2
C5Q C 0.9322(10) 0.4531(6) 0.4123(6) 0.083(3) Uani 1 1 d . . .
H51Q H 0.9461 0.4987 0.3924 0.099 Uiso 0.50 1 d PR A 1
H52Q H 0.9391 0.4576 0.4649 0.099 Uiso 0.50 1 d PR A 1
H53Q H 0.9494 0.4932 0.4451 0.099 Uiso 0.50 1 d PR A 2
H54Q H 0.9247 0.4119 0.4413 0.099 Uiso 0.50 1 d PR A 2
C6Q C 0.7949(16) 0.4234(10) 0.3723(9) 0.046(3) Uiso 0.50 1 d P A 1
H6Q H 0.7814 0.3772 0.3905 0.056 Uiso 0.50 1 d PR A 1
C6Q' C 0.8006(16) 0.4627(10) 0.3522(9) 0.046(3) Uiso 0.50 1 d P A 2
H6Q' H 0.8102 0.5008 0.3194 0.056 Uiso 0.50 1 d PR A 2
N6Q N 0.6851(6) 0.4749(3) 0.3825(3) 0.0460(16) Uani 1 1 d . . .
H61Q H 0.6671 0.4682 0.4273 0.055 Uiso 0.50 1 d PR A 1
H62Q H 0.7138 0.5197 0.3804 0.055 Uiso 0.50 1 d PR A 1
H63Q H 0.6878 0.4445 0.4203 0.055 Uiso 0.50 1 d PR A 2
H64Q H 0.6856 0.5192 0.4003 0.055 Uiso 0.50 1 d PR A 2
N1N N 0.7303(13) 0.6560(6) 0.4536(6) 0.103(3) Uani 1 1 d . . .
O1N O 0.6363(11) 0.6199(5) 0.4564(6) 0.131(4) Uani 1 1 d . A .
O2N O 0.8004(13) 0.6382(8) 0.4125(5) 0.166(6) Uani 1 1 d . A .
O3N O 0.7560(19) 0.7058(8) 0.4969(10) 0.244(9) Uani 1 1 d . A .
N2N N 0.5770(13) 0.4102(6) 0.0616(5) 0.087(3) Uani 1 1 d . . .
O4N O 0.6742(11) 0.4301(6) 0.1078(5) 0.123(3) Uani 1 1 d . A .
O5N O 0.4692(13) 0.4404(7) 0.0596(7) 0.162(5) Uani 1 1 d . A .
O6N O 0.5777(10) 0.3633(4) 0.0142(4) 0.103(3) Uani 1 1 d . A .
O1W O 0.4796(10) 0.3248(5) 0.4133(5) 0.118(3) Uani 1 1 d . . .
O2W O 0.2946(9) 0.7439(4) 0.0933(5) 0.106(3) Uani 1 1 d . . .
O3W O 0.0487(19) 0.7433(11) -0.0271(10) 0.158(6) Uiso 0.682(15) 1 d P B 1
O3W' O 0.127(4) 0.687(2) -0.039(2) 0.158(6) Uiso 0.318(15) 1 d P B 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
Pd1 0.0427(3) 0.0328(3) 0.0330(3) -0.0024(2) 0.0155(2) -0.0014(3)
Pd2 0.0466(4) 0.0277(3) 0.0339(3) -0.0035(2) 0.0152(3) -0.0019(3)
N1A 0.059(5) 0.066(5) 0.063(5) 0.007(4) -0.007(4) -0.010(4)
C2A 0.054(5) 0.056(6) 0.064(6) 0.009(5) -0.001(5) 0.000(5)
N3A 0.051(4) 0.041(4) 0.044(4) -0.004(3) 0.014(3) -0.009(3)
C3AA 0.040(4) 0.050(5) 0.040(4) -0.009(4) 0.017(4) -0.003(4)
N4A 0.046(4) 0.041(4) 0.040(4) -0.009(3) 0.016(3) -0.003(3)
C5A 0.059(5) 0.041(5) 0.061(5) -0.009(4) 0.022(5) -0.009(4)
O5A 0.084(5) 0.043(3) 0.067(4) 0.004(3) 0.010(3) -0.013(3)
C6A 0.074(6) 0.064(6) 0.071(6) -0.015(5) 0.021(5) -0.038(5)
C7A 0.064(6) 0.080(7) 0.052(5) 0.000(5) 0.005(5) -0.025(6)
N8A 0.051(4) 0.053(4) 0.054(4) -0.004(4) 0.010(3) -0.013(4)
N1B 0.084(5) 0.056(4) 0.049(4) 0.005(4) 0.042(4) 0.001(4)
C2B 0.065(5) 0.045(5) 0.050(5) 0.003(4) 0.032(4) -0.001(4)
N3B 0.056(4) 0.033(4) 0.041(3) -0.001(3) 0.025(3) 0.002(3)
C3AB 0.041(4) 0.037(4) 0.038(4) -0.005(3) 0.017(3) -0.003(3)
N4B 0.045(4) 0.030(3) 0.042(3) -0.002(3) 0.018(3) 0.001(3)
C5B 0.057(5) 0.038(5) 0.056(5) -0.004(4) 0.021(4) 0.006(4)
O5B 0.112(5) 0.035(3) 0.069(4) 0.012(3) 0.047(4) 0.009(3)
C6B 0.093(7) 0.041(5) 0.062(6) -0.002(4) 0.044(5) 0.019(5)
C7B 0.086(7) 0.058(6) 0.054(5) -0.007(5) 0.040(5) 0.020(5)
N8B 0.069(4) 0.046(4) 0.039(4) 0.000(3) 0.031(3) 0.005(3)
N1P 0.050(4) 0.035(4) 0.045(4) -0.007(3) 0.016(3) -0.005(3)
C2P 0.054(5) 0.069(6) 0.095(7) -0.020(6) 0.033(5) -0.010(5)
C5P 0.069(7) 0.119(9) 0.088(7) -0.037(7) 0.051(6) -0.014(7)
N6P 0.055(4) 0.055(4) 0.036(3) -0.006(3) 0.019(3) -0.004(3)
N1Q 0.053(4) 0.032(3) 0.039(3) -0.010(3) 0.018(3) 0.002(3)
C2Q 0.056(5) 0.079(7) 0.062(6) -0.012(5) 0.016(5) 0.008(5)
C5Q 0.063(6) 0.113(9) 0.063(6) -0.039(6) -0.001(5) 0.000(6)
N6Q 0.059(4) 0.048(4) 0.033(3) -0.011(3) 0.015(3) -0.002(3)
N1N 0.124(9) 0.093(8) 0.081(7) 0.012(6) 0.007(7) -0.036(8)
O1N 0.122(8) 0.096(7) 0.162(10) 0.006(6) 0.010(7) -0.022(6)
O2N 0.194(12) 0.240(15) 0.076(6) 0.045(8) 0.056(7) 0.072(11)
O3N 0.271(19) 0.153(12) 0.274(19) -0.101(13) 0.001(15) -0.081(12)
N2N 0.116(9) 0.099(8) 0.054(5) 0.004(5) 0.034(6) 0.001(7)
O4N 0.142(8) 0.162(9) 0.054(5) 0.015(5) 0.002(5) -0.036(7)
O5N 0.151(10) 0.179(11) 0.177(11) -0.069(9) 0.080(9) 0.009(9)
O6N 0.166(8) 0.077(5) 0.072(5) -0.007(4) 0.038(5) 0.032(5)
O1W 0.146(8) 0.107(7) 0.094(6) 0.010(5) 0.015(6) 0.020(6)
O2W 0.141(7) 0.088(5) 0.089(6) -0.012(5) 0.030(5) -0.005(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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
N6P Pd1 N1P 83.2(2) . . ?
N6P Pd1 N3A 90.5(3) . . ?
N1P Pd1 N3A 173.2(2) . . ?
N6P Pd1 N4B 175.7(2) . . ?
N1P Pd1 N4B 93.1(2) . . ?
N3A Pd1 N4B 93.1(2) . . ?
N6P Pd1 Pd2 103.4(2) . . ?
N1P Pd1 Pd2 108.22(18) . . ?
N3A Pd1 Pd2 75.60(18) . . ?
N4B Pd1 Pd2 79.76(16) . . ?
N6Q Pd2 N1Q 83.8(2) . . ?
N6Q Pd2 N3B 90.5(2) . . ?
N1Q Pd2 N3B 174.3(3) . . ?
N6Q Pd2 N4A 176.3(2) . . ?
N1Q Pd2 N4A 92.9(2) . . ?
N3B Pd2 N4A 92.8(2) . . ?
N6Q Pd2 Pd1 101.26(19) . . ?
N1Q Pd2 Pd1 103.80(17) . . ?
N3B Pd2 Pd1 77.01(17) . . ?
N4A Pd2 Pd1 81.07(18) . . ?
C2A N1A N8A 101.1(7) . . ?
N1A C2A N3A 115.8(8) . . ?
C3AA N3A C2A 104.2(7) . . ?
C3AA N3A Pd1 130.4(5) . . ?
C2A N3A Pd1 124.7(6) . . ?
N3A C3AA N4A 130.2(7) . . ?
N3A C3AA N8A 107.3(7) . . ?
N4A C3AA N8A 122.4(7) . . ?
C3AA N4A C5A 118.4(7) . . ?
C3AA N4A Pd2 122.3(5) . . ?
C5A N4A Pd2 119.2(6) . . ?
O5A C5A N4A 119.6(8) . . ?
O5A C5A C6A 122.9(8) . . ?
N4A C5A C6A 117.4(8) . . ?
C7A C6A C5A 122.5(9) . . ?
C6A C7A N8A 117.2(8) . . ?
C7A N8A C3AA 121.9(8) . . ?
C7A N8A N1A 126.6(7) . . ?
C3AA N8A N1A 111.5(7) . . ?
C2B N1B N8B 102.3(6) . . ?
N1B C2B N3B 114.7(7) . . ?
C3AB N3B C2B 104.9(6) . . ?
C3AB N3B Pd2 128.5(5) . . ?
C2B N3B Pd2 125.6(5) . . ?
N3B C3AB N4B 130.3(6) . . ?
N3B C3AB N8B 107.9(6) . . ?
N4B C3AB N8B 121.9(7) . . ?
C3AB N4B C5B 118.2(6) . . ?
C3AB N4B Pd1 123.8(5) . . ?
C5B N4B Pd1 117.9(5) . . ?
O5B C5B N4B 119.2(7) . . ?
O5B C5B C6B 122.7(7) . . ?
N4B C5B C6B 118.2(7) . . ?
C7B C6B C5B 122.2(8) . . ?
C6B C7B N8B 117.2(7) . . ?
C7B N8B C3AB 122.3(7) . . ?
C7B N8B N1B 127.3(6) . . ?
C3AB N8B N1B 110.3(6) . . ?
C2P C1P N1P 114.7(13) . . ?
C2P C1P C6P 106.7(14) . . ?
N1P C1P C6P 99.0(12) . . ?
C6P' C1P' N1P 115.8(14) . . ?
C6P' C1P' C2P 121.3(15) . . ?
N1P C1P' C2P 115.1(13) . . ?
C1P' N1P Pd1 108.3(8) . . ?
C1P N1P Pd1 109.6(8) . . ?
C1P C2P C3P 111.8(13) . . ?
C1P' C2P C3P' 108.0(12) . . ?
C2P C3P C4P 103.4(15) . . ?
C5P C4P C3P 104.1(15) . . ?
C4P' C3P' C2P 117.4(18) . . ?
C3P' C4P' C5P 113.0(19) . . ?
C4P' C5P C6P' 107.9(12) . . ?
C6P C5P C4P 102.5(12) . . ?
N6P C6P C5P 106.2(11) . . ?
N6P C6P C1P 102.3(12) . . ?
C5P C6P C1P 106.1(13) . . ?
C1P' C6P' N6P 112.5(14) . . ?
C1P' C6P' C5P 113.9(14) . . ?
N6P C6P' C5P 115.6(11) . . ?
C6P' N6P Pd1 109.8(7) . . ?
C6P N6P Pd1 108.7(7) . . ?
C2Q C1Q N1Q 114.5(11) . . ?
C2Q C1Q C6Q 110.1(13) . . ?
N1Q C1Q C6Q 102.7(12) . . ?
N1Q C1Q' C6Q' 109.8(12) . . ?
N1Q C1Q' C2Q 112.3(11) . . ?
C6Q' C1Q' C2Q 113.8(13) . . ?
C1Q' N1Q Pd2 108.2(7) . . ?
C1Q N1Q Pd2 109.1(7) . . ?
C1Q C2Q C3Q 108.6(12) . . ?
C1Q' C2Q C3Q' 109.6(11) . . ?
C2Q C3Q C4Q 106.9(15) . . ?
C3Q C4Q C5Q 103.4(16) . . ?
C4Q' C3Q' C2Q 111.3(16) . . ?
C3Q' C4Q' C5Q 112.3(18) . . ?
C4Q' C5Q C6Q' 108.8(12) . . ?
C6Q C5Q C4Q 104.5(12) . . ?
C5Q C6Q N6Q 109.1(11) . . ?
C5Q C6Q C1Q 108.3(13) . . ?
N6Q C6Q C1Q 105.3(12) . . ?
N6Q C6Q' C1Q' 106.5(13) . . ?
N6Q C6Q' C5Q 113.6(11) . . ?
C1Q' C6Q' C5Q 107.7(13) . . ?
C6Q' N6Q Pd2 108.4(7) . . ?
C6Q N6Q Pd2 109.2(7) . . ?
O1N N1N O2N 118.5(14) . . ?
O1N N1N O3N 117.5(16) . . ?
O2N N1N O3N 123.8(16) . . ?
O4N N2N O5N 117.4(12) . . ?
O4N N2N O6N 124.9(13) . . ?
O5N N2N O6N 117.7(12) . . ?
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
Pd1 N6P 2.019(6) . ?
Pd1 N1P 2.035(6) . ?
Pd1 N3A 2.036(6) . ?
Pd1 N4B 2.052(6) . ?
Pd1 Pd2 3.2378(9) . ?
Pd2 N6Q 2.024(6) . ?
Pd2 N1Q 2.029(6) . ?
Pd2 N3B 2.031(6) . ?
Pd2 N4A 2.052(6) . ?
N1A C2A 1.296(11) . ?
N1A N8A 1.381(10) . ?
C2A N3A 1.370(10) . ?
N3A C3AA 1.327(10) . ?
C3AA N4A 1.336(10) . ?
C3AA N8A 1.357(10) . ?
N4A C5A 1.377(10) . ?
C5A O5A 1.253(10) . ?
C5A C6A 1.437(13) . ?
C6A C7A 1.329(13) . ?
C7A N8A 1.353(11) . ?
N1B C2B 1.308(10) . ?
N1B N8B 1.386(9) . ?
C2B N3B 1.375(9) . ?
N3B C3AB 1.323(9) . ?
C3AB N4B 1.345(9) . ?
C3AB N8B 1.372(9) . ?
N4B C5B 1.372(10) . ?
C5B O5B 1.242(10) . ?
C5B C6B 1.460(11) . ?
C6B C7B 1.317(12) . ?
C7B N8B 1.362(10) . ?
C1P C2P 1.48(2) . ?
C1P N1P 1.518(19) . ?
C1P C6P 1.62(2) . ?
C1P' C6P' 1.39(2) . ?
C1P' N1P 1.471(19) . ?
C1P' C2P 1.52(2) . ?
C2P C3P 1.48(2) . ?
C2P C3P' 1.60(2) . ?
C3P C4P 1.74(3) . ?
C4P C5P 1.59(2) . ?
C3P' C4P' 1.34(3) . ?
C4P' C5P 1.53(2) . ?
C5P C6P' 1.539(18) . ?
C5P C6P 1.589(18) . ?
C6P N6P 1.551(18) . ?
C6P' N6P 1.428(17) . ?
C1Q C2Q 1.480(18) . ?
C1Q N1Q 1.524(17) . ?
C1Q C6Q 1.55(2) . ?
C1Q' N1Q 1.485(16) . ?
C1Q' C6Q' 1.50(2) . ?
C1Q' C2Q 1.557(18) . ?
C2Q C3Q 1.54(2) . ?
C2Q C3Q' 1.56(2) . ?
C3Q C4Q 1.57(3) . ?
C4Q C5Q 1.64(2) . ?
C3Q' C4Q' 1.47(3) . ?
C4Q' C5Q 1.53(2) . ?
C5Q C6Q 1.531(18) . ?
C5Q C6Q' 1.537(18) . ?
C6Q N6Q 1.537(17) . ?
C6Q' N6Q 1.450(17) . ?
N1N O1N 1.195(13) . ?
N1N O2N 1.215(14) . ?
N1N O3N 1.221(15) . ?
N2N O4N 1.204(12) . ?
N2N O5N 1.239(14) . ?
N2N O6N 1.249(12) . ?
O5A O1W 2.832(11) . ?
O5B O2W 2.817(10) . ?
N1P O2N 2.956(11) . ?
N1P O5A 3.019(8) 2_655 ?
N6P O6N 2.936(10) 3_665 ?
N6P O4N 3.153(13) . ?
N1Q O4N 2.860(10) . ?
N1Q O5B 2.921(8) 2_645 ?
N6Q N1B 3.155(9) 3_666 ?
O1W O2W 2.809(13) 2_645 ?
O2W O3W' 2.84(4) . ?
O2W O3W 2.93(2) . ?
|
1100172.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100172.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_1100172
loop_
_publ_author_name
'Bouchouit, Karim'
'Bendheif, Leulmi'
'Benali-Cherif, Nouredine'
_publ_section_title
;
D-Phenylglycinium nitrate
;
_journal_name_full 'Acta Crystallographica, Section E'
_journal_page_first o272
_journal_page_last o274
_journal_paper_doi 10.1107/S1600536804000972
_journal_volume 60
_journal_year 2004
_chemical_formula_iupac 'C8 H10 N O2 + , N O3 -'
_chemical_formula_moiety 'C8 H10 N O2 + , N O3 -'
_chemical_formula_structural 'C8 H10 N2 O5'
_chemical_formula_sum 'C8 H10 N2 O5'
_chemical_formula_weight 214.18
_chemical_name_common 'D-Phynylglycinium nitrate'
_chemical_name_systematic
;
D-Phenylglycinium nitrate
;
_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
_cell_angle_beta 94.943(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.4320(3)
_cell_length_b 5.6450(2)
_cell_length_c 16.7830(2)
_cell_measurement_reflns_used 3980
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 26.30
_cell_measurement_theta_min 1.96
_cell_volume 984.65(5)
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device 'Nonius KappaCCD area-detector'
_diffrn_measurement_method \f
_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 0.0686
_diffrn_reflns_av_sigmaI/netI 0.0929
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 6
_diffrn_reflns_limit_k_min -6
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 7185
_diffrn_reflns_theta_full 26.30
_diffrn_reflns_theta_max 26.30
_diffrn_reflns_theta_min 1.96
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.122
_exptl_absorpt_correction_type none
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.445
_exptl_crystal_density_meas ?
_exptl_crystal_density_method .
_exptl_crystal_description prism
_exptl_crystal_F_000 448
_exptl_crystal_size_max 0.25
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.15
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
_refine_diff_density_max 0.246
_refine_diff_density_min -0.274
_refine_ls_extinction_coef ?
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.158
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 328
_refine_ls_number_reflns 3752
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.158
_refine_ls_R_factor_all 0.0858
_refine_ls_R_factor_gt 0.0563
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0724P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1160
_refine_ls_wR_factor_ref 0.1381
_reflns_number_gt 2831
_reflns_number_total 3752
_reflns_threshold_expression I>2\s(I)
_cod_original_sg_symbol_H-M 'P 21'
_cod_database_code 1100172
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
C1A 0.1469(4) 0.4257(8) 0.4835(2) 0.0249(9) Uani d . 1 . . C
C1B 0.1415(4) 0.7185(7) -0.0142(2) 0.0263(10) Uani d . 1 . . C
C2A 0.1714(4) 0.2955(8) 0.5622(2) 0.0245(9) Uani d . 1 . . C
H2 0.1462 0.1248 0.5531 0.014(9) Uiso d R 1 . . H
C2B 0.1869(3) 0.5997(7) 0.0639(2) 0.0213(9) Uani d . 1 . . C
H22 0.1759 0.4347 0.0539 0.032(12) Uiso d R 1 . . H
C3A 0.3143(4) 0.2959(8) 0.5912(3) 0.0285(10) Uani d . 1 . . C
C3B 0.3260(4) 0.6582(8) 0.0902(2) 0.0251(9) Uani d . 1 . . C
C4A 0.3722(5) 0.4762(9) 0.6352(3) 0.0482(14) Uani d . 1 . . C
H4 0.3345 0.6174 0.6443 0.048(14) Uiso d R 1 . . H
C4B 0.3981(4) 0.4990(10) 0.1380(3) 0.0455(13) Uani d . 1 . . C
H44 0.3606 0.3541 0.1508 0.032(12) Uiso d R 1 . . H
C5A 0.5039(5) 0.4687(13) 0.6568(4) 0.0649(18) Uani d . 1 . . C
H5 0.5389 0.6080 0.6802 0.061(17) Uiso d R 1 . . H
C5B 0.5256(5) 0.5495(12) 0.1627(4) 0.0654(19) Uani d . 1 . . C
H55 0.5668 0.4342 0.1966 0.069(18) Uiso d R 1 . . H
C6A 0.5762(5) 0.2815(14) 0.6332(4) 0.0659(17) Uani d . 1 . . C
H6 0.6636 0.2574 0.6490 0.13(3) Uiso d R 1 . . H
C6B 0.5817(5) 0.7518(12) 0.1387(4) 0.0565(15) Uani d . 1 . . C
H66 0.6694 0.7846 0.1531 0.070(18) Uiso d R 1 . . H
C7A 0.5185(5) 0.1051(12) 0.5888(4) 0.0664(18) Uani d . 1 . . C
H7 0.5581 -0.0329 0.5690 0.059(17) Uiso d R 1 . . H
C7B 0.5107(5) 0.9092(12) 0.0901(4) 0.0589(16) Uani d . 1 . . C
H77 0.5451 1.0546 0.0721 0.071(19) Uiso d R 1 . . H
C8A 0.3882(5) 0.1093(10) 0.5671(3) 0.0500(14) Uani d . 1 . . C
H8 0.3462 -0.0228 0.5437 0.049(15) Uiso d R 1 . . H
C8B 0.3828(4) 0.8655(9) 0.0671(3) 0.0432(13) Uani d . 1 . . C
H88 0.3309 0.9665 0.0323 0.046(14) Uiso d R 1 . . H
N1A 0.0896(3) 0.3989(7) 0.6226(2) 0.0291(9) Uani d . 1 . . N
H10 -0.0042 0.3649 0.6087 0.050(15) Uiso d R 1 . . H
H11 0.1036 0.5605 0.6336 0.053(17) Uiso d R 1 . . H
H12 0.1105 0.3164 0.6637 0.07(2) Uiso d R 1 . . H
N1B 0.0990(3) 0.6691(6) 0.12531(19) 0.0245(8) Uani d . 1 . . N
H100 0.0989 0.8453 0.1335 0.018(11) Uiso d R 1 . . H
H110 0.0160 0.6233 0.1050 0.034(12) Uiso d R 1 . . H
H120 0.1270 0.5971 0.1791 0.08(2) Uiso d R 1 . . H
N2A 0.8659(3) 0.3989(6) 0.2635(2) 0.0284(8) Uani d . 1 . . N
N2B 0.1387(3) 0.1677(6) 0.2384(2) 0.0277(8) Uani d . 1 . . N
O1A 0.1060(3) 0.6267(6) 0.47733(18) 0.0381(8) Uani d . 1 . . O
O1B 0.0802(3) 0.9000(6) -0.01840(17) 0.0342(8) Uani d . 1 . . O
O2A 0.1759(3) 0.2876(7) 0.42532(18) 0.0449(9) Uani d . 1 . . O
H 0.1607 0.3380 0.3724 0.039(14) Uiso d R 1 . . H
O2B 0.1820(3) 0.6028(6) -0.07435(19) 0.0474(10) Uani d . 1 . . O
H' 0.1647 0.6729 -0.1198 0.055(16) Uiso d R 1 . . H
O3A 0.8728(3) 0.5946(6) 0.2296(2) 0.0452(9) Uani d . 1 . . O
O3B 0.1315(3) -0.0109(6) 0.2801(2) 0.0428(9) Uani d . 1 . . O
O4A 0.8454(4) 0.2135(6) 0.22480(19) 0.0492(10) Uani d . 1 . . O
O4B 0.1270(4) 0.1552(6) 0.16386(17) 0.0424(9) Uani d . 1 . . O
O5A 0.8820(3) 0.3867(6) 0.33787(19) 0.0438(9) Uani d . 1 . . O
O5B 0.1552(3) 0.3716(5) 0.2692(2) 0.0368(8) Uani d . 1 . . O
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1A 0.020(2) 0.032(2) 0.023(2) -0.0022(17) 0.0011(17) 0.0021(17)
C1B 0.023(2) 0.032(2) 0.024(2) 0.0016(17) 0.0000(17) 0.0002(17)
C2A 0.023(2) 0.030(2) 0.020(2) -0.0011(17) 0.0021(17) -0.0019(17)
C2B 0.021(2) 0.024(2) 0.018(2) 0.0022(16) 0.0007(16) 0.0021(15)
C3A 0.032(2) 0.032(2) 0.021(2) 0.0014(18) 0.0028(19) 0.0072(18)
C3B 0.022(2) 0.034(2) 0.019(2) 0.0014(17) 0.0002(16) 0.0013(18)
C4A 0.039(3) 0.044(3) 0.060(4) 0.006(2) -0.008(2) -0.019(3)
C4B 0.030(3) 0.052(3) 0.052(3) -0.001(2) -0.005(2) 0.023(3)
C5A 0.047(4) 0.074(5) 0.071(5) -0.011(3) -0.013(3) -0.013(4)
C5B 0.032(3) 0.082(4) 0.078(5) -0.002(3) -0.020(3) 0.039(4)
C6A 0.032(3) 0.084(4) 0.080(5) 0.005(3) -0.006(3) 0.005(4)
C6B 0.022(3) 0.077(4) 0.070(4) -0.008(3) -0.003(2) 0.010(4)
C7A 0.035(3) 0.069(4) 0.096(5) 0.016(3) 0.010(3) -0.009(4)
C7B 0.036(3) 0.055(3) 0.085(5) -0.017(3) 0.002(3) 0.019(3)
C8A 0.044(3) 0.043(3) 0.064(4) 0.007(2) 0.005(3) -0.007(3)
C8B 0.032(3) 0.041(3) 0.056(4) -0.003(2) -0.002(2) 0.016(2)
N1A 0.031(2) 0.031(2) 0.026(2) -0.0006(16) 0.0073(16) 0.0015(18)
N1B 0.029(2) 0.0260(17) 0.0181(19) -0.0045(15) 0.0009(14) 0.0030(15)
N2A 0.0297(19) 0.033(2) 0.023(2) 0.0031(16) 0.0021(16) -0.0003(17)
N2B 0.035(2) 0.0240(17) 0.024(2) 0.0007(15) 0.0025(15) 0.0012(16)
O1A 0.0435(19) 0.0393(19) 0.0308(19) 0.0074(16) -0.0007(14) 0.0059(15)
O1B 0.0377(18) 0.0392(18) 0.0248(17) 0.0136(14) -0.0024(13) 0.0070(13)
O2A 0.066(2) 0.051(2) 0.0175(18) 0.0122(18) 0.0036(15) -0.0011(15)
O2B 0.065(2) 0.057(2) 0.0213(18) 0.0336(19) 0.0078(15) 0.0072(15)
O3A 0.045(2) 0.041(2) 0.050(2) 0.0010(16) 0.0034(16) 0.0170(17)
O3B 0.068(2) 0.0303(19) 0.0308(19) 0.0023(15) 0.0082(16) 0.0128(14)
O4A 0.083(3) 0.042(2) 0.0228(19) -0.0085(18) 0.0029(17) -0.0089(15)
O4B 0.078(3) 0.0325(17) 0.0174(17) -0.0082(17) 0.0063(15) -0.0003(15)
O5A 0.076(3) 0.0323(18) 0.0239(19) -0.0014(16) 0.0069(16) -0.0073(15)
O5B 0.053(2) 0.0312(18) 0.0262(19) -0.0035(15) 0.0041(15) -0.0047(14)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1A C1A O2A . . 126.6(4) ?
O1A C1A C2A . . 124.1(4) ?
O2A C1A C2A . . 109.3(4) ?
O1B C1B O2B . . 125.8(4) ?
O1B C1B C2B . . 123.6(4) ?
O2B C1B C2B . . 110.6(3) ?
N1A C2A C1A . . 109.7(3) ?
N1A C2A C3A . . 112.4(3) ?
C1A C2A C3A . . 111.4(3) ?
N1A C2A H2 . . 108.7 ?
C1A C2A H2 . . 108.0 ?
C3A C2A H2 . . 106.5 ?
N1B C2B C1B . . 108.5(3) ?
N1B C2B C3B . . 111.9(3) ?
C1B C2B C3B . . 112.1(3) ?
N1B C2B H22 . . 107.9 ?
C1B C2B H22 . . 104.9 ?
C3B C2B H22 . . 111.3 ?
C4A C3A C8A . . 119.5(4) ?
C4A C3A C2A . . 123.1(4) ?
C8A C3A C2A . . 117.2(4) ?
C8B C3B C4B . . 119.2(4) ?
C8B C3B C2B . . 121.7(4) ?
C4B C3B C2B . . 119.1(4) ?
C3A C4A C5A . . 119.9(5) ?
C3A C4A H4 . . 124.5 ?
C5A C4A H4 . . 114.6 ?
C3B C4B C5B . . 119.9(5) ?
C3B C4B H44 . . 118.8 ?
C5B C4B H44 . . 121.2 ?
C6A C5A C4A . . 120.2(6) ?
C6A C5A H5 . . 124.1 ?
C4A C5A H5 . . 115.0 ?
C6B C5B C4B . . 120.6(5) ?
C6B C5B H55 . . 124.9 ?
C4B C5B H55 . . 114.4 ?
C7A C6A C5A . . 119.6(5) ?
C7A C6A H6 . . 115.1 ?
C5A C6A H6 . . 125.1 ?
C5B C6B C7B . . 119.5(5) ?
C5B C6B H66 . . 121.4 ?
C7B C6B H66 . . 119.1 ?
C6A C7A C8A . . 121.0(5) ?
C6A C7A H7 . . 127.4 ?
C8A C7A H7 . . 111.6 ?
C6B C7B C8B . . 120.6(5) ?
C6B C7B H77 . . 122.9 ?
C8B C7B H77 . . 116.5 ?
C7A C8A C3A . . 119.8(5) ?
C7A C8A H8 . . 120.9 ?
C3A C8A H8 . . 118.5 ?
C7B C8B C3B . . 120.1(5) ?
C7B C8B H88 . . 123.4 ?
C3B C8B H88 . . 116.4 ?
C2A N1A H10 . . 111.6 ?
C2A N1A H11 . . 114.9 ?
H10 N1A H11 . . 111.3 ?
C2A N1A H12 . . 102.4 ?
H10 N1A H12 . . 105.2 ?
H11 N1A H12 . . 110.6 ?
C2B N1B H100 . . 111.3 ?
C2B N1B H110 . . 106.2 ?
H100 N1B H110 . . 108.1 ?
C2B N1B H120 . . 111.4 ?
H100 N1B H120 . . 106.3 ?
H110 N1B H120 . . 113.6 ?
O4A N2A O5A . . 118.7(4) ?
O4A N2A O3A . . 121.5(4) ?
O5A N2A O3A . . 119.8(4) ?
O3B N2B O4B . . 121.2(3) ?
O3B N2B O5B . . 121.5(4) ?
O4B N2B O5B . . 117.3(3) ?
C1A O2A H . . 119.9 ?
C1B O2B H' . . 113.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1A O1A . 1.213(5) ?
C1A O2A . 1.306(5) ?
C1A C2A . 1.514(6) ?
C1B O1B . 1.207(5) ?
C1B O2B . 1.303(5) ?
C1B C2B . 1.512(5) ?
C2A N1A . 1.499(5) ?
C2A C3A . 1.528(5) ?
C2A H2 . 1.0072 ?
C2B N1B . 1.489(5) ?
C2B C3B . 1.516(5) ?
C2B H22 . 0.9512 ?
C3A C4A . 1.367(6) ?
C3A C8A . 1.385(7) ?
C3B C8B . 1.382(6) ?
C3B C4B . 1.384(6) ?
C4A C5A . 1.391(7) ?
C4A H4 . 0.9076 ?
C4B C5B . 1.388(7) ?
C4B H44 . 0.9392 ?
C5A C6A . 1.376(9) ?
C5A H5 . 0.9386 ?
C5B C6B . 1.361(9) ?
C5B H55 . 0.9428 ?
C6A C7A . 1.354(9) ?
C6A H6 . 0.9372 ?
C6B C7B . 1.378(8) ?
C6B H66 . 0.9440 ?
C7A C8A . 1.377(7) ?
C7A H7 . 0.9547 ?
C7B C8B . 1.379(6) ?
C7B H77 . 0.9553 ?
C8A H8 . 0.9344 ?
C8B H88 . 0.9511 ?
N1A H10 . 1.0044 ?
N1A H11 . 0.9397 ?
N1A H12 . 0.8441 ?
N1B H100 . 1.0040 ?
N1B H110 . 0.9396 ?
N1B H120 . 1.0105 ?
N2A O4A . 1.241(5) ?
N2A O5A . 1.246(5) ?
N2A O3A . 1.248(5) ?
N2B O3B . 1.234(5) ?
N2B O4B . 1.248(4) ?
N2B O5B . 1.268(5) ?
O2A H . 0.9336 ?
O2B H' . 0.8650 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O2A H O3B 1_555 0.93 2.51 2.966(5) 110
O2A H O5B 1_555 0.93 1.74 2.653(5) 166
O2B H' O4A 2_655 0.87 1.77 2.593(5) 158
N1A H10 O1A 2_546 1.01 2.18 2.958(5) 133
N1A H10 O3B 2_556 1.01 2.48 2.982(5) 110
N1A H11 O4A 2_656 0.94 2.54 3.142(5) 122
N1A H11 O5A 2_656 0.94 1.91 2.842(5) 174
N1A H12 O3A 2_646 0.85 2.18 3.015(5) 170
N1A H12 O5A 2_646 0.85 2.43 2.976(5) 123
N1B H100 O3B 1_565 1.00 2.59 3.158(5) 116
N1B H100 O4B 1_565 1.00 1.84 2.829(5) 168
N1B H110 O1B 2_545 0.94 2.11 2.906(4) 142
N1B H120 O4B 1_555 1.01 2.51 2.981(5) 108
N1B H120 O5B 1_555 1.01 1.98 2.958(5) 163
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1A C1A C2A N1A . . . . 24.1(5) ?
O2A C1A C2A N1A . . . . -155.8(3) ?
O1A C1A C2A C3A . . . . -101.2(4) ?
O2A C1A C2A C3A . . . . 78.9(4) ?
O1B C1B C2B N1B . . . . 25.4(4) ?
O2B C1B C2B N1B . . . . -156.6(3) ?
O1B C1B C2B C3B . . . . -98.6(4) ?
O2B C1B C2B C3B . . . . 79.4(4) ?
N1A C2A C3A C4A . . . . -37.6(5) ?
C1A C2A C3A C4A . . . . 86.0(4) ?
N1A C2A C3A C8A . . . . 146.1(4) ?
C1A C2A C3A C8A . . . . -90.3(4) ?
N1B C2B C3B C8B . . . . -95.9(4) ?
C1B C2B C3B C8B . . . . 26.1(5) ?
N1B C2B C3B C4B . . . . 84.8(4) ?
C1B C2B C3B C4B . . . . -153.2(4) ?
C8A C3A C4A C5A . . . . -1.3(7) ?
C2A C3A C4A C5A . . . . -177.5(4) ?
C8B C3B C4B C5B . . . . 0.6(7) ?
C2B C3B C4B C5B . . . . 179.9(4) ?
C3A C4A C5A C6A . . . . 1.0(8) ?
C3B C4B C5B C6B . . . . -1.7(8) ?
C4A C5A C6A C7A . . . . 0.1(9) ?
C4B C5B C6B C7B . . . . 1.1(9) ?
C5A C6A C7A C8A . . . . -0.8(9) ?
C5B C6B C7B C8B . . . . 0.6(9) ?
C6A C7A C8A C3A . . . . 0.4(8) ?
C4A C3A C8A C7A . . . . 0.7(7) ?
C2A C3A C8A C7A . . . . 177.1(4) ?
C4B C3B C8B C7B . . . . 1.1(7) ?
C2B C3B C8B C7B . . . . -178.2(4) ?
C6B C7B C8B C3B . . . . -1.7(8) ?
|
1100173.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-07 04:14:33 +0200 (Mon, 07 Mar 2016) $
#$Revision: 177980 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100173.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_1100173
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 H22 N2 O4'
_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 9.3531(11)
_cell_length_b 10.5002(13)
_cell_length_c 15.900(2)
_cod_database_code 1100173
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
O1 O 0.49095(9) 0.59203(7) 0.07262(5)
O2 O 0.73684(9) 0.60253(8) -0.07116(5)
O3 O 0.49893(10) 0.25460(7) 0.11004(5)
N1 N 0.61035(12) 0.38080(9) 0.01426(6)
N2 N 0.67015(11) 0.77638(8) 0.00380(6)
C1 C 0.44679(13) 0.47806(10) 0.11498(7)
C2 C 0.47452(14) 0.49977(11) 0.20881(7)
C3 C 0.60023(15) 0.59207(11) 0.20779(7)
C4 C 0.57011(13) 0.67345(10) 0.12980(6)
C5 C 0.52342(12) 0.36099(9) 0.07957(7)
C6 C 0.67957(16) 0.27638(12) -0.03006(8)
C7 C 0.70488(13) 0.72036(10) 0.08561(7)
C8 C 0.69011(12) 0.71368(10) -0.06864(7)
C9 C 0.78395(15) 0.81861(12) 0.13883(9)
C10 C 0.65359(12) 0.78058(10) -0.14936(7)
C11 C 0.58175(13) 0.89688(11) -0.15350(8)
C12 C 0.54659(16) 0.94832(13) -0.23173(9)
C13 C 0.58206(17) 0.88497(14) -0.30541(8)
C14 C 0.65528(17) 0.77048(14) -0.30186(8)
C15 C 0.69145(14) 0.71878(12) -0.22388(8)
O4 O 1.00838(12) 0.49545(9) -0.04533(7)
H1 H 0.342(2) 0.4665(14) 0.1036(10)
H2 H 0.694(2) 0.5473(15) 0.1993(10)
H3 H 0.6084(19) 0.6413(14) 0.2606(10)
H4 H 0.5075(16) 0.7480(12) 0.1439(8)
H5 H 0.6224(19) 0.4575(16) -0.0012(10)
H6 H 0.389(2) 0.5406(15) 0.2338(10)
H7 H 0.4935(19) 0.4213(15) 0.2398(10)
H8 H 0.7664(16) 0.6450(12) 0.0738(8)
H9 H 0.722(2) 0.8948(17) 0.1471(11)
H10 H 0.870(2) 0.8448(15) 0.109(1)
H11 H 0.810(2) 0.7836(18) 0.1971(11)
H12 H 0.6326(18) 0.8561(14) 0.0037(9)
H13 H 0.605(2) 0.2173(17) -0.0554(10)
H14 H 0.733(2) 0.2197(18) 0.0085(11)
H15 H 0.736(2) 0.311(2) -0.0763(12)
H16 H 0.550(2) 0.9401(15) -0.0996(11)
H17 H 0.496(2) 1.0300(16) -0.2346(11)
H18 H 0.556(2) 0.9265(16) -0.3636(11)
H19 H 0.685(2) 0.7302(16) -0.3551(12)
H20 H 0.7418(17) 0.6362(14) -0.2216(9)
H21 H 1.018(2) 0.423(2) -0.0652(12)
H22 H 0.918(3) 0.532(2) -0.0555(13)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100174.cif | #------------------------------------------------------------------------------
#$Date: 2016-06-16 14:46:25 +0300 (Thu, 16 Jun 2016) $
#$Revision: 183538 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/01/1100174.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_1100174
loop_
_publ_author_name
'Gr\"ob, Thorsten'
'Neum\"uller, Bernhard'
'Harms, Klaus'
'Schmock, Fritjof'
'Greiner, Andreas'
'Dehnicke, Kurt'
_publ_section_title
;
Die Kristallstrukturen vontrans-[NiBr~2~(Pyridin)~4~] und
[Ni(HNPEt~3~)~4~]I~2~
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1928
_journal_page_last 1931
_journal_paper_doi
10.1002/1521-3749(200108)627:8<1928::AID-ZAAC1928>3.0.CO;2-V
_journal_volume 627
_journal_year 2001
_chemical_formula_moiety
;
C24 H64 N4 Ni1 P4 2+,2(I1 1-)
;
_chemical_formula_sum 'C24 H64 I2 N4 Ni P4'
_chemical_name_systematic
;
tetrakis(Triethylphosphoraneimino-N)-nickel(ii) di-iodide
;
_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 111.040(8)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 19.349(2)
_cell_length_b 10.7833(7)
_cell_length_c 19.663(2)
_cell_volume 3829.087
_diffrn_ambient_temperature 193
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.466
_exptl_crystal_description prism
_refine_ls_R_factor_gt 4.3
_refine_ls_wR_factor_gt 4.3
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C24 H64 I2 N4 Ni1 P4'
_cod_database_code 1100174
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_disorder_group
_atom_site_disorder_assembly
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
. . I1 I 0.11116(2) 0.38770(3) 0.17339(2)
. . Ni1 Ni 0.25438(3) 0.05871(5) 0.33709(3)
. . P1 P 0.10804(6) -0.02781(12) 0.19181(6)
. . N1 N 0.1684(2) 0.0640(4) 0.2438(2)
. . H1 H 0.156(3) 0.123(5) 0.238(3)
. . I2 I 0.37223(2) -0.27445(3) 0.52034(2)
. . P2 P 0.38973(7) -0.04050(12) 0.29256(7)
. . N2 N 0.3377(2) -0.0521(4) 0.3391(2)
. . H2 H 0.354(3) -0.092(5) 0.374(3)
. . P3 P 0.31882(7) 0.33841(11) 0.38993(7)
. . N3 N 0.2731(3) 0.2389(4) 0.3311(2)
. . H3 H 0.255(3) 0.265(6) 0.299(3)
. . P4 P 0.18975(8) 0.00140(15) 0.46637(7)
. . N4 N 0.2478(3) -0.0106(5) 0.4270(2)
. . H4 H 0.270(3) -0.064(6) 0.442(3)
. . C1 C 0.0250(3) -0.0434(5) 0.2124(3)
. . H5 H -0.00990 -0.09890 0.17600
. . H6 H 0.03760 -0.08250 0.26090
. . C2 C -0.0129(3) 0.0805(6) 0.2123(4)
. . H7 H -0.05430 0.06840 0.22920
. . H8 H -0.03150 0.11440 0.16270
. . H9 H 0.02280 0.13850 0.24490
. . C3 C 0.1444(3) -0.1817(5) 0.1941(3)
. . H10 H 0.10540 -0.23400 0.15950
. . H11 H 0.18620 -0.17780 0.17630
. . C4 C 0.1711(4) -0.2449(5) 0.2677(3)
. . H12 H 0.18550 -0.33050 0.26220
. . H13 H 0.13130 -0.24530 0.28740
. . H14 H 0.21390 -0.20000 0.30100
. . C5 C 0.0763(3) 0.0215(6) 0.0975(3)
. . H15 H 0.04290 -0.04300 0.06710
. . H16 H 0.04690 0.09840 0.09250
. . C6 C 0.1371(4) 0.0452(7) 0.0684(3)
. . H17 H 0.11550 0.07220 0.01750
. . H18 H 0.16540 -0.03130 0.07120
. . H19 H 0.17010 0.11000 0.09750
. . C7 C 0.4115(3) -0.1874(5) 0.2604(3)
. . H20 H 0.44220 -0.17140 0.23050
. . H21 H 0.44150 -0.23730 0.30300
. . C8 C 0.3440(3) -0.2630(6) 0.2154(3)
. . H22 H 0.36020 -0.34210 0.20170
. . H23 H 0.31560 -0.21680 0.17130
. . H24 H 0.31280 -0.27870 0.24420
. . C9 C 0.3413(3) 0.0543(6) 0.2153(3)
. . H25 H 0.29450 0.01190 0.18650
. . H26 H 0.32800 0.13330 0.23310
. . C10 C 0.3827(4) 0.0845(7) 0.1647(3)
. . H27 H 0.35210 0.13830 0.12520
. . H28 H 0.39370 0.00760 0.14410
. . H29 H 0.42910 0.12720 0.19220
. . C11 C 0.4788(3) 0.0303(5) 0.3388(3)
. . H30 H 0.50750 0.03080 0.30600
. . H31 H 0.47160 0.11740 0.35070
. . C12 C 0.5222(4) -0.0380(6) 0.4080(4)
. . H32 H 0.56780 0.00760 0.43420
. . H33 H 0.53460 -0.12120 0.39590
. . H34 H 0.49230 -0.04470 0.43890
. . C13 C 0.2686(3) 0.4078(5) 0.4416(3)
. . H35 H 0.25610 0.34260 0.47080
. . H36 H 0.30100 0.46900 0.47600
. . C14 C 0.1985(3) 0.4715(7) 0.3948(3)
. . H37 H 0.17060 0.49810 0.42510
. . H38 H 0.16830 0.41390 0.35740
. . H39 H 0.21090 0.54410 0.37140
. . C15 C 0.3964(3) 0.2633(5) 0.4559(3)
. . H40 H 0.37810 0.19510 0.47870
. . H41 H 0.42730 0.22590 0.43060
. . C16 C 0.4447(3) 0.3488(5) 0.5158(3)
. . H42 H 0.48920 0.30400 0.54610
. . H43 H 0.41690 0.37630 0.54600
. . H44 H 0.45920 0.42110 0.49370
. . C17 C 0.3522(3) 0.4653(5) 0.3511(3)
. . H45 H 0.31010 0.50220 0.31120
. . H46 H 0.37260 0.52980 0.38890
. . C18 C 0.4121(4) 0.4270(6) 0.3212(3)
. . H47 H 0.42570 0.49860 0.29800
. . H48 H 0.39310 0.36060 0.28530
. . H49 H 0.45580 0.39740 0.36130
2 A C19? C 0.1603(8) -0.1151(11) 0.5132(7)
2 A H50? H 0.20540 -0.16200 0.54150
2 A H51? H 0.14460 -0.07090 0.54940
1 A C20 C 0.1341(7) -0.1471(10) 0.4426(5)
1 A H52 H 0.09270 -0.13000 0.39630
1 A H53 H 0.16630 -0.20810 0.43080
. . C21 C 0.1059(8) -0.2038(12) 0.4818(7)
1 A H54 H 0.08370 -0.28130 0.45790
1 A H55 H 0.06760 -0.15190 0.48920
1 A H56 H 0.14430 -0.22240 0.52910
2 A H57? H 0.09990 -0.25570 0.51900
2 A H58? H 0.12120 -0.25340 0.44920
2 A H59? H 0.05960 -0.16420 0.45510
1 A C22 C 0.2300(5) 0.0019(8) 0.5616(4)
1 A H60 H 0.19090 -0.00620 0.58280
1 A H61 H 0.26410 -0.06940 0.57820
2 A C23? C 0.2340(9) 0.1106(15) 0.5468(7)
2 A H62? H 0.25300 0.18360 0.52850
2 A H63? H 0.19430 0.14060 0.56330
1 A C24 C 0.2710(7) 0.1188(10) 0.5864(7)
1 A H64 H 0.29780 0.11520 0.63910
1 A H65 H 0.23610 0.18840 0.57490
1 A H66 H 0.30630 0.13040 0.56160
2 A C25? C 0.2935(10) 0.064(2) 0.6101(10)
2 A H67? H 0.33500 0.03840 0.59590
2 A H68? H 0.27590 -0.00710 0.63020
2 A H69? H 0.31000 0.12960 0.64700
. . C26 C 0.1240(4) 0.1170(6) 0.4207(4)
. . H70 H 0.15110 0.19600 0.42410
. . H71 H 0.10300 0.09420 0.36850
. . C27 C 0.0607(3) 0.1411(7) 0.4459(3)
. . H72 H 0.03550 0.21790 0.42360
. . H73 H 0.07950 0.14960 0.49910
. . H74 H 0.02570 0.07180 0.43140
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
I 1.40
N 0.68
Ni 1.50
P 1.05
|
1100175.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 14:16:41 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176967 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100175.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_1100175
loop_
_publ_author_name
'Gr\"ob, Thorsten'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Phosphaniminato-Komplexe des Hafniums. Die Kristallstrukturen von
[Hf(NPPh~3~)~4~] · 3 THF und [Hf(NPPh~3~)~2~Cl~2~(HNPPh~3~)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1801
_journal_page_last 1806
_journal_paper_doi
10.1002/1521-3749(200108)627:8<1801::AID-ZAAC1801>3.0.CO;2-9
_journal_volume 627
_journal_year 2001
_chemical_formula_moiety 'C72 H60 Hf1 N4 P4,3(C4 H8 O1)'
_chemical_formula_sum 'C84 H84 Hf N4 O3 P4'
_chemical_name_systematic
;
tetrakis(Triphenylphosphoraneiminato)-hafnium tetrahydrofuran solvate
;
_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 109.193(4)
_cell_angle_beta 111.285(4)
_cell_angle_gamma 96.879(4)
_cell_formula_units_Z 4
_cell_length_a 20.0757(10)
_cell_length_b 20.642(1)
_cell_length_c 21.1595(11)
_cell_volume 7425.962
_diffrn_ambient_temperature 193
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.342
_exptl_crystal_description prism
_refine_ls_R_factor_gt 5.06
_refine_ls_wR_factor_gt 5.06
_cod_original_formula_sum 'C84 H84 Hf1 N4 O3 P4'
_cod_database_code 1100175
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
Hf1 Hf 0.61194(1) 0.94426(1) 0.30210(1)
P1 P 0.68552(8) 1.12333(8) 0.39233(8)
N1 N 0.6474(3) 1.0464(3) 0.3753(3)
C1 C 0.6504(3) 1.1489(3) 0.3143(3)
C2 C 0.6472(3) 1.1035(3) 0.2464(3)
H1 H 0.66690 1.06360 0.24370
C3 C 0.6154(4) 1.1168(4) 0.1833(3)
H2 H 0.61380 1.08610 0.13770
C4 C 0.5863(4) 1.1742(4) 0.1864(4)
H3 H 0.56470 1.18300 0.14300
C5 C 0.5885(4) 1.2194(4) 0.2531(4)
H4 H 0.56800 1.25880 0.25520
C6 C 0.6205(4) 1.2068(3) 0.3162(4)
H5 H 0.62220 1.23800 0.36160
C7 C 0.6724(3) 1.1898(3) 0.4653(3)
C8 C 0.6092(3) 1.1694(4) 0.4744(3)
H6 H 0.57720 1.12240 0.44540
C9 C 0.5932(4) 1.2183(4) 0.5262(4)
H7 H 0.54970 1.20460 0.53210
C10 C 0.6394(4) 1.2863(4) 0.5691(4)
H8 H 0.62830 1.31920 0.60470
C11 C 0.7020(5) 1.3063(4) 0.5598(4)
H9 H 0.73370 1.35330 0.58880
C12 C 0.7192(4) 1.2584(4) 0.5087(4)
H10 H 0.76290 1.27250 0.50320
C13 C 0.7856(3) 1.1425(3) 0.4203(3)
C14 C 0.8263(3) 1.1984(4) 0.4159(4)
H11 H 0.80190 1.22920 0.39690
C15 C 0.9032(4) 1.2103(4) 0.4390(4)
H12 H 0.93060 1.24870 0.43540
C16 C 0.9387(3) 1.1666(4) 0.4667(4)
H13 H 0.99100 1.17510 0.48340
C17 C 0.8983(4) 1.1099(4) 0.4703(4)
H14 H 0.92290 1.07890 0.48860
C18 C 0.8225(3) 1.0979(4) 0.4475(4)
H15 H 0.79540 1.05890 0.45060
P2 P 0.42438(7) 0.89226(8) 0.17431(8)
N2 N 0.5080(2) 0.9201(3) 0.2235(3)
C19 C 0.3748(3) 0.8340(3) 0.2007(4)
C20 C 0.4125(4) 0.8304(4) 0.2682(4)
H16 H 0.46260 0.85800 0.29900
C21 C 0.3771(6) 0.7862(5) 0.2912(5)
H17 H 0.40300 0.78460 0.33790
C22 C 0.3055(6) 0.7452(5) 0.2466(7)
H18 H 0.28180 0.71460 0.26180
C23 C 0.2681(5) 0.7488(5) 0.1798(7)
H19 H 0.21770 0.72190 0.14990
C24 C 0.3026(4) 0.7913(4) 0.1546(5)
H20 H 0.27700 0.79080 0.10680
C25 C 0.4008(3) 0.8372(3) 0.0777(3)
C26 C 0.4340(4) 0.7823(4) 0.0649(4)
H21 H 0.46650 0.77450 0.10550
C27 C 0.4201(4) 0.7383(4) -0.0072(4)
H22 H 0.44300 0.70060 -0.01550
C28 C 0.3730(4) 0.7498(4) -0.0662(4)
H23 H 0.36250 0.71900 -0.11530
C29 C 0.3412(4) 0.8048(4) -0.0549(4)
H24 H 0.31020 0.81330 -0.09580
C30 C 0.3544(3) 0.8489(4) 0.0178(3)
H25 H 0.33160 0.88670 0.02580
C31 C 0.3798(3) 0.9640(3) 0.1731(3)
C32 C 0.3027(3) 0.9546(4) 0.1454(4)
H26 H 0.27020 0.90860 0.12690
C33 C 0.2743(4) 1.0123(4) 0.1451(4)
H27 H 0.22210 1.00570 0.12640
C34 C 0.3215(5) 1.0803(4) 0.1721(4)
H28 H 0.30190 1.12010 0.17240
C35 C 0.3962(4) 1.0883(4) 0.1980(5)
H29 H 0.42860 1.13420 0.21570
C36 C 0.4257(4) 1.0321(3) 0.1992(4)
H30 H 0.47800 1.03950 0.21800
P3 P 0.69358(7) 0.88784(8) 0.18478(7)
N3 N 0.6804(3) 0.9294(3) 0.2527(2)
C37 C 0.6511(3) 0.7924(3) 0.1415(3)
C38 C 0.6357(4) 0.7588(3) 0.1843(3)
H31 H 0.64830 0.78570 0.23500
C39 C 0.6024(5) 0.6868(4) 0.1526(5)
H32 H 0.59220 0.66440 0.18210
C40 C 0.5834(5) 0.6458(4) 0.0785(5)
H33 H 0.56070 0.59600 0.05740
C41 C 0.5985(4) 0.6796(4) 0.0360(4)
H34 H 0.58570 0.65260 -0.01470
C42 C 0.6314(3) 0.7513(3) 0.0668(3)
H35 H 0.64100 0.77360 0.03700
C43 C 0.6572(3) 0.9144(3) 0.1077(3)
C44 C 0.5835(3) 0.9166(3) 0.0833(3)
H36 H 0.55520 0.90610 0.10800
C45 C 0.5507(4) 0.9342(4) 0.0230(4)
H37 H 0.50020 0.93510 0.00660
C46 C 0.5910(4) 0.9502(3) -0.0127(3)
H38 H 0.56830 0.96220 -0.05380
C47 C 0.6651(4) 0.9490(4) 0.0112(3)
H39 H 0.69310 0.96030 -0.01340
C48 C 0.6981(3) 0.9313(3) 0.0710(3)
H40 H 0.74870 0.93060 0.08720
C49 C 0.7919(3) 0.8989(3) 0.2085(3)
C50 C 0.8417(3) 0.9610(4) 0.2663(4)
H41 H 0.82360 0.99610 0.29210
C51 C 0.9180(4) 0.9730(5) 0.2873(4)
H42 H 0.95150 1.01620 0.32670
C52 C 0.9447(4) 0.9213(5) 0.2501(4)
H43 H 0.99660 0.92920 0.26400
C53 C 0.8961(3) 0.8588(4) 0.1932(4)
H44 H 0.91460 0.82360 0.16810
C54 C 0.8198(3) 0.8467(4) 0.1722(3)
H45 H 0.78670 0.80310 0.13330
P4 P 0.65865(7) 0.87054(8) 0.42859(7)
N4 N 0.6157(3) 0.8797(3) 0.3561(2)
C55 C 0.6316(3) 0.9115(3) 0.5025(3)
C56 C 0.6201(4) 0.8797(4) 0.5473(4)
H46 H 0.62690 0.83360 0.54080
C57 C 0.5986(4) 0.9151(4) 0.6020(4)
H47 H 0.59180 0.89320 0.63310
C58 C 0.5874(4) 0.9798(5) 0.6112(4)
H48 H 0.57300 1.00350 0.64880
C59 C 0.5969(6) 1.0121(5) 0.5660(5)
H49 H 0.58860 1.05770 0.57210
C60 C 0.6186(5) 0.9775(4) 0.5120(4)
H50 H 0.62480 0.99960 0.48080
C61 C 0.7599(3) 0.9063(3) 0.4697(3)
C62 C 0.7923(3) 0.9067(4) 0.4223(3)
H51 H 0.76180 0.89240 0.37100
C63 C 0.8690(3) 0.9276(4) 0.4488(4)
H52 H 0.89090 0.92610 0.41550
C64 C 0.9135(3) 0.9505(4) 0.5236(4)
H53 H 0.96600 0.96520 0.54200
C65 C 0.8813(4) 0.9519(4) 0.5719(4)
H54 H 0.91160 0.96780 0.62340
C66 C 0.8050(3) 0.9301(4) 0.5447(3)
H55 H 0.78310 0.93140 0.57790
C67 C 0.6494(3) 0.7773(3) 0.4138(3)
C68 C 0.6956(3) 0.7548(4) 0.4647(4)
H56 H 0.73150 0.78920 0.51160
C69 C 0.6896(4) 0.6825(4) 0.4478(5)
H57 H 0.72060 0.66750 0.48310
C70 C 0.6381(4) 0.6328(4) 0.3790(5)
H58 H 0.63470 0.58360 0.36650
C71 C 0.5914(4) 0.6545(4) 0.3281(4)
H59 H 0.55540 0.62000 0.28140
C72 C 0.5969(3) 0.7262(3) 0.3452(3)
H60 H 0.56490 0.74070 0.31000
Hf2 Hf 0.85588(1) 0.65584(1) 0.76212(1)
P5 P 0.94750(8) 0.78056(9) 0.72991(9)
N5 N 0.9324(3) 0.7357(3) 0.7710(3)
C73 C 0.8964(3) 0.8469(4) 0.7283(3)
C74 C 0.8182(4) 0.8229(5) 0.7018(4)
H61 H 0.79550 0.77340 0.68380
C75 C 0.7747(4) 0.8688(5) 0.7012(4)
H62 H 0.72250 0.85140 0.68350
C76 C 0.8065(5) 0.9399(5) 0.7263(5)
H63 H 0.77630 0.97190 0.72600
C77 C 0.8828(5) 0.9659(5) 0.7524(5)
H64 H 0.90450 1.01540 0.76950
C78 C 0.9271(4) 0.9190(4) 0.7533(4)
H65 H 0.97920 0.93690 0.77130
C79 C 0.9257(3) 0.7318(4) 0.6329(4)
C80 C 0.9018(4) 0.7598(5) 0.5801(4)
H66 H 0.89740 0.80720 0.59460
C81 C 0.8842(5) 0.7195(7) 0.5055(5)
H67 H 0.86720 0.73900 0.46960
C82 C 0.8918(6) 0.6516(7) 0.4855(6)
H68 H 0.88070 0.62400 0.43530
C83 C 0.9152(5) 0.6230(6) 0.5369(6)
H69 H 0.92100 0.57610 0.52220
C84 C 1.0457(3) 0.8281(3) 0.7719(4)
C85 C 0.9305(4) 0.6618(5) 0.6096(5)
H70 H 0.94450 0.64050 0.64430
C86 C 1.0818(4) 0.8477(4) 0.7335(5)
H71 H 1.05440 0.83940 0.68300
C87 C 1.1576(4) 0.8794(5) 0.7682(6)
H72 H 1.18170 0.89210 0.74110
C88 C 1.1977(4) 0.8926(4) 0.8398(5)
H73 H 1.24960 0.91500 0.86320
C89 C 1.1631(4) 0.8734(5) 0.8789(5)
H74 H 1.19130 0.88280 0.92960
C90 C 1.0863(4) 0.8401(5) 0.8447(4)
H75 H 1.06280 0.82600 0.87160
P6 P 0.95280(8) 0.53055(8) 0.78706(9)
N6 N 0.9050(3) 0.5833(3) 0.7870(3)
C91 C 0.9314(4) 0.4686(4) 0.8257(4)
C92 C 0.9322(6) 0.3997(5) 0.8040(6)
H76 H 0.94300 0.37770 0.76310
C93 C 0.9168(7) 0.3602(6) 0.8437(8)
H77 H 0.91610 0.31130 0.82720
C94 C 0.9037(6) 0.3877(8) 0.9010(7)
H78 H 0.89860 0.36120 0.92890
C95 C 0.8976(11) 0.4541(10) 0.9197(10)
H79 H 0.88490 0.47450 0.95960
C96 C 0.9099(9) 0.4941(7) 0.8806(8)
H80 H 0.90280 0.54050 0.89320
C97 C 0.9448(4) 0.4770(4) 0.6964(4)
C98 C 0.8864(4) 0.4754(4) 0.6337(4)
H81 H 0.85170 0.50150 0.63980
C99 C 0.8785(6) 0.4366(5) 0.5633(5)
H82 H 0.83820 0.43590 0.52150
C100 C 0.9288(7) 0.3989(5) 0.5531(6)
H83 H 0.92410 0.37340 0.50460
C101 C 0.9854(6) 0.3982(6) 0.6130(6)
H84 H 1.01890 0.37090 0.60600
C102 C 0.9938(5) 0.4378(5) 0.6844(5)
H85 H 1.03400 0.43790 0.72570
C103 C 1.0520(3) 0.5735(4) 0.8437(4)
C104 C 1.0800(4) 0.6399(4) 0.8474(4)
H86 H 1.04750 0.66090 0.82030
C105 C 1.1546(4) 0.6764(5) 0.8901(5)
H87 H 1.17300 0.72190 0.89180
C106 C 1.2017(4) 0.6462(6) 0.9301(5)
H88 H 1.25270 0.67140 0.96000
C107 C 1.1749(5) 0.5786(7) 0.9268(7)
H89 H 1.20750 0.55800 0.95440
C108 C 1.0999(4) 0.5419(6) 0.8826(6)
H90 H 1.08150 0.49560 0.87900
P7 P 0.69511(7) 0.57083(8) 0.61050(7)
N7 N 0.7793(2) 0.6095(3) 0.6562(2)
C109 C 0.6569(3) 0.5153(3) 0.6480(3)
C110 C 0.7060(3) 0.4911(3) 0.6952(3)
H91 H 0.75710 0.50160 0.70510
C111 C 0.6801(4) 0.4518(4) 0.7274(4)
H92 H 0.71350 0.43620 0.76040
C112 C 0.6054(4) 0.4352(4) 0.7116(4)
H93 H 0.58750 0.40750 0.73310
C113 C 0.5567(4) 0.4588(4) 0.6648(4)
H94 H 0.50550 0.44740 0.65400
C114 C 0.5828(3) 0.4990(4) 0.6336(3)
H95 H 0.54930 0.51560 0.60190
C115 C 0.6725(3) 0.5119(3) 0.5155(3)
C116 C 0.6081(4) 0.4575(4) 0.4691(3)
H96 H 0.57210 0.44880 0.48670
C117 C 0.5950(5) 0.4152(4) 0.3973(4)
H97 H 0.55010 0.37820 0.36610
C118 C 0.6468(5) 0.4268(4) 0.3715(4)
H98 H 0.63780 0.39790 0.32230
C119 C 0.7126(4) 0.4809(4) 0.4175(4)
H99 H 0.74870 0.48880 0.39980
C120 C 0.7255(3) 0.5232(4) 0.4891(3)
H100 H 0.77050 0.56000 0.52040
C121 C 0.6347(3) 0.6295(3) 0.6024(3)
C122 C 0.6406(4) 0.6800(4) 0.6681(4)
H101 H 0.67500 0.68220 0.71410
C123 C 0.5972(4) 0.7268(4) 0.6671(4)
H102 H 0.60100 0.76030 0.71240
C124 C 0.5481(4) 0.7255(4) 0.6004(5)
H103 H 0.51800 0.75770 0.59980
C125 C 0.5434(4) 0.6775(4) 0.5354(4)
H104 H 0.51060 0.67710 0.48960
C126 C 0.5859(3) 0.6297(4) 0.5358(4)
H105 H 0.58180 0.59640 0.49020
P8 P 0.78721(8) 0.72716(9) 0.89302(8)
N8 N 0.8057(3) 0.6916(3) 0.8276(3)
C127 C 0.8313(3) 0.8228(3) 0.9403(3)
C128 C 0.8591(4) 0.8563(4) 0.9050(4)
H106 H 0.85360 0.82920 0.85650
C129 C 0.8949(4) 0.9283(4) 0.9381(4)
H107 H 0.91370 0.95010 0.91260
C130 C 0.9031(4) 0.9685(4) 1.0089(4)
H108 H 0.92730 1.01810 1.03190
C131 C 0.8759(4) 0.9360(4) 1.0463(4)
H109 H 0.88130 0.96320 1.09470
C132 C 0.8407(3) 0.8634(4) 1.0117(3)
H110 H 0.82270 0.84100 1.03720
C133 C 0.6880(3) 0.7159(3) 0.8689(3)
C134 C 0.6580(3) 0.7695(4) 0.8948(3)
H111 H 0.68910 0.81680 0.92400
C135 C 0.5833(3) 0.7558(4) 0.8791(4)
H112 H 0.56370 0.79330 0.89840
C136 C 0.5370(3) 0.6870(4) 0.8351(4)
H113 H 0.48580 0.67720 0.82450
C137 C 0.5659(3) 0.6331(4) 0.8068(4)
H114 H 0.53410 0.58630 0.77580
C138 C 0.6410(3) 0.6465(4) 0.8233(3)
H115 H 0.66050 0.60900 0.80390
C139 C 0.8144(4) 0.6915(4) 0.9648(3)
C140 C 0.7755(4) 0.6880(4) 1.0055(4)
H116 H 0.73250 0.70510 0.99710
C141 C 0.7977(5) 0.6598(4) 1.0595(4)
H117 H 0.77010 0.65710 1.08710
C142 C 0.8600(6) 0.6363(6) 1.0713(5)
H118 H 0.87650 0.61760 1.10800
C143 C 0.8987(7) 0.6396(7) 1.0305(6)
H119 H 0.94310 0.62490 1.04070
C144 C 0.8748(5) 0.6637(7) 0.9753(5)
H120 H 0.89960 0.66120 0.94430
O1 O 1.1331(10) 0.6714(8) 0.6839(14)
C145 C 1.1046(7) 0.5953(9) 0.6604(10)
H121 H 1.07620 0.58570 0.68750
H122 H 1.07200 0.57230 0.60660
C146 C 1.1644(9) 0.5722(8) 0.6765(18)
H123 H 1.16760 0.54500 0.63000
H124 H 1.15970 0.53930 0.70060
C147 C 1.2282(7) 0.6255(10) 0.7220(9)
H125 H 1.27060 0.61290 0.71220
H126 H 1.24000 0.63680 0.77470
C148 C 1.2116(8) 0.6815(10) 0.7037(13)
H127 H 1.22250 0.68060 0.66140
H128 H 1.24080 0.72760 0.74630
O2 O 0.5991(13) 0.4760(11) 0.1026(12)
C149 C 0.5817(12) 0.4640(15) 0.1578(18)
H129 H 0.57500 0.50810 0.18920
H130 H 0.53470 0.42590 0.13420
C150 C 0.6370(16) 0.4450(17) 0.1995(13)
H131 H 0.62740 0.39250 0.17920
H132 H 0.64200 0.46180 0.25100
C151 C 0.6994(13) 0.476(3) 0.198(2)
H133 H 0.73650 0.44820 0.20660
H134 H 0.72180 0.52510 0.23620
C152 C 0.6760(14) 0.4749(13) 0.1283(15)
H135 H 0.68120 0.43150 0.09440
H136 H 0.70650 0.51710 0.12950
O3 O 0.3387(8) 0.5999(8) 0.0985(10)
C153 C 0.3284(8) 0.5238(7) 0.0742(9)
H137 H 0.29790 0.50360 0.09440
H138 H 0.30350 0.50000 0.01940
C154 C 0.3995(7) 0.5151(6) 0.1013(6)
H139 H 0.40040 0.48090 0.12490
H140 H 0.41320 0.49540 0.05980
C155 C 0.4494(4) 0.5786(4) 0.1515(4)
H141 H 0.49600 0.58280 0.14510
H142 H 0.46120 0.58250 0.20250
C156 C 0.4176(7) 0.6307(6) 0.1394(7)
H143 H 0.43730 0.65030 0.11080
H144 H 0.42910 0.67000 0.18720
O4 O 0.9073(12) 0.2310(9) 0.9271(12)
C157 C 0.9176(14) 0.2256(14) 0.9953(11)
H145 H 0.95800 0.26640 1.03760
H146 H 0.87140 0.22500 1.00230
C158 C 0.9355(17) 0.1641(14) 0.9901(11)
H147 H 0.98190 0.17330 1.03390
H148 H 0.89570 0.13090 0.99030
C159 C 0.9447(14) 0.1334(11) 0.9286(11)
H149 H 0.91720 0.08220 0.90310
H150 H 0.99800 0.13750 0.94100
C160 C 0.9180(17) 0.1681(11) 0.8847(9)
H151 H 0.87040 0.13750 0.84220
H152 H 0.95370 0.17980 0.86520
O5 O 1.1835(10) 0.2591(11) 0.6999(11)
C161 C 1.1982(12) 0.3352(10) 0.7307(15)
H153 H 1.23590 0.35570 0.78290
H154 H 1.21710 0.35570 0.70230
C162 C 1.1335(14) 0.3498(9) 0.7268(16)
H155 H 1.11330 0.36650 0.68660
H156 H 1.14200 0.38830 0.77400
C163 C 1.0839(12) 0.2905(13) 0.7133(15)
H157 H 1.03230 0.29130 0.68650
H158 H 1.08960 0.28590 0.76000
C164 C 1.1022(11) 0.2352(8) 0.6696(9)
H159 H 1.07870 0.22820 0.61690
H160 H 1.08620 0.19000 0.67350
O6 O 0.8762(6) 1.1193(6) 0.7047(5)
C165 C 0.9040(7) 1.1653(10) 0.6783(10)
H161 H 0.92080 1.13880 0.64130
H162 H 0.94710 1.20420 0.71970
C166 C 0.8470(7) 1.1940(7) 0.6455(8)
H163 H 0.84980 1.24030 0.68190
H164 H 0.85080 1.20120 0.60280
C167 C 0.7804(7) 1.1430(8) 0.6223(7)
H165 H 0.76510 1.10690 0.57170
H166 H 0.74000 1.16580 0.62320
C168 C 0.7987(7) 1.1114(8) 0.6755(7)
H167 H 0.78470 1.13540 0.71570
H168 H 0.77130 1.06030 0.65130
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Hf 1.57
N 0.68
O 0.68
P 1.05
|
1100176.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 14:16:41 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176967 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100176.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_1100176
loop_
_publ_author_name
'Gr\"ob, Thorsten'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Phosphaniminato-Komplexe des Hafniums. Die Kristallstrukturen von
[Hf(NPPh~3~)~4~] · 3 THF und [Hf(NPPh~3~)~2~Cl~2~(HNPPh~3~)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 8
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 1801
_journal_page_last 1806
_journal_paper_doi
10.1002/1521-3749(200108)627:8<1801::AID-ZAAC1801>3.0.CO;2-9
_journal_volume 627
_journal_year 2001
_chemical_formula_moiety 'C72 H62 Cl2 Hf1 N4 P4'
_chemical_formula_sum 'C72 H62 Cl2 Hf N4 P4'
_chemical_name_systematic
;
trans-Dichloro-bis(triphenylphosphoraneimine)-bis(triphenylphosphoraneiminato)-hafnium
;
_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 67.273(8)
_cell_angle_beta 87.445(8)
_cell_angle_gamma 87.082(8)
_cell_formula_units_Z 4
_cell_length_a 14.4397(10)
_cell_length_b 19.2812(14)
_cell_length_c 24.5579(17)
_cell_volume 6295.928
_diffrn_ambient_temperature 193
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.431
_exptl_crystal_description irregular
_refine_ls_R_factor_gt 3.12
_refine_ls_wR_factor_gt 3.12
_cod_original_formula_sum 'C72 H62 Cl2 Hf1 N4 P4'
_cod_database_code 1100176
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
Hf1 Hf 0.96775(1) -0.76247(1) 0.20474(1)
Cl1 Cl 0.93164(8) -0.62294(6) 0.16172(6)
Cl2 Cl 0.97724(9) -0.90588(6) 0.24548(5)
N1 N 0.8594(2) -0.7766(2) 0.14401(16)
H1 H 0.88160 -0.81840 0.14110
P1 P 0.77106(7) -0.76089(6) 0.10384(5)
C1 C 0.7227(3) -0.8474(2) 0.1081(2)
N2 N 0.8358(2) -0.7793(2) 0.26079(15)
H2 H 0.79430 -0.78290 0.23690
P2 P 0.77480(7) -0.78846(6) 0.31842(5)
C2 C 0.6945(4) -0.8607(3) 0.0607(3)
H3 H 0.70530 -0.82530 0.02160
N3 N 1.0466(2) -0.75500(19) 0.26631(16)
P3 P 1.11752(8) -0.72501(6) 0.29610(5)
C3 C 0.6504(5) -0.9259(5) 0.0705(5)
H4 H 0.62890 -0.93460 0.03780
N4 N 1.0629(2) -0.75783(19) 0.14133(15)
P4 P 1.13483(7) -0.75889(7) 0.09318(5)
C4 C 0.6368(5) -0.9783(4) 0.1256(6)
H5 H 0.60630 -1.02320 0.13150
C5 C 0.6662(6) -0.9661(3) 0.1712(4)
H6 H 0.65770 -1.00300 0.20990
C6 C 0.7086(5) -0.9016(3) 0.1635(3)
H7 H 0.72870 -0.89380 0.19700
C7 C 0.6770(3) -0.7134(2) 0.12777(19)
C8 C 0.5851(3) -0.7298(3) 0.1250(2)
H8 H 0.57110 -0.76650 0.10980
C9 C 0.5140(4) -0.6935(3) 0.1440(2)
H9 H 0.45140 -0.70520 0.14220
C10 C 0.5344(4) -0.6402(3) 0.1654(2)
H10 H 0.48540 -0.61500 0.17840
C11 C 0.6244(3) -0.6226(3) 0.1682(2)
H11 H 0.63750 -0.58570 0.18320
C12 C 0.6957(3) -0.6585(2) 0.14931(19)
H12 H 0.75800 -0.64590 0.15090
C13 C 0.7960(3) -0.7033(2) 0.02708(19)
C14 C 0.8844(4) -0.6845(3) 0.0103(3)
H13 H 0.93210 -0.70170 0.03840
C15 C 0.9056(4) -0.6394(4) -0.0486(3)
H14 H 0.96760 -0.62520 -0.06030
C16 C 0.8373(4) -0.6158(3) -0.0892(3)
H15 H 0.85240 -0.58670 -0.12940
C17 C 0.7485(4) -0.6337(3) -0.0723(2)
H16 H 0.70110 -0.61680 -0.10070
C18 C 0.7259(3) -0.6767(3) -0.0136(2)
H17 H 0.66310 -0.68780 -0.00140
C19 C 0.7191(3) -0.7015(2) 0.31592(17)
C20 C 0.6272(3) -0.6953(3) 0.3327(2)
H18 H 0.59120 -0.73890 0.34900
C21 C 0.5880(4) -0.6251(4) 0.3257(2)
H19 H 0.52480 -0.62050 0.33690
C22 C 0.6405(5) -0.5624(3) 0.3026(2)
H20 H 0.61330 -0.51450 0.29760
C23 C 0.7309(5) -0.5681(3) 0.2867(2)
H21 H 0.76720 -0.52460 0.27190
C24 C 0.7701(4) -0.6369(3) 0.2921(2)
H22 H 0.83270 -0.64030 0.27940
C25 C 0.6845(3) -0.8530(2) 0.32783(19)
C26 C 0.6148(3) -0.8326(3) 0.2865(2)
H23 H 0.61220 -0.78300 0.25710
C27 C 0.5496(4) -0.8827(4) 0.2872(3)
H24 H 0.50240 -0.86750 0.25870
C28 C 0.5533(4) -0.9548(3) 0.3294(3)
H25 H 0.50990 -0.99030 0.32940
C29 C 0.6192(3) -0.9750(3) 0.3709(3)
H26 H 0.62040 -1.02440 0.40070
C30 C 0.6849(3) -0.9248(2) 0.3707(2)
H27 H 0.73030 -0.94000 0.40030
C31 C 0.8414(3) -0.8256(2) 0.38445(18)
C32 C 0.8124(3) -0.8134(2) 0.4346(2)
H28 H 0.76020 -0.78070 0.43310
C33 C 0.8586(3) -0.8484(3) 0.4872(2)
H29 H 0.83750 -0.84050 0.52160
C34 C 0.9349(3) -0.8945(3) 0.4891(2)
H30 H 0.96700 -0.91830 0.52500
C35 C 0.9652(3) -0.9062(3) 0.4394(2)
H31 H 1.01870 -0.93770 0.44110
C36 C 0.9188(3) -0.8728(2) 0.3871(2)
H32 H 0.93960 -0.88190 0.35310
C37 C 1.2030(3) -0.7976(2) 0.33524(19)
C38 C 1.2908(3) -0.7832(3) 0.3483(2)
H33 H 1.30740 -0.73280 0.33920
C39 C 1.3538(4) -0.8413(3) 0.3742(3)
H34 H 1.41450 -0.83040 0.38110
C40 C 1.3306(4) -0.9144(3) 0.3902(2)
H35 H 1.37390 -0.95420 0.40970
C41 C 1.2432(4) -0.9300(3) 0.3779(3)
H36 H 1.22650 -0.98080 0.38870
C42 C 1.1805(3) -0.8723(3) 0.3500(2)
H37 H 1.12130 -0.88340 0.34060
C43 C 1.0667(3) -0.6887(2) 0.34901(19)
C44 C 1.0705(3) -0.7274(3) 0.4092(2)
H38 H 1.10720 -0.77280 0.42450
C45 C 1.0222(4) -0.7017(3) 0.4475(2)
H39 H 1.02510 -0.72980 0.48880
C46 C 0.9696(3) -0.6356(3) 0.4267(2)
H40 H 0.93630 -0.61810 0.45340
C47 C 0.9659(3) -0.5953(3) 0.3668(3)
H41 H 0.93070 -0.54920 0.35190
C48 C 1.0134(3) -0.6218(3) 0.3282(2)
H42 H 1.00980 -0.59400 0.28690
C49 C 1.1873(3) -0.6494(2) 0.2465(2)
C50 C 1.2355(3) -0.6027(3) 0.2649(2)
H43 H 1.22690 -0.60610 0.30450
C51 C 1.2954(3) -0.5514(3) 0.2277(3)
H44 H 1.32810 -0.51990 0.24130
C52 C 1.3074(3) -0.5462(3) 0.1707(3)
H45 H 1.34960 -0.51150 0.14480
C53 C 1.2591(3) -0.5907(3) 0.1506(2)
H46 H 1.26670 -0.58590 0.11070
C54 C 1.1990(3) -0.6427(3) 0.1888(2)
H47 H 1.16590 -0.67370 0.17500
C55 C 1.0938(3) -0.8003(3) 0.0442(2)
C56 C 1.0455(3) -0.8658(3) 0.0697(3)
H48 H 1.03910 -0.88850 0.11150
C57 C 1.0060(4) -0.8991(4) 0.0358(4)
H49 H 0.97240 -0.94370 0.05390
C58 C 1.0167(4) -0.8656(5) -0.0256(4)
H50 H 0.99130 -0.88820 -0.04940
C59 C 1.0638(4) -0.8003(5) -0.0517(3)
H51 H 1.06910 -0.77710 -0.09350
C60 C 1.1032(4) -0.7684(3) -0.0173(2)
H52 H 1.13730 -0.72410 -0.03560
C61 C 1.1694(3) -0.6645(3) 0.0458(2)
C62 C 1.1068(3) -0.6068(3) 0.0419(2)
H53 H 1.04890 -0.61800 0.06280
C63 C 1.1264(4) -0.5319(3) 0.0080(3)
H54 H 1.08240 -0.49280 0.00610
C64 C 1.2093(4) -0.5152(4) -0.0224(2)
H55 H 1.22320 -0.46440 -0.04550
C65 C 1.2716(4) -0.5716(4) -0.0194(3)
H56 H 1.32900 -0.56020 -0.04090
C66 C 1.2521(4) -0.6457(3) 0.0146(2)
H57 H 1.29680 -0.68440 0.01640
C67 C 1.2399(3) -0.8138(3) 0.1236(2)
C68 C 1.2513(3) -0.8380(3) 0.1842(2)
H58 H 1.20550 -0.82480 0.20790
C69 C 1.3283(3) -0.8809(3) 0.2099(3)
H59 H 1.33560 -0.89670 0.25130
C70 C 1.3955(4) -0.9014(3) 0.1764(3)
H60 H 1.44800 -0.93190 0.19460
C71 C 1.3855(3) -0.8772(3) 0.1166(3)
H61 H 1.43240 -0.88960 0.09320
C72 C 1.3072(3) -0.8347(3) 0.0900(2)
H62 H 1.29970 -0.82000 0.04870
Hf2 Hf 0.56661(1) -0.25599(1) 0.29561(1)
Cl3 Cl 0.55732(8) -0.11889(6) 0.27722(5)
Cl4 Cl 0.55290(8) -0.39672(6) 0.33792(5)
N5 N 0.7014(2) -0.26042(19) 0.27599(15)
P5 P 0.80441(7) -0.28815(6) 0.27302(5)
N6 N 0.5983(2) -0.27632(18) 0.39213(14)
H63 H 0.59710 -0.32550 0.41080
P6 P 0.62102(7) -0.24682(6) 0.44191(4)
N7 N 0.4097(2) -0.24858(19) 0.32040(14)
H64 H 0.39450 -0.20220 0.29690
P7 P 0.31407(6) -0.27614(6) 0.35366(4)
N8 N 0.5192(2) -0.24079(18) 0.21625(14)
P8 P 0.49704(7) -0.21602(6) 0.15061(5)
C73 C 0.8530(3) -0.3437(2) 0.34503(18)
C74 C 0.8163(3) -0.4128(3) 0.3772(2)
H65 H 0.77150 -0.43190 0.36000
C75 C 0.8438(3) -0.4543(3) 0.4337(2)
H66 H 0.81790 -0.50180 0.45510
C76 C 0.9080(3) -0.4280(3) 0.4595(2)
H67 H 0.92670 -0.45690 0.49870
C77 C 0.9449(3) -0.3600(3) 0.4285(2)
H68 H 0.99030 -0.34150 0.44590
C78 C 0.9165(3) -0.3171(3) 0.3713(2)
H69 H 0.94130 -0.26900 0.35030
C79 C 0.8825(3) -0.2109(2) 0.23928(18)
C80 C 0.9787(3) -0.2211(3) 0.2346(2)
H70 H 1.00590 -0.27050 0.24660
C81 C 1.0344(4) -0.1596(3) 0.2125(2)
H71 H 1.09970 -0.16680 0.20980
C82 C 0.9958(4) -0.0881(4) 0.1945(2)
H72 H 1.03450 -0.04610 0.18000
C83 C 0.9019(4) -0.0770(3) 0.1974(2)
H73 H 0.87530 -0.02740 0.18400
C84 C 0.8446(3) -0.1390(3) 0.2202(2)
H74 H 0.77930 -0.13120 0.22250
C85 C 0.8217(3) -0.3475(2) 0.23070(18)
C86 C 0.7500(3) -0.3500(2) 0.19571(19)
H75 H 0.69250 -0.32430 0.19670
C87 C 0.7619(3) -0.3898(3) 0.1596(2)
H76 H 0.71270 -0.39070 0.13550
C88 C 0.8446(4) -0.4283(3) 0.1581(2)
H77 H 0.85240 -0.45490 0.13260
C89 C 0.9150(4) -0.4281(3) 0.1933(2)
H78 H 0.97150 -0.45530 0.19280
C90 C 0.9041(3) -0.3883(3) 0.2299(2)
H79 H 0.95320 -0.38870 0.25450
C91 C 0.5244(3) -0.1952(2) 0.45935(18)
C92 C 0.4567(3) -0.1612(2) 0.4192(2)
H80 H 0.45790 -0.16800 0.38280
C93 C 0.3867(3) -0.1174(3) 0.4313(2)
H81 H 0.34070 -0.09380 0.40290
C94 C 0.3827(3) -0.1075(2) 0.4834(2)
H82 H 0.33350 -0.07790 0.49150
C95 C 0.4496(4) -0.1404(3) 0.5239(2)
H83 H 0.44860 -0.13240 0.55980
C96 C 0.5184(4) -0.1853(3) 0.5125(2)
H84 H 0.56300 -0.21020 0.54170
C97 C 0.7154(3) -0.1824(2) 0.42388(19)
C98 C 0.7551(3) -0.1556(3) 0.3677(2)
H85 H 0.73670 -0.17400 0.33920
C99 C 0.8223(3) -0.1014(3) 0.3530(2)
H86 H 0.84840 -0.08200 0.31400
C100 C 0.8512(3) -0.0758(3) 0.3944(2)
H87 H 0.89750 -0.03920 0.38400
C101 C 0.8130(3) -0.1033(3) 0.4508(2)
H88 H 0.83270 -0.08570 0.47950
C102 C 0.7467(3) -0.1562(2) 0.4654(2)
H89 H 0.72120 -0.17550 0.50450
C103 C 0.6487(3) -0.3241(2) 0.51008(17)
C104 C 0.7383(3) -0.3432(2) 0.53010(19)
H90 H 0.78790 -0.31260 0.50920
C105 C 0.7560(3) -0.4064(2) 0.5802(2)
H91 H 0.81780 -0.41920 0.59340
C106 C 0.6849(3) -0.4509(2) 0.61096(19)
H92 H 0.69730 -0.49420 0.64560
C107 C 0.5956(3) -0.4328(2) 0.5916(2)
H93 H 0.54640 -0.46390 0.61270
C108 C 0.5773(3) -0.3693(2) 0.5413(2)
H94 H 0.51540 -0.35670 0.52820
C109 C 0.2522(3) -0.3335(2) 0.32406(18)
C110 C 0.1780(3) -0.3760(2) 0.3539(2)
H95 H 0.15990 -0.37900 0.39240
C111 C 0.1301(3) -0.4143(3) 0.3269(3)
H96 H 0.07820 -0.44270 0.34680
C112 C 0.1570(4) -0.4117(3) 0.2720(3)
H97 H 0.12420 -0.43850 0.25410
C113 C 0.2310(4) -0.3705(3) 0.2429(2)
H98 H 0.24950 -0.36870 0.20480
C114 C 0.2793(3) -0.3313(3) 0.2687(2)
H99 H 0.33100 -0.30290 0.24840
C115 C 0.3272(2) -0.3337(2) 0.43101(17)
C116 C 0.3689(3) -0.4039(2) 0.44550(19)
H100 H 0.39160 -0.41960 0.41500
C117 C 0.3784(3) -0.4522(2) 0.5039(2)
H101 H 0.40710 -0.50070 0.51340
C118 C 0.3463(3) -0.4296(2) 0.54787(19)
H102 H 0.35240 -0.46290 0.58800
C119 C 0.3058(3) -0.3603(3) 0.53493(19)
H103 H 0.28390 -0.34490 0.56570
C120 C 0.2965(3) -0.3117(2) 0.47588(19)
H104 H 0.26880 -0.26290 0.46670
C121 C 0.2323(3) -0.1992(2) 0.34655(17)
C122 C 0.1437(3) -0.2104(3) 0.3733(2)
H105 H 0.12680 -0.25990 0.39810
C123 C 0.0809(3) -0.1519(3) 0.3645(2)
H106 H 0.02160 -0.16090 0.38380
C124 C 0.1031(4) -0.0810(3) 0.3283(2)
H107 H 0.05860 -0.04070 0.32160
C125 C 0.1889(4) -0.0674(3) 0.3016(2)
H108 H 0.20410 -0.01760 0.27650
C126 C 0.2548(3) -0.1266(2) 0.3111(2)
H109 H 0.31480 -0.11680 0.29300
C127 C 0.3845(3) -0.1671(2) 0.13143(18)
C128 C 0.3163(3) -0.1883(3) 0.1036(2)
H110 H 0.32810 -0.22960 0.09200
C129 C 0.2317(4) -0.1502(4) 0.0928(2)
H111 H 0.18530 -0.16530 0.07380
C130 C 0.2141(4) -0.0907(4) 0.1092(2)
H112 H 0.15600 -0.06380 0.10090
C131 C 0.2797(4) -0.0694(3) 0.1376(2)
H113 H 0.26690 -0.02870 0.14980
C132 C 0.3646(3) -0.1077(3) 0.1485(2)
H114 H 0.41020 -0.09270 0.16810
C133 C 0.5795(3) -0.1538(2) 0.09975(18)
C134 C 0.5589(3) -0.1047(3) 0.0425(2)
H115 H 0.49710 -0.09940 0.02930
C135 C 0.6284(4) -0.0636(3) 0.0046(2)
H116 H 0.61440 -0.03110 -0.03470
C136 C 0.7174(4) -0.0700(3) 0.0239(2)
H117 H 0.76500 -0.04270 -0.00240
C137 C 0.7383(3) -0.1157(3) 0.0811(2)
H118 H 0.79970 -0.11880 0.09440
C138 C 0.6695(3) -0.1571(3) 0.1190(2)
H119 H 0.68390 -0.18800 0.15860
C139 C 0.4980(3) -0.2958(2) 0.12779(19)
C140 C 0.4981(3) -0.3672(3) 0.1726(2)
H120 H 0.49480 -0.37270 0.21280
C141 C 0.5031(3) -0.4303(3) 0.1587(2)
H121 H 0.50300 -0.47890 0.18950
C142 C 0.5082(3) -0.4237(3) 0.1011(2)
H122 H 0.51060 -0.46740 0.09210
C143 C 0.5098(3) -0.3527(3) 0.0560(2)
H123 H 0.51480 -0.34790 0.01600
C144 C 0.5041(3) -0.2895(3) 0.0692(2)
H124 H 0.50440 -0.24110 0.03810
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
Hf 1.57
N 0.68
P 1.05
|
1100177.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-04 15:42:05 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177552 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100177.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_1100177
loop_
_publ_author_name
'Hoffmann, Reinhard W.'
'Nell, Peter G.'
'Leo, Roland'
'Harms, Klaus'
_publ_section_title
;
Highly Enantiomerically Enriched \a-Haloalkyl Grignard Reagents
;
_journal_coden_ASTM CEUJED
_journal_issue 18
_journal_name_full 'Chemistry - A European Journal'
_journal_page_first 3359
_journal_page_last 3365
_journal_paper_doi
10.1002/1521-3765(20000915)6:18<3359::AID-CHEM3359>3.0.CO;2-U
_journal_volume 6
_journal_year 2000
_chemical_formula_moiety 'C15 H15 Cl1 O1 S1'
_chemical_formula_sum 'C15 H15 Cl O S'
_chemical_melting_point 335.15
_chemical_name_systematic
'(S,R)-1-Chloro-2-phenylethyl p-tolyl sulfoxide'
_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 97.94(2)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 7.685(2)
_cell_length_b 5.006(1)
_cell_length_c 18.580(5)
_cell_volume 707.941
_diffrn_ambient_temperature 213
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.308
_exptl_crystal_description plate
_refine_ls_R_factor_gt 7.0
_refine_ls_wR_factor_gt 7.0
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C15 H15 Cl1 O1 S1'
_cod_database_code 1100177
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
S1 S 0.2866(3) 0.2971(6) 0.71160(15)
Cl1 Cl 0.2329(3) 0.6613(7) 0.82812(14)
O1 O 0.4166(8) 0.2423(14) 0.6607(4)
C1 C 0.3869(12) 0.557(2) 0.7720(5)
H1 H 0.41500 0.71090 0.74220
C2 C 0.5589(14) 0.451(3) 0.8142(7)
H2 H 0.63020 0.36730 0.78060
H3 H 0.53290 0.31520 0.84930
H4? H 0.53200 0.28770 0.83980
H5? H 0.63690 0.40010 0.77900
C3 C 0.665(6) 0.693(8) 0.8559(14)
C4 C 0.796(5) 0.822(8) 0.8237(15)
H6 H 0.81760 0.77260 0.77690
C5 C 0.895(4) 1.023(6) 0.8612(16)
H7 H 0.98080 1.11380 0.83890
C6 C 0.869(3) 1.093(6) 0.9328(13)
H8 H 0.93640 1.22750 0.95860
C7 C 0.747(3) 0.963(7) 0.9625(17)
H9 H 0.73030 1.00580 1.01030
C8 C 0.644(3) 0.770(7) 0.9272(12)
H10 H 0.55820 0.68670 0.95070
C9? C 0.650(5) 0.624(8) 0.8648(15)
C10? C 0.763(6) 0.815(9) 0.8412(18)
H11? H 0.77430 0.82720 0.79160
C11? C 0.857(4) 0.988(7) 0.8905(18)
H12? H 0.93330 1.11460 0.87430
C12? C 0.838(4) 0.974(8) 0.965(2)
H13? H 0.90390 1.08550 0.99930
C13? C 0.724(3) 0.800(8) 0.9855(15)
H14? H 0.70300 0.80140 1.03410
C14? C 0.638(3) 0.621(7) 0.9394(14)
H15? H 0.56730 0.49050 0.95780
C15 C 0.1093(13) 0.4811(19) 0.6641(5)
C16 C 0.1428(12) 0.692(2) 0.6166(5)
H16 H 0.25830 0.74230 0.61160
C17 C 0.0015(12) 0.821(2) 0.5784(5)
H17 H 0.02320 0.95960 0.54680
C18 C -0.1710(13) 0.756(2) 0.5840(5)
C19 C -0.1974(13) 0.545(2) 0.6308(6)
H18 H -0.31290 0.49540 0.63610
C20 C -0.0612(13) 0.411(2) 0.6686(6)
H19 H -0.08410 0.26800 0.69860
C21 C -0.3212(15) 0.894(3) 0.5417(7)
H20 H -0.41990 0.89450 0.56910
H21 H -0.35400 0.80170 0.49600
H22 H -0.28850 1.07650 0.53240
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
O 0.68
S 1.02
|
1100178.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 06:21:20 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176899 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100178.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_1100178
loop_
_publ_author_name
'Bromm, Lars O.'
'Laaziri, Hamid'
'Lhermitte, Fr\'ed\'eric'
'Harms, Klaus'
'Knochel, Paul'
_publ_section_title
;
Highly Regio- and Stereoselective Thermal Migration of Organoboranes
in Acyclic Molecules
;
_journal_coden_ASTM JACSAT
_journal_issue 41
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 10218
_journal_page_last 10219
_journal_paper_doi 10.1021/ja001283y
_journal_volume 122
_journal_year 2000
_chemical_formula_moiety 'C25 H24 N2 O6'
_chemical_formula_sum 'C25 H24 N2 O6'
_chemical_name_systematic
;
3-(Diphenylmethyl)pent-2-yl 3,5-dinitrobenzoate
;
_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 65.76(1)
_cell_angle_beta 86.43(1)
_cell_angle_gamma 81.31(1)
_cell_formula_units_Z 2
_cell_length_a 7.842(1)
_cell_length_b 12.127(1)
_cell_length_c 12.973(1)
_cell_volume 1112.044
_diffrn_ambient_temperature 223
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.339
_refine_ls_R_factor_gt 4.44
_refine_ls_wR_factor_gt 4.44
_cod_database_code 1100178
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 0.67355(19) -0.00061(14) 0.39666(13)
N2 N 0.6714(2) 0.05984(15) 0.00114(14)
O1 O 0.25526(14) 0.38044(10) 0.20579(9)
O2 O 0.27707(18) 0.42720(11) 0.01864(10)
O3 O 0.65453(19) 0.04898(14) 0.46234(11)
O4 O 0.7457(2) -0.10485(13) 0.41925(13)
O5 O 0.7800(3) -0.03065(16) 0.02690(15)
O6 O 0.6159(2) 0.11959(15) -0.09435(12)
C1 C -0.1238(2) 0.38201(13) 0.29096(12)
C2 C 0.0174(2) 0.45807(14) 0.29297(13)
C3 C 0.1322(2) 0.49107(14) 0.18682(13)
C4 C 0.3139(2) 0.36061(14) 0.11564(13)
C5 C 0.2390(3) 0.59290(17) 0.16584(17)
C6 C -0.0654(3) 0.57211(16) 0.31121(17)
C7 C -0.1927(3) 0.66030(18) 0.2194(2)
C8 C 0.43543(19) 0.24376(14) 0.14841(13)
C9 C 0.4929(2) 0.17618(14) 0.25873(13)
C10 C 0.6064(2) 0.06980(14) 0.28108(13)
C11 C 0.6642(2) 0.02816(15) 0.19956(15)
C12 C 0.6046(2) 0.09865(15) 0.09099(14)
C13 C 0.4916(2) 0.20532(14) 0.06320(13)
C14 C -0.2305(2) 0.34629(14) 0.39924(13)
C15 C -0.4094(2) 0.36766(18) 0.39265(18)
C16 C -0.5103(3) 0.3349(2) 0.4894(2)
C17 C -0.4337(3) 0.2804(2) 0.5946(2)
C18 C -0.2580(3) 0.25975(17) 0.60288(16)
C19 C -0.1564(2) 0.29257(15) 0.50641(14)
C20 C -0.05741(19) 0.27263(13) 0.26247(12)
C21 C 0.0244(2) 0.16286(14) 0.34190(13)
C22 C 0.0895(2) 0.06751(15) 0.31223(14)
C23 C 0.0751(2) 0.07918(15) 0.20220(14)
C24 C -0.0070(2) 0.18733(15) 0.12274(13)
C25 C -0.0740(2) 0.28275(14) 0.15271(13)
H1 H -0.20390 0.43740 0.22920
H2 H 0.09260 0.40690 0.35890
H3 H 0.06070 0.51140 0.11950
H4 H 0.32120 0.59720 0.10580
H5 H 0.30040 0.57640 0.23440
H6 H 0.16360 0.67000 0.14400
H7 H -0.12570 0.54550 0.38400
H8 H 0.02660 0.61630 0.31590
H9 H -0.22340 0.73530 0.23040
H10 H -0.29560 0.62310 0.22390
H11 H -0.13980 0.67850 0.14570
H12 H 0.45580 0.20190 0.31660
H13 H 0.74060 -0.04470 0.21690
H14 H 0.45530 0.25110 -0.01160
H15 H -0.46300 0.40500 0.32140
H16 H -0.63120 0.34990 0.48320
H17 H -0.50200 0.25770 0.66020
H18 H -0.20540 0.22300 0.67450
H19 H -0.03560 0.27830 0.51350
H20 H 0.03540 0.15350 0.41690
H21 H 0.14410 -0.00590 0.36710
H22 H 0.12040 0.01460 0.18190
H23 H -0.01750 0.19630 0.04780
H24 H -0.13130 0.35520 0.09810
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100179.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 06:21:20 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176899 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100179.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_1100179
loop_
_publ_author_name
'Bromm, Lars O.'
'Laaziri, Hamid'
'Lhermitte, Fr\'ed\'eric'
'Harms, Klaus'
'Knochel, Paul'
_publ_section_title
;
Highly Regio- and Stereoselective Thermal Migration of Organoboranes
in Acyclic Molecules
;
_journal_coden_ASTM JACSAT
_journal_issue 41
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 10218
_journal_page_last 10219
_journal_paper_doi 10.1021/ja001283y
_journal_volume 122
_journal_year 2000
_chemical_formula_moiety 'C18 H22 O1'
_chemical_formula_sum 'C18 H22 O'
_chemical_name_systematic 3,4-Diphenylhexan-2-ol
_space_group_IT_number 146
_symmetry_cell_setting rhombohedral
_symmetry_space_group_name_Hall 'R 3'
_symmetry_space_group_name_H-M 'R 3 :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 9
_cell_length_a 23.056(1)
_cell_length_b 23.056(1)
_cell_length_c 7.325(1)
_cell_volume 3372.145
_diffrn_ambient_temperature 223
_exptl_crystal_density_diffrn 1.127
_exptl_crystal_preparation colorless
_refine_ls_R_factor_gt 3.05
_refine_ls_wR_factor_gt 3.05
_cod_original_sg_symbol_H-M 'R 3'
_cod_original_formula_sum 'C18 H22 O1'
_cod_database_code 1100179
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 1/3+x,2/3+y,2/3+z
5 1/3-y,2/3+x-y,2/3+z
6 1/3-x+y,2/3-x,2/3+z
7 2/3+x,1/3+y,1/3+z
8 2/3-y,1/3+x-y,1/3+z
9 2/3-x+y,1/3-x,1/3+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O1 O 0.32062(8) 0.03022(7) 0.0072(2)
C1 C 0.24681(10) 0.08089(9) 0.2331(3)
C2 C 0.32137(9) 0.11919(9) 0.1919(3)
C3 C 0.47456(10) 0.23009(11) 0.2208(3)
C4 C 0.20208(10) 0.09816(11) 0.1573(3)
C5 C 0.15308(11) -0.01020(12) 0.3903(3)
C6 C 0.35142(10) 0.19578(10) 0.2173(3)
C7 C 0.42304(10) 0.2378(1) 0.1502(3)
C8 C 0.10989(11) 0.00814(12) 0.3153(3)
C9 C 0.50527(14) 0.32898(12) -0.0356(4)
C10 C 0.1345(11) 0.06227(12) 0.1985(3)
C11 C 0.43927(12) 0.28766(11) 0.0209(3)
C12 C 0.54013(11) 0.27133(13) 0.1639(3)
C13 C 0.22075(10) 0.02589(10) 0.3501(3)
C14 C 0.55529(11) 0.32055(12) 0.0362(4)
C15 C 0.33806(10) 0.0994(1) 0.0053(3)
C16 C 0.34730(12) 0.20976(12) 0.4225(3)
C17 C 0.37286(13) 0.28268(13) 0.4690(4)
C18 C 0.30359(14) 0.10812(13) -0.1600(3)
H1 H 0.34280 0.10520 0.28560
H2 H 0.46500 0.19660 0.30810
H3 H 0.21810 0.13480 0.07690
H4 H 0.13660 -0.04730 0.46900
H5 H 0.32320 0.20940 0.14840
H6 H 0.06400 -0.01600 0.34340
H7 H 0.51530 0.36260 -0.12290
H8 H 0.10510 0.07490 0.14650
H9 H 0.40510 0.29370 -0.02940
H10 H 0.57450 0.26550 0.21320
H11 H 0.24980 0.01300 0.40280
H12 H 0.59980 0.34830 -0.00170
H13 H 0.38700 0.12690 -0.01380
H14 H 0.30050 0.18340 0.46180
H15 H 0.37310 0.19420 0.49240
H16 H 0.36600 0.28670 0.59800
H17 H 0.34860 0.29920 0.39780
H18 H 0.42020 0.30880 0.44090
H19 H 0.32030 0.09800 -0.26990
H20 H 0.31270 0.15400 -0.16510
H21 H 0.25570 0.07790 -0.15070
H22 H 0.3364(19) 0.0237(17) 0.110(6)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
O 0.68
|
1100180.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 06:21:20 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176899 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100180.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_1100180
loop_
_publ_author_name
'Bromm, Lars O.'
'Laaziri, Hamid'
'Lhermitte, Fr\'ed\'eric'
'Harms, Klaus'
'Knochel, Paul'
_publ_section_title
;
Highly Regio- and Stereoselective Thermal Migration of Organoboranes
in Acyclic Molecules
;
_journal_coden_ASTM JACSAT
_journal_issue 41
_journal_name_full 'Journal of the American Chemical Society'
_journal_page_first 10218
_journal_page_last 10219
_journal_paper_doi 10.1021/ja001283y
_journal_volume 122
_journal_year 2000
_chemical_formula_moiety 'C17 H20 O1'
_chemical_formula_sum 'C17 H20 O'
_chemical_name_systematic 3,4-Diphenylpentan-2-ol
_space_group_IT_number 146
_symmetry_cell_setting rhombohedral
_symmetry_space_group_name_Hall 'R 3'
_symmetry_space_group_name_H-M 'R 3 :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 9
_cell_length_a 22.864(1)
_cell_length_b 22.864(1)
_cell_length_c 7.229(1)
_cell_volume 3272.753
_diffrn_ambient_temperature 223
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.097
_refine_ls_R_factor_gt 4.89
_refine_ls_wR_factor_gt 4.89
_cod_original_sg_symbol_H-M 'R 3'
_cod_original_formula_sum 'C17 H20 O1'
_cod_database_code 1100180
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 1/3+x,2/3+y,2/3+z
5 1/3-y,2/3+x-y,2/3+z
6 1/3-x+y,2/3-x,2/3+z
7 2/3+x,1/3+y,1/3+z
8 2/3-y,1/3+x-y,1/3+z
9 2/3-x+y,1/3-x,1/3+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O1 O 0.63588(8) 0.62161(9) -0.1401(2)
C1 C 0.55920(18) 0.53035(16) -0.3253(4)
C2 C 0.56643(13) 0.57092(13) -0.1527(3)
C3 C 0.54211(12) 0.52938(13) 0.0290(3)
C4 C 0.46503(13) 0.48022(14) 0.0339(4)
C5 C 0.44245(18) 0.4494(2) 0.2283(6)
C6 C 0.42352(12) 0.51215(14) -0.0229(3)
C7 C 0.37278(15) 0.48114(15) -0.1543(4)
C8 C 0.33227(15) 0.50865(17) -0.2026(5)
C9 C 0.34226(14) 0.56660(16) -0.1213(4)
C10 C 0.39241(16) 0.59802(16) 0.0107(4)
C11 C 0.43204(14) 0.57069(15) 0.0597(4)
C12 C 0.58234(12) 0.49467(12) 0.0729(3)
C13 C 0.63620(14) 0.52449(14) 0.1968(4)
C14 C 0.67470(15) 0.49503(15) 0.2375(4)
C15 C 0.65927(15) 0.43404(14) 0.1583(4)
C16 C 0.60629(16) 0.40359(14) 0.0356(4)
C17 C 0.56785(15) 0.43355(14) -0.0066(4)
H1 H 0.644(2) 0.643(2) -0.026(6)
H2 H 0.512(2) 0.488(2) -0.334(6)
H3 H 0.5769(16) 0.5612(16) -0.440(5)
H4 H 0.5921(14) 0.5096(14) -0.316(4)
H5 H 0.5416(14) 0.5946(13) -0.172(3)
H6 H 0.5526(15) 0.5605(16) 0.124(4)
H7 H 0.4558(13) 0.4442(14) -0.064(4)
H8 H 0.4682(17) 0.4265(17) 0.254(4)
H9 H 0.390(2) 0.4170(18) 0.241(5)
H10 H 0.458(3) 0.491(3) 0.322(9)
H11 H 0.3640(17) 0.4393(18) -0.225(5)
H12 H 0.300(2) 0.484(2) -0.293(6)
H13 H 0.3161(16) 0.5890(16) -0.152(4)
H14 H 0.3967(19) 0.637(2) 0.066(6)
H15 H 0.4671(17) 0.5887(16) 0.155(5)
H16 H 0.6463(16) 0.5683(19) 0.259(5)
H17 H 0.7137(17) 0.5143(17) 0.324(4)
H18 H 0.6998(18) 0.4244(17) 0.195(4)
H19 H 0.5961(13) 0.3599(13) -0.015(4)
H20 H 0.5334(18) 0.4103(16) -0.086(5)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
O 0.68
|
1100181.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-25 13:50:25 +0200 (Thu, 25 Feb 2016) $
#$Revision: 176964 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100181.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_1100181
loop_
_publ_author_name
'Gr\"ob, Thorsten'
'Harms, Klaus'
'Dehnicke, Kurt'
_publ_section_title
;
Kristallstruktur des Isothiocyanato-Komplexes
[Ph~3~PNH~2~(OEt~2~)][Sm(NCS)~4~(DME)~2~]
;
_journal_coden_ASTM ZAACAB
_journal_issue 2
_journal_name_full
;
Zeitschrift fuer Anorganische und Allgemeine Chemie
;
_journal_page_first 125
_journal_page_last 127
_journal_paper_doi
10.1002/1521-3749(200102)627:2<125::AID-ZAAC125>3.0.CO;2-O
_journal_volume 627
_journal_year 2001
_chemical_formula_moiety
;
C18 H17 N1 P1 1+,C12 H20 N4 O4 S4 Sm1 1-,C4 H10 O1
;
_chemical_formula_sum 'C34 H47 N5 O5 P S4 Sm'
_chemical_name_systematic
;
Amino-triphenylphosphonium tetrakis(isothiocyanato)-bis(1,2-dimethoxyethane-O,
O')-samarium(iii) diethyl ether solvate
;
_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 96.748(10)
_cell_angle_beta 94.827(10)
_cell_angle_gamma 91.720(11)
_cell_formula_units_Z 4
_cell_length_a 9.1900(8)
_cell_length_b 19.6516(18)
_cell_length_c 24.0125(19)
_cell_volume 4287.808
_diffrn_ambient_temperature 193
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.418
_exptl_crystal_description nugget
_exptl_crystal_preparation 'dimethoxyethane/diethyl ether'
_refine_ls_R_factor_gt 2.91
_refine_ls_wR_factor_gt 2.91
_cod_original_formula_sum 'C34 H47 N5 O5 P1 S4 Sm1'
_cod_database_code 1100181
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 0.97459(2) 0.02011(1) 0.28191(1)
S1 S 0.59007(13) -0.16116(7) 0.19309(6)
S2 S 0.98813(12) 0.03528(6) 0.06909(5)
S3 S 1.00715(18) 0.28291(7) 0.33377(7)
S4 S 1.36087(12) 0.01343(7) 0.45242(5)
N1 N 0.8062(4) -0.07902(19) 0.25822(18)
N2 N 0.9406(4) 0.0239(2) 0.18073(17)
N3 N 1.0085(4) 0.1420(2) 0.30778(18)
N4 N 1.1441(4) 0.0178(2) 0.36452(17)
O1 O 0.8200(3) 0.02090(17) 0.36431(13)
O2 O 0.7258(3) 0.07227(16) 0.26709(15)
O3 O 1.2228(3) 0.04801(16) 0.24679(13)
O4 O 1.1313(3) -0.08111(15) 0.26402(15)
C1 C 0.7152(4) -0.1127(2) 0.2311(2)
C2 C 0.9590(4) 0.0290(2) 0.1339(2)
C3 C 1.0073(4) 0.2009(3) 0.3189(2)
C4 C 1.2351(4) 0.0158(2) 0.4009(2)
C5 C 0.6678(5) 0.0317(3) 0.3514(2)
H1 H 0.62000 0.04270 0.38670
H2 H 0.61920 -0.01050 0.33050
C6 C 0.6544(5) 0.0890(3) 0.3170(3)
H3 H 0.55000 0.09680 0.30710
H4 H 0.69990 0.13150 0.33850
C7 C 0.8400(6) -0.0281(4) 0.4038(3)
H5 H 0.79630 -0.01160 0.43850
H6 H 0.94470 -0.03390 0.41240
H7 H 0.79270 -0.07210 0.38760
C8 C 0.7026(5) 0.1222(3) 0.2288(3)
H8 H 0.60100 0.11800 0.21240
H9 H 0.76830 0.11450 0.19880
H10 H 0.72250 0.16830 0.24910
C9 C 1.2929(5) -0.0111(3) 0.2223(3)
H11 H 1.39660 0.00080 0.21820
H12 H 1.24420 -0.02720 0.18450
C10 C 1.2837(5) -0.0657(3) 0.2592(3)
H13 H 1.33110 -0.10710 0.24300
H14 H 1.33420 -0.05010 0.29680
C11 C 1.2448(5) 0.1060(3) 0.2163(2)
H15 H 1.34770 0.12180 0.22210
H16 H 1.18330 0.14320 0.22990
H17 H 1.21830 0.09240 0.17600
C12 C 1.1136(6) -0.1390(3) 0.2943(3)
H18 H 1.15540 -0.17910 0.27420
H19 H 1.00940 -0.14840 0.29720
H20 H 1.16410 -0.12910 0.33210
Sm2 Sm 0.46987(2) 0.48820(1) 0.78098(1)
S5 S 0.08010(12) 0.29493(6) 0.71506(6)
S6 S 0.51644(13) 0.49801(7) 0.57011(5)
S7 S 0.50041(17) 0.74988(7) 0.81604(8)
S8 S 0.85923(13) 0.48314(8) 0.94828(6)
N5 N 0.2845(4) 0.3956(2) 0.76479(18)
N6 N 0.4500(4) 0.4787(2) 0.67857(17)
N7 N 0.5239(4) 0.6097(2) 0.79998(19)
N8 N 0.6286(4) 0.4859(2) 0.86702(17)
O5 O 0.3061(3) 0.50774(16) 0.86077(13)
O6 O 0.2350(3) 0.54922(15) 0.75716(14)
O7 O 0.7269(3) 0.50429(18) 0.74764(14)
O8 O 0.6102(3) 0.38038(17) 0.76967(16)
C13 C 0.1984(4) 0.3545(2) 0.74404(19)
C14 C 0.4772(4) 0.4862(2) 0.6329(2)
C15 C 0.5140(5) 0.6681(3) 0.8069(2)
C16 C 0.7246(5) 0.4844(2) 0.9006(2)
C17 C 0.1585(5) 0.5240(3) 0.8445(3)
H21 H 0.10980 0.54220 0.87800
H22 H 0.10280 0.48230 0.82610
C18 C 0.1632(5) 0.5759(3) 0.8050(3)
H23 H 0.06250 0.58800 0.79280
H24 H 0.21650 0.61800 0.82380
C19 C 0.3117(6) 0.4634(3) 0.9045(2)
H25 H 0.26850 0.48600 0.93740
H26 H 0.41370 0.45370 0.91500
H27 H 0.25670 0.42040 0.89070
C20 C 0.2251(5) 0.5951(3) 0.7149(3)
H28 H 0.12270 0.59760 0.70040
H29 H 0.28290 0.57820 0.68400
H30 H 0.26290 0.64090 0.73140
C21 C 0.7886(6) 0.4406(3) 0.7273(3)
H31 H 0.89460 0.44790 0.72430
H32 H 0.74170 0.42350 0.68940
C22 C 0.7650(6) 0.3897(3) 0.7665(3)
H33 H 0.80670 0.34560 0.75280
H34 H 0.81370 0.40610 0.80420
C23 C 0.7613(6) 0.5582(3) 0.7147(3)
H35 H 0.86680 0.56870 0.71950
H36 H 0.70930 0.59920 0.72720
H37 H 0.73120 0.54330 0.67490
C24 C 0.5816(7) 0.3246(3) 0.8011(3)
H38 H 0.61440 0.28200 0.78140
H39 H 0.47650 0.32010 0.80490
H40 H 0.63440 0.33350 0.83860
P1 P 0.78252(10) 0.22069(6) 0.01060(5)
N9 N 0.7228(5) 0.1457(2) 0.02094(18)
H41 H 0.768(5) 0.120(2) 0.029(2)
H42 H 0.628(6) 0.124(3) 0.005(2)
C25 C 0.9048(4) 0.2527(2) 0.07014(18)
C26 C 1.0195(5) 0.3002(3) 0.0667(2)
H43 H 1.03250 0.31780 0.03210
C27 C 1.1144(5) 0.3215(3) 0.1144(3)
H44 H 1.19170 0.35410 0.11230
C28 C 1.0976(5) 0.2963(3) 0.1639(2)
H45 H 1.16490 0.31030 0.19570
C29 C 0.9852(6) 0.2510(3) 0.1684(2)
H46 H 0.97320 0.23440 0.20330
C30 C 0.8879(5) 0.2293(2) 0.1216(2)
H47 H 0.80910 0.19800 0.12500
C31 C 0.6274(4) 0.2726(2) 0.00319(19)
C32 C 0.5976(5) 0.3235(2) 0.0452(2)
H48 H 0.66440 0.33370 0.07770
C33 C 0.4707(5) 0.3599(2) 0.0401(2)
H49 H 0.45140 0.39500 0.06890
C34 C 0.3736(5) 0.3449(2) -0.0065(2)
H50 H 0.28650 0.36950 -0.00980
C35 C 0.4015(4) 0.2945(3) -0.0484(2)
H51 H 0.33360 0.28440 -0.08060
C36 C 0.5281(4) 0.2581(2) -0.0440(2)
H52 H 0.54690 0.22330 -0.07320
C37 C 0.8754(4) 0.2213(2) -0.05183(18)
C38 C 0.9342(4) 0.1619(2) -0.0759(2)
H53 H 0.92030 0.12020 -0.06030
C39 C 1.0123(5) 0.1627(3) -0.1221(2)
H54 H 1.05290 0.12180 -0.13810
C40 C 1.0319(5) 0.2229(3) -0.1453(2)
H55 H 1.08570 0.22340 -0.17730
C41 C 0.9739(5) 0.2825(3) -0.1222(2)
H56 H 0.98740 0.32390 -0.13830
C42 C 0.8956(5) 0.2819(3) -0.0753(2)
H57 H 0.85590 0.32300 -0.05910
P2 P 0.69272(10) 0.28023(6) 0.51145(5)
N10 N 0.7400(5) 0.3603(2) 0.5230(2)
H58 H 0.672(5) 0.393(2) 0.525(2)
H59 H 0.820(5) 0.371(2) 0.5271(19)
C43 C 0.5807(4) 0.2614(2) 0.44667(19)
C44 C 0.4752(4) 0.2081(2) 0.4376(2)
H60 H 0.46210 0.17960 0.46630
C45 C 0.3895(5) 0.1963(3) 0.3872(2)
H61 H 0.31730 0.15990 0.38150
C46 C 0.4075(5) 0.2364(3) 0.3454(2)
H62 H 0.34810 0.22790 0.31070
C47 C 0.5111(6) 0.2887(3) 0.3534(3)
H63 H 0.52370 0.31640 0.32430
C48 C 0.5976(5) 0.3015(3) 0.4037(2)
H64 H 0.66920 0.33810 0.40880
C49 C 0.8568(4) 0.2340(2) 0.51012(19)
C50 C 0.8929(5) 0.1939(2) 0.4627(2)
H65 H 0.82950 0.19050 0.42900
C51 C 1.0208(5) 0.1588(3) 0.4638(2)
H66 H 1.04510 0.13130 0.43090
C52 C 1.1135(5) 0.1637(2) 0.5125(2)
H67 H 1.20130 0.13930 0.51320
C53 C 1.0788(5) 0.2040(2) 0.5603(2)
H68 H 1.14270 0.20770 0.59380
C54 C 0.9506(4) 0.2388(2) 0.5590(2)
H69 H 0.92630 0.26630 0.59190
C55 C 0.5944(4) 0.2541(2) 0.56711(19)
C56 C 0.5249(5) 0.3023(3) 0.6013(2)
H70 H 0.52970 0.34930 0.59550
C57 C 0.4485(5) 0.2812(3) 0.6440(2)
H71 H 0.40150 0.31420 0.66770
C58 C 0.4395(5) 0.2132(3) 0.6526(2)
H72 H 0.38640 0.19950 0.68190
C59 C 0.5072(5) 0.1655(3) 0.6188(2)
H73 H 0.50010 0.11850 0.62440
C60 C 0.5860(4) 0.1854(2) 0.5764(2)
H74 H 0.63460 0.15220 0.55350
O9 O 0.4349(3) 0.09409(17) -0.01937(15)
C61 C 0.3022(6) 0.1183(3) -0.0009(3)
H75 H 0.23460 0.07890 0.00180
H76 H 0.25610 0.14630 -0.02880
C62 C 0.3264(6) 0.1603(3) 0.0546(3)
H77 H 0.23210 0.17360 0.06770
H78 H 0.38610 0.20150 0.05120
H79 H 0.37710 0.13350 0.08160
C63 C 0.4119(6) 0.0452(3) -0.0697(3)
H80 H 0.35450 0.06600 -0.09970
H81 H 0.35630 0.00410 -0.06160
C64 C 0.5539(7) 0.0254(3) -0.0888(3)
H82 H 0.53960 -0.01400 -0.11810
H83 H 0.61710 0.01290 -0.05690
H84 H 0.59980 0.06400 -0.10410
O10 O 1.0336(3) 0.40605(18) 0.52367(15)
C65 C 1.1228(6) 0.4338(4) 0.5726(3)
H85 H 1.17150 0.47740 0.56580
H86 H 1.19940 0.40140 0.58150
C66 C 1.0328(6) 0.4464(3) 0.6200(2)
H87 H 1.09480 0.46540 0.65380
H88 H 0.98550 0.40310 0.62670
H89 H 0.95810 0.47900 0.61130
C67 C 1.1079(6) 0.4028(3) 0.4733(2)
H90 H 1.15210 0.44860 0.47030
H91 H 1.03570 0.39080 0.44030
C68 C 1.2225(6) 0.3526(3) 0.4716(3)
H92 H 1.26300 0.34940 0.43490
H93 H 1.18100 0.30770 0.47720
H94 H 1.30030 0.36710 0.50150
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
P 1.05
S 1.02
Sm 1.80
|
1100182.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-04 12:18:45 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177462 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100182.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_1100182
loop_
_publ_author_name
'Bach, Thorsten'
'Schlummer, Bj\"orn'
'Harms, Klaus'
_publ_section_title
;
Iron(II)-catalyzed intramolecular aminochlorination of alkenes
;
_journal_coden_ASTM CHCOFS
_journal_issue 4
_journal_name_full
;
Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first 287
_journal_page_last 288
_journal_paper_doi 10.1039/a909009f
_journal_year 2000
_chemical_formula_moiety 'C10 H10 Cl1 N1 O2'
_chemical_formula_sum 'C10 H10 Cl N O2'
_chemical_name_systematic
;
threo-4-(Chloro(phenyl)methyl)-1,3-oxazolidin-2-one
;
_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 94.175(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.8902(2)
_cell_length_b 5.8375(3)
_cell_length_c 20.5524(7)
_cell_volume 944.112
_diffrn_ambient_temperature 213
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.489
_exptl_crystal_description plate
_refine_ls_R_factor_gt 4.59
_refine_ls_wR_factor_gt 4.59
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_original_formula_sum 'C10 H10 Cl1 N1 O2'
_cod_database_code 1100182
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 0.51420(6) 0.37874(10) 0.91426(3)
O1 O 0.90458(19) 0.3620(3) 1.06105(7)
N1 N 0.88553(19) 0.2441(4) 0.95366(8)
C1 C 0.8494(2) 0.2388(4) 1.01657(9)
O2 O 0.74148(17) 0.0648(3) 1.02684(6)
C2 C 0.7122(3) -0.0645(4) 0.96675(10)
C3 C 0.7841(2) 0.0859(4) 0.91370(9)
C4 C 0.6434(2) 0.1948(4) 0.86765(9)
C5 C 0.7028(2) 0.3185(4) 0.80906(9)
C6 C 0.6672(2) 0.2221(4) 0.74783(10)
C7 C 0.7180(3) 0.3322(5) 0.69242(11)
C8 C 0.8020(2) 0.5390(5) 0.69764(11)
C9 C 0.8403(3) 0.6349(5) 0.75884(12)
C10 C 0.7906(3) 0.5255(4) 0.81417(11)
H1 H 0.950(4) 0.362(5) 0.9416(14)
H2 H 0.585(3) -0.092(4) 0.9572(11)
H3 H 0.773(3) -0.214(5) 0.9734(10)
H4 H 0.859(3) -0.001(4) 0.8867(10)
H5 H 0.569(3) 0.060(4) 0.8530(11)
H6 H 0.597(3) 0.077(5) 0.7429(12)
H7 H 0.703(3) 0.263(5) 0.6532(13)
H8 H 0.831(3) 0.611(5) 0.6617(14)
H9 H 0.902(3) 0.780(5) 0.7617(11)
H10 H 0.820(3) 0.590(5) 0.8578(14)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
N 0.68
O 0.68
|
1100183.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100183.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_1100183
loop_
_publ_author_name
T.Bach
H.Bergmann
K.Harms
_journal_name_full Angew.Chem.,Int.Ed.Engl.
_journal_page_first 2302
_journal_paper_doi
10.1002/1521-3773(20000703)39:13<2302::AID-ANIE2302>3.0.CO;2-6
_journal_volume 39
_journal_year 2000
_chemical_formula_moiety
;
C22 H37 N1 O3,C1 H2 Cl2
;
_chemical_formula_sum 'C23 H39 Cl2 N O3'
_chemical_name_systematic
;
Menthan-7-yl 2,4,7-trimethyl-2,4-trimethylene-5-pentane lactam-7-carboxylate d
ichloromethane solvate
;
_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 8.520(1)
_cell_length_b 12.123(1)
_cell_length_c 24.105(1)
_cell_volume 2489.756
_diffrn_ambient_temperature ?
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.196
_exptl_crystal_description Regular
_refine_ls_R_factor_gt 6.08
_refine_ls_wR_factor_gt 6.08
_cod_original_formula_sum 'C23 H39 Cl2 N1 O3'
_cod_database_code 1100183
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
Cl1 Cl 0.7129(3) 0.06368(17) 0.12892(10)
O1 O 0.0731(5) 0.2762(3) 0.02385(18)
C1 C 0.1525(7) 0.3614(4) 0.0277(2)
Cl2 Cl 0.8022(2) 0.26518(16) 0.18279(7)
N1 N 0.3080(6) 0.3602(3) 0.02144(17)
C2 C 0.4147(7) 0.4538(4) 0.0183(2)
H1 H 0.44680 0.46390 -0.02000
H2 H 0.50800 0.43740 0.03980
C3 C 0.3427(6) 0.5610(4) 0.0395(2)
C4 C 0.1747(7) 0.5669(4) 0.0192(2)
H3 H 0.17280 0.56290 -0.02100
H4 H 0.12850 0.63670 0.03020
C5 C 0.0786(6) 0.4719(4) 0.0434(2)
C6 C 0.0757(6) 0.4826(4) 0.1066(2)
H5 H 0.02120 0.41910 0.12160
H6 H 0.01450 0.54740 0.11610
C7 C 0.2352(5) 0.4917(3) 0.13543(18)
C8 C 0.3442(6) 0.5699(4) 0.10298(19)
H7 H 0.31690 0.64500 0.11290
H8 H 0.45080 0.55720 0.11560
C9 C -0.0905(7) 0.4746(5) 0.0216(3)
H9 H -0.08990 0.46770 -0.01800
H10 H -0.13870 0.54330 0.03180
H11 H -0.14880 0.41470 0.03750
C10 C 0.2105(8) 0.5388(4) 0.1945(2)
H12 H 0.13350 0.49530 0.21370
H13 H 0.17470 0.61370 0.19190
H14 H 0.30790 0.53650 0.21440
C11 C 0.4404(9) 0.6575(5) 0.0167(3)
H15 H 0.43320 0.65870 -0.02310
H16 H 0.54810 0.64840 0.02750
H17 H 0.40100 0.72570 0.03140
O2 O 0.4530(4) 0.3640(3) 0.13972(17)
C12 C 0.3164(6) 0.3808(4) 0.14475(18)
O3 O 0.2149(4) 0.3064(2) 0.16446(14)
C13 C 0.2707(6) 0.1980(3) 0.1809(2)
H18 H 0.38570 0.19780 0.18040
C14 C 0.2114(8) 0.1162(4) 0.1389(2)
H19 H 0.25440 0.13410 0.10270
H20 H 0.09800 0.12140 0.13650
C15 C 0.2574(7) -0.0023(4) 0.1543(2)
H21 H 0.37210 -0.00850 0.15320
C16 C 0.2022(8) -0.0262(4) 0.2130(2)
H22 H 0.08840 -0.02530 0.21380
H23 H 0.23670 -0.09940 0.22360
C17 C 0.2643(7) 0.0570(4) 0.2547(2)
H24 H 0.37800 0.05270 0.25580
H25 H 0.22490 0.03880 0.29130
C18 C 0.2146(6) 0.1754(4) 0.23965(19)
H26 H 0.09960 0.17640 0.23880
C19 C 0.1883(9) -0.0844(5) 0.1135(2)
H27 H 0.21910 -0.15770 0.12380
H28 H 0.22610 -0.06840 0.07690
H29 H 0.07590 -0.07890 0.11400
C20 C 0.2663(6) 0.2630(4) 0.2819(2)
H30 H 0.22630 0.33380 0.26830
C21 C 0.4432(7) 0.2761(6) 0.2880(3)
H31 H 0.46540 0.32430 0.31860
H32 H 0.48570 0.30710 0.25460
H33 H 0.48990 0.20530 0.29470
C22 C 0.1912(10) 0.2440(6) 0.3382(3)
H34 H 0.20780 0.30760 0.36120
H35 H 0.23790 0.18050 0.35540
H36 H 0.08060 0.23190 0.33360
C23 C 0.7525(8) 0.2036(5) 0.1206(2)
H37 H 0.83810 0.21260 0.09450
H38 H 0.66070 0.23990 0.10540
H39 H 0.332(5) 0.294(4) 0.0149(16)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
N 0.68
O 0.68
|
1100184.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100184.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_1100184
loop_
_publ_author_name
T.Grob
G.Seybert
W.Massa
K.Harms
K.Dehnicke
_journal_name_full Z.Anorg.Allg.Chem.
_journal_page_first 1361
_journal_paper_doi
10.1002/(SICI)1521-3749(200006)626:6<1361::AID-ZAAC1361>3.0.CO;2-X
_journal_volume 626
_journal_year 2000
_chemical_formula_moiety
;
C12 H30 Eu1 I2 O6
;
_chemical_formula_sum 'C12 H30 Eu I2 O6'
_chemical_name_systematic
;
Di-iodo-tris(dimethoxyethane)-europium
;
_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 93.793(6)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 8.4889(8)
_cell_length_b 10.5945(8)
_cell_length_c 12.2789(7)
_cell_volume 1101.892
_diffrn_ambient_temperature 188
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 2.038
_exptl_crystal_description 'triangular platelet'
_refine_ls_R_factor_gt 2.46
_refine_ls_wR_factor_gt 2.46
_cod_original_sg_symbol_H-M 'P 21'
_cod_original_formula_sum 'C12 H30 Eu1 I2 O6'
_cod_database_code 1100184
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
Eu1 Eu 0.14493(2) 0.99983(2) 0.25875(2)
I1 I 0.31186(5) 0.98191(4) 0.51256(3)
I2 I -0.14107(4) 0.99037(5) 0.05505(3)
O1 O 0.3252(6) 0.7986(5) 0.2284(4)
O2 O 0.3048(5) 0.9832(5) 0.0820(3)
O3 O 0.3833(5) 1.1607(5) 0.2543(4)
O4 O 0.0880(5) 1.2449(4) 0.2601(4)
O5 O -0.0968(5) 1.0313(4) 0.3843(3)
O6 O -0.0187(5) 0.7932(4) 0.3026(4)
C1 C 0.381(1) 0.7124(8) 0.3097(6)
H1 H 0.44550 0.64770 0.27710
H2 H 0.29100 0.67220 0.34200
H3 H 0.44500 0.75750 0.36660
C2 C 0.3985(9) 0.7791(8) 0.1294(6)
H4 H 0.39190 0.68880 0.10870
H5 H 0.51140 0.80290 0.13870
C3 C 0.3172(12) 0.8576(10) 0.0428(6)
H6 H 0.37780 0.85680 -0.02340
H7 H 0.21060 0.82310 0.02330
C4 C 0.2898(13) 1.0789(11) 0.0020(8)
H8 H 0.35730 1.05890 -0.05750
H9 H 0.32230 1.15990 0.03480
H10 H 0.17960 1.08430 -0.02690
C5 C 0.5420(9) 1.1139(11) 0.2707(9)
H11 H 0.61650 1.18430 0.26740
H12 H 0.56190 1.05250 0.21350
H13 H 0.55590 1.07310 0.34230
C6 C 0.3570(12) 1.2732(8) 0.3130(8)
H14 H 0.44860 1.33050 0.30980
H15 H 0.34250 1.25340 0.39050
C7 C 0.2111(8) 1.3349(6) 0.2616(6)
H16 H 0.18320 1.40980 0.30450
H17 H 0.22910 1.36240 0.18640
C8 C -0.0612(10) 1.3017(7) 0.2202(8)
H18 H -0.05440 1.39360 0.22810
H19 H -0.14640 1.26960 0.26270
H20 H -0.08320 1.28000 0.14310
C9 C -0.1001(10) 1.1335(7) 0.4631(6)
H21 H -0.19770 1.12860 0.50130
H22 H -0.09580 1.21460 0.42510
H23 H -0.00900 1.12610 0.51610
C10 C -0.1532(8) 0.9182(6) 0.4292(5)
H24 H -0.25690 0.93340 0.45930
H25 H -0.07850 0.88890 0.48930
C11 C -0.1691(7) 0.8204(6) 0.3424(6)
H26 H -0.21430 0.74250 0.37210
H27 H -0.24190 0.85080 0.28170
C12 C -0.0279(11) 0.6899(7) 0.2263(7)
H28 H -0.09210 0.62210 0.25470
H29 H 0.07850 0.65820 0.21610
H30 H -0.07650 0.71910 0.15620
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Eu 1.99
I 1.40
O 0.68
|
1100185.cif | #------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100185.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_1100185
loop_
_publ_author_name
T.Grob
G.Seybert
W.Massa
K.Harms
K.Dehnicke
_journal_name_full Z.Anorg.Allg.Chem.
_journal_page_first 1361
_journal_paper_doi
10.1002/(SICI)1521-3749(200006)626:6<1361::AID-ZAAC1361>3.0.CO;2-X
_journal_volume 626
_journal_year 2000
_chemical_formula_moiety
;
C94 H85 Eu2 I1 N5 O2 P5,2(C4 H10 O2)
;
_chemical_formula_sum 'C102 H105 Eu2 I N5 O6 P5'
_chemical_name_systematic
;
bis(\m~2~-Triphenylphosphoraneiminato)-iodo-tris(triphenylphosphoraneiminato)-
dimethoxyethane-di-europium dimethoxyethane solvate
;
_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 89.404(11)
_cell_angle_beta 72.958(11)
_cell_angle_gamma 78.657(11)
_cell_formula_units_Z 2
_cell_length_a 14.0550(14)
_cell_length_b 16.5220(15)
_cell_length_c 22.037(2)
_cell_volume 4790.995
_diffrn_ambient_temperature 193
_exptl_crystal_colour light-yellow.
_exptl_crystal_density_diffrn 1.444
_exptl_crystal_description 'triangular platelet'
_refine_ls_R_factor_gt 3.91
_refine_ls_wR_factor_gt 3.91
_cod_original_formula_sum 'C102 H105 Eu2 I1 N5 O6 P5'
_cod_database_code 1100185
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
Eu1 Eu 0.51706(2) 0.76670(2) 0.23415(2)
Eu2 Eu 0.40631(2) 0.97301(2) 0.20082(2)
I1 I 0.51288(3) 1.11919(3) 0.13308(2)
O1 O 0.4620(4) 0.9159(4) 0.0842(2)
O2 O 0.2891(3) 1.0298(3) 0.1365(3)
N1 N 0.5554(3) 0.9004(3) 0.2220(2)
N2 N 0.3632(3) 0.8400(3) 0.2203(2)
N3 N 0.4942(4) 0.7056(3) 0.3252(3)
N4 N 0.6186(4) 0.6841(4) 0.1555(3)
N5 N 0.3060(4) 1.0454(3) 0.2860(3)
P1 P 0.66254(11) 0.91934(11) 0.21584(8)
P2 P 0.25735(11) 0.81487(10) 0.23827(8)
P3 P 0.49604(12) 0.63976(11) 0.37473(8)
P4 P 0.67903(12) 0.60995(12) 0.10954(9)
P5 P 0.24330(11) 1.09806(11) 0.34743(9)
C1 C 0.5368(8) 0.8434(7) 0.0617(4)
H1 H 0.54640 0.83290 0.01640
H2 H 0.51470 0.79640 0.08540
H3 H 0.60110 0.85040 0.06780
C2 C 0.3800(7) 0.9229(9) 0.0576(4)
H4 H 0.33500 0.88480 0.07780
H5 H 0.40620 0.90850 0.01140
C3 C 0.3229(7) 1.0097(9) 0.0694(5)
H6 H 0.36730 1.04730 0.04730
H7 H 0.26380 1.01660 0.05280
C4 C 0.2312(6) 1.1123(6) 0.1520(6)
H8 H 0.18910 1.12630 0.12350
H9 H 0.27740 1.15090 0.14720
H10 H 0.18740 1.11630 0.19610
C5 C 0.6618(4) 1.0112(4) 0.2594(3)
C6 C 0.7507(5) 1.0308(5) 0.2664(4)
H11 H 0.81410 0.99580 0.24560
C7 C 0.7498(6) 1.0978(6) 0.3020(4)
H12 H 0.81180 1.10940 0.30510
C8 C 0.6589(6) 1.1490(5) 0.3335(4)
H13 H 0.65720 1.19570 0.35890
C9 C 0.5700(6) 1.1308(5) 0.3273(4)
H14 H 0.50680 1.16600 0.34820
C10 C 0.5714(5) 1.0634(5) 0.2918(4)
H15 H 0.50910 1.05190 0.28910
C11 C 0.7443(4) 0.9252(4) 0.1356(3)
C12 C 0.7797(4) 0.9968(5) 0.1133(3)
H16 H 0.75900 1.04600 0.13980
C13 C 0.8456(5) 0.9955(6) 0.0517(4)
H17 H 0.86830 1.04450 0.03640
C14 C 0.8776(5) 0.9259(6) 0.0135(4)
H18 H 0.92400 0.92550 -0.02770
C15 C 0.8423(5) 0.8557(5) 0.0350(4)
H19 H 0.86360 0.80700 0.00800
C16 C 0.7758(5) 0.8552(5) 0.0960(3)
H20 H 0.75210 0.80620 0.11020
C17 C 0.7436(4) 0.8426(4) 0.2479(3)
C18 C 0.8502(4) 0.8224(4) 0.2218(3)
H21 H 0.88150 0.84690 0.18390
C19 C 0.9103(5) 0.7678(5) 0.2502(4)
H22 H 0.98190 0.75470 0.23150
C20 C 0.8667(6) 0.7329(5) 0.3049(4)
H23 H 0.90820 0.69650 0.32490
C21 C 0.7616(6) 0.7502(5) 0.3319(4)
H24 H 0.73150 0.72460 0.36950
C22 C 0.7007(5) 0.8050(5) 0.3037(3)
H25 H 0.62910 0.81710 0.32260
C23 C 0.1637(4) 0.8784(4) 0.2072(3)
C24 C 0.1412(5) 0.8554(5) 0.1533(3)
H26 H 0.17310 0.80290 0.13220
C25 C 0.0713(5) 0.9096(5) 0.1299(4)
H27 H 0.05680 0.89370 0.09280
C26 C 0.0243(5) 0.9844(5) 0.1597(4)
H28 H -0.02270 1.02060 0.14340
C27 C 0.0448(4) 1.0083(5) 0.2138(4)
H29 H 0.01160 1.06050 0.23500
C28 C 0.1141(4) 0.9552(4) 0.2370(3)
H30 H 0.12800 0.97190 0.27410
C29 C 0.1897(4) 0.8173(4) 0.3224(3)
C30 C 0.0855(4) 0.8178(4) 0.3448(3)
H31 H 0.04750 0.82130 0.31530
C31 C 0.0371(5) 0.8134(5) 0.4079(4)
H32 H -0.03310 0.81170 0.42160
C32 C 0.0904(6) 0.8113(5) 0.4522(4)
H33 H 0.05650 0.80950 0.49620
C33 C 0.1929(5) 0.8120(4) 0.4317(3)
H34 H 0.22970 0.81080 0.46180
C34 C 0.2424(4) 0.8143(4) 0.3676(3)
H35 H 0.31320 0.81400 0.35400
C35 C 0.2646(4) 0.7102(4) 0.2104(3)
C36 C 0.3405(5) 0.6770(5) 0.1542(4)
H36 H 0.38850 0.70870 0.13270
C37 C 0.3462(6) 0.5994(6) 0.1302(5)
H37 H 0.39960 0.57750 0.09310
C38 C 0.2769(6) 0.5529(5) 0.1584(5)
H38 H 0.27990 0.50040 0.13990
C39 C 0.2025(6) 0.5829(5) 0.2139(5)
H39 H 0.15590 0.54960 0.23470
C40 C 0.1947(5) 0.6608(4) 0.2397(4)
H40 H 0.14190 0.68110 0.27750
C41 C 0.5746(5) 0.5384(5) 0.3462(3)
C42 C 0.6687(5) 0.5327(6) 0.3009(4)
H41 H 0.69080 0.58180 0.28540
C43 C 0.7303(5) 0.4571(6) 0.2783(4)
H42 H 0.79350 0.45440 0.24640
C44 C 0.7011(6) 0.3855(5) 0.3014(5)
H43 H 0.74440 0.33340 0.28650
C45 C 0.6076(7) 0.3900(6) 0.3469(5)
H44 H 0.58620 0.34060 0.36220
C46 C 0.5456(6) 0.4652(5) 0.3700(4)
H45 H 0.48300 0.46750 0.40220
C47 C 0.3720(5) 0.6172(4) 0.4156(3)
C48 C 0.3103(5) 0.6015(4) 0.3796(4)
H46 H 0.33500 0.60060 0.33460
C49 C 0.2128(5) 0.5869(5) 0.4085(4)
H47 H 0.17140 0.57640 0.38350
C50 C 0.1774(6) 0.5882(5) 0.4747(5)
H48 H 0.11150 0.57810 0.49490
C51 C 0.2364(6) 0.6038(5) 0.5106(4)
H49 H 0.21130 0.60450 0.55570
C52 C 0.3334(5) 0.6186(5) 0.4820(4)
H50 H 0.37360 0.62980 0.50760
C53 C 0.5422(4) 0.6675(4) 0.4386(3)
C54 C 0.6020(5) 0.6121(5) 0.4679(4)
H51 H 0.61870 0.55510 0.45500
C55 C 0.6369(5) 0.6382(5) 0.5149(4)
H52 H 0.67750 0.59920 0.53390
C56 C 0.6137(5) 0.7199(5) 0.5346(4)
H53 H 0.63790 0.73790 0.56710
C57 C 0.5554(6) 0.7754(5) 0.5071(4)
H54 H 0.53910 0.83210 0.52090
C58 C 0.5198(5) 0.7507(5) 0.4597(4)
H55 H 0.47960 0.79060 0.44120
C59 C 0.8058(4) 0.5687(4) 0.1158(3)
C60 C 0.8399(5) 0.6065(5) 0.1588(4)
H56 H 0.79850 0.65450 0.18330
C61 C 0.9341(6) 0.5745(6) 0.1662(5)
H57 H 0.95650 0.60150 0.19580
C62 C 0.9954(6) 0.5061(6) 0.1329(5)
H58 H 1.06070 0.48590 0.13780
C63 C 0.9608(6) 0.4662(5) 0.0914(4)
H59 H 1.00120 0.41650 0.06890
C64 C 0.8672(5) 0.4984(5) 0.0826(4)
H60 H 0.84520 0.47130 0.05290
C65 C 0.6990(4) 0.6316(4) 0.0268(3)
C66 C 0.7860(5) 0.6562(5) -0.0095(4)
H61 H 0.84130 0.65390 0.00750
C67 C 0.7947(6) 0.6842(6) -0.0701(4)
H62 H 0.85480 0.70140 -0.09390
C68 C 0.7158(7) 0.6868(6) -0.0954(4)
H63 H 0.72100 0.70530 -0.13700
C69 C 0.6307(8) 0.6627(7) -0.0603(5)
H64 H 0.57620 0.66380 -0.07780
C70 C 0.6218(6) 0.6366(6) 0.0000(4)
H65 H 0.56030 0.62160 0.02380
C71 C 0.6240(5) 0.5176(5) 0.1194(4)
C72 C 0.6421(6) 0.4583(6) 0.0715(5)
H66 H 0.67980 0.46720 0.02950
C73 C 0.6050(7) 0.3841(6) 0.0845(6)
H67 H 0.61810 0.34270 0.05190
C74 C 0.5496(9) 0.3741(8) 0.1458(7)
H68 H 0.52580 0.32420 0.15570
C75 C 0.5282(9) 0.4324(8) 0.1920(6)
H69 H 0.48840 0.42360 0.23350
C76 C 0.5634(6) 0.5065(6) 0.1801(4)
H70 H 0.54610 0.54840 0.21290
C77 C 0.1065(4) 1.1009(4) 0.3727(3)
C78 C 0.0679(4) 1.0368(4) 0.4064(3)
H71 H 0.11280 0.99330 0.41850
C79 C -0.0341(5) 1.0351(5) 0.4224(4)
H72 H -0.05840 0.99000 0.44440
C80 C -0.1012(5) 1.0984(5) 0.4067(4)
H73 H -0.17180 1.09800 0.41930
C81 C -0.0654(5) 1.1625(5) 0.3724(4)
H74 H -0.11100 1.20570 0.36060
C82 C 0.0392(5) 1.1631(4) 0.3553(3)
H75 H 0.06400 1.20680 0.33140
C83 C 0.2791(5) 1.0662(4) 0.4184(3)
C84 C 0.3615(6) 1.0019(5) 0.4121(4)
H76 H 0.39600 0.97450 0.37170
C85 C 0.3948(7) 0.9765(6) 0.4647(6)
H77 H 0.45280 0.93360 0.45960
C86 C 0.3429(7) 1.0141(6) 0.5235(5)
H78 H 0.36410 0.99620 0.55940
C87 C 0.2611(6) 1.0771(5) 0.5306(4)
H79 H 0.22540 1.10320 0.57130
C88 C 0.2304(5) 1.1026(5) 0.4784(4)
H80 H 0.17370 1.14690 0.48390
C89 C 0.2519(4) 1.2073(4) 0.3440(3)
C90 C 0.3297(6) 1.2269(5) 0.2942(4)
H81 H 0.37330 1.18490 0.26400
C91 C 0.3436(7) 1.3074(5) 0.2886(5)
H82 H 0.39740 1.31990 0.25460
C92 C 0.2823(7) 1.3687(6) 0.3303(5)
H83 H 0.29400 1.42350 0.32580
C93 C 0.2033(6) 1.3520(5) 0.3791(4)
H84 H 0.15900 1.39510 0.40810
C94 C 0.1893(5) 1.2717(4) 0.3855(4)
H85 H 0.13480 1.26010 0.41950
O3 O 0.91550 0.30220 0.01710
O4 O 0.90790 0.20700 0.12410
O5 O 1.04080 0.44580 0.29040
O6 O 0.97820 0.55520 0.38950
C95 C 0.93170 0.31180 -0.04860
H86 H 0.96870 0.35650 -0.06190
H87 H 0.86610 0.32530 -0.05730
H88 H 0.97160 0.26020 -0.07210
C96 C 0.86530 0.24210 0.03750
H89 H 0.91010 0.18910 0.01810
H90 H 0.80580 0.25040 0.02110
C97 C 0.82730 0.23360 0.11000
H91 H 0.79140 0.28760 0.13240
H92 H 0.78110 0.19390 0.12070
C98 C 0.93930 0.23210 0.17140
H93 H 1.01320 0.21440 0.16080
H94 H 0.90680 0.20770 0.21080
H95 H 0.92070 0.29250 0.17690
C99 C 1.08710 0.36480 0.24960
H96 H 1.14300 0.37360 0.21300
H97 H 1.03490 0.34710 0.23470
H98 H 1.11300 0.32200 0.27520
C100 C 0.96870 0.44270 0.33760
H99 H 0.99350 0.40530 0.36760
H100 H 0.91840 0.41830 0.32450
C101 C 0.92110 0.51710 0.36880
H101 H 0.89220 0.55320 0.33970
H102 H 0.86380 0.50850 0.40530
C102 C 0.92790 0.60930 0.44050
H103 H 0.97700 0.63360 0.45410
H104 H 0.89080 0.57980 0.47550
H105 H 0.87990 0.65320 0.42850
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Eu 1.60
I 1.40
N 0.68
O 0.68
P 1.05
|
1100186.cif | #------------------------------------------------------------------------------
#$Date: 2015-01-27 21:58:39 +0200 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100186.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_1100186
loop_
_publ_author_name
T.Grob
G.Seybert
W.Massa
K.Harms
K.Dehnicke
_journal_name_full Z.Anorg.Allg.Chem.
_journal_page_first 1361
_journal_paper_doi
10.1002/(SICI)1521-3749(200006)626:6<1361::AID-ZAAC1361>3.0.CO;2-X
_journal_volume 626
_journal_year 2000
_chemical_formula_moiety
;
C88 H92 I1 N4 O4 P4 Y2 1+,I3 1-,6.5(C4 H8 O1)
;
_chemical_formula_sum 'C114 H144 I4 N4 O10.5 P4 Y2'
_chemical_name_systematic
;
(\m~2~-Iodo)-bis((\m~2~-triphenylphosphoraneiminato)-triphenylphosphoraneimina
to-bis(tetrahydrofuran)-yttrium) tri-iodide tetrahydrofuran solvate
;
_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 74.929(15)
_cell_angle_beta 84.223(14)
_cell_angle_gamma 64.612(12)
_cell_formula_units_Z 2
_cell_length_a 17.3969(18)
_cell_length_b 17.701(2)
_cell_length_c 21.538(3)
_cell_volume 5785.395
_diffrn_ambient_temperature 103
_exptl_crystal_colour dark.
_exptl_crystal_density_diffrn 1.464
_exptl_crystal_description plate
_refine_ls_R_factor_gt 6.38
_refine_ls_wR_factor_gt 6.38
_cod_database_code 1100186
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
I1 I 0.91915(4) 0.82227(4) 0.12771(3)
Y1 Y 0.82207(6) 0.89035(5) 0.25381(4)
P1 P 0.95873(16) 0.69401(14) 0.35904(11)
N1 N 0.9454(5) 0.7729(4) 0.3012(3)
O1 O 0.7363(4) 0.8185(4) 0.2365(3)
Y2 Y 1.03857(6) 0.82083(5) 0.23820(4)
P2 P 0.91004(15) 1.04495(14) 0.22295(11)
N2 N 0.9179(4) 0.9514(4) 0.2319(3)
O2 O 0.7284(4) 0.9936(4) 0.1666(3)
P3 P 0.66801(16) 0.96660(14) 0.37917(11)
O3 O 1.1194(4) 0.6794(4) 0.2164(3)
N3 N 0.7389(5) 0.9338(4) 0.3299(3)
P4 P 1.20898(16) 0.81265(15) 0.33291(12)
O4 O 1.1214(4) 0.8490(4) 0.1432(3)
N4 N 1.1336(5) 0.8194(5) 0.2964(3)
C1 C 0.6788(6) 0.7983(6) 0.2865(5)
H1 H 0.70820 0.74080 0.31350
H2 H 0.65920 0.83920 0.31340
C2 C 0.6076(11) 0.8036(13) 0.2524(7)
H3 H 0.56100 0.86040 0.24720
H4 H 0.58750 0.76110 0.27620
C3 C 0.6400(9) 0.7864(9) 0.1908(8)
H5 H 0.59770 0.82380 0.15730
H6 H 0.65410 0.72700 0.19110
C4 C 0.7197(7) 0.8037(7) 0.1784(5)
H7 H 0.76740 0.75470 0.16780
H8 H 0.70990 0.85400 0.14320
C5 C 1.0949(6) 0.6203(6) 0.1969(5)
H9 H 1.06610 0.64590 0.15540
H10 H 1.05740 0.60390 0.22840
C6 C 1.1784(7) 0.5423(6) 0.1938(6)
H11 H 1.19210 0.49980 0.23470
H12 H 1.17550 0.51550 0.16060
C7 C 1.2425(7) 0.5800(6) 0.1773(5)
H13 H 1.24020 0.60820 0.13200
H14 H 1.29990 0.53670 0.18890
C8 C 1.2127(6) 0.6441(6) 0.2199(5)
H15 H 1.23350 0.61600 0.26380
H16 H 1.23200 0.68940 0.20300
C9 C 1.1292(6) 0.8204(6) 0.0845(4)
H17 H 1.07970 0.85730 0.05690
H18 H 1.13440 0.76170 0.09430
C10 C 1.2071(9) 0.8246(10) 0.0530(7)
H19 H 1.24790 0.76770 0.04940
H20 H 1.19280 0.86180 0.01000
C11 C 1.2421(10) 0.8589(12) 0.0886(7)
H21 H 1.24580 0.91080 0.06240
H22 H 1.29900 0.81690 0.10320
C12 C 1.1862(6) 0.8793(6) 0.1449(5)
H23 H 1.21890 0.84960 0.18470
H24 H 1.16090 0.94070 0.14210
C13 C 0.7434(7) 1.0355(6) 0.1010(4)
H25 H 0.76280 0.99450 0.07430
H26 H 0.78630 1.05690 0.10110
C14 C 0.6589(7) 1.1087(7) 0.0759(6)
H27 H 0.65270 1.11810 0.02990
H28 H 0.65260 1.16170 0.08540
C15 C 0.5947(8) 1.0763(10) 0.1135(6)
H29 H 0.54050 1.12360 0.11740
H30 H 0.58550 1.03790 0.09310
C16 C 0.6366(7) 1.0303(7) 0.1749(5)
H31 H 0.61880 0.98470 0.19510
H32 H 0.62090 1.06970 0.20280
C17 C 1.0638(6) 0.6034(5) 0.3672(4)
C18 C 1.0766(7) 0.5218(6) 0.3629(5)
H33 H 1.03020 0.51130 0.35400
C19 C 1.1594(8) 0.4549(6) 0.3719(6)
H34 H 1.16890 0.39890 0.36880
C20 C 1.2255(7) 0.4699(6) 0.3848(5)
H35 H 1.28110 0.42450 0.38980
C21 C 1.2139(6) 0.5486(6) 0.3907(5)
H36 H 1.26060 0.55780 0.40090
C22 C 1.1318(6) 0.6166(6) 0.3814(5)
H37 H 1.12330 0.67200 0.38500
C23 C 0.9472(6) 0.7174(5) 0.4374(4)
C24 C 0.9099(6) 0.8034(6) 0.4423(5)
H38 H 0.88920 0.84870 0.40470
C25 C 0.9029(6) 0.8229(6) 0.5017(5)
H39 H 0.87830 0.88140 0.50420
C26 C 0.9314(7) 0.7579(7) 0.5571(5)
H40 H 0.92650 0.77190 0.59750
C27 C 0.9670(6) 0.6728(6) 0.5539(5)
H41 H 0.98550 0.62800 0.59210
C28 C 0.9755(6) 0.6531(6) 0.4950(5)
H42 H 1.00130 0.59430 0.49310
C29 C 0.8916(6) 0.6399(5) 0.3560(5)
C30 C 0.8620(6) 0.5965(6) 0.4097(5)
H43 H 0.86950 0.60110 0.45140
C31 C 0.8218(7) 0.5469(6) 0.4023(5)
H44 H 0.80260 0.51710 0.43930
C32 C 0.8091(7) 0.5396(6) 0.3426(6)
H45 H 0.78130 0.50530 0.33830
C33 C 0.8370(7) 0.5825(6) 0.2891(5)
H46 H 0.82920 0.57700 0.24770
C34 C 0.8764(6) 0.6336(6) 0.2950(5)
H47 H 0.89340 0.66480 0.25750
C35 C 0.8053(6) 1.1337(5) 0.1988(4)
C36 C 0.7915(7) 1.2003(6) 0.1433(5)
H48 H 0.83680 1.19930 0.11440
C37 C 0.7111(7) 1.2683(6) 0.1306(5)
H49 H 0.70090 1.31260 0.09220
C38 C 0.6462(7) 1.2711(7) 0.1736(5)
H50 H 0.59190 1.31850 0.16500
C39 C 0.6582(7) 1.2072(6) 0.2284(5)
H51 H 0.61260 1.20980 0.25730
C40 C 0.7386(6) 1.1377(5) 0.2415(5)
H52 H 0.74770 1.09330 0.27970
C41 C 0.9795(6) 1.0732(5) 0.1606(4)
C42 C 0.9861(6) 1.0450(5) 0.1038(4)
H53 H 0.95740 1.01120 0.10020
C43 C 1.0344(6) 1.0669(6) 0.0537(5)
H54 H 1.03930 1.04760 0.01570
C44 C 1.0753(7) 1.1159(6) 0.0583(5)
H55 H 1.10840 1.13050 0.02340
C45 C 1.0688(6) 1.1443(6) 0.1131(5)
H56 H 1.09690 1.17910 0.11590
C46 C 1.0215(6) 1.1223(5) 0.1642(5)
H57 H 1.01800 1.14130 0.20220
C47 C 0.9325(6) 1.0682(5) 0.2950(4)
C48 C 0.9101(6) 1.1533(6) 0.3003(5)
H58 H 0.88100 1.20040 0.26550
C49 C 0.9294(7) 1.1695(6) 0.3543(5)
H59 H 0.91420 1.22700 0.35670
C50 C 0.9717(6) 1.1006(6) 0.4056(5)
H60 H 0.98660 1.11050 0.44300
C51 C 0.9918(6) 1.0170(6) 0.4014(4)
H61 H 1.01890 0.96990 0.43670
C52 C 0.9732(6) 1.0021(5) 0.3475(4)
H62 H 0.98860 0.94430 0.34560
C53 C 0.5600(6) 0.9922(6) 0.3533(4)
C54 C 0.5178(7) 1.0643(7) 0.3041(5)
H63 H 0.54150 1.10500 0.28880
C55 C 0.4438(7) 1.0786(8) 0.2770(5)
H64 H 0.41750 1.12770 0.24280
C56 C 0.4075(7) 1.0218(8) 0.2996(5)
H65 H 0.35610 1.03120 0.28060
C57 C 0.4456(7) 0.9503(7) 0.3501(6)
H66 H 0.42030 0.91110 0.36630
C58 C 0.5205(7) 0.9371(6) 0.3764(5)
H67 H 0.54590 0.88880 0.41140
C59 C 0.6778(6) 0.8911(5) 0.4572(4)
C60 C 0.7205(6) 0.8022(5) 0.4609(5)
H68 H 0.74630 0.78280 0.42360
C61 C 0.7252(7) 0.7435(6) 0.5173(5)
H69 H 0.75350 0.68380 0.51850
C62 C 0.6895(6) 0.7690(6) 0.5735(5)
H70 H 0.69320 0.72770 0.61270
C63 C 0.6480(6) 0.8572(6) 0.5702(5)
H71 H 0.62360 0.87630 0.60790
C64 C 0.6422(6) 0.9164(6) 0.5135(4)
H72 H 0.61330 0.97610 0.51240
C65 C 0.6601(6) 1.0620(5) 0.4015(4)
C66 C 0.7332(7) 1.0716(6) 0.4073(4)
H73 H 0.78610 1.02890 0.39820
C67 C 0.7327(8) 1.1406(7) 0.4258(5)
H74 H 0.78410 1.14570 0.42980
C68 C 0.6543(10) 1.2028(7) 0.4384(5)
H75 H 0.65240 1.25170 0.45020
C69 C 0.5811(8) 1.1955(7) 0.4343(6)
H76 H 0.52860 1.23840 0.44400
C70 C 0.5820(7) 1.1258(6) 0.4160(5)
H77 H 0.53030 1.12080 0.41320
C71 C 1.3119(7) 0.7696(7) 0.2931(5)
C72 C 1.3500(7) 0.8228(8) 0.2587(5)
H78 H 1.32760 0.88090 0.26200
C73 C 1.4200(8) 0.7928(9) 0.2198(6)
H79 H 1.44510 0.82960 0.19600
C74 C 1.4523(9) 0.7060(11) 0.2171(7)
H80 H 1.49960 0.68410 0.19040
C75 C 1.4172(9) 0.6527(10) 0.2520(7)
H81 H 1.44050 0.59390 0.25020
C76 C 1.3483(7) 0.6840(7) 0.2895(5)
H82 H 1.32450 0.64620 0.31370
C77 C 1.2264(6) 0.7448(6) 0.4158(4)
C78 C 1.3050(7) 0.6821(6) 0.4420(5)
H83 H 1.35480 0.67310 0.41680
C79 C 1.3111(8) 0.6327(6) 0.5044(6)
H84 H 1.36480 0.59020 0.52180
C80 C 1.2398(8) 0.6453(6) 0.5407(5)
H85 H 1.24370 0.61120 0.58340
C81 C 1.1619(8) 0.7080(6) 0.5153(5)
H86 H 1.11280 0.71690 0.54120
C82 C 1.1537(6) 0.7574(6) 0.4536(5)
H87 H 1.09960 0.79970 0.43680
C83 C 1.2038(6) 0.9135(6) 0.3446(4)
C84 C 1.2360(6) 0.9186(6) 0.3977(5)
H88 H 1.26080 0.86770 0.43080
C85 C 1.2346(7) 0.9951(7) 0.4058(5)
H89 H 1.25780 0.99670 0.44330
C86 C 1.1973(6) 1.0693(6) 0.3561(5)
H90 H 1.19550 1.12230 0.36000
C87 C 1.1633(7) 1.0671(6) 0.3020(5)
H91 H 1.13900 1.11770 0.26840
C88 C 1.1651(6) 0.9893(6) 0.2974(5)
H92 H 1.13930 0.98790 0.26110
I2 I 0.3955(2) 1.3331(2) 0.2041(3)
I3 I 0.44888(12) 1.39191(12) 0.29960(9)
I4 I 0.34001(15) 1.28183(11) 0.10518(11)
I5? I 0.3956(3) 1.3097(3) 0.1363(3)
I6? I 0.4147(3) 1.3424(3) 0.2595(3)
I7? I 0.3856(5) 1.2821(4) 0.0085(5)
I8? I 0.460(1) 1.4333(10) 0.3430(14)
I9? I 0.4037(7) 1.2765(7) 0.0853(5)
I10? I 0.4289(15) 1.2442(15) -0.0385(6)
I11? I 0.3776(12) 1.3126(10) 0.2153(9)
O5 O 0.4501(13) 1.4785(12) -0.0845(9)
C89 C 0.4466(18) 1.3976(16) -0.0582(15)
H93 H 0.43940 1.37430 -0.09220
H94 H 0.40300 1.39980 -0.02600
C90 C 0.544(2) 1.350(2) -0.0268(14)
H95 H 0.54030 1.32980 0.01930
H96 H 0.57520 1.30010 -0.04400
C91 C 0.581(2) 1.3890(19) -0.0449(18)
H97 H 0.63810 1.35520 -0.05810
H98 H 0.58620 1.40320 -0.00530
C92 C 0.5339(14) 1.470(2) -0.0934(11)
H99 H 0.53680 1.51920 -0.08440
H100 H 0.55520 1.46370 -0.13600
O6 O 0.7995(9) 1.3531(6) -0.0114(6)
O7? O 0.861(2) 1.3950(19) -0.0501(15)
C93 C 0.7583(5) 1.4440(4) -0.0033(3)
H101 H 0.74100 1.48450 -0.04480
H102 H 0.70810 1.45170 0.02310
H103? H 0.71310 1.49520 -0.02770
H104? H 0.73760 1.40330 0.02320
C94 C 0.8183(5) 1.4586(4) 0.0270(3)
H105 H 0.79150 1.48980 0.05990
H106 H 0.84430 1.49080 -0.00410
C95 C 0.8853(5) 1.3655(4) 0.0571(3)
H107 H 0.94090 1.36410 0.06150
H108 H 0.86750 1.34100 0.09860
C96 C 0.8844(5) 1.3205(4) 0.0061(3)
H109 H 0.91820 1.33270 -0.03060
H110 H 0.90700 1.25860 0.02340
H111? H 0.94000 1.27610 0.00060
H112? H 0.84280 1.29620 0.01500
O8 O 1.4618(5) 0.9644(4) 0.0954(3)
C97 C 1.4041(5) 1.0205(4) 0.1262(3)
H113 H 1.41980 1.06760 0.12360
H114 H 1.40560 0.99140 0.17130
C98 C 1.3200(12) 1.0547(16) 0.1015(11)
H115 H 1.28850 1.11500 0.10170
H116 H 1.28860 1.02200 0.12410
C99 C 1.3468(14) 1.0396(17) 0.0312(10)
H117 H 1.30310 1.03360 0.01080
H118 H 1.35950 1.08580 0.00400
C100 C 1.4229(15) 0.9585(15) 0.0461(11)
H119 H 1.40770 0.91000 0.05990
H120 H 1.45950 0.95100 0.00910
O9 O 0.2188(8) 1.6205(6) -0.2865(6)
C101 C 0.2978(14) 1.6285(14) -0.2895(10)
H121 H 0.29510 1.67040 -0.26690
H122 H 0.31640 1.64300 -0.33320
C102 C 0.3506(17) 1.5383(18) -0.2519(15)
H123 H 0.39920 1.53780 -0.23300
H124 H 0.37170 1.50210 -0.28220
C103 C 0.301(2) 1.5094(18) -0.2018(15)
H125 H 0.31650 1.50620 -0.15900
H126 H 0.30470 1.45390 -0.20460
C104 C 0.2176(14) 1.5782(13) -0.2253(8)
H127 H 0.17550 1.55500 -0.22100
H128 H 0.20110 1.61810 -0.19770
O10 O 0.8242(11) 0.6140(8) 0.1148(6)
C105 C 0.9069(14) 0.5990(15) 0.0983(14)
H129 H 0.93900 0.54850 0.13140
H130 H 0.91720 0.64600 0.10490
C106 C 0.9525(17) 0.5644(19) 0.0486(19)
H131 H 0.94740 0.51790 0.03610
H132 H 1.00900 0.56290 0.04160
C107 C 0.8719(19) 0.6658(16) 0.0142(13)
H133 H 0.88840 0.70840 0.02200
H134 H 0.86320 0.67820 -0.03180
C108 C 0.7919(19) 0.6831(16) 0.0509(12)
H135 H 0.76010 0.74040 0.05810
H136 H 0.75670 0.66870 0.02810
O11 O 1.1039(18) 1.2778(15) 0.1896(9)
C109 C 1.0250(18) 1.3327(16) 0.2210(16)
H137 H 0.98220 1.37120 0.18810
H138 H 1.00460 1.29270 0.24900
C110 C 1.047(2) 1.3717(15) 0.2547(13)
H139 H 1.01770 1.37160 0.29550
H140 H 1.03220 1.43070 0.23060
C111 C 1.1458(18) 1.3191(13) 0.2619(13)
H141 H 1.17080 1.35640 0.26770
H142 H 1.15780 1.27240 0.30030
C112 C 1.179(2) 1.283(2) 0.2033(17)
H143 H 1.19670 1.32120 0.17040
H144 H 1.22570 1.22590 0.21480
O12 O 0.5230(6) 0.5789(5) 0.4443(5)
C113 C 0.5363(11) 0.5906(10) 0.5026(8)
H145 H 0.55590 0.53570 0.53420
H146 H 0.48430 0.63060 0.51800
C114 C 0.6007(10) 0.6232(9) 0.4930(7)
H147 H 0.65730 0.57740 0.49350
H148 H 0.59800 0.65360 0.52530
C115 C 0.5769(10) 0.6840(9) 0.4257(8)
H149 H 0.53030 0.73880 0.42800
H150 H 0.62510 0.69420 0.40540
C116 C 0.5520(11) 0.6357(12) 0.3907(9)
H151 H 0.59930 0.60150 0.36740
H152 H 0.50560 0.67490 0.36080
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
I 1.45
N 0.68
O 0.68
P 1.05
Y 1.46
|
1100187.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-10 17:02:39 +0200 (Thu, 10 Mar 2016) $
#$Revision: 178092 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100187.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_1100187
loop_
_publ_author_name
'Bach, Thorsten'
'Bergmann, Hermann'
'Grosch, Benjamin'
'Harms, Klaus'
'Herdtweck, Eberhardt'
_publ_section_title
;
Synthesis of Enantiomerically Pure
1,5,7-Trimethyl-3-azabicyclo[3.3.1]nonan-2-ones
as Chiral Host Compounds for Enantioselective Photochemical
Reactions in Solution
;
_journal_coden_ASTM SYNTBF
_journal_issue 9
_journal_name_full Synthesis
_journal_page_first 1395
_journal_page_last 1405
_journal_paper_doi 10.1055/s-2001-15231
_journal_volume 2001
_journal_year 2001
_chemical_formula_moiety 'C22 H35 N1 O4,0.17(C1 H2 Cl2)'
_chemical_formula_sum 'C22.17 H35.34 Cl0.34 N O4'
_chemical_melting_point 427.15
_chemical_name_systematic
;
p-Menth-3-yl 1,3,5-trimethylcyclohexane-1,3-dicarboximide-5-carboxylate dichloromethane solvate
;
_space_group_IT_number 146
_symmetry_cell_setting rhombohedral
_symmetry_space_group_name_Hall 'R 3'
_symmetry_space_group_name_H-M 'R 3 :H'
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_formula_units_Z 18
_cell_length_a 28.224(1)
_cell_length_b 28.224(1)
_cell_length_c 15.262(1)
_cell_volume 10528.808
_diffrn_ambient_temperature 293
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.112
_exptl_crystal_description prism
_refine_ls_R_factor_gt 5.16
_refine_ls_wR_factor_gt 5.16
_cod_original_sg_symbol_H-M 'R 3'
_cod_original_formula_sum 'C22.17 H35.34 Cl0.34 N1 O4'
_cod_database_code 1100187
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 -1/3+x,1/3+y,1/3+z
5 -1/3-y,1/3+x-y,1/3+z
6 -1/3-x+y,1/3-x,1/3+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
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
O1 O 1.03743(12) 0.47384(14) 0.1488(3)
O2 O 0.86434(13) 0.42169(12) 0.0758(2)
O3 O 0.95044(13) 0.35552(14) 0.2508(2)
O4 O 0.86219(11) 0.31848(11) 0.21611(16)
O5 O 0.80123(12) 0.09440(14) -0.0992(2)
O6 O 0.75808(12) 0.22126(13) -0.0205(2)
O7 O 0.69078(14) 0.07445(13) -0.19329(18)
O8 O 0.65253(11) 0.12472(11) -0.16148(16)
N1 N 0.95031(14) 0.44476(14) 0.1109(2)
H1 H 0.94970 0.46630 0.15010
N2 N 0.77776(12) 0.15608(14) -0.0553(2)
H2 H 0.80060 0.17840 -0.09310
C1 C 1.00000(16) 0.40582(18) 0.0354(3)
C2 C 0.99793(18) 0.44392(17) 0.1032(3)
C3 C 0.90235(19) 0.41469(16) 0.0623(3)
C4 C 0.90294(18) 0.37573(17) -0.0059(3)
C5 C 0.96078(19) 0.3982(2) -0.0383(3)
H3 H 0.97280 0.43320 -0.06670
H4 H 0.96150 0.37350 -0.08160
C6 C 0.98166(17) 0.34981(19) 0.0780(3)
H5 H 1.00420 0.35560 0.12930
H6 H 0.98880 0.32790 0.03700
C7 C 0.92108(17) 0.31665(16) 0.1062(3)
C8 C 0.88415(17) 0.31941(16) 0.0370(3)
H7 H 0.84850 0.30690 0.06320
H8 H 0.87940 0.29370 -0.00910
C9 C 0.91396(17) 0.33391(16) 0.1978(3)
C10 C 0.8645(2) 0.3691(2) -0.0802(3)
H9 H 0.87450 0.40440 -0.10380
H10 H 0.82770 0.35200 -0.05860
H11 H 0.86700 0.34680 -0.12530
C11 C 1.0590(2) 0.4291(2) 0.0025(4)
H12 H 1.07120 0.46410 -0.02440
H13 H 1.06020 0.40450 -0.03980
H14 H 1.08240 0.43320 0.05090
C12 C 0.9053(2) 0.25595(18) 0.1193(4)
H15 H 0.86850 0.23560 0.14100
H16 H 0.92980 0.25390 0.16070
H17 H 0.90780 0.24080 0.06430
C13 C 0.84647(17) 0.31623(17) 0.3078(3)
H18 H 0.87690 0.34510 0.34100
C14 C 0.79766(16) 0.32474(15) 0.3116(3)
H19 H 0.76990 0.29770 0.27230
C15 C 0.7734(2) 0.3119(2) 0.4039(3)
H20 H 0.79940 0.33880 0.44440
H21 H 0.74050 0.31460 0.40490
C16 C 0.7596(2) 0.2554(2) 0.4342(4)
H22 H 0.74450 0.24920 0.49290
H23 H 0.73200 0.22820 0.39580
C17 C 0.8096(2) 0.24886(19) 0.4341(3)
H24 H 0.83670 0.27630 0.47380
C18 C 0.8338(2) 0.26044(18) 0.3422(3)
H25 H 0.86720 0.25860 0.34260
H26 H 0.80820 0.23230 0.30270
C19 C 0.8110(2) 0.3810(2) 0.2782(4)
H27 H 0.82880 0.38610 0.22100
C20 C 0.8499(3) 0.4273(2) 0.3354(6)
H28 H 0.88470 0.42890 0.33600
H29 H 0.83560 0.42160 0.39390
H30 H 0.85440 0.46100 0.31290
C21 C 0.7586(3) 0.3837(3) 0.2631(5)
H31 H 0.73610 0.35680 0.22040
H32 H 0.76800 0.41950 0.24240
H33 H 0.73880 0.37650 0.31730
C22 C 0.7971(3) 0.1929(2) 0.4658(4)
H34 H 0.78080 0.18620 0.52290
H35 H 0.83040 0.19160 0.46870
H36 H 0.77220 0.16540 0.42580
C23 C 0.73329(16) 0.06526(17) 0.0157(3)
C24 C 0.77352(16) 0.10529(18) -0.0509(3)
C25 C 0.74980(16) 0.17557(17) -0.0066(3)
C26 C 0.70963(15) 0.13669(17) 0.0607(3)
C27 C 0.72885(18) 0.09814(19) 0.0919(3)
H37 H 0.70330 0.07320 0.13510
H38 H 0.76430 0.11910 0.11990
C28 C 0.67649(16) 0.03156(15) -0.0244(3)
H39 H 0.67960 0.01270 -0.07530
H40 H 0.65340 0.00390 0.01770
C29 C 0.64750(13) 0.06223(14) -0.0524(2)
C30 C 0.65282(14) 0.10324(16) 0.0190(2)
H41 H 0.64270 0.12850 -0.00640
H42 H 0.62670 0.08320 0.06500
C31 C 0.66741(14) 0.08802(15) -0.1431(2)
C32 C 0.7051(2) 0.1704(2) 0.1360(3)
H43 H 0.74010 0.19130 0.16390
H44 H 0.67880 0.14620 0.17800
H45 H 0.69360 0.19470 0.11310
C33 C 0.7539(2) 0.0276(2) 0.0472(4)
H46 H 0.75430 0.00600 -0.00090
H47 H 0.73010 0.00400 0.09230
H48 H 0.79030 0.04920 0.07020
C34 C 0.58596(15) 0.02049(19) -0.0649(3)
H49 H 0.56680 0.03960 -0.07940
H50 H 0.57140 0.00030 -0.01160
H51 H 0.58150 -0.00430 -0.11140
C35 C 0.66811(16) 0.15227(17) -0.2472(2)
H52 H 0.68370 0.13500 -0.28400
C36 C 0.61731(15) 0.14672(15) -0.2904(2)
H53 H 0.60220 0.16300 -0.25050
C37 C 0.63503(19) 0.18172(19) -0.3736(3)
H54 H 0.65010 0.16660 -0.41480
H55 H 0.60320 0.18020 -0.40060
C38 C 0.67736(18) 0.24113(19) -0.3555(3)
H56 H 0.66150 0.25720 -0.31790
H57 H 0.68770 0.26130 -0.41020
C39 C 0.72801(18) 0.24594(18) -0.3117(3)
H58 H 0.74450 0.23130 -0.35210
C40 C 0.71099(17) 0.21081(18) -0.2290(3)
H59 H 0.74290 0.21170 -0.20360
H60 H 0.69680 0.22620 -0.18660
C41 C 0.57246(17) 0.08709(16) -0.3052(3)
H61 H 0.56560 0.06850 -0.24850
C42 C 0.5896(2) 0.0565(2) -0.3684(4)
H62 H 0.62200 0.05740 -0.34670
H63 H 0.59700 0.07370 -0.42500
H64 H 0.56070 0.01920 -0.37340
C43 C 0.51933(19) 0.0835(2) -0.3335(4)
H65 H 0.49070 0.04590 -0.33380
H66 H 0.52350 0.09860 -0.39120
H67 H 0.51010 0.10380 -0.29320
C44 C 0.7707(2) 0.3051(2) -0.2917(4)
H68 H 0.78460 0.32480 -0.34560
H69 H 0.80020 0.30610 -0.25890
H70 H 0.75420 0.32180 -0.25800
C45? C 0.66670 0.33330 -0.0348(12)
Cl1? Cl 0.6612(12) 0.2884(10) -0.073(2)
Cl2? Cl 0.676(3) 0.296(2) 0.0270(18)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
N 0.68
O 0.68
|
1100188.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-10 17:02:39 +0200 (Thu, 10 Mar 2016) $
#$Revision: 178092 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100188.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_1100188
loop_
_publ_author_name
'Bach, Thorsten'
'Bergmann, Hermann'
'Grosch, Benjamin'
'Harms, Klaus'
'Herdtweck, Eberhardt'
_publ_section_title
;
Synthesis of Enantiomerically Pure
1,5,7-Trimethyl-3-azabicyclo[3.3.1]nonan-2-ones
as Chiral Host Compounds for Enantioselective Photochemical
Reactions in Solution
;
_journal_coden_ASTM SYNTBF
_journal_issue 9
_journal_name_full Synthesis
_journal_page_first 1395
_journal_page_last 1405
_journal_paper_doi 10.1055/s-2001-15231
_journal_volume 2001
_journal_year 2001
_chemical_formula_moiety 'C22 H24 N2 O2'
_chemical_formula_sum 'C22 H24 N2 O2'
_chemical_melting_point 565.15
_chemical_name_systematic
;
rac-1,5,7-Trimethyl-7-(1'-oxa-3'-azacyclopenta(b)naphthalen-2'-yl)-3-azabicyclo(3.3.1)nonan-2-one
;
_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 111.665(19)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.372(2)
_cell_length_b 14.9124(13)
_cell_length_c 11.545(3)
_cell_volume 1819.540
_diffrn_ambient_temperature 223
_exptl_crystal_colour 'light yellow.'
_exptl_crystal_density_diffrn 1.272
_exptl_crystal_description Prism
_refine_ls_R_factor_gt 6.49
_refine_ls_wR_factor_gt 6.49
_cod_original_sg_symbol_H-M 'P 21/c'
_cod_database_code 1100188
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
C1 C -0.2754(3) 0.0700(3) 0.2458(3)
C2 C -0.3082(4) 0.0119(3) 0.1276(4)
H1 H -0.33650 -0.04740 0.14320
H2 H -0.37770 0.03990 0.05930
C3 C -0.1954(4) 0.0014(3) 0.0900(4)
C4 C -0.1547(4) 0.0951(3) 0.0608(4)
H3 H -0.07610 0.08820 0.04540
H4 H -0.21950 0.11670 -0.01670
C5 C -0.1336(3) 0.1680(3) 0.1612(3)
C6 C -0.2381(3) 0.1646(3) 0.2145(3)
H5 H -0.31380 0.19300 0.15440
H6 H -0.21120 0.20080 0.29070
C7 C -0.3877(4) 0.0802(3) 0.2856(4)
H7 H -0.41100 0.02190 0.30790
H8 H -0.45870 0.10520 0.21740
H9 H -0.36550 0.12000 0.35700
C8 C -0.2295(4) -0.0568(3) -0.0303(4)
H10 H -0.29840 -0.02880 -0.09740
H11 H -0.25520 -0.11610 -0.01440
H12 H -0.15620 -0.06170 -0.05370
C9 C -0.1342(4) 0.2607(3) 0.1016(4)
H13 H -0.07380 0.26080 0.06030
H14 H -0.11110 0.30640 0.16580
H15 H -0.21820 0.27310 0.04110
C10 C -0.0930(4) -0.0470(3) 0.1981(4)
H16 H -0.11230 -0.11130 0.19230
H17 H -0.01130 -0.03940 0.18890
N1 N -0.0814(4) -0.0148(2) 0.3235(3)
H18 H -0.016(4) -0.026(3) 0.389(4)
O1 O -0.1488(2) 0.05006(19) 0.4653(3)
C11 C -0.1657(4) 0.0330(3) 0.3530(4)
C12 C -0.0066(4) 0.1589(3) 0.2631(4)
N2 N 0.0920(3) 0.1265(2) 0.2488(3)
C13 C 0.1881(4) 0.1389(3) 0.3657(4)
C14 C 0.3114(4) 0.1156(3) 0.4059(4)
H19 H 0.34560 0.08660 0.35300
C15 C 0.3878(4) 0.1367(3) 0.5318(4)
C16 C 0.5179(4) 0.1147(3) 0.5823(4)
H20 H 0.55530 0.08670 0.53150
C17 C 0.5900(4) 0.1334(3) 0.7033(5)
H21 H 0.67640 0.11830 0.73400
C18 C 0.5379(4) 0.1753(3) 0.7844(5)
H22 H 0.58900 0.18740 0.86780
C19 C 0.4155(4) 0.1971(3) 0.7404(4)
H23 H 0.38130 0.22550 0.79350
C20 C 0.3350(4) 0.1784(3) 0.6145(4)
C21 C 0.2076(4) 0.2013(3) 0.5682(4)
H24 H 0.17000 0.23020 0.61820
C22 C 0.1398(3) 0.1801(3) 0.4478(4)
O2 O 0.0133(2) 0.19455(19) 0.3790(2)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100189.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-10 17:02:39 +0200 (Thu, 10 Mar 2016) $
#$Revision: 178092 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100189.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_1100189
loop_
_publ_author_name
'Bach, Thorsten'
'Bergmann, Hermann'
'Grosch, Benjamin'
'Harms, Klaus'
'Herdtweck, Eberhardt'
_publ_section_title
;
Synthesis of Enantiomerically Pure
1,5,7-Trimethyl-3-azabicyclo[3.3.1]nonan-2-ones
as Chiral Host Compounds for Enantioselective Photochemical
Reactions in Solution
;
_journal_coden_ASTM SYNTBF
_journal_issue 9
_journal_name_full Synthesis
_journal_page_first 1395
_journal_page_last 1405
_journal_paper_doi 10.1055/s-2001-15231
_journal_volume 2001
_journal_year 2001
_chemical_formula_moiety 'C22 H28 N2 O2,0.33(H2 O1)'
_chemical_formula_sum 'C22 H28.66 N2 O2.33'
_chemical_name_systematic
;
ent-1,5,7-Trimethyl-7-(5',6',7',8'-tetrahydro-1'-oxa-3'-azacyclopenta(b)naphthalen-2'-yl)-3-azabicyclo(3.3.1)nonan-2-one hydrate
;
_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 7.6041(8)
_cell_length_b 15.9342(11)
_cell_length_c 16.4592(11)
_cell_volume 1994.283
_diffrn_ambient_temperature 173
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.194
_exptl_crystal_description fragment
_refine_ls_R_factor_gt 3.05
_refine_ls_wR_factor_gt 3.05
_cod_database_code 1100189
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
O1 O -0.02644(15) 0.19869(7) 0.50173(6)
O2 O -0.10080(13) 0.35399(6) 0.62452(6)
N1 N 0.21282(14) 0.20677(7) 0.58063(7)
N2 N 0.15403(16) 0.37758(7) 0.69103(7)
C1 C -0.04439(18) 0.13067(9) 0.63303(9)
C2 C 0.04882(17) 0.18117(8) 0.56615(8)
C3 C 0.32426(18) 0.18614(10) 0.65017(9)
C4 C 0.22310(18) 0.14683(8) 0.72102(8)
C5 C -0.14810(19) 0.19223(9) 0.68724(10)
C6 C -0.0356(2) 0.25581(9) 0.73469(8)
C7 C 0.1235(2) 0.21162(10) 0.77308(8)
C8 C 0.0912(2) 0.08472(9) 0.68525(9)
C9 C -0.1721(3) 0.06844(12) 0.59422(14)
C10 C 0.3565(3) 0.10163(13) 0.77563(12)
C11 C -0.1487(3) 0.29613(14) 0.80255(12)
C12 C -0.09444(19) 0.47647(9) 0.53157(9)
C13 C -0.02847(18) 0.42646(8) 0.59271(8)
C14 C 0.12760(19) 0.44167(8) 0.63285(8)
C15 C 0.2275(2) 0.51122(9) 0.61150(8)
C16 C 0.2814(2) 0.63646(9) 0.52248(9)
C17 C 0.1792(3) 0.70239(12) 0.47241(13)
C18 C 0.0768(3) 0.65919(13) 0.40465(17)
C19 C -0.0613(2) 0.60184(9) 0.44114(10)
C20 C 0.00681(18) 0.54630(8) 0.50955(8)
C21 C 0.16715(18) 0.56345(8) 0.54930(8)
C22 C 0.01851(18) 0.32930(8) 0.68254(8)
C23? C -0.0613(2) 0.60184(9) 0.44114(10)
C24? C 0.088(3) 0.6839(13) 0.4487(17)
C25? C 0.2814(2) 0.63646(9) 0.52248(9)
C26? C 0.281(3) 0.6641(13) 0.4480(14)
O3 O 0.0376(5) 0.1191(3) 0.3144(3)
H1 H 0.384(2) 0.2394(11) 0.6682(9)
H2 H 0.204(2) 0.2559(11) 0.7912(10)
H3 H -0.240(2) 0.2206(10) 0.6569(9)
H4 H -0.210(2) 0.1577(11) 0.7291(10)
H5 H 0.418(2) 0.1436(11) 0.6323(10)
H6 H -0.236(3) 0.0361(16) 0.6350(15)
H7 H -0.267(3) 0.0994(12) 0.5592(12)
H8 H -0.102(3) 0.0286(14) 0.5574(13)
H9 H 0.424(3) 0.0549(15) 0.7426(14)
H10 H 0.073(2) 0.1792(10) 0.8226(9)
H11 H 0.156(2) 0.0440(11) 0.6512(10)
H12 H 0.027(2) 0.0531(11) 0.730(1)
H13 H -0.075(4) 0.3377(17) 0.8362(14)
H14 H -0.195(3) 0.2500(15) 0.8383(13)
H15 H -0.208(2) 0.4656(10) 0.5071(10)
H16 H 0.336(2) 0.5203(11) 0.6375(10)
H17 H 0.338(2) 0.6607(11) 0.5721(11)
H18 H 0.380(2) 0.6121(11) 0.4927(11)
H19 H 0.262(3) 0.7437(12) 0.4485(11)
H20 H 0.090(2) 0.7363(11) 0.5079(11)
H21 H 0.162(3) 0.6244(13) 0.3716(11)
H22 H 0.018(3) 0.7007(13) 0.3699(12)
H23 H -0.168(3) 0.6377(12) 0.4612(11)
H24 H -0.116(2) 0.5658(12) 0.3982(11)
H25 H 0.441(3) 0.1412(13) 0.7967(12)
H26 H 0.290(3) 0.0786(13) 0.8226(13)
H27 H -0.256(3) 0.3274(14) 0.7775(12)
H28 H 0.270(2) 0.2373(10) 0.5418(10)
H29? H 0.25070 0.68460 0.55770
H30? H 0.40440 0.62120 0.53550
H31? H 0.31240 0.62030 0.40780
H32? H 0.35550 0.71440 0.44040
H33? H 0.06440 0.72310 0.40330
H34? H 0.06230 0.71450 0.49970
H35? H -0.18350 0.62070 0.45110
H36? H -0.05430 0.57350 0.38770
H37 H -0.08640 0.12590 0.28430
H38 H 0.06060 0.07550 0.36190
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100190.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-10 17:02:39 +0200 (Thu, 10 Mar 2016) $
#$Revision: 178092 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100190.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_1100190
loop_
_publ_author_name
'Bach, Thorsten'
'Bergmann, Hermann'
'Grosch, Benjamin'
'Harms, Klaus'
'Herdtweck, Eberhardt'
_publ_section_title
;
Synthesis of Enantiomerically Pure
1,5,7-Trimethyl-3-azabicyclo[3.3.1]nonan-2-ones
as Chiral Host Compounds for Enantioselective Photochemical
Reactions in Solution
;
_journal_coden_ASTM SYNTBF
_journal_issue 9
_journal_name_full Synthesis
_journal_page_first 1395
_journal_page_last 1405
_journal_paper_doi 10.1055/s-2001-15231
_journal_volume 2001
_journal_year 2001
_chemical_formula_moiety 'C22 H28 N2 O2,0.33(H2 O1)'
_chemical_formula_sum 'C22 H28.66 N2 O2.33'
_chemical_name_systematic
;
ent-1,5,7-Trimethyl-7-(5',6',7',8'-tetrahydro-1'-oxa-3'-azacyclopenta(b)naphthalen-2'-yl)-3-azabicyclo(3.3.1)nonan-2-one hydrate
;
_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 7.6183(2)
_cell_length_b 16.0920(6)
_cell_length_c 16.4887(6)
_cell_volume 2021.410
_diffrn_ambient_temperature 293
_exptl_crystal_colour colorless.
_exptl_crystal_density_diffrn 1.178
_exptl_crystal_description fragment
_refine_ls_R_factor_gt 3.06
_refine_ls_wR_factor_gt 3.06
_cod_database_code 1100190
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
O1 O -0.02002(17) 0.20040(9) 0.50120(7)
O2 O -0.10083(14) 0.35455(7) 0.62429(7)
N1 N 0.21504(15) 0.20798(9) 0.58119(7)
N2 N 0.15219(19) 0.37678(9) 0.69045(7)
C1 C -0.0416(2) 0.13309(10) 0.63173(10)
C2 C 0.05256(19) 0.18259(10) 0.56590(9)
C3 C 0.3238(2) 0.18771(13) 0.65057(10)
C4 C 0.2219(2) 0.14892(10) 0.72074(9)
C5 C -0.1456(2) 0.19310(12) 0.68485(12)
C6 C -0.0365(2) 0.25605(11) 0.73271(9)
C7 C 0.1220(3) 0.21300(13) 0.77161(9)
C8 C 0.0925(2) 0.08780(11) 0.68461(11)
C9 C -0.1667(4) 0.07089(17) 0.5921(2)
C10 C 0.3549(4) 0.10456(18) 0.77546(16)
C11 C -0.1522(5) 0.2955(2) 0.80029(17)
C12 C -0.0932(2) 0.47634(11) 0.53307(11)
C13 C -0.0290(2) 0.42606(9) 0.59331(9)
C14 C 0.1265(2) 0.44068(10) 0.63328(8)
C15 C 0.2251(2) 0.50921(10) 0.61239(10)
C16 C 0.2804(3) 0.63306(11) 0.52471(12)
C17 C 0.1768(6) 0.6996(2) 0.4744(2)
C18 C 0.0741(6) 0.6571(3) 0.4063(3)
C19 C -0.0591(3) 0.60109(13) 0.44426(14)
C20 C 0.0069(2) 0.54521(9) 0.51176(9)
C21 C 0.1664(2) 0.56136(9) 0.55084(9)
C22 C 0.0179(2) 0.3292(1) 0.68186(9)
C23? C -0.0591(3) 0.60109(13) 0.44426(14)
C24? C 0.073(3) 0.6787(12) 0.4442(14)
C25? C 0.2804(3) 0.63306(11) 0.52471(12)
C26? C 0.265(2) 0.6635(9) 0.4499(9)
O3 O 0.0362(6) 0.1161(4) 0.3136(4)
H1 H 0.381(2) 0.2431(12) 0.6688(10)
H2 H 0.202(3) 0.2616(13) 0.7889(12)
H3 H -0.232(3) 0.2248(12) 0.6547(11)
H4 H -0.212(3) 0.1594(13) 0.7236(12)
H5 H 0.415(3) 0.1424(13) 0.6331(12)
H6 H -0.218(4) 0.0354(18) 0.6274(16)
H7 H -0.256(4) 0.1004(15) 0.5572(16)
H8 H -0.097(4) 0.0289(18) 0.5560(17)
H9 H 0.423(4) 0.053(2) 0.7490(17)
H10 H 0.071(3) 0.1777(13) 0.8225(12)
H11 H 0.157(3) 0.0454(13) 0.6521(11)
H12 H 0.028(3) 0.0567(14) 0.7294(13)
H13 H -0.075(5) 0.333(3) 0.834(2)
H14 H -0.186(3) 0.2501(17) 0.8312(16)
H15 H -0.209(3) 0.4650(12) 0.5111(12)
H16 H 0.338(3) 0.5164(13) 0.6382(12)
H17 H 0.339(3) 0.6572(15) 0.5713(15)
H18 H 0.384(3) 0.6096(15) 0.4976(15)
H19 H 0.258(4) 0.742(2) 0.4506(17)
H20 H 0.086(3) 0.7327(15) 0.5113(15)
H21 H 0.156(4) 0.6197(17) 0.3743(16)
H22 H 0.014(4) 0.700(2) 0.3736(19)
H23 H -0.161(4) 0.6387(19) 0.4695(17)
H24 H -0.109(4) 0.563(2) 0.4059(18)
H25 H 0.444(3) 0.1493(16) 0.7995(15)
H26 H 0.291(4) 0.0866(17) 0.8207(16)
H27 H -0.262(5) 0.334(2) 0.7750(19)
H28 H 0.265(3) 0.2424(14) 0.5443(13)
H29? H 0.25950 0.67840 0.56220
H30? H 0.40160 0.61610 0.53180
H31? H 0.30340 0.62350 0.40960
H32? H 0.33100 0.71450 0.44350
H33? H 0.05170 0.71000 0.39490
H34? H 0.04020 0.71440 0.48920
H35? H -0.17850 0.61910 0.45490
H36? H -0.05600 0.57240 0.39250
H37 H -0.08640 0.12590 0.28430
H38 H 0.06060 0.07550 0.36190
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
N 0.68
O 0.68
|
1100191.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-04 12:31:23 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177463 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100191.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_1100191
loop_
_publ_author_name
'Uhl, Werner'
'Cuypers, Lars'
'Geiseler, Gertraud'
'Harms, Klaus'
'Neum\"uller, Bernhard'
_publ_section_title
;
Unexpected formation of gallium--gallium single bonds by irradiation of
the hydride [(Me~3~C)~2~GaH]~3~
;
_journal_coden_ASTM JCSDAA
_journal_issue 16
_journal_name_full
;
Journal of the Chemical Society, Dalton Transactions
;
_journal_page_first 2398
_journal_page_last 2400
_journal_paper_doi 10.1039/b103409j
_journal_year 2001
_chemical_formula_moiety 'C32 H78 Ga6'
_chemical_formula_sum 'C32 H78 Ga6'
_chemical_melting_point 431.15
_chemical_name_common octakis(t-Butyl)-hypho-hexagallane(6)
_chemical_name_systematic
;
hexakis(\m~2~-Hydrido)-octakis(t-butyl)-hexa-gallium
;
_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 101.582(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 14.4126(8)
_cell_length_b 17.328(2)
_cell_length_c 18.359(1)
_cell_volume 4491.647
_diffrn_ambient_temperature 193
_exptl_crystal_density_diffrn 1.303
_exptl_crystal_preparation pentafluorobenzene
_refine_ls_R_factor_gt 5.76
_refine_ls_wR_factor_gt 5.76
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1100191
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
H1 H 0.471(6) 0.224(5) 0.654(4)
Ga1 Ga 0.43899(6) 0.13926(6) 0.68597(5)
C1 C 0.3907(6) 0.0611(5) 0.6059(5)
C2 C 0.4473(9) -0.0139(6) 0.6214(7)
H2 H 0.43900 -0.03500 0.66800
H3 H 0.51320 -0.00340 0.62360
H4 H 0.42510 -0.05020 0.58230
C3 C 0.2895(8) 0.0416(10) 0.6077(9)
H5 H 0.24960 0.08460 0.58940
H6 H 0.28410 0.03050 0.65790
H7 H 0.27030 -0.00270 0.57700
C4 C 0.4014(14) 0.0903(7) 0.5331(5)
H8 H 0.38390 0.05070 0.49630
H9 H 0.46610 0.10500 0.53520
H10 H 0.36110 0.13440 0.52010
Ga2 Ga 0.51312(7) 0.29563(6) 0.68082(5)
C5 C 0.5092(7) 0.3768(5) 0.6021(5)
C6 C 0.5523(13) 0.4509(8) 0.6426(8)
H11 H 0.55210 0.49150 0.60700
H12 H 0.61610 0.44080 0.66790
H13 H 0.51520 0.46640 0.67810
C7 C 0.5680(18) 0.3525(11) 0.5473(11)
H14 H 0.56770 0.39270 0.51130
H15 H 0.54210 0.30620 0.52250
H16 H 0.63180 0.34300 0.57290
C8 C 0.4082(10) 0.3961(10) 0.5628(9)
H17 H 0.37360 0.41580 0.59830
H18 H 0.37770 0.35040 0.54010
H19 H 0.40980 0.43440 0.52530
C9? C 0.617(3) 0.399(3) 0.602(2)
H20? H 0.61980 0.43020 0.55950
H21? H 0.65360 0.35320 0.60130
H22? H 0.64230 0.42810 0.64660
C10? C 0.458(3) 0.4452(19) 0.619(2)
H23? H 0.49380 0.49040 0.61120
H24? H 0.45080 0.44320 0.66930
H25? H 0.39740 0.44690 0.58610
C11? C 0.471(4) 0.338(2) 0.529(2)
H26? H 0.40720 0.32060 0.52800
H27? H 0.50980 0.29430 0.52300
H28? H 0.47060 0.37370 0.48900
Ga3 Ga 0.27617(6) 0.21307(5) 0.76843(4)
H29 H 0.334(4) 0.173(3) 0.710(3)
H30 H 0.621(4) 0.261(3) 0.688(3)
C12 C 0.2454(7) 0.1409(6) 0.8451(6)
C13 C 0.311(4) 0.156(2) 0.9182(14)
H31 H 0.32450 0.10850 0.94480
H32 H 0.28090 0.19120 0.94690
H33 H 0.36850 0.17860 0.90960
C14 C 0.268(3) 0.0543(13) 0.828(2)
H34 H 0.33410 0.04900 0.82820
H35 H 0.23160 0.03990 0.78030
H36 H 0.25120 0.02140 0.86560
C15 C 0.146(2) 0.138(3) 0.852(3)
H37 H 0.13940 0.10380 0.89200
H38 H 0.10770 0.11930 0.80650
H39 H 0.12500 0.18870 0.86240
C16? C 0.783(4) 0.194(2) 0.599(2)
H40? H 0.79890 0.16390 0.55900
H41? H 0.83690 0.22370 0.62200
H42? H 0.73130 0.22780 0.57930
C17? C 0.680(3) 0.095(3) 0.631(3)
H43? H 0.68410 0.07390 0.58380
H44? H 0.62290 0.12450 0.62700
H45? H 0.68010 0.05400 0.66640
C18? C 0.841(3) 0.097(2) 0.6966(19)
H46? H 0.82740 0.07710 0.74210
H47? H 0.89390 0.13160 0.70770
H48? H 0.85520 0.05550 0.66640
C19 C 0.1875(6) 0.2829(6) 0.7044(5)
C20 C 0.1436(11) 0.3377(9) 0.7545(8)
H49 H 0.19320 0.36390 0.78810
H50 H 0.10620 0.30840 0.78230
H51 H 0.10420 0.37490 0.72410
C21 C 0.1081(9) 0.2401(10) 0.6580(8)
H52 H 0.06190 0.27600 0.63280
H53 H 0.07930 0.20700 0.68910
H54 H 0.13160 0.20950 0.62210
C22 C 0.2382(11) 0.3319(11) 0.6579(9)
H55 H 0.25590 0.30080 0.61960
H56 H 0.29400 0.35340 0.68860
H57 H 0.19730 0.37280 0.63560
Ga1F* Ga 0.56101(6) 0.13926(6) 0.81403(5)
H1F* H 0.529(6) 0.224(5) 0.846(4)
Ga2F* Ga 0.48688(7) 0.29563(6) 0.81918(5)
Ga3F* Ga 0.72383(6) 0.21307(5) 0.73157(4)
H29F* H 0.666(4) 0.173(3) 0.790(3)
C1F* C 0.6093(6) 0.0611(5) 0.8941(5)
C2F* C 0.5527(9) -0.0139(6) 0.8786(7)
H2F* H 0.56100 -0.03500 0.83200
H3F* H 0.48680 -0.00340 0.87640
H4F* H 0.57490 -0.05020 0.91770
C3F* C 0.7105(8) 0.0416(10) 0.8923(9)
H5F* H 0.75040 0.08460 0.91060
H6F* H 0.71590 0.03050 0.84210
H7F* H 0.72970 -0.00270 0.92300
C4F* C 0.5986(14) 0.0903(7) 0.9669(5)
H8F* H 0.61610 0.05070 1.00370
H9F* H 0.53390 0.10500 0.96480
H10F* H 0.63890 0.13440 0.97990
C12F* C 0.7546(7) 0.1409(6) 0.6549(6)
C13F* C 0.689(4) 0.156(2) 0.5818(14)
H31F* H 0.67550 0.10850 0.55520
H32F* H 0.71910 0.19120 0.55310
H33F* H 0.63150 0.17860 0.59040
C14F* C 0.732(3) 0.0543(13) 0.672(2)
H34F* H 0.66590 0.04900 0.67180
H35F* H 0.76840 0.03990 0.71970
H36F* H 0.74880 0.02140 0.63440
C15F* C 0.854(2) 0.138(3) 0.648(3)
H37F* H 0.86060 0.10380 0.60800
H38F* H 0.89230 0.11930 0.69350
H39F* H 0.87500 0.18870 0.63760
C19F* C 0.8125(6) 0.2829(6) 0.7956(5)
C20F* C 0.8564(11) 0.3377(9) 0.7455(8)
H49F* H 0.80680 0.36390 0.71190
H50F* H 0.89380 0.30840 0.71770
H51F* H 0.89580 0.37490 0.77590
C21F* C 0.8919(9) 0.2401(10) 0.8420(8)
H52F* H 0.93810 0.27600 0.86720
H53F* H 0.92070 0.20700 0.81090
H54F* H 0.86840 0.20950 0.87790
C22F* C 0.7618(11) 0.3319(11) 0.8421(9)
H55F* H 0.74410 0.30080 0.88040
H56F* H 0.70600 0.35340 0.81140
H57F* H 0.80270 0.37280 0.86440
C5F* C 0.4908(7) 0.3768(5) 0.8979(5)
C6F* C 0.4477(13) 0.4509(8) 0.8574(8)
H11F* H 0.44790 0.49150 0.89300
H12F* H 0.38390 0.44080 0.83210
H13F* H 0.48480 0.46640 0.82190
C7F* C 0.4320(18) 0.3525(11) 0.9527(11)
H14F* H 0.43230 0.39270 0.98870
H15F* H 0.45790 0.30620 0.97750
H16F* H 0.36820 0.34300 0.92710
C8F* C 0.5918(10) 0.3961(10) 0.9372(9)
H17F* H 0.62640 0.41580 0.90170
H18F* H 0.62230 0.35040 0.95990
H19F* H 0.59020 0.43440 0.97470
H30F* H 0.379(4) 0.261(3) 0.812(3)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Ga 1.25
|
1100192.cif | #------------------------------------------------------------------------------
#$Date: 2016-03-04 15:57:10 +0200 (Fri, 04 Mar 2016) $
#$Revision: 177554 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/01/1100192.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_1100192
loop_
_publ_author_name
'Breit, Bernhard'
'Winde, Roland'
'Mackewitz, Thomas'
'Paciello, Rocco'
'Harms, Klaus'
_publ_section_title
;
Phosphabenzenes as Monodentate \p-Acceptor Ligands for Rhodium-Catalyzed
Hydroformylation
;
_journal_coden_ASTM CEUJED
_journal_issue 14
_journal_name_full 'Chemistry - A European Journal'
_journal_page_last 3121
_journal_paper_doi
10.1002/1521-3765(20010716)7:14<3106::aid-chem3106>3.0.co;2-y
_journal_volume 7
_journal_year 2001
_chemical_formula_moiety
;
C47 H34 Cl1 O1 P2 Rh1,0.5(C1 H2 Cl2)
;
_chemical_formula_sum 'C47.5 H35 Cl2 O P2 Rh'
_chemical_name_systematic
;
trans-Carbonyl-chloro-bis(2,4,6-triphenylphosphabenzene)-rhodium dichloromethane solvate
;
_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 79.09(1)
_cell_angle_beta 74.83(1)
_cell_angle_gamma 74.74(1)
_cell_formula_units_Z 2
_cell_length_a 10.966(1)
_cell_length_b 13.868(1)
_cell_length_c 14.306(1)
_cell_volume 2008.754
_diffrn_ambient_temperature 193
_exptl_crystal_colour yellow.
_exptl_crystal_density_diffrn 1.418
_exptl_crystal_description irregular
_refine_ls_R_factor_gt 7.16
_refine_ls_wR_factor_gt 7.16
_cod_original_formula_sum 'C47.5 H35 Cl2 O1 P2 Rh1'
_cod_database_code 1100192
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
Rh1 Rh 0.31564(3) 0.25385(2) 0.28112(2)
Cl1 Cl 0.26249(16) 0.43066(10) 0.26317(11)
C1 C 0.3567(5) 0.1165(4) 0.2921(4)
O1 O 0.3817(5) 0.0334(3) 0.2991(4)
P1 P 0.13322(11) 0.25234(9) 0.40231(9)
C2 C 0.0836(4) 0.3081(3) 0.5075(3)
C3 C -0.0362(5) 0.3049(4) 0.5686(3)
H1 H -0.05920 0.33810 0.62510
C4 C -0.1279(5) 0.2567(4) 0.5549(3)
C5 C -0.1007(4) 0.2026(4) 0.4762(3)
H2 H -0.16430 0.16940 0.47210
C6 C 0.0130(4) 0.1934(3) 0.4029(3)
C7 C 0.1702(4) 0.3623(4) 0.5325(3)
C8 C 0.3039(5) 0.3229(4) 0.5166(4)
H3 H 0.34080 0.26100 0.49020
C9 C 0.3828(5) 0.3748(5) 0.5395(4)
H4 H 0.47370 0.34810 0.52890
C10 C 0.3291(6) 0.4651(4) 0.5778(4)
H5 H 0.38370 0.49970 0.59340
C11 C 0.1970(5) 0.5053(4) 0.5935(4)
H6 H 0.16090 0.56760 0.61920
C12 C 0.1177(5) 0.4536(4) 0.5711(3)
H7 H 0.02680 0.48060 0.58230
C13 C -0.2571(5) 0.2702(4) 0.6244(3)
C14 C -0.3164(5) 0.3609(4) 0.6583(4)
H8 H -0.27390 0.41520 0.63640
C15 C -0.4358(5) 0.3765(4) 0.7232(4)
H9 H -0.47490 0.44020 0.74550
C16 C -0.4976(5) 0.2956(5) 0.7553(4)
H10 H -0.57940 0.30420 0.80020
C17 C -0.4406(5) 0.2047(4) 0.7222(4)
H11 H -0.48350 0.15060 0.74450
C18 C -0.3210(5) 0.1897(4) 0.6564(4)
H12 H -0.28270 0.12620 0.63330
C19 C 0.0322(4) 0.1361(4) 0.3213(3)
C20 C 0.0245(5) 0.0343(4) 0.3395(4)
H13 H -0.00110 0.00390 0.40470
C21 C 0.0539(6) -0.0210(4) 0.2637(5)
H14 H 0.04560 -0.08900 0.27650
C22 C 0.0951(6) 0.0205(5) 0.1696(5)
H15 H 0.11650 -0.01970 0.11820
C23 C 0.1059(5) 0.1170(5) 0.1485(4)
H16 H 0.13660 0.14420 0.08300
C24 C 0.0711(5) 0.1781(4) 0.2250(4)
H17 H 0.07450 0.24720 0.21040
P2 P 0.49853(11) 0.25691(9) 0.16179(9)
C25 C 0.5162(4) 0.3124(3) 0.0422(3)
C26 C 0.6391(5) 0.3064(4) -0.0185(3)
H18 H 0.64380 0.33860 -0.08370
C27 C 0.7558(5) 0.2574(4) 0.0077(3)
C28 C 0.7604(4) 0.2025(4) 0.0996(4)
H19 H 0.84290 0.16700 0.11130
C29 C 0.6519(4) 0.1962(4) 0.1755(3)
C30 C 0.4006(4) 0.3675(4) 0.0037(3)
C31 C 0.4016(5) 0.4578(4) -0.0592(3)
H20 H 0.47700 0.48460 -0.07700
C32 C 0.2938(6) 0.5086(4) -0.0959(4)
H21 H 0.29590 0.56980 -0.13870
C33 C 0.1835(5) 0.4711(5) -0.0710(4)
H22 H 0.10960 0.50680 -0.09600
C34 C 0.1803(5) 0.3810(5) -0.0091(4)
H23 H 0.10470 0.35450 0.00750
C35 C 0.2869(5) 0.3304(4) 0.0282(4)
H24 H 0.28370 0.26930 0.07110
C36 C 0.8800(5) 0.2653(4) -0.0648(3)
C37 C 0.9890(5) 0.1867(4) -0.0730(4)
H25 H 0.98610 0.12400 -0.03280
C38 C 1.1026(5) 0.1996(5) -0.1404(4)
H26 H 1.17670 0.14520 -0.14650
C39 C 1.1091(5) 0.2905(6) -0.1985(4)
H27 H 1.18740 0.29870 -0.24380
C40 C 1.0034(6) 0.3676(5) -0.1907(4)
H28 H 1.00770 0.43000 -0.23110
C41 C 0.8890(5) 0.3570(4) -0.1247(4)
H29 H 0.81580 0.41220 -0.11980
C42 C 0.6639(4) 0.1320(4) 0.2699(4)
C43 C 0.6088(5) 0.1673(4) 0.3588(4)
H30 H 0.56680 0.23630 0.36110
C44 C 0.6146(6) 0.1019(5) 0.4450(4)
H31 H 0.57600 0.12650 0.50610
C45 C 0.6753(6) 0.0027(6) 0.4425(5)
H32 H 0.67830 -0.04130 0.50190
C46 C 0.7320(7) -0.0338(5) 0.3553(5)
H33 H 0.77400 -0.10300 0.35400
C47 C 0.7278(6) 0.0304(4) 0.2691(4)
H34 H 0.76880 0.00520 0.20850
C48? C 0.539(3) 0.048(3) -0.050(2)
H35? H 0.53050 0.12010 -0.06330
H36? H 0.60380 0.01900 -0.10270
Cl2? Cl 0.3993(11) 0.0232(13) -0.0523(9)
Cl3? Cl 0.5956(12) 0.0076(8) 0.0499(9)
loop_
_atom_type_symbol
_atom_type_radius_bond
C 0.68
H 0.23
Cl 0.99
O 0.68
P 1.05
Rh 1.45
|