#------------------------------------------------------------------------------
#$Date: 2024-06-05 05:22:05 +0300 (Wed, 05 Jun 2024) $
#$Revision: 292201 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571777.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_1571777
loop_
_publ_author_name
'Qin, Hui-Yu'
'Zhang, Bing-Guang'
'Sun, Qiao-Zhen'
_publ_section_title
;
Poly[[{\m2-5-[(dimethylamino)(thioxo)methoxy]benzene-1,3-dicarboxylato-\k4
O 1,O 1′:O 3,O 3′}(\m2-4,4′-dipyridylamine-\k2 N 4:N
4′)cobalt(II)] dimethylformamide hemisolvate monohydrate]
;
_journal_coeditor_code WM4212
_journal_issue 6
_journal_name_full IUCrData
_journal_paper_doi 10.1107/S2414314624004899
_journal_volume 9
_journal_year 2024
_chemical_formula_iupac
'[Co (C11 H9 N1 O5 S1) (C10 H9 N3)], 0.5C3 H7 N O, H2 O'
_chemical_formula_moiety 'C21 H18 Co1 N4 O5 S1, 0.5(C3 H7 N O), H2 O'
_chemical_formula_sum 'C22.5 H23.5 Co N4.5 O6.5 S'
_chemical_formula_weight 551.95
_chemical_name_systematic
;Poly[[{\m~2~-5-[(dimethylamino)(thioxo)methoxy]benzene-1,3-dicarboxylato-\k^4^O^1^,O^1'^:O^3^,O^3'^}(\m~2-~4,4'-dipyridylamine-\k^2^N^4^:N^4'^)cobalt(II)]
dimethylformamide hemisolvate monohydrate]
;
_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 mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 103.485(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 11.2451(14)
_cell_length_b 14.4734(17)
_cell_length_c 15.232(2)
_cell_measurement_reflns_used 4852
_cell_measurement_temperature 298.0
_cell_measurement_theta_max 26.309
_cell_measurement_theta_min 2.922
_cell_volume 2410.7(5)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov et al., 2009), XP (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 298.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker APEXII CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0685
_diffrn_reflns_av_unetI/netI 0.0532
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 21131
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.021
_diffrn_reflns_theta_min 2.479
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.849
_exptl_absorpt_correction_T_max 0.7454
_exptl_absorpt_correction_T_min 0.6430
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 1.521
_exptl_crystal_description prism
_exptl_crystal_F_000 1140
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.18
_refine_diff_density_max 0.759
_refine_diff_density_min -0.421
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 355
_refine_ls_number_reflns 4711
_refine_ls_number_restraints 64
_refine_ls_restrained_S_all 1.059
_refine_ls_R_factor_all 0.0898
_refine_ls_R_factor_gt 0.0531
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+2.1129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1290
_refine_ls_wR_factor_ref 0.1495
_reflns_number_gt 3216
_reflns_number_total 4711
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file wm4212.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 1571777
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
2 0 0 1737.03 54.39
-2 0 0 1764.42 54.29
3 0 0 0.70 1.90
-3 0 0 1.30 1.70
-4 0 0 3589.54 111.79
4 0 0 3632.54 112.19
-5 0 0 -5.20 1.80
5 0 0 -1.70 2.70
6 0 0 3093.29 95.59
-6 0 0 2992.80 94.49
-7 0 0 -2.60 1.70
7 0 0 3.40 3.50
8 0 0 72.89 7.40
9 0 0 4.10 4.50
9 0 0 3.90 4.60
10 0 0 161.58 12.00
10 0 0 196.48 12.20
11 0 0 0.40 6.10
12 0 0 34.20 8.30
13 0 0 12.10 8.80
-2 -1 0 104.49 5.20
2 1 0 98.79 5.00
3 -1 0 3.40 1.40
-3 -1 0 2.40 2.40
3 1 0 5.70 2.60
4 -1 0 3.80 1.90
-4 -1 0 2.80 2.50
4 1 0 5.30 2.70
-5 -1 0 443.66 15.80
5 -1 0 445.06 15.40
5 1 0 449.76 16.30
6 -1 0 280.17 11.40
-6 -1 0 307.37 11.60
6 1 0 290.47 12.30
-7 -1 0 26.70 3.50
7 -1 0 38.00 4.20
7 1 0 33.10 4.70
8 -1 0 17.80 4.20
-8 -1 0 9.90 3.20
8 1 0 17.80 4.70
9 -1 0 5.60 4.40
-9 -1 0 7.10 2.90
9 -1 0 7.80 4.30
9 1 0 3.30 4.80
9 1 0 11.90 5.40
10 -1 0 119.49 10.30
10 -1 0 111.39 10.00
10 1 0 109.39 11.30
11 -1 0 31.60 6.60
11 1 0 33.30 7.40
11 1 0 27.60 7.40
12 -1 0 2.00 6.80
12 1 0 0.60 8.30
12 1 0 8.00 7.80
13 -1 0 2.50 8.80
13 -1 0 21.00 8.60
13 1 0 36.30 10.30
13 1 0 28.30 10.10
0 -2 0 15.40 1.70
0 2 0 17.10 1.80
-1 -2 0 4246.88 132.59
1 2 0 4324.37 132.59
-2 -2 0 418.56 14.90
2 2 0 439.36 14.90
-3 -2 0 1446.96 46.80
3 2 0 1493.05 47.00
-4 -2 0 333.97 12.70
4 -2 0 342.07 11.00
4 2 0 325.57 13.10
-5 -2 0 1024.80 33.90
5 -2 0 1034.10 32.60
5 2 0 1019.50 34.10
6 -2 0 39.50 4.30
-6 -2 0 30.00 4.20
6 2 0 49.10 5.10
7 -2 0 344.87 13.00
-7 -2 0 332.37 13.80
7 2 0 344.37 14.40
-8 -2 0 -1.10 3.70
8 -2 0 -2.10 3.20
8 2 0 -1.70 4.60
9 -2 0 27.10 4.60
-9 -2 0 21.60 4.40
9 -2 0 27.20 4.80
9 2 0 14.20 6.00
9 2 0 9.50 5.20
-10 -2 0 5.60 3.90
10 -2 0 10.10 5.20
10 -2 0 6.00 4.70
10 2 0 18.60 6.90
11 -2 0 33.30 6.40
-11 -2 0 30.70 3.80
11 -2 0 36.00 6.50
11 2 0 32.30 8.20
11 2 0 36.90 9.40
12 -2 0 -8.00 6.00
12 2 0 5.50 8.50
13 -2 0 5.40 8.70
13 -2 0 7.60 8.40
13 2 0 1.10 9.00
13 2 0 -22.00 9.70
0 -3 0 0.20 2.00
0 3 0 3.30 2.10
0 3 0 2.40 2.10
1 -3 0 38.90 3.00
-1 -3 0 38.60 4.50
-1 3 0 41.00 2.50
1 3 0 36.50 3.50
-1 3 0 47.40 2.40
-2 -3 0 2.20 3.00
2 3 0 1.10 2.90
-3 -3 0 17.50 3.50
3 3 0 20.10 3.60
-4 -3 0 622.04 21.70
4 3 0 608.04 21.60
-5 -3 0 295.27 12.40
5 3 0 299.17 12.70
6 -3 0 1.30 1.90
-6 -3 0 3.20 3.60
6 3 0 1.40 3.90
7 -3 0 12.30 2.80
-7 -3 0 17.20 4.40
7 3 0 12.80 4.70
-8 -3 0 2.40 4.30
8 -3 0 4.40 3.20
8 -3 0 2.90 2.90
8 3 0 2.30 5.00
9 -3 0 59.59 5.70
-9 -3 0 65.09 6.70
9 -3 0 61.69 6.80
9 3 0 68.69 7.80
10 -3 0 23.40 5.10
10 -3 0 20.30 4.70
-10 -3 0 9.40 5.20
10 3 0 19.30 6.70
10 3 0 17.10 7.20
11 -3 0 37.30 6.10
-11 -3 0 27.40 5.90
11 -3 0 40.30 6.30
11 3 0 24.40 8.10
12 -3 0 21.10 6.60
12 -3 0 7.30 6.00
-12 -3 0 2.80 4.20
12 3 0 7.40 8.80
12 3 0 14.30 9.40
13 -3 0 -1.50 7.40
13 3 0 13.10 10.90
13 3 0 -9.30 9.90
0 -4 0 50.99 4.40
0 4 0 46.90 4.50
0 4 0 50.29 4.20
-1 -4 0 7.90 3.10
1 -4 0 9.40 2.10
-1 4 0 9.70 1.80
-1 4 0 10.30 1.90
1 4 0 9.80 3.10
2 -4 0 276.07 9.30
-2 -4 0 276.27 11.30
2 4 0 276.67 11.30
-3 -4 0 554.24 20.00
3 4 0 567.74 20.10
-4 -4 0 98.89 7.40
4 4 0 103.79 7.60
-5 -4 0 3.80 3.90
5 4 0 5.80 4.10
-6 -4 0 227.28 11.40
6 4 0 213.68 11.80
-7 -4 0 -2.50 4.20
7 -4 0 0.30 2.10
7 -4 0 1.60 2.00
7 4 0 0.60 4.70
8 -4 0 14.20 3.00
-8 -4 0 11.60 5.20
8 -4 0 14.20 3.20
8 4 0 28.60 5.70
9 -4 0 43.30 4.50
9 -4 0 47.70 4.80
-9 -4 0 44.80 6.50
9 4 0 47.60 7.50
9 4 0 50.09 7.80
10 -4 0 5.60 4.10
10 -4 0 6.50 4.40
-10 -4 0 6.40 6.10
10 4 0 4.70 6.90
10 4 0 3.10 6.70
11 -4 0 -5.80 4.40
-11 -4 0 0.10 6.00
11 -4 0 -4.70 5.10
11 4 0 -1.20 8.60
11 4 0 3.00 7.60
-12 -4 0 2.90 6.50
12 -4 0 -1.30 6.00
12 -4 0 0.30 5.60
12 4 0 7.10 10.00
12 4 0 4.90 9.30
-13 -4 0 6.80 5.60
13 -4 0 -2.10 6.80
13 4 0 3.10 12.20
13 4 0 19.30 11.10
0 -5 0 -1.90 2.60
0 5 0 -1.00 2.60
0 5 0 0.40 2.50
1 -5 0 1.70 2.30
-1 -5 0 0.70 2.90
-1 5 0 1.20 2.00
-1 5 0 0.90 1.90
1 5 0 0.40 3.00
-2 -5 0 4.90 3.50
2 -5 0 4.70 1.90
2 5 0 6.70 3.60
3 -5 0 -0.80 1.40
-3 -5 0 -1.50 3.60
3 5 0 0.00 3.70
4 -5 0 261.87 8.50
-4 -5 0 261.97 12.20
4 5 0 257.67 12.10
-5 -5 0 0.30 4.00
5 -5 0 1.70 0.90
5 5 0 -2.70 4.00
6 -5 0 40.80 2.70
-6 -5 0 35.20 5.60
6 5 0 36.90 5.80
7 -5 0 10.20 2.00
7 -5 0 11.90 2.20
-7 -5 0 3.10 4.90
8 -5 0 18.60 3.00
-8 -5 0 9.20 5.60
8 -5 0 18.70 2.90
8 5 0 14.90 6.40
-9 -5 0 26.40 6.80
9 -5 0 21.60 3.60
9 -5 0 23.80 3.90
9 5 0 7.00 6.60
-10 -5 0 8.50 6.70
10 -5 0 12.10 3.90
10 -5 0 18.60 4.50
10 5 0 -0.30 7.20
-11 -5 0 -6.20 6.90
11 -5 0 0.50 5.00
11 -5 0 7.70 4.70
11 5 0 2.70 8.00
11 5 0 -8.50 8.00
12 -5 0 -5.00 5.70
-12 -5 0 2.20 7.70
12 -5 0 -0.80 5.30
12 5 0 -22.40 9.30
12 5 0 -4.00 10.20
0 -6 0 8.60 3.20
0 6 0 11.00 3.20
0 6 0 6.10 2.80
1 -6 0 8.80 2.80
-1 -6 0 9.80 3.50
-1 6 0 10.80 2.50
-1 6 0 9.10 2.50
1 6 0 13.40 3.50
1 6 0 10.20 3.60
2 -6 0 21.40 2.80
-2 -6 0 14.50 4.10
2 6 0 17.00 4.10
-3 -6 0 637.34 23.10
3 -6 0 632.64 20.80
3 6 0 635.14 23.00
-4 -6 0 538.05 21.10
4 -6 0 557.94 18.00
4 6 0 573.24 21.20
5 -6 0 27.00 2.50
-5 -6 0 30.20 5.50
5 6 0 40.40 5.80
-6 -6 0 16.70 5.30
6 -6 0 16.80 1.80
6 6 0 40.30 5.50
7 -6 0 261.17 9.50
-7 -6 0 271.17 14.70
7 6 0 273.37 14.70
8 -6 0 7.80 2.60
-8 -6 0 5.80 6.10
8 -6 0 2.20 2.30
8 6 0 -1.70 6.20
8 6 0 18.80 6.80
-9 -6 0 28.70 7.50
9 -6 0 21.40 3.50
9 -6 0 20.00 3.40
9 6 0 17.90 7.90
9 6 0 19.80 7.90
10 -6 0 -0.80 3.70
-10 -6 0 -2.20 7.40
10 -6 0 2.10 3.50
10 6 0 5.90 8.00
10 6 0 -0.70 8.30
11 -6 0 15.20 4.60
11 -6 0 15.40 5.30
-11 -6 0 18.60 8.70
11 6 0 29.30 10.10
11 6 0 22.10 9.80
12 -6 0 -15.10 5.50
-12 -6 0 1.30 9.20
12 -6 0 -1.70 5.00
12 6 0 4.10 10.40
12 6 0 3.50 10.30
0 -7 0 -5.80 3.00
0 7 0 2.10 3.00
0 7 0 -3.60 3.10
1 -7 0 82.49 6.20
-1 -7 0 84.49 7.00
-1 7 0 77.29 5.40
-1 7 0 71.49 5.40
1 7 0 81.79 6.60
1 7 0 89.59 6.70
-2 -7 0 5.80 4.30
2 -7 0 4.00 2.70
-2 7 0 5.40 1.60
2 7 0 7.50 4.10
-2 7 0 5.20 1.50
2 7 0 6.30 3.90
3 -7 0 202.18 8.40
-3 -7 0 200.98 11.10
3 7 0 206.38 10.90
3 7 0 191.98 10.70
4 -7 0 10.50 2.20
-4 -7 0 6.40 4.80
4 7 0 11.40 4.50
4 7 0 4.50 4.50
-5 -7 0 -1.70 4.90
5 -7 0 -0.20 1.70
5 7 0 -2.70 4.30
5 7 0 4.20 4.80
6 -7 0 128.79 5.40
-6 -7 0 128.29 11.10
6 7 0 140.69 10.90
6 7 0 87.59 9.30
-7 -7 0 46.20 7.40
7 -7 0 45.00 3.70
7 7 0 52.79 7.70
7 7 0 36.50 7.30
-8 -7 0 15.90 7.10
8 -7 0 19.90 2.70
8 7 0 28.10 7.70
8 7 0 23.30 7.60
9 -7 0 86.59 6.00
9 -7 0 86.49 6.40
-9 -7 0 94.29 10.20
9 7 0 99.49 10.90
9 7 0 76.79 10.30
10 -7 0 67.09 6.80
-10 -7 0 25.50 11.60
10 -7 0 46.30 4.50
10 7 0 29.90 10.00
10 7 0 46.20 10.10
-11 -7 0 14.10 10.70
11 -7 0 8.50 4.80
11 -7 0 9.70 4.00
11 7 0 5.70 10.00
11 7 0 6.50 10.10
12 -7 0 0.70 5.70
-12 -7 0 16.90 10.70
12 -7 0 13.20 5.10
12 7 0 1.80 11.20
12 7 0 0.70 11.50
0 -8 0 25.30 4.40
0 8 0 17.10 3.70
0 8 0 17.10 4.00
1 -8 0 218.58 10.10
-1 -8 0 233.98 11.30
1 8 0 222.18 10.70
1 8 0 210.68 10.60
-1 8 0 227.68 9.50
-1 8 0 215.28 9.50
2 -8 0 80.49 6.30
-2 -8 0 72.89 8.10
-2 8 0 75.49 4.30
2 8 0 58.49 6.20
-2 8 0 77.19 4.20
2 8 0 84.49 7.80
3 -8 0 694.03 23.10
-3 -8 0 680.53 25.30
3 8 0 655.83 25.00
3 8 0 675.43 25.10
-4 -8 0 228.18 12.80
4 -8 0 220.88 9.30
4 8 0 208.58 12.40
4 8 0 247.38 12.80
5 -8 0 51.39 4.40
-5 -8 0 47.50 6.90
5 8 0 43.80 6.60
6 -8 0 5.10 2.20
-6 -8 0 7.50 5.90
6 8 0 1.40 5.80
6 8 0 -1.50 5.40
-7 -8 0 22.50 7.00
7 -8 0 21.60 2.70
7 8 0 14.80 7.10
7 8 0 11.30 11.30
8 -8 0 108.09 5.90
-8 -8 0 110.09 12.50
8 8 0 117.39 13.30
-9 -8 0 298.07 18.30
9 -8 0 282.67 11.30
9 -8 0 298.87 11.80
9 8 0 300.47 19.00
9 8 0 303.87 18.80
10 -8 0 60.09 6.20
10 -8 0 55.09 5.00
-10 -8 0 50.19 10.50
10 8 0 51.49 10.60
10 8 0 61.09 11.20
11 -8 0 12.70 4.80
-11 -8 0 5.30 12.00
11 -8 0 9.00 4.10
11 8 0 24.80 10.50
11 8 0 7.70 11.10
12 -8 0 11.10 5.80
12 -8 0 8.50 4.90
12 8 0 4.00 12.60
12 8 0 12.10 11.70
0 -9 0 -3.80 3.90
0 9 0 -2.60 3.50
0 9 0 5.10 3.80
-1 -9 0 16.00 4.90
1 -9 0 13.10 4.30
1 9 0 12.10 4.30
-1 9 0 20.10 3.60
-1 9 0 8.40 3.30
1 9 0 9.70 4.50
2 -9 0 228.08 10.90
-2 -9 0 235.98 12.70
-2 9 0 241.08 8.90
-2 9 0 228.98 8.90
2 9 0 237.18 12.00
2 9 0 229.98 12.10
-3 -9 0 73.29 7.70
3 -9 0 92.49 6.90
3 9 0 96.59 8.90
3 9 0 70.39 7.30
4 -9 0 162.38 8.10
-4 -9 0 165.98 11.40
4 9 0 133.49 11.00
5 -9 0 22.30 3.40
-5 -9 0 18.70 6.40
5 9 0 31.00 6.30
5 9 0 24.30 6.30
-6 -9 0 16.90 6.80
6 -9 0 26.00 3.30
6 9 0 35.00 7.10
7 -9 0 222.88 9.20
-7 -9 0 206.88 16.20
-8 -9 0 5.60 7.50
8 -9 0 5.70 2.80
8 9 0 5.60 7.60
9 -9 0 35.60 3.80
9 9 0 27.50 9.50
9 9 0 28.70 9.10
10 -9 0 -4.20 3.70
10 -9 0 0.20 3.30
10 9 0 12.00 10.50
10 9 0 -0.20 9.10
11 -9 0 9.40 4.10
11 -9 0 15.70 4.70
-11 -9 0 18.00 10.60
11 9 0 9.40 11.70
11 9 0 8.40 10.70
0 -10 0 566.84 22.30
0 10 0 571.14 21.20
0 10 0 575.04 21.20
-1 -10 0 169.08 11.10
1 -10 0 169.28 10.00
1 10 0 143.09 10.60
1 10 0 182.48 10.10
-1 10 0 164.28 8.90
-1 10 0 167.38 8.90
2 -10 0 92.09 7.90
-2 -10 0 91.39 9.80
-2 10 0 88.39 5.40
2 10 0 93.49 8.90
2 10 0 99.29 9.20
-2 10 0 87.39 5.30
-3 -10 0 -2.70 5.40
3 -10 0 1.00 3.60
3 10 0 5.20 5.30
-4 -10 0 212.78 13.50
4 -10 0 209.78 10.40
4 10 0 235.88 14.10
4 10 0 214.88 13.40
-5 -10 0 25.90 7.70
5 -10 0 17.80 3.70
5 10 0 19.70 6.70
5 10 0 3.60 6.00
6 -10 0 139.99 7.90
-6 -10 0 139.39 13.40
6 10 0 110.09 13.00
-7 -10 0 3.50 7.70
7 -10 0 7.10 3.30
7 10 0 8.90 8.00
8 -10 0 11.10 3.30
8 10 0 22.40 9.00
-9 -10 0 17.00 9.40
9 -10 0 28.60 3.90
9 10 0 16.60 9.80
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_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 63601
_shelx_res_file
;
TITL mo_0322_3_P 1 21/n 1 R = 0.08
mo_0322_3_0m.res
created by SHELXL-2018/3 at 13:28:44 on 22-Apr-2024
CELL 0.71073 11.2451 14.4734 15.232 90 103.485 90
ZERR 2 0.0014 0.0017 0.002 0 0.004 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Co N O S
UNIT 90 94 4 18 26 4
EQIV $1 -0.5+X,0.5-Y,-0.5+Z
EQIV $2 2-X,1-Y,1-Z
EQIV $3 0.5+X,0.5-Y,0.5+Z
EQIV $4 1+X,+Y,1+Z
DFIX 2.4 H7e O2_$1
ISOR 0.01 0.02 C23
SIMU 0.01 0.02 2 N5 O6 C22 C24 C23
DFIX 2.1 H7d O4
DFIX 1.4 C24 N5 N5 C23
DFIX 2.4 C24 C23
DFIX 2.4 C24 C22 C22 C23
DFIX 1.2 C22 O6
DFIX 1.4 N5 C22
ISOR 0.01 0.02 O6 C22 N5 C24 C23
DFIX 2.3 N5 O6
ISOR 0.005 0.01 O6
L.S. 20 0 11
PLAN 5
TEMP 25
CONF
HTAB N3 O6
HTAB N3 O8
HTAB C13 O2_$2
HTAB O7 O2_$1
HTAB O7 O4
HTAB O8 O5_$3
HTAB O8 O7_$4
MORE -1
BOND $H
fmap 2
acta
OMIT 0 1 5
OMIT 0 2 1
OMIT 0 2 2
OMIT 1 0 1
OMIT 1 3 1
OMIT 10 0 4
OMIT 11 0 3
REM
REM
REM
WGHT 0.074200 2.112900
FVAR 0.37468
CO1 3 0.739270 0.606960 0.448751 11.00000 0.04959 0.02677 =
0.02676 -0.00185 0.01366 -0.00251
S1 6 0.212935 0.445894 0.062542 11.00000 0.07048 0.06710 =
0.07502 0.02949 0.00235 0.00371
O1 5 0.579282 0.534363 0.383637 11.00000 0.04471 0.04348 =
0.05236 -0.02070 0.01577 -0.00225
O2 5 0.752858 0.492682 0.354779 11.00000 0.04308 0.07061 =
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O3 5 0.265242 0.322389 0.192962 11.00000 0.02962 0.05166 =
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O4 5 0.595021 0.180670 0.053986 11.00000 0.05525 0.03901 =
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O5 5 0.760210 0.213397 0.155316 11.00000 0.05051 0.06453 =
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N1 4 0.068167 0.355433 0.150053 11.00000 0.03532 0.04917 =
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N2 4 0.811856 0.523883 0.560982 11.00000 0.05291 0.03046 =
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N3 4 0.964450 0.379061 0.799984 11.00000 0.05485 0.03753 =
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AFIX 43
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AFIX 0
N4 4 0.835027 0.202527 0.975035 11.00000 0.06234 0.03013 =
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C2 1 0.574523 0.415086 0.273336 11.00000 0.03533 0.03219 =
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C3 1 0.447919 0.406208 0.257373 11.00000 0.03982 0.03286 =
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AFIX 43
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AFIX 0
C4 1 0.389306 0.340158 0.197472 11.00000 0.03442 0.03869 =
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C5 1 0.178994 0.374064 0.136178 11.00000 0.04615 0.03657 =
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C6 1 -0.038525 0.403471 0.098087 11.00000 0.04289 0.05723 =
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AFIX 137
H6A 2 -0.061594 0.451505 0.134299 11.00000 -1.50000
H6B 2 -0.104911 0.360578 0.080358 11.00000 -1.50000
H6C 2 -0.019640 0.430104 0.045232 11.00000 -1.50000
AFIX 0
C7 1 0.046989 0.290007 0.215735 11.00000 0.04479 0.07760 =
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AFIX 137
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H7C 2 0.093632 0.307415 0.274533 11.00000 -1.50000
AFIX 0
C8 1 0.452662 0.284292 0.150617 11.00000 0.04188 0.03353 =
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AFIX 43
H8 2 0.411067 0.242145 0.108353 11.00000 -1.20000
AFIX 0
C9 1 0.578271 0.291629 0.167133 11.00000 0.03931 0.03367 =
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C10 1 0.648817 0.225613 0.123200 11.00000 0.04553 0.03156 =
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C11 1 0.639414 0.356889 0.228857 11.00000 0.03174 0.03680 =
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AFIX 43
H11 2 0.724132 0.361467 0.240303 11.00000 -1.20000
AFIX 0
C12 1 0.931558 0.523976 0.601784 11.00000 0.05214 0.04162 =
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AFIX 43
H12 2 0.983755 0.557585 0.574663 11.00000 -1.20000
AFIX 0
C13 1 0.982032 0.478553 0.679814 11.00000 0.04593 0.04334 =
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AFIX 43
H13 2 1.065719 0.482183 0.704535 11.00000 -1.20000
AFIX 0
C14 1 0.906938 0.426114 0.722831 11.00000 0.05317 0.02654 =
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C15 1 0.916471 0.323445 0.857650 11.00000 0.05809 0.03041 =
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C16 1 0.798439 0.327479 0.868788 11.00000 0.05872 0.03567 =
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AFIX 43
H16 2 0.743752 0.371028 0.837599 11.00000 -1.20000
AFIX 0
C17 1 0.762526 0.266005 0.926858 11.00000 0.05132 0.04011 =
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AFIX 43
H17 2 0.682131 0.269181 0.932704 11.00000 -1.20000
AFIX 0
C18 1 0.950891 0.202038 0.967004 11.00000 0.06561 0.03429 =
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AFIX 43
H18 2 1.004311 0.159659 1.001410 11.00000 -1.20000
AFIX 0
C19 1 0.995921 0.259636 0.911640 11.00000 0.05685 0.04111 =
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AFIX 43
H19 2 1.077847 0.256815 0.909575 11.00000 -1.20000
AFIX 0
C20 1 0.783675 0.423815 0.680844 11.00000 0.05789 0.04084 =
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AFIX 43
H20 2 0.729663 0.389357 0.705490 11.00000 -1.20000
AFIX 0
C21 1 0.741852 0.472819 0.602536 11.00000 0.04902 0.03921 =
0.03597 0.00280 0.00982 -0.01132
AFIX 43
H21 2 0.658501 0.470415 0.576267 11.00000 -1.20000
AFIX 0
PART -1
O6 5 1.210182 0.365611 0.830351 10.50000 0.13366 0.10762 =
0.10962 -0.00288 0.03134 0.00073
PART 1
O7 5 0.347001 0.202055 -0.069212 10.50000 0.08503 0.07457 =
0.08355 -0.03176 -0.03369 0.02289
AFIX 3
H7D 2 0.414831 0.198915 -0.032112 10.50000 -1.50000
H7E 2 0.317801 0.146795 -0.086502 10.50000 -1.50000
AFIX 0
PART -1
C23 1 1.493459 0.454610 0.945196 10.50000 0.16638 0.20553 =
0.21088 0.08675 0.01756 -0.06399
AFIX 3
H23A 2 1.466619 0.517120 0.949026 10.50000 -1.50000
H23B 2 1.561309 0.453770 0.916886 10.50000 -1.50000
H23C 2 1.518269 0.428940 1.004746 10.50000 -1.50000
AFIX 0
N5 4 1.406006 0.402416 0.899380 10.50000 0.18957 0.19285 =
0.17870 0.02987 0.03080 0.00318
C22 1 1.276712 0.429630 0.868280 10.50000 0.16751 0.16937 =
0.16115 0.02015 0.03963 0.00238
AFIX 43
H22 2 1.247808 0.488525 0.876167 10.50000 -1.20000
AFIX 0
C24 1 1.423796 0.308654 0.879183 10.50000 0.23343 0.24946 =
0.21924 -0.03621 0.03397 0.06738
AFIX 137
H24A 2 1.509290 0.297487 0.884281 10.50000 -1.50000
H24B 2 1.379160 0.295245 0.818744 10.50000 -1.50000
H24C 2 1.394999 0.269661 0.920830 10.50000 -1.50000
AFIX 0
PART 1
O8 5 1.236210 0.381214 0.833076 10.50000 0.09983 0.19239 =
0.03429 0.01991 0.01257 -0.05450
AFIX 3
H8A 2 1.283550 0.349024 0.876365 10.50000 -1.50000
H8B 2 1.255520 0.363564 0.785015 10.50000 -1.50000
AFIX 0
HKLF 4
REM mo_0322_3_P 1 21/n 1 R = 0.08
REM wR2 = 0.1495, GooF = S = 1.036, Restrained GooF = 1.059 for all data
REM R1 = 0.0531 for 3216 Fo > 4sig(Fo) and 0.0898 for all 4711 data
REM 355 parameters refined using 64 restraints
END
WGHT 0.0739 2.1454
REM Highest difference peak 0.759, deepest hole -0.421, 1-sigma level 0.076
Q1 1 1.5141 0.4053 0.8930 11.00000 0.05 0.76
Q2 1 0.2434 0.4007 0.1073 11.00000 0.05 0.42
Q3 1 1.4087 0.4412 0.9045 11.00000 0.05 0.39
Q4 1 0.3574 0.1846 -0.1000 11.00000 0.05 0.37
Q5 1 -0.0158 0.4859 0.0976 11.00000 0.05 0.36
;
_shelx_res_checksum 67755
loop_
_space_group_symop_operation_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_type_symbol
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.73927(5) 0.60696(3) 0.44875(3) 0.03359(18) Uani d 1 . .
S S1 0.21293(14) 0.44589(10) 0.06254(10) 0.0733(4) Uani d 1 . .
O O1 0.5793(2) 0.53436(19) 0.38364(19) 0.0461(7) Uani d 1 . .
O O2 0.7529(3) 0.4927(2) 0.3548(2) 0.0535(8) Uani d 1 . .
O O3 0.2652(2) 0.32239(19) 0.19296(19) 0.0456(7) Uani d 1 . .
O O4 0.5950(3) 0.18067(18) 0.05399(18) 0.0460(7) Uani d 1 . .
O O5 0.7602(3) 0.2134(2) 0.15532(19) 0.0510(8) Uani d 1 . .
N N1 0.0682(3) 0.3554(2) 0.1501(2) 0.0469(9) Uani d 1 . .
N N2 0.8119(3) 0.5239(2) 0.5610(2) 0.0372(7) Uani d 1 . .
N N3 0.9644(3) 0.3791(2) 0.8000(2) 0.0412(8) Uani d 1 . .
H H3 1.042657 0.385181 0.814726 0.049 Uiso calc 1 . .
N N4 0.8350(3) 0.2025(2) 0.9750(2) 0.0393(8) Uani d 1 . .
C C1 0.6393(4) 0.4844(2) 0.3406(2) 0.0349(8) Uani d 1 . .
C C2 0.5745(3) 0.4151(2) 0.2733(2) 0.0327(8) Uani d 1 . .
C C3 0.4479(4) 0.4062(2) 0.2574(3) 0.0366(9) Uani d 1 . .
H H3A 0.403355 0.444495 0.286860 0.044 Uiso calc 1 . .
C C4 0.3893(3) 0.3402(3) 0.1975(3) 0.0372(9) Uani d 1 . .
C C5 0.1790(4) 0.3741(3) 0.1362(3) 0.0440(10) Uani d 1 . .
C C6 -0.0385(4) 0.4035(3) 0.0981(3) 0.0567(12) Uani d 1 . .
H H6A -0.061594 0.451505 0.134299 0.085 Uiso calc 1 . .
H H6B -0.104911 0.360578 0.080358 0.085 Uiso calc 1 . .
H H6C -0.019640 0.430104 0.045232 0.085 Uiso calc 1 . .
C C7 0.0470(4) 0.2900(4) 0.2157(4) 0.0664(14) Uani d 1 . .
H H7A 0.071609 0.229571 0.200946 0.100 Uiso calc 1 . .
H H7B -0.038419 0.289331 0.215602 0.100 Uiso calc 1 . .
H H7C 0.093632 0.307415 0.274533 0.100 Uiso calc 1 . .
C C8 0.4527(4) 0.2843(3) 0.1506(3) 0.0376(9) Uani d 1 . .
H H8 0.411067 0.242145 0.108353 0.045 Uiso calc 1 . .
C C9 0.5783(3) 0.2916(2) 0.1671(2) 0.0331(8) Uani d 1 . .
C C10 0.6488(4) 0.2256(2) 0.1232(2) 0.0359(9) Uani d 1 . .
C C11 0.6394(3) 0.3569(2) 0.2289(2) 0.0328(8) Uani d 1 . .
H H11 0.724132 0.361467 0.240303 0.039 Uiso calc 1 . .
C C12 0.9316(4) 0.5240(3) 0.6018(3) 0.0432(10) Uani d 1 . .
H H12 0.983755 0.557585 0.574663 0.052 Uiso calc 1 . .
C C13 0.9820(4) 0.4786(3) 0.6798(3) 0.0419(9) Uani d 1 . .
H H13 1.065719 0.482183 0.704535 0.050 Uiso calc 1 . .
C C14 0.9069(4) 0.4261(2) 0.7228(2) 0.0359(9) Uani d 1 . .
C C15 0.9165(4) 0.3234(2) 0.8576(2) 0.0374(9) Uani d 1 . .
C C16 0.7984(4) 0.3275(3) 0.8688(2) 0.0418(9) Uani d 1 . .
H H16 0.743752 0.371028 0.837599 0.050 Uiso calc 1 . .
C C17 0.7625(4) 0.2660(3) 0.9269(2) 0.0418(9) Uani d 1 . .
H H17 0.682131 0.269181 0.932704 0.050 Uiso calc 1 . .
C C18 0.9509(4) 0.2020(3) 0.9670(3) 0.0459(10) Uani d 1 . .
H H18 1.004311 0.159659 1.001410 0.055 Uiso calc 1 . .
C C19 0.9959(4) 0.2596(3) 0.9116(3) 0.0441(10) Uani d 1 . .
H H19 1.077847 0.256815 0.909575 0.053 Uiso calc 1 . .
C C20 0.7837(4) 0.4238(3) 0.6808(3) 0.0439(10) Uani d 1 . .
H H20 0.729663 0.389357 0.705490 0.053 Uiso calc 1 . .
C C21 0.7419(4) 0.4728(3) 0.6025(3) 0.0414(9) Uani d 1 . .
H H21 0.658501 0.470415 0.576267 0.050 Uiso calc 1 . .
O O6 1.2102(17) 0.3656(14) 0.8304(14) 0.116(6) Uani d 0.5 A -1
O O7 0.3470(7) 0.2021(5) -0.0692(5) 0.090(3) Uani d 0.5 B 1
H H7D 0.414831 0.198915 -0.032112 0.135 Uiso d 0.5 B 1
H H7E 0.317801 0.146795 -0.086502 0.135 Uiso d 0.5 B 1
C C23 1.4935(17) 0.4546(13) 0.9452(13) 0.199(8) Uani d 0.5 A -1
H H23A 1.466619 0.517120 0.949026 0.298 Uiso d 0.5 A -1
H H23B 1.561309 0.453770 0.916886 0.298 Uiso d 0.5 A -1
H H23C 1.518269 0.428940 1.004746 0.298 Uiso d 0.5 A -1
N N5 1.4060(15) 0.4024(12) 0.8994(13) 0.189(6) Uani d 0.5 A -1
C C22 1.2767(15) 0.4296(13) 0.8683(16) 0.166(6) Uani d 0.5 A -1
H H22 1.247808 0.488525 0.876167 0.199 Uiso calc 0.5 A -1
C C24 1.424(2) 0.3087(13) 0.8792(19) 0.237(9) Uani d 0.5 A -1
H H24A 1.509290 0.297487 0.884281 0.356 Uiso calc 0.5 A -1
H H24B 1.379160 0.295245 0.818744 0.356 Uiso calc 0.5 A -1
H H24C 1.394999 0.269661 0.920830 0.356 Uiso calc 0.5 A -1
O O8 1.2362(15) 0.3812(15) 0.8331(9) 0.109(6) Uani d 0.5 A 1
H H8A 1.283550 0.349024 0.876365 0.164 Uiso d 0.5 A 1
H H8B 1.255520 0.363564 0.785015 0.164 Uiso d 0.5 A 1
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
Co1 0.0496(3) 0.0268(3) 0.0268(3) -0.0025(2) 0.0137(2) -0.0018(2)
S1 0.0705(9) 0.0671(9) 0.0750(9) 0.0037(7) 0.0023(7) 0.0295(7)
O1 0.0447(16) 0.0435(16) 0.0524(17) -0.0023(13) 0.0158(14) -0.0207(13)
O2 0.0431(18) 0.071(2) 0.0508(18) -0.0167(15) 0.0189(14) -0.0265(15)
O3 0.0296(15) 0.0517(16) 0.0523(17) 0.0015(12) 0.0033(13) 0.0137(13)
O4 0.0552(18) 0.0390(15) 0.0452(16) -0.0038(13) 0.0146(14) -0.0154(13)
O5 0.0505(19) 0.0645(19) 0.0398(16) 0.0128(15) 0.0140(14) -0.0109(14)
N1 0.035(2) 0.049(2) 0.049(2) 0.0063(16) -0.0050(16) -0.0034(17)
N2 0.053(2) 0.0305(16) 0.0321(16) -0.0019(15) 0.0178(15) 0.0024(13)
N3 0.055(2) 0.0375(18) 0.0328(17) -0.0046(15) 0.0133(15) 0.0085(14)
N4 0.062(2) 0.0301(16) 0.0278(16) -0.0028(15) 0.0155(15) 0.0016(13)
C1 0.044(2) 0.0323(19) 0.0303(19) -0.0057(17) 0.0131(17) -0.0028(15)
C2 0.035(2) 0.0322(19) 0.0317(19) -0.0007(15) 0.0100(16) -0.0002(15)
C3 0.040(2) 0.033(2) 0.039(2) 0.0070(16) 0.0119(17) -0.0028(16)
C4 0.034(2) 0.039(2) 0.037(2) 0.0013(17) 0.0052(17) 0.0078(17)
C5 0.046(3) 0.037(2) 0.040(2) 0.0086(18) -0.0076(19) -0.0092(17)
C6 0.043(3) 0.057(3) 0.059(3) 0.015(2) -0.010(2) -0.011(2)
C7 0.045(3) 0.078(3) 0.076(3) 0.000(2) 0.013(2) 0.015(3)
C8 0.042(2) 0.034(2) 0.034(2) -0.0048(17) 0.0021(17) -0.0014(16)
C9 0.039(2) 0.0337(19) 0.0284(18) -0.0011(16) 0.0120(16) -0.0033(15)
C10 0.046(2) 0.0316(19) 0.033(2) -0.0005(17) 0.0148(18) 0.0021(16)
C11 0.032(2) 0.0368(19) 0.0307(19) -0.0009(16) 0.0091(15) -0.0024(16)
C12 0.052(3) 0.042(2) 0.043(2) -0.0035(19) 0.025(2) 0.0106(18)
C13 0.046(2) 0.043(2) 0.042(2) -0.0049(18) 0.0210(19) 0.0059(18)
C14 0.053(2) 0.0265(18) 0.0313(19) 0.0003(17) 0.0167(18) -0.0002(15)
C15 0.058(3) 0.0304(19) 0.0250(18) -0.0051(18) 0.0122(17) -0.0012(15)
C16 0.059(3) 0.036(2) 0.031(2) -0.0003(19) 0.0096(18) 0.0046(16)
C17 0.051(3) 0.040(2) 0.034(2) -0.0045(19) 0.0088(18) 0.0073(17)
C18 0.066(3) 0.034(2) 0.040(2) 0.015(2) 0.018(2) 0.0077(17)
C19 0.057(3) 0.041(2) 0.040(2) 0.007(2) 0.022(2) 0.0036(18)
C20 0.058(3) 0.041(2) 0.036(2) -0.014(2) 0.0167(19) 0.0061(17)
C21 0.049(2) 0.039(2) 0.036(2) -0.0113(18) 0.0098(18) 0.0028(17)
O6 0.134(10) 0.108(8) 0.110(9) 0.001(7) 0.031(7) -0.003(6)
O7 0.085(6) 0.075(5) 0.084(5) 0.023(4) -0.034(4) -0.032(4)
C23 0.166(13) 0.206(13) 0.211(14) -0.064(11) 0.018(11) 0.087(11)
N5 0.190(8) 0.193(8) 0.179(8) 0.003(7) 0.031(7) 0.030(7)
C22 0.168(9) 0.169(8) 0.161(8) 0.002(7) 0.040(7) 0.020(7)
C24 0.233(14) 0.249(15) 0.219(14) 0.067(13) 0.034(12) -0.036(13)
O8 0.100(9) 0.192(16) 0.034(5) -0.055(9) 0.013(5) 0.020(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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Co1 O2 . . 60.43(10) ?
O1 Co1 O4 . 2_655 151.57(11) ?
O1 Co1 O5 . 2_655 98.85(11) ?
O1 Co1 C1 . . 30.50(11) ?
O2 Co1 C1 . . 29.96(11) ?
O4 Co1 O2 2_655 . 99.60(11) ?
O4 Co1 O5 2_655 2_655 59.65(10) ?
O4 Co1 C1 2_655 . 126.57(12) ?
O5 Co1 O2 2_655 . 92.57(12) ?
O5 Co1 C1 2_655 . 95.62(11) ?
N2 Co1 O1 . . 102.95(12) ?
N2 Co1 O2 . . 91.51(12) ?
N2 Co1 O4 . 2_655 97.23(12) ?
N2 Co1 O5 . 2_655 156.87(12) ?
N2 Co1 N4 . 2_656 93.24(12) ?
N2 Co1 C1 . . 99.22(12) ?
N4 Co1 O1 2_656 . 100.46(12) ?
N4 Co1 O2 2_656 . 160.89(13) ?
N4 Co1 O4 2_656 2_655 98.15(12) ?
N4 Co1 O5 2_656 2_655 90.30(11) ?
N4 Co1 C1 2_656 . 130.93(14) ?
C1 O1 Co1 . . 91.7(2) ?
C1 O2 Co1 . . 87.8(2) ?
C5 O3 C4 . . 118.8(3) ?
C10 O4 Co1 . 2_645 91.3(2) ?
C10 O5 Co1 . 2_645 89.3(2) ?
C5 N1 C6 . . 119.9(4) ?
C5 N1 C7 . . 123.6(3) ?
C7 N1 C6 . . 116.4(4) ?
C12 N2 Co1 . . 122.3(2) ?
C21 N2 Co1 . . 122.8(3) ?
C21 N2 C12 . . 114.6(3) ?
C14 N3 H3 . . 114.8 ?
C14 N3 C15 . . 130.5(4) ?
C15 N3 H3 . . 114.8 ?
C17 N4 Co1 . 2_646 119.2(3) ?
C17 N4 C18 . . 116.0(3) ?
C18 N4 Co1 . 2_646 124.7(3) ?
O1 C1 Co1 . . 57.84(18) ?
O1 C1 C2 . . 120.2(3) ?
O2 C1 Co1 . . 62.2(2) ?
O2 C1 O1 . . 120.0(3) ?
O2 C1 C2 . . 119.8(3) ?
C2 C1 Co1 . . 176.8(3) ?
C3 C2 C1 . . 119.7(3) ?
C11 C2 C1 . . 120.9(3) ?
C11 C2 C3 . . 119.4(3) ?
C2 C3 H3A . . 120.3 ?
C4 C3 C2 . . 119.4(3) ?
C4 C3 H3A . . 120.3 ?
C3 C4 O3 . . 118.4(3) ?
C3 C4 C8 . . 121.6(4) ?
C8 C4 O3 . . 119.6(3) ?
O3 C5 S1 . . 122.5(3) ?
N1 C5 S1 . . 127.6(3) ?
N1 C5 O3 . . 109.9(4) ?
N1 C6 H6A . . 109.5 ?
N1 C6 H6B . . 109.5 ?
N1 C6 H6C . . 109.5 ?
H6A C6 H6B . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N1 C7 H7A . . 109.5 ?
N1 C7 H7B . . 109.5 ?
N1 C7 H7C . . 109.5 ?
H7A C7 H7B . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C4 C8 H8 . . 120.3 ?
C9 C8 C4 . . 119.4(3) ?
C9 C8 H8 . . 120.3 ?
C8 C9 C10 . . 119.8(3) ?
C8 C9 C11 . . 119.8(3) ?
C11 C9 C10 . . 120.3(3) ?
O4 C10 C9 . . 120.0(4) ?
O5 C10 O4 . . 119.7(4) ?
O5 C10 C9 . . 120.3(3) ?
C2 C11 C9 . . 120.4(3) ?
C2 C11 H11 . . 119.8 ?
C9 C11 H11 . . 119.8 ?
N2 C12 H12 . . 117.6 ?
N2 C12 C13 . . 124.9(4) ?
C13 C12 H12 . . 117.6 ?
C12 C13 H13 . . 120.2 ?
C12 C13 C14 . . 119.6(4) ?
C14 C13 H13 . . 120.2 ?
N3 C14 C13 . . 116.7(4) ?
N3 C14 C20 . . 126.9(4) ?
C20 C14 C13 . . 116.3(4) ?
N3 C15 C19 . . 117.5(4) ?
C16 C15 N3 . . 125.5(4) ?
C16 C15 C19 . . 117.0(3) ?
C15 C16 H16 . . 120.5 ?
C15 C16 C17 . . 119.1(4) ?
C17 C16 H16 . . 120.5 ?
N4 C17 C16 . . 124.5(4) ?
N4 C17 H17 . . 117.8 ?
C16 C17 H17 . . 117.8 ?
N4 C18 H18 . . 117.9 ?
N4 C18 C19 . . 124.3(4) ?
C19 C18 H18 . . 117.9 ?
C15 C19 H19 . . 120.5 ?
C18 C19 C15 . . 119.0(4) ?
C18 C19 H19 . . 120.5 ?
C14 C20 H20 . . 120.3 ?
C21 C20 C14 . . 119.5(4) ?
C21 C20 H20 . . 120.3 ?
N2 C21 C20 . . 125.1(4) ?
N2 C21 H21 . . 117.5 ?
C20 C21 H21 . . 117.5 ?
H7D O7 H7E . . 111.7 ?
H23A C23 H23B . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
N5 C23 H23A . . 111.7 ?
N5 C23 H23B . . 109.3 ?
N5 C23 H23C . . 107.3 ?
C23 N5 C22 . . 125.5(15) ?
C23 N5 C24 . . 122.9(15) ?
C24 N5 C22 . . 111.4(13) ?
O6 C22 N5 . . 113.0(15) ?
O6 C22 H22 . . 123.5 ?
N5 C22 H22 . . 123.5 ?
O8 C22 O6 . . 10.1(19) ?
O8 C22 N5 . . 107(2) ?
O8 C22 H22 . . 128.6 ?
N5 C24 H24A . . 109.5 ?
N5 C24 H24B . . 109.5 ?
N5 C24 H24C . . 109.5 ?
H24A C24 H24B . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C22 O8 H8A . . 80.7 ?
C22 O8 H8B . . 122.1 ?
H8A O8 H8B . . 104.8 ?
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
Co1 O1 . 2.119(3) ?
Co1 O2 . 2.216(3) ?
Co1 O4 2_655 2.156(3) ?
Co1 O5 2_655 2.211(3) ?
Co1 N2 . 2.094(3) ?
Co1 N4 2_656 2.100(3) ?
Co1 C1 . 2.502(4) ?
S1 C5 . 1.638(5) ?
O1 C1 . 1.271(4) ?
O2 C1 . 1.251(5) ?
O3 C4 . 1.404(4) ?
O3 C5 . 1.363(4) ?
O4 C10 . 1.266(4) ?
O5 C10 . 1.247(5) ?
N1 C5 . 1.339(6) ?
N1 C6 . 1.451(5) ?
N1 C7 . 1.437(6) ?
N2 C12 . 1.345(5) ?
N2 C21 . 1.341(5) ?
N3 H3 . 0.8600 ?
N3 C14 . 1.382(5) ?
N3 C15 . 1.390(5) ?
N4 C17 . 1.330(5) ?
N4 C18 . 1.337(5) ?
C1 C2 . 1.496(5) ?
C2 C3 . 1.393(5) ?
C2 C11 . 1.390(5) ?
C3 H3A . 0.9300 ?
C3 C4 . 1.379(5) ?
C4 C8 . 1.381(5) ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C7 H7A . 0.9600 ?
C7 H7B . 0.9600 ?
C7 H7C . 0.9600 ?
C8 H8 . 0.9300 ?
C8 C9 . 1.380(5) ?
C9 C10 . 1.496(5) ?
C9 C11 . 1.395(5) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C12 C13 . 1.361(5) ?
C13 H13 . 0.9300 ?
C13 C14 . 1.406(5) ?
C14 C20 . 1.385(6) ?
C15 C16 . 1.378(6) ?
C15 C19 . 1.409(5) ?
C16 H16 . 0.9300 ?
C16 C17 . 1.380(5) ?
C17 H17 . 0.9300 ?
C18 H18 . 0.9300 ?
C18 C19 . 1.364(6) ?
C19 H19 . 0.9300 ?
C20 H20 . 0.9300 ?
C20 C21 . 1.373(5) ?
C21 H21 . 0.9300 ?
O6 C22 . 1.245(17) ?
O7 H7D . 0.8380 ?
O7 H7E . 0.8812 ?
C23 H23A . 0.9598 ?
C23 H23B . 0.9600 ?
C23 H23C . 0.9595 ?
C23 N5 . 1.306(14) ?
N5 C22 . 1.474(15) ?
N5 C24 . 1.416(15) ?
C22 H22 . 0.9300 ?
C22 O8 . 0.93(3) ?
C24 H24A . 0.9600 ?
C24 H24B . 0.9600 ?
C24 H24C . 0.9600 ?
O8 H8A . 0.8784 ?
O8 H8B . 0.8500 ?
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
_geom_hbond_publ_flag
N3 H3 O6 . 0.86 1.86 2.700(19) 163.5 yes
N3 H3 O8 . 0.86 2.13 2.979(17) 169.5 yes
C13 H13 O2 3_766 0.93 2.44 3.174(5) 135.4 yes
O7 H7D O4 . 0.84 2.16 2.992(7) 174.0 yes
O7 H7E O2 4_565 0.88 2.26 3.136(7) 173.1 yes
O8 H8A O7 1_656 0.88 2.33 3.10(2) 146.3 yes
O8 H8B O5 4_666 0.85 2.28 3.102(17) 162.9 yes
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
Co1 O1 C1 O2 . . . . 3.4(4) ?
Co1 O1 C1 C2 . . . . -177.0(3) ?
Co1 O2 C1 O1 . . . . -3.2(4) ?
Co1 O2 C1 C2 . . . . 177.2(3) ?
Co1 O4 C10 O5 2_645 . . . 2.2(4) ?
Co1 O4 C10 C9 2_645 . . . -176.6(3) ?
Co1 O5 C10 O4 2_645 . . . -2.1(4) ?
Co1 O5 C10 C9 2_645 . . . 176.7(3) ?
Co1 N2 C12 C13 . . . . 173.3(3) ?
Co1 N2 C21 C20 . . . . -173.9(3) ?
Co1 N4 C17 C16 2_646 . . . -174.6(3) ?
Co1 N4 C18 C19 2_646 . . . 174.4(3) ?
O1 C1 C2 C3 . . . . 0.7(5) ?
O1 C1 C2 C11 . . . . -176.9(3) ?
O2 C1 C2 C3 . . . . -179.7(4) ?
O2 C1 C2 C11 . . . . 2.7(5) ?
O3 C4 C8 C9 . . . . -169.0(3) ?
N2 C12 C13 C14 . . . . 0.6(6) ?
N3 C14 C20 C21 . . . . -178.0(4) ?
N3 C15 C16 C17 . . . . 178.3(4) ?
N3 C15 C19 C18 . . . . -178.0(4) ?
N4 C18 C19 C15 . . . . -1.1(6) ?
C1 C2 C3 C4 . . . . -177.9(3) ?
C1 C2 C11 C9 . . . . 179.1(3) ?
C2 C3 C4 O3 . . . . 170.1(3) ?
C2 C3 C4 C8 . . . . -2.0(6) ?
C3 C2 C11 C9 . . . . 1.5(5) ?
C3 C4 C8 C9 . . . . 3.1(6) ?
C4 O3 C5 S1 . . . . 8.9(5) ?
C4 O3 C5 N1 . . . . -171.9(3) ?
C4 C8 C9 C10 . . . . 174.4(3) ?
C4 C8 C9 C11 . . . . -1.8(5) ?
C5 O3 C4 C3 . . . . 87.8(4) ?
C5 O3 C4 C8 . . . . -100.0(4) ?
C6 N1 C5 S1 . . . . -1.8(6) ?
C6 N1 C5 O3 . . . . 179.0(3) ?
C7 N1 C5 S1 . . . . 179.1(4) ?
C7 N1 C5 O3 . . . . -0.1(6) ?
C8 C9 C10 O4 . . . . 19.2(5) ?
C8 C9 C10 O5 . . . . -159.6(4) ?
C8 C9 C11 C2 . . . . -0.5(5) ?
C10 C9 C11 C2 . . . . -176.6(3) ?
C11 C2 C3 C4 . . . . -0.3(5) ?
C11 C9 C10 O4 . . . . -164.7(3) ?
C11 C9 C10 O5 . . . . 16.5(5) ?
C12 N2 C21 C20 . . . . 0.5(6) ?
C12 C13 C14 N3 . . . . 177.7(4) ?
C12 C13 C14 C20 . . . . 0.6(6) ?
C13 C14 C20 C21 . . . . -1.2(6) ?
C14 N3 C15 C16 . . . . -23.9(6) ?
C14 N3 C15 C19 . . . . 158.4(4) ?
C14 C20 C21 N2 . . . . 0.6(6) ?
C15 N3 C14 C13 . . . . 178.9(4) ?
C15 N3 C14 C20 . . . . -4.3(6) ?
C15 C16 C17 N4 . . . . 1.0(6) ?
C16 C15 C19 C18 . . . . 4.1(6) ?
C17 N4 C18 C19 . . . . -2.0(6) ?
C18 N4 C17 C16 . . . . 2.0(6) ?
C19 C15 C16 C17 . . . . -4.0(5) ?
C21 N2 C12 C13 . . . . -1.2(6) ?
C23 N5 C22 O6 . . . . -176(2) ?
C23 N5 C22 O8 . . . . 175(2) ?
C24 N5 C22 O6 . . . . -1(3) ?
C24 N5 C22 O8 . . . . -9(3) ?