Crystal structure of rac-trans-6,6′-((cyclohexane-1,2-diylbis(azanylylidene))bis(methanylylidene))bis(2-bromophenolato-κ4 N,N′,O,O′)-bis(methanol)cobalt(III) chloride, C22H25Br2Co8N2O4Cl
Wu, Qiong; Zi, Qiaoli; Li, Jindong; Li, Yajuan; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 269–270; doi:10.1515/ncrs-2018-0309

data_8105614
_publ_section_title
;
 Crystal structure of
 rac-trans-6,6&#x2032;-((cyclohexane-1,2-diylbis(azanylylidene))bis(methanylylidene))bis(2-bromophenolato-\k4
 N,N&#x2032;,O,O&#x2032;)-bis(methanol)cobalt(III) chloride,
 C22H25Br2Co8N2O4Cl
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              269
_journal_page_last               270
_journal_paper_doi               10.1515/ncrs-2018-0309
_journal_volume                  234
_journal_year                    2019
_chemical_formula_sum            'C22 H25 Br2 Cl Co N2 O4'
_chemical_formula_weight         635.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        '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                 95.987(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8246(13)
_cell_length_b                   23.695(4)
_cell_length_c                   13.225(2)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      18.6710
_cell_measurement_theta_min      3.6520
_cell_volume                     2438.6(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Diamond 3.2k)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_av_unetI/netI     0.1852
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9593
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.122
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_refine_diff_density_max         0.835
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4290
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.2142
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.2192
_reflns_number_gt                1747
_reflns_number_total             4290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2018-0309_suppl.cif
_cod_data_source_block           5722
_cod_depositor_comments
;

2025-04-22
Formula modified to eliminate an spurious "8" after the Co symbol
                 miguel
;
_cod_original_formula_weight         1048.17
_cod_original_formula_sum        'C22 H25 Br2 Co8 N2 O4 Cl'
_cod_database_code               8105614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 O4-H4
 0.87 with sigma of 0.01
 C21-H3
 1.926143 with sigma of 0.02
 Co1-H3
 2.614861 with sigma of 0.02
 C22-H4
 1.961404 with sigma of 0.02
 Co1-H4
 2.590349 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5), C7(H7), C14(H14), C16(H16), C17(H17), C18(H18)
3.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;