Synthesis and Crystal Structure of (μ-Acetato)bis(μ-Alkoxo)dicobalt(II, III) Complex with an Unsymmetric Dinucleating Ligand
SHINDE, Naho; HANDA, Ryunosuke; FURUTACHI, Hideki; SAKATA, Yoko; AKINE, Shigehisa; FUJINAMI, Shuhei; SUZUKI, Masatatsu; X-ray Structure Analysis Online 37 (2021) 13–14; doi:10.2116/xraystruct.37.13

data_1561478
_publ_section_title
;
 Synthesis and Crystal Structure of (\m-Acetato)bis(\m-Alkoxo)dicobalt(II,
 III) Complex with an Unsymmetric Dinucleating Ligand
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              13
_journal_page_last               14
_journal_paper_doi               10.2116/xraystruct.37.13
_journal_volume                  37
_journal_year                    2021
_chemical_formula_moiety         C32.25H40.75Cl2Co2N6.25O12.75
_chemical_formula_sum            'C32.25 H40.75 Cl2 Co2 N6.25 O12.75'
_chemical_formula_weight         908.72
_chemical_name_common
(C28H31N6O)Co2(CH3CO2)(MeO)(ClO4)2(MeOH)0.75(MeCN)0.25
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 102.8116(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4372(4)
_cell_length_b                   27.8578(10)
_cell_length_c                   13.5496(5)
_cell_measurement_reflns_used    71351
_cell_measurement_temperature    90
_cell_measurement_theta_max      66.902
_cell_measurement_theta_min      3.173
_cell_volume                     3841.6(2)
_computing_cell_refinement       'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_data_collection       'Bruker Instrument Service V4.2.9 '
_computing_data_reduction        'SAINT V8.37A/APEX3 (Bruker AXS Inc., 2015)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  ORTEP-3
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            71351
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.902
_diffrn_reflns_theta_max         66.902
_diffrn_reflns_theta_min         3.173
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    8.659
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Sheldrick, 1996 / Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     185
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+4.7096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6620
_reflns_number_total             6799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            37_13_1.txt
_cod_data_source_block           handa015
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1561478
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.221
_shelx_estimated_absorpt_t_max   0.449
_shelx_res_checksum              87319
_shelx_hkl_checksum              71022