The crystal structure bis{hexakis(1-methyl-1H-imidazole-κ1N)cobalt(II)} tetrakis(μ3-oxido)-octakis(μ2-oxido)-tetradecaoxido-octamolybdate(VI), C24H36CoMo4N12O13
Zhang, Gang; Luan, Jian; Wang, Xiao-Jie; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1307–1309; doi:10.1515/ncrs-2020-0289

data_8105452
_publ_section_title
;
 The crystal structure bis{hexakis(1-methyl-1H-imidazole-\k1N)cobalt(II)}
 tetrakis(\m3-oxido)-octakis(\m2-oxido)-tetradecaoxido-octamolybdate(VI),
 C24H36CoMo4N12O13
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1307
_journal_page_last               1309
_journal_paper_doi               10.1515/ncrs-2020-0289
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C24 H36 Co N12, Mo4 O13'
_chemical_formula_sum            'C24 H36 Co Mo4 N12 O13'
_chemical_formula_weight         1143.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                64.544(12)
_cell_angle_beta                 79.558(14)
_cell_angle_gamma                87.084(14)
_cell_formula_units_Z            2
_cell_length_a                   11.155(5)
_cell_length_b                   13.889(6)
_cell_length_c                   14.081(6)
_cell_measurement_reflns_used    9010
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.36
_cell_volume                     1936.3(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015) [1]'
_computing_data_collection       'Bruker APEX-II'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [3]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [3]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015) [2]'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34372
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.625
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1126
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.546
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.281
_refine_ls_extinction_coef       0.0113(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         6975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0654P)^2^+0.9450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5844
_reflns_number_total             6975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0289_suppl.cif
_cod_data_source_block           a
_cod_database_code               8105452
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.668
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C)
;