Templated syntheses of heterometal tungsten-cobalt-sulfur clusters with different nuclearities.
Guo, Jia-Ting; Chen, Xu-Dong; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5523–5530; doi:10.1039/d0dt00765j

data_7704004
_publ_section_title
;
 Templated syntheses of heterometal tungsten-cobalt-sulfur clusters with
 different nuclearities.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5523
_journal_page_last               5530
_journal_paper_doi               10.1039/d0dt00765j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C30 H44 B2 Co N12 S6 W2, C8 H20 N, C2 H3 N'
_chemical_formula_sum            'C40 H67 B2 Co N14 S6 W2'
_chemical_formula_weight         1384.68
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-16 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.37920(10)
_cell_length_b                   14.4818(2)
_cell_length_c                   31.9209(3)
_cell_measurement_reflns_used    12149
_cell_measurement_temperature    298
_cell_measurement_theta_max      4.7580
_cell_measurement_theta_min      74.099
_cell_volume                     5260.09(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25392
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.885
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.925
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.154
_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     603
_refine_ls_number_reflns         9109
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0382
_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^+10.7067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7827
_reflns_number_total             9109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00765j1.cif
_cod_data_source_block           aa
_cod_depositor_comments
'Adding full bibliography for 7704003--7704007.cif.'
_cod_database_code               7704004
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.782
_shelx_estimated_absorpt_t_min   0.564
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1 = B2-H2
 1.05 with sigma of 0.002
3.a Riding coordinates:
 B2(H2), B1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C36(H36A,H36B), C32(H32A,H32B), C38(H38A,H38B)
3.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C8(H8), C3(H3), C13(H13), C23(H23), C18(H18)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C10(H10A,H10B,H10C), C1(H1A,H1B,H1C), C25(H25A,H25B,
 H25C), C21(H21A,H21B,H21C), C5(H5A,H5B,H5C), C15(H15A,H15B,H15C), C16(H16A,
 H16B,H16C), C30(H30A,H30B,H30C), C20(H20A,H20B,H20C), C11(H11A,H11B,H11C),
 C6(H6A,H6B,H6C), C37(H37A,H37B,H37C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C),
  C35(H35A,H35B,H35C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              85601
_olex2_submission_special_instructions 'No special instructions were received'