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_7704003
_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'
_chemical_formula_sum            'C30 H44 B2 Co N12 S6 W2'
_chemical_formula_weight         1213.38
_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     iterative
_audit_creation_date             2020-01-16
_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                 103.248(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.154(10)
_cell_length_b                   16.190(14)
_cell_length_c                   12.030(11)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.320
_cell_measurement_theta_min      2.247
_cell_volume                     2115(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16332
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.146
_exptl_absorpt_coefficient_mu    6.150
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0441 before and 0.0358 after correction. The Ratio of minimum to maximum transmission is 0.9309. The \l/2 correction factor is Not present.'
_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    1.906
_exptl_crystal_description       block
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.9958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3564
_reflns_number_total             4861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00765j1.cif
_cod_data_source_block           mo_lan_0m
_cod_depositor_comments
'Adding full bibliography for 7704003--7704007.cif.'
_cod_database_code               7704003
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.749
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B1-H1
 1.05 with sigma of 0.002
3.a Riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C1(H1A,H1B,
 H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              3414
_olex2_submission_special_instructions 'No special instructions were received'