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_7704006
_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 Cl0.5 Co1.5 N12 S6 W2, C8 H20 N, 2(C2 H3 N)'
_chemical_formula_sum            'C42 H70 B2 Cl0.5 Co1.5 N15 S6 W2'
_chemical_formula_weight         1472.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 92.876(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.638(12)
_cell_length_b                   15.620(15)
_cell_length_c                   29.22(3)
_cell_measurement_reflns_used    3395
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.358
_cell_measurement_theta_min      2.455
_cell_volume                     5761(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            19595
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.197
_diffrn_reflns_theta_min         2.074
_exptl_absorpt_coefficient_mu    4.692
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0782 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.7732.
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    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.921
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5689
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0373P)^2^+18.0359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3764
_reflns_number_total             5689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00765j1.cif
_cod_data_source_block           15a
_cod_depositor_comments
'Adding full bibliography for 7704003--7704007.cif.'
_cod_original_cell_volume        5761(9)
_cod_original_formula_sum        'C42 H70 B2 Cl0.50 Co1.50 N15 S6 W2'
_cod_database_code               7704006
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.799
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N8-C20
 1.52 with sigma of 0.02
 N8-C21
 1.52 with sigma of 0.02
 N8-C19
 1.52 with sigma of 0.02
 N8-C22
 1.52 with sigma of 0.02
 C23-C21
 1.5 with sigma of 0.02
 C18-C19
 1.5 with sigma of 0.02
 H1-B1
 1.05 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
N8 \\sim C23 \\sim C18 \\sim C21 \\sim C19 \\sim C22 \\sim C20: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: Co2(0.25) Cl1(0.25) H23A(0.5) H23B(0.5) H23C(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5) H18D(0.5) H18E(0.5) H18F(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C21(0.5) H21A(0.5) H21B(0.5) C19(0.5) H19A(0.5) H19B(0.5) C22(0.5)
 H22A(0.5) H22B(0.5) C20(0.5) H20A(0.5) H20B(0.5)
5.a Riding coordinates:
 C23(H23A,H23B,H23C), C23(H23D,H23E,H23F), C18(H18D,H18E,H18F), C18(H18A,H18B,
 H18C), C21(H21A,H21B), C19(H19A,H19B), C22(H22A,H22B), C20(H20A,H20B), B1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C3(H3)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C1(H1A,H1B,
 H1C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              2561
_olex2_submission_special_instructions 'No special instructions were received'