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_7704005
_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 Cl Co2 N12 S6 W2, 2(C2 H3 N), C8 H20 N'
_chemical_formula_sum            'C42 H70 B2 Cl Co2 N15 S6 W2'
_chemical_formula_weight         1520.12
_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                 93.167(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7233(14)
_cell_length_b                   15.7004(18)
_cell_length_c                   29.118(3)
_cell_measurement_reflns_used    8945
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.407
_cell_measurement_theta_min      2.206
_cell_volume                     5807.8(11)
_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_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13160
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.062
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.816
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5941
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0685 before and 0.0345 after correction. The Ratio of minimum to maximum transmission is 0.7968. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.773
_refine_diff_density_min         -2.230
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5178
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0321P)^2^+26.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4077
_reflns_number_total             5178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00765j1.cif
_cod_data_source_block           ee
_cod_depositor_comments
'Adding full bibliography for 7704003--7704007.cif.'
_cod_database_code               7704005
_shelx_shelxl_version_number     2018/3
_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
 1 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
C37 \\sim N14 \\sim C38 \\sim C33 \\sim C35 \\sim C39 \\sim C34 \\sim C40 \\sim
C36: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(C34)=Sof(H34a)=Sof(H34b)=Sof(H34c)=1-FVAR(1)
 Sof(C36)=Sof(H36a)=Sof(H36b)=Sof(H36c)=Sof(C35)=Sof(H35a)=Sof(H35b)=FVAR(1)
 Sof(C37)=Sof(H37a)=Sof(H37b)=Sof(C40)=Sof(H40a)=Sof(H40b)=Sof(H40c)=1-FVAR(2)
 Sof(C39)=Sof(H39a)=Sof(H39b)=Sof(H39c)=Sof(C38)=Sof(H38a)=Sof(H38b)=FVAR(2)
 Fixed Sof: Co2(0.5)
5.a Riding coordinates:
 C40(H40a,H40b,H40c)
5.b Secondary CH2 refined with riding coordinates:
 C37(H37a,H37b), C35(H35a,H35b), C33(H33a,H33b), C38(H38a,H38b)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13)
5.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C10(H10a,H10b,H10c),
 C11(H11a,H11b,H11c), C15(H15a,H15b,H15c), C31(H31a,H31b,H31c), C36(H36a,H36b,
 H36c), C39(H39a,H39b,H39c), C34(H34a,H34b,H34c)
;
_shelx_res_checksum              5201
_olex2_submission_special_instructions 'No special instructions were received'