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_7704007
_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
'C33 H51 B2 Cl2 Co4 N13 O S6 W2, C9 H21 Co0.5 N3 O3, C4 H10 O, C3 H7 N O'
_chemical_formula_sum            'C49 H89 B2 Cl2 Co4.5 N17 O6 S6 W2'
_chemical_formula_weight         1930.13
_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   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                112.024(2)
_cell_angle_beta                 95.703(2)
_cell_angle_gamma                100.406(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9709(3)
_cell_length_b                   17.0437(3)
_cell_length_c                   20.5403(4)
_cell_measurement_reflns_used    47156
_cell_measurement_temperature    100
_cell_measurement_theta_max      49.099
_cell_measurement_theta_min      4.7670
_cell_volume                     3756.37(16)
_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      100
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43385
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         4.106
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    15.734
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.53
_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    1.706
_exptl_crystal_description       needle
_exptl_crystal_F_000             1919
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.910
_refine_diff_density_min         -2.915
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         12762
_refine_ls_number_restraints     492
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0608
_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^)+(0.1137P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10358
_reflns_number_total             12762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00765j1.cif
_cod_data_source_block           gjtr138a
_cod_depositor_comments
'Adding full bibliography for 7704003--7704007.cif.'
_cod_original_cell_volume        3756.37(15)
_cod_original_formula_sum        'C49 H89 B2 Cl2 Co4.50 N17 O6 S6 W2'
_cod_database_code               7704007
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.507
_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. Rigid bond restraints
 O6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3. Uiso/Uaniso restraints and constraints
C52 \\sim C53: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
4. Others
 Fixed Sof: Co1(0.822) Co1A(0.178) C40(0.5) H40(0.5) C46(0.5) H46A(0.5)
 H46B(0.5) H46C(0.5) C41(0.5) H41(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
 C43(0.5) H43A(0.5) H43B(0.5) H43C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
5.a Riding coordinates:
 C53(H53A,H53B,H53C)
5.b Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B)
5.d Aromatic/amide H refined with riding coordinates:
 C32(H32), C18(H18), C28(H28), C23(H23), C3(H3), C13(H13), C39(H39), C36(H36),
 C8(H8), C40(H40), C41(H41), C47(H47)
5.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C26(H26A,H26B,H26C), C38(H38A,H38B,
 H38C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C25(H25A,
 H25B,H25C), C10(H10A,H10B,H10C), C37(H37A,H37B,H37C), C31(H31A,H31B,H31C),
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C20(H20A,H20B,H20C), C11(H11A,H11B,
 H11C), C1(H1A,H1B,H1C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C34(H34A,
 H34B,H34C), C46(H46A,H46B,H46C), C6(H6A,H6B,H6C), C48(H48A,H48B,H48C),
 C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              40883
_shelx_fab_checksum              44331
_olex2_submission_special_instructions 'No special instructions were received'