Nitride-incorporated W-Fe-S double cubane clusters: terminal ligand substitutions and redox behaviors.
Xue, Lian; Xu, Gan; Wang, Zheng; Chen, Xu-Dong; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6840–6847; doi:10.1039/d1dt00414j

data_7707281
_publ_section_title
;
 Nitride-incorporated W-Fe-S double cubane clusters: terminal ligand
 substitutions and redox behaviors.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6840
_journal_page_last               6847
_journal_paper_doi               10.1039/d1dt00414j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C38 H64 B2 Fe6 N14 S10 W2, 2(C8 H20 N)'
_chemical_formula_sum            'C54 H104 B2 Fe6 N16 S10 W2'
_chemical_formula_weight         2022.55
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.057(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.814(5)
_cell_length_b                   18.930(8)
_cell_length_c                   15.716(6)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.15
_cell_volume                     3797(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            72626
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.688
_diffrn_source                   'SSRF, Beamline B17B'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.449
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1238 before and 0.0490 after correction. The Ratio of minimum to maximum transmission is 0.7625. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       plate
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6446
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0481P)^2^+59.9717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5830
_reflns_number_total             6446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00414j2.cif
_cod_data_source_block           mo_204_0m_a
_cod_depositor_comments
'Adding full bibliography for 7707281--7707285.cif.'
_cod_database_code               7707281
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.617
_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
 C18-C19
 1.47 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B), C26(H26A,H26B), C24(H24A,H24B), C20(H20A,
 H20B), C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C),
 C21(H21A,H21B,H21C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C),
  C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              83525
_shelx_hkl_checksum              35655
_olex2_submission_special_instructions 'No special instructions were received'