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_7707284
_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
'C30 H44 B2 Fe6 N26 S6 W2, 2(C3 H7 N O), 2(C8 H20 N)'
_chemical_formula_sum            'C52 H98 B2 Fe6 N30 O2 S6 W2'
_chemical_formula_weight         2092.38
_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     dual
_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
;
2021-02-05 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                72.820(2)
_cell_angle_beta                 83.033(2)
_cell_angle_gamma                81.869(2)
_cell_formula_units_Z            1
_cell_length_a                   10.9698(17)
_cell_length_b                   11.9853(18)
_cell_length_c                   15.905(2)
_cell_measurement_reflns_used    6986
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.07
_cell_measurement_theta_min      2.22
_cell_volume                     1970.7(5)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25488
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.790
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.194
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0786 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.7967. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             1046
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.453
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         7735
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0411P)^2^+1.5030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6293
_reflns_number_total             7735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00414j2.cif
_cod_data_source_block           xla
_cod_depositor_comments
'Adding full bibliography for 7707281--7707285.cif.'
_cod_database_code               7707284
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.572
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N11, N12, N13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, N9, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N11 \\sim N12 \\sim N13: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N9 \\sim N8 \\sim N10: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C26(H26)
4.c 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), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,
 H22B,H22C)
;
_shelx_res_checksum              34711
_shelx_hkl_checksum              18167
_olex2_submission_special_instructions 'No special instructions were received'