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_7707282
_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         'C54 H64 B2 Fe6 N14 S10 W2, 2(C8 H20 N)'
_chemical_formula_sum            'C70 H104 B2 Fe6 N16 S10 W2'
_chemical_formula_weight         2214.71
_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             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                90
_cell_angle_beta                 98.477(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.096(4)
_cell_length_b                   19.118(3)
_cell_length_c                   20.286(3)
_cell_measurement_reflns_used    8738
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.17
_cell_measurement_theta_min      2.32
_cell_volume                     10394(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29145
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.211
_diffrn_reflns_theta_max         25.211
_diffrn_reflns_theta_min         2.319
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.258
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0914 before and 0.0412 after correction. The Ratio of minimum to maximum transmission is 0.7907. 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    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9295
_refine_ls_number_restraints     735
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+16.2035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7013
_reflns_number_total             9295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00414j2.cif
_cod_data_source_block           xl19a_sq
_cod_depositor_comments
'Adding full bibliography for 7707281--7707285.cif.'
_cod_original_cell_volume        10393(3)
_cod_database_code               7707282
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.293
_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. Restrained distances
 C18-C17 \\sim C16-C21 \\sim C20-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C21: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C23 \\sim C24
\\sim C25 \\sim C26 \\sim C27 \\sim C22 \\sim C39 \\sim C34 \\sim C35 \\sim C36
\\sim C37 \\sim C38 \\sim C19 \\sim C20 \\sim C21 \\sim C16 \\sim C17 \\sim C18
\\sim C32 \\sim C33 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C28)=
 Sof(C29)=Sof(H29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=1-FVAR(1)
 Sof(C23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(C22)=Sof(H22)=Sof(C39)=Sof(H39)=Sof(C34)=Sof(C35)=Sof(H35)=
 Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C42(H42A,H42B), C44(H44A,H44B), C46(H46A,H46B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C24(H24), C25(H25), C26(H26), C27(H27), C22(H22),
 C39(H39), C35(H35), C36(H36), C37(H37), C38(H38), C19(H19), C20(H20), C21(H21),
  C17(H17), C18(H18), C32(H32), C33(H33), C29(H29), C30(H30), C31(H31)
5.c Fitted hexagon refined as free rotating group:
 C23(C24,C25,C26,C27,C22), C39(C34,C35,C36,C37,C38), C19(C20,C21,C16,C17,C18),
 C32(C33,C28,C29,C30,C31)
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), C41(H41A,H41B,H41C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              75738
_shelx_hkl_checksum              8710
_shelx_fab_checksum              27302
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'