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_7707283
_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
'C34 H56 B2 Fe6 N14 O4 S6 W2, C8 H17 N, C8 H20 N, 8(C3 H7 N O)'
_chemical_formula_sum            'C74 H149 B2 Fe6 N24 O12 S6 W2'
_chemical_formula_weight         2483.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0221(8)
_cell_length_b                   18.0186(6)
_cell_length_c                   23.9879(7)
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      30.17
_cell_measurement_theta_min      2.41
_cell_volume                     10383.0(6)
_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      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0944
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47821
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.413
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.203
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1690 before and 0.1210 after correction. The Ratio of minimum to maximum transmission is 0.4413. 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    1.589
_exptl_crystal_description       block
_exptl_crystal_F_000             5068
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.982
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0797P)^2^+40.8429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4687
_reflns_number_total             5051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00414j2.cif
_cod_data_source_block           123
_cod_depositor_comments
'Adding full bibliography for 7707281--7707285.cif.'
_cod_database_code               7707283
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.807
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O2-H16A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O3 \\sim C21 \\sim O3': within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O2 \\sim C20 \\sim N8 \\sim C19: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(H21A)=Sof(O3)=1-FVAR(1)
 Sof(H21)=Sof(O3')=FVAR(1)
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C17(0.25)
 H17A(0.25) H17B(0.25) H16A(0.25) H16C(0.25) H16B(0.25) H16D(0.25) H16F(0.25)
 H16E(0.25) C15(0.5) H15A(0.5) H15B(0.5) H14A(0.25) H14B(0.25) H14C(0.25)
 C17'(0.25) H17C(0.25) H17D(0.25)
5.a Riding coordinates:
 C16(H16D,H16F,H16E), C19(H19A,H19B,H19C)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C17(H17A,H17B), C15(H15A,H15B), C17'(H17C,H17D)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C21(H21A), C21(H21), C20(H20)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C13(H13A,H13B,
 H13C), C18(H18A,H18B,H18C), C16(H16A,H16C,H16B), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              14297
_shelx_hkl_checksum              20133
_olex2_submission_special_instructions 'No special instructions were received'