Cubane-type Tungsten-Iron-Sulfur Clusters with Nitrogen Atom in the Core: Terminal Ligand Substitutions and Redox Behaviors
Zhang, Hong-Ying; Qiu, Shu-Juan; Yang, Huan-Huan; Wang, Meng-Ting; Yang, Jie; Wang, Han-Bin; Liu, Nai-Hao; Chen, Xu-Dong; Dalton Transactions  (2023) –; doi:10.1039/D3DT00865G

data_7712900
_publ_section_title
;
 Cubane-type Tungsten-Iron-Sulfur Clusters with Nitrogen Atom in the Core:
 Terminal Ligand Substitutions and Redox Behaviors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00865G
_journal_year                    2023
_chemical_formula_moiety         'C21 H40 B Fe3 N7 S6 Si W, C8 H20 N'
_chemical_formula_sum            'C29 H60 B Fe3 N8 S6 Si W'
_chemical_formula_weight         1103.51
_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
_audit_creation_date             2022-07-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                77.61(15)
_cell_angle_beta                 86.91(2)
_cell_angle_gamma                79.50(4)
_cell_formula_units_Z            2
_cell_length_a                   10.768(16)
_cell_length_b                   11.02(3)
_cell_length_c                   21.39(4)
_cell_measurement_reflns_used    5105
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.278
_cell_measurement_theta_min      2.506
_cell_volume                     2437(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.946
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25655
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.136
_diffrn_reflns_theta_min         1.922
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1393 before and 0.0626 after correction.
The Ratio of minimum to maximum transmission is 0.6250.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1114
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         9208
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0787P)^2^+3.3935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8063
_reflns_number_total             9208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00865g2.cif
_cod_data_source_block           mo_zhy25b_0m_a
_cod_original_cell_volume        2437(8)
_cod_database_code               7712900
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
C8 \\sim C9 \\sim C2 \\sim C12 \\sim C7 \\sim C13 \\sim C14 \\sim C4 \\sim C3
\\sim C11 \\sim C1 \\sim C28 \\sim C6 \\sim C21 \\sim C20 \\sim C10 \\sim C26
\\sim C5 \\sim C19 \\sim C24 \\sim C15 \\sim C18 \\sim C23 \\sim C17 \\sim C25
\\sim C16 \\sim C29 \\sim C27 \\sim C22: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
3.a Riding coordinates:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C25(H25A,H25B,H25C)
3.b Ternary CH refined with riding coordinates:
 B00P(H00P)
3.c Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C26(H26A,H26B), C24(H24A,H24B), C23(H23A,H23B)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C13(H13), C3(H3)
3.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C),
 C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C),
  C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C27(H27A,H27B,
 H27C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61254
_shelx_hkl_checksum              25218
_shelx_fab_checksum              94781
_olex2_submission_special_instructions 'No special instructions were received'