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_7712901
_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         'C39 H52 B Fe3 N7 S6 Si W, C8 H20 N'
_chemical_formula_sum            'C47 H72 B Fe3 N8 S6 Si W'
_chemical_formula_weight         1331.78
_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     iterative
_audit_creation_date             2022-08-03
_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                92.02(15)
_cell_angle_beta                 101.28(9)
_cell_angle_gamma                90.5(2)
_cell_formula_units_Z            2
_cell_length_a                   10.49(4)
_cell_length_b                   10.76(5)
_cell_length_c                   24.74(8)
_cell_measurement_reflns_used    1005
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.26
_cell_volume                     2736(19)
_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    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.0953
_diffrn_reflns_av_unetI/netI     0.1391
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22323
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.022
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         1.980
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.166
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             1354
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         9436
_refine_ls_number_restraints     1150
_refine_ls_restrained_S_all      7.959
_refine_ls_R_factor_all          0.1681
_refine_ls_R_factor_gt           0.0892
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+33.1999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5348
_reflns_number_total             9436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00865g2.cif
_cod_data_source_block           mo_zhy72_0m_a
_cod_original_cell_volume        2737(19)
_cod_database_code               7712901
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C41-C38
 2.2 with sigma of 0.001
 C38-C37
 1.55 with sigma of 0.001
 C38-C41
 2.2 with sigma of 0.005
 C39-C40
 1.55 with sigma of 0.001
 H40C-C46
 1.9 with sigma of 0.02
 H46B-H40C
 1.9 with sigma of 0.02
 C43-C42
 1.54 with sigma of 0.0001
 C45-C46
 1.54 with sigma of 0.0001
 C44-C47
 1.54 with sigma of 0.0001
 C43-C41
 1.54 with sigma of 0.0001
 C5-C4
 1.51 with sigma of 0.0001
 C1-C2
 1.51 with sigma of 0.0001
 C10-C9
 1.51 with sigma of 0.0001
 C15-C14
 1.51 with sigma of 0.0001
 C11-C12
 1.51 with sigma of 0.0001
 C7-C6
 1.51 with sigma of 0.0001
 C33-C36
 1.46 with sigma of 0.0001
 C4-C3
 1.39 with sigma of 0.0001
 C8-C9
 1.39 with sigma of 0.0001
 C12-C13
 1.39 with sigma of 0.0001
 C2-C3
 1.39 with sigma of 0.0001
 C13-C14
 1.39 with sigma of 0.0001
 C7-C8
 1.39 with sigma of 0.0001
 C26-C29
 1.54 with sigma of 0.0001
 C36-C33
 1.54 with sigma of 0.0001
 C19-C22
 1.51 with sigma of 0.0001
 C19-C18
 1.39 with sigma of 0.0001
 C17-C18
 1.39 with sigma of 0.0001
 C21-C20
 1.39 with sigma of 0.0001
 C20-C19
 1.39 with sigma of 0.0001
 C16-C21
 1.39 with sigma of 0.0001
 C16-C17
 1.39 with sigma of 0.0001
 H40A-H45B
 2.3 with sigma of 0.02
 C45-C40
 2.3 with sigma of 0.02
 C40-C45
 2.5 with sigma of 0.02
3. Restrained planarity
 C20, C21, C16, C18, C17, C19, C22
 with sigma of 0.1
4. Rigid bond restraints
 Si1, C52
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
N8 \\sim C44 \\sim C41 \\sim C50 \\sim C45 \\sim C42 \\sim C48 \\sim C39 \\sim
C37 \\sim C38 \\sim C47 \\sim C46 \\sim C40 \\sim C43 \\sim C49: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
N8 \\sim C45 \\sim C41 \\sim C42 \\sim C50 \\sim C44 \\sim C48 \\sim C46 \\sim
C43 \\sim C49 \\sim C47: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C37 \\sim C39 \\sim C40 \\sim C38: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C20 \\sim C21 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C22: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C26 \\sim C25 \\sim C29 \\sim C27 \\sim C28 \\sim C23 \\sim C24: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C4 \\sim C14 \\sim C7 \\sim C3 \\sim C2 \\sim C9 \\sim C8 \\sim C13 \\sim C12
\\sim C6 \\sim C1 \\sim C15 \\sim C5 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C30 \\sim C11 \\sim C10 \\sim C36 \\sim C01A \\sim C22 \\sim
C25 \\sim C24 \\sim C23 \\sim C28 \\sim C27 \\sim C26 \\sim C51 \\sim C52 \\sim
C20 \\sim C21 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C29 \\sim C43 \\sim
C41 \\sim C49 \\sim C50 \\sim C44 \\sim C46 \\sim C48 \\sim C45 \\sim C42 \\sim
C47 \\sim C37 \\sim C39 \\sim C40 \\sim C38: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
6. Others
 Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H49D)=
 Sof(H49E)=Sof(H49F)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(H38C)=1-FVAR(1)
 Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(1)
7.a Riding coordinates:
 C43(H43D,H43E,H43F), C43(H43A,H43B,H43C), C49(H49D,H49E,H49F), C49(H49A,H49B,
 H49C), C38(H38A,H38B,H38C)
7.b Ternary CH refined with riding coordinates:
 B1(H1)
7.c Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C50(H50A,H50B), C44(H44A,H44B), C48(H48A,H48B), C45(H45A,
 H45B), C42(H42A,H42B), C37(H37A,H37B), C39(H39A,H39B)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C31(H31), C32(H32), C34(H34), C35(H35), C25(H25),
 C24(H24), C28(H28), C27(H27), C20(H20), C21(H21), C17(H17), C18(H18)
7.e Fitted hexagon refined as free rotating group:
 C31(C32,C33,C34,C35,C30), C25(C24,C23,C28,C27,C26), C20(C21,C16,C17,C18,C19)
7.f Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C5(H5A,H5B,H5C),
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C36(H36A,H36B,H36C), C01A(H01A,H01B,
 H01C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C29(H29A,
 H29B,H29C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              35073
_shelx_hkl_checksum              37345
_olex2_submission_special_instructions 'No special instructions were received'