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_7712905
_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         'C36 H46 B Fe3 N7 S6 Si W, 2(C8 H20 N)'
_chemical_formula_sum            'C52 H86 B Fe3 N9 S6 Si W'
_chemical_formula_weight         1419.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-16
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-02-01 deposited with the CCDC.	2023-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.171(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.981(12)
_cell_length_b                   14.821(13)
_cell_length_c                   35.11(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.027
_cell_measurement_theta_min      2.277
_cell_volume                     7264(11)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0801
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            49254
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.004
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'brownish yellow'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         12544
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+10.1153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9944
_reflns_number_total             12544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00865g2.cif
_cod_data_source_block           mo_zhy55_1_0m_a
_cod_database_code               7712905
_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
 C27-C28
 1.4 with sigma of 0.02
 C22-C23
 1.4 with sigma of 0.02
 C23-C24
 1.4 with sigma of 0.02
 C32-C27
 1.4 with sigma of 0.02
 C25-C26
 1.4 with sigma of 0.02
 C31B-C30B
 1.4 with sigma of 0.02
 C22-C21
 1.4 with sigma of 0.02
 C32B-C31B
 1.4 with sigma of 0.02
 C28-C29
 1.4 with sigma of 0.02
 C32B-C27B
 1.4 with sigma of 0.02
 C31-C32
 1.4 with sigma of 0.02
 C29-C30
 1.4 with sigma of 0.02
 C28B-C29B
 1.4 with sigma of 0.02
 C21-C26
 1.4 with sigma of 0.02
 C27B-C28B
 1.4 with sigma of 0.02
 C30-C31
 1.4 with sigma of 0.02
 C30B-C29B
 1.4 with sigma of 0.02
3. Restrained planarity
 C30, C31, C32, C27, C28, C29
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N9 \\sim C33 \\sim C44 \\sim C38 \\sim C39 \\sim C41 \\sim C35 \\sim C34 \\sim
C43 \\sim C37 \\sim C40: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C28B \\sim C27B \\sim C29B \\sim C30B \\sim C31B \\sim C32B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C21: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C16 \\sim C18 \\sim C19 \\sim C17 \\sim C20 \\sim C15: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C27 \\sim C32 \\sim C30 \\sim C31 \\sim C29 \\sim C28: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C36 \\sim C42 \\sim C44 \\sim C38: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Uanis(C42) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(H34D)=
 Sof(H34E)=Sof(H34F)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41)=Sof(H41A)=Sof(H41B)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C36)=Sof(H36A)=
 Sof(H36B)=1-FVAR(1)
 Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H43A)=
 Sof(H43B)=Sof(H43C)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=FVAR(1)
 Fixed Sof: S6B(0.35) C27B(0.65) C30B(0.65) H30B(0.65) C28B(0.65) H28B(0.65)
 C31B(0.65) H31B(0.65) C32B(0.65) H32B(0.65) C29B(0.65) H29B(0.65) C27(0.35)
 C31(0.35) H31(0.35) C28(0.35) H28(0.35) C32(0.35) H32(0.35) C29(0.35)
 H29(0.35) C30(0.35) H30(0.35) S6A(0.65)
6.a Riding coordinates:
 C5(H5A,H5B,H5C), C37(H37A,H37B,H37C), C37(H37D,H37E,H37F), C43(H43A,H43B,
 H43C), C43(H43D,H43E,H43F), C34(H34A,H34B,H34C), C34(H34D,H34E,H34F), C40(H40A,
 H40B,H40C), C40(H40D,H40E,H40F)
6.b Ternary CH refined with riding coordinates:
 B00Y(H00Y)
6.c Secondary CH2 refined with riding coordinates:
 C011(H01M,H01N), C012(H01O,H01P), C01C(H01T,H01U), C01D(H01V,H01W), C33(H33A,
 H33B), C44(H44A,H44B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B),
 C35(H35A,H35B), C42(H42A,H42B), C36(H36A,H36B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C12(H12), C7(H7), C20(H20), C26(H26), C19(H19), C18(H18), C16(H16),
 C22(H22), C17(H17), C30B(H30B), C25(H25), C28B(H28B), C24(H24), C31B(H31B),
 C32B(H32B), C29B(H29B), C23(H23), C31(H31), C28(H28), C32(H32), C29(H29),
 C30(H30)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C14(H14A,H14B,H14C),
 C014(H01A,H01B,H01C), C015(H01D,H01E,H01F), C017(H01Q,H01R,H01S), C018(H01G,
 H01H,H01I), C019(H01J,H01K,H01L), C01G(H01X,H01Y,H), C01H(H01Z,HA,HB),
 C01M(H01,HC,HD)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96226
_shelx_hkl_checksum              1296
_shelx_fab_checksum              31021
_olex2_submission_special_instructions 'No special instructions were received'