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_7712903
_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
'C18 H31 B Cl3 Fe3 N7 S3 Si W, 2(C8 H20 N), C2 H3 N'
_chemical_formula_sum            'C36 H74 B Cl3 Fe3 N10 S3 Si W'
_chemical_formula_weight         1239.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.825(15)
_cell_length_b                   19.385(14)
_cell_length_c                   28.47(2)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.357
_cell_measurement_theta_min      2.220
_cell_volume                     10941(14)
_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 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54342
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.397
_diffrn_reflns_theta_min         1.634
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1232 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.6439.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'brownish red'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             5040
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         9993
_refine_ls_number_restraints     737
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.0960
_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^)+398.8586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.2041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7218
_reflns_number_total             9993
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00865g2.cif
_cod_data_source_block           mo_zhy84d_0ma_a
_cod_database_code               7712903
_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-C42
 1.54 with sigma of 0.001
 C37-C39
 1.54 with sigma of 0.001
 C40-C42
 1.54 with sigma of 0.001
 C39-C38
 1.54 with sigma of 0.001
 C32-C31
 1.54 with sigma of 0.001
 N9-C41
 1.54 with sigma of 0.001
 C30-C31
 1.54 with sigma of 0.001
 C34-C35
 1.54 with sigma of 0.001
 N9-C40
 1.54 with sigma of 0.001
 C35-C33
 1.54 with sigma of 0.001
 C27-C24
 1.54 with sigma of 0.02
 C25-C26
 1.54 with sigma of 0.02
 C21-C20
 1.54 with sigma of 0.02
 C29-C28
 1.54 with sigma of 0.02
 C43-C44
 1.46 with sigma of 0.02
 C10-C9
 1.51 with sigma of 0.0001
 C12-C11
 1.51 with sigma of 0.0001
 C3-C4
 1.47 with sigma of 0.0001
 C7-C6
 1.51 with sigma of 0.0001
 C2-C1
 1.51 with sigma of 0.0001
 C12-C13
 1.47 with sigma of 0.0001
 C3-C2
 1.47 with sigma of 0.0001
 C14-C13
 1.47 with sigma of 0.0001
 C4-C5
 1.51 with sigma of 0.0001
 C9-C8
 1.47 with sigma of 0.0001
 C8-C7
 1.47 with sigma of 0.0001
 C15-C14
 1.51 with sigma of 0.0001
3. Rigid bond restraints
 N8, C21
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 N8, C25
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C37 \\sim C1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C14 \\sim C15 \\sim C13 \\sim C3 \\sim C2 \\sim C12 \\sim C6 \\sim C4 \\sim C7
\\sim C1 \\sim C19 \\sim C16 \\sim C11 \\sim C8 \\sim C9 \\sim C5 \\sim C17
\\sim C29 \\sim C10 \\sim C27 \\sim C28 \\sim C39 \\sim C44 \\sim C20 \\sim C24
\\sim C43 \\sim C21 \\sim C25 \\sim C35 \\sim C26 \\sim C42 \\sim C38 \\sim C41
\\sim C34 \\sim C33 \\sim C37 \\sim C31 \\sim C30 \\sim C40 \\sim C32: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
5. Others
 Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(H42D)=
 Sof(H42E)=Sof(H42F)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C41)=Sof(H41A)=Sof(H41B)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=1-FVAR(1)
 Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(H42A)=
 Sof(H42B)=Sof(H42C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C32)=Sof(H32A)=
 Sof(H32B)=FVAR(1)
6.a Riding coordinates:
 C6(H6A,H6B,H6C), C29(H29A,H29B,H29C), C39(H39D,H39E,H39F), C39(H39A,H39B,
 H39C), C35(H35A,H35B,H35C), C35(H35D,H35E,H35F), C42(H42D,H42E,H42F), C42(H42A,
 H42B,H42C), C31(H31D,H31E,H31F), C31(H31A,H31B,H31C)
6.b Ternary CH refined with riding coordinates:
 B1(H1)
6.c Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C21(H21A,H21B), C25(H25A,H25B), C38(H38A,
 H38B), C41(H41A,H41B), C34(H34A,H34B), C33(H33A,H33B), C37(H37A,H37B),
 C30(H30A,H30B), C40(H40A,H40B), C32(H32A,H32B)
6.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C8(H8)
6.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C16(H16A,H16B,
 H16C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C10(H10A,
 H10B,H10C), C44(H44A,H44B,H44C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20229
_shelx_hkl_checksum              1105
_shelx_fab_checksum              47991
_olex2_submission_special_instructions 'No special instructions were received'