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_7712904
_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 Fe3 N16 S3 Si W, C8 H20 N'
_chemical_formula_sum            'C26 H51 B Fe3 N17 S3 Si W'
_chemical_formula_weight         1088.31
_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             2022-12-12
_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                83.765(5)
_cell_angle_beta                 86.492(5)
_cell_angle_gamma                87.819(5)
_cell_formula_units_Z            2
_cell_length_a                   10.742(4)
_cell_length_b                   11.078(5)
_cell_length_c                   21.227(9)
_cell_measurement_reflns_used    7289
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.598
_cell_measurement_theta_min      2.530
_cell_volume                     2505.1(18)
_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 0.980
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_unetI/netI     0.1058
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25230
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         2.530
_exptl_absorpt_coefficient_mu    3.325
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             1090
_refine_diff_density_max         1.678
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         11110
_refine_ls_number_restraints     404
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0598P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7337
_reflns_number_total             11110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00865g2.cif
_cod_data_source_block           mo_zhy30_0m_a
_cod_original_cell_volume        2505.0(18)
_cod_database_code               7712904
_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. Restrained distances
 C24-C26
 1.55 with sigma of 0.005
 C30-C21
 1.55 with sigma of 0.02
 C22-N17
 1.55 with sigma of 0.02
 C33-C21
 3 with sigma of 0.02
 C19-C31
 1.55 with sigma of 0.02
 C22-C20
 1.55 with sigma of 0.02
 C23-C25
 1.55 with sigma of 0.005
 C31-C19
 1.55 with sigma of 0.02
 C33-C32
 1.55 with sigma of 0.02
 N17-C23
 1.55 with sigma of 0.005
 C29-C27
 1.55 with sigma of 0.02
 N17-C22
 1.55 with sigma of 0.02
 N17-C25
 2.5 with sigma of 0.005
 C29-N17
 2.5 with sigma of 0.02
 N17-C32
 2.5 with sigma of 0.02
 N17-C30
 1.55 with sigma of 0.02
 C25-C30
 2.5 with sigma of 0.02
 C24-N17
 1.55 with sigma of 0.005
 C27-C25
 2.5 with sigma of 0.02
 C19-N17
 1.55 with sigma of 0.02
 C33-N17
 1.55 with sigma of 0.02
 C27-N17
 1.55 with sigma of 0.02
 C30-C33
 2.2 with sigma of 0.02
 C27-C33
 2.2 with sigma of 0.02
 C27-C23
 2.2 with sigma of 0.02
 C30-C23
 2.2 with sigma of 0.02
 C27-C30
 2.2 with sigma of 0.02
3. Rigid bond restraints
 N7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, N6, N7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N4, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C20, C22
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
N10 \\sim N9: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
N6 \\sim N7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N7) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(1)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C34)=
 Sof(H34A)=Sof(H34B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C20)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C31)=Sof(H31A)=Sof(H31B)=
 Sof(H31C)=Sof(C24)=Sof(H24A)=Sof(H24B)=FVAR(1)
6.a Riding coordinates:
 C5(H5A,H5B,H5C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C), C20(H20A,H20B,H20C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C29(H29A,
 H29B,H29C), C21(H21A,H21B,H21C)
6.b Ternary CH refined with riding coordinates:
 B00X(H00X)
6.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C34(H34A,H34B), C33(H33A,H33B), C19(H19A,H19B), C23(H23A,
 H23B), C27(H27A,H27B), C24(H24A,H24B), C30(H30A,H30B)
6.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C3(H3)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6277
_shelx_hkl_checksum              17678
_shelx_fab_checksum              85236
_olex2_submission_special_instructions 'No special instructions were received'