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_7712906
_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 H67 B Fe3 N13 S3 Si W, C24 H20 B'
_chemical_formula_sum            'C63 H87 B2 Fe3 N13 S3 Si W'
_chemical_formula_weight         1523.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 109.78(05)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.87(14)
_cell_length_b                   31.70(9)
_cell_length_c                   25.83(9)
_cell_measurement_reflns_used    6850
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      22.540
_cell_measurement_theta_min      2.211
_cell_volume                     15310(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            149896
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.583
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.196
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4828
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0921 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.6475.
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    1.322
_exptl_crystal_description       block
_exptl_crystal_F_000             6240
_refine_diff_density_max         1.150
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1590
_refine_ls_number_reflns         35042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0006P)^2^+61.0186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22746
_reflns_number_total             35042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00865g2.cif
_cod_data_source_block           mo_zhy71_0m_a
_cod_original_cell_volume        15308(129)
_cod_database_code               7712906
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 C01P(H01A,H01B,H01C)
2.b Ternary CH refined with riding coordinates:
 B3(H3), B1(H1A)
2.c Aromatic/amide H refined with riding coordinates:
 C01J(H01J), C01U(H01U), C01V(H01V), C01X(H01X), C022(H022), C025(H025),
 C027(H027), C028(H028), C02G(H11), C02H(H12), C02N(H02), C02Q(H13), C02R(H14),
 C02T(H15), C02U(H24), C032(H032), C033(H033), C034(H034), C036(H036),
 C03C(H16), C03D(H03P), C03H(H25), C03I(H26), C03L(H27), C03Q(H28), C03U(H17),
 C03V(H18), C03X(H19), C03Z(H29), C041(H041), C043(H043), C044(H044),
 C045(H045), C046(H046), C047(H047), C048(H048), C049(H049), C04B(H30),
 C04D(H20), C04G(H31), C04I(H32), C04L(H21), C04M(H22), C04N(H23), C04O(H33),
 C04P(H34)
2.d Idealised Me refined as rotating group:
 C01Z(H01D,H01E,H01F), C023(H02V,H02W,H02X), C02A(H02A,H02B,H02C), C02C(H02Y,H,
 HA), C02E(H02D,H02E,H02F), C02F(H02Z,HB,HC), C02L(H02G,H02H,H02I), C02O(H02J,
 H02K,H02L), C02P(H02M,H02N,H02O), C02W(H1,HD,HE), C02X(H02P,H02Q,H02R),
 C02Z(H02S,H02T,H02U), C030(H03A,H03B,H03C), C031(H03W,H03X,H03Y), C035(H03D,
 H03E,H03F), C037(H03G,H03H,H03I), C038(H03J,H03K,H03L), C039(H03Z,HF,HG),
 C03A(H03M,H03N,H03O), C03F(H03,HH,HI), C03G(H2,HJ,HK), C03J(H4,HL,HM), C03M(H5,
 HN,HO), C03N(H03Q,H03R,H03S), C03O(H6,HP,HQ), C03P(H7,HR,HS), C03S(H8,HT,HU),
 C03T(H9,HV,HW), C03Y(H03T,H03U,H03V), C040(H04P,H04Q,H04R), C042(H04S,H04T,
 H04U), C04A(H04A,H04B,H04C), C04C(H04D,H04E,H04F), C04E(H04G,H04H,H04I),
 C04F(H04V,H04W,H04X), C04H(H04J,H04K,H04L), C04J(H04M,H04N,H04O), C04K(H04Y,HX,
 HY), C04Q(H04Z,HZ,H35), C04R(H04,H36,H37), C04S(H10,H38,H39)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92427
_shelx_hkl_checksum              66949
_shelx_fab_checksum              51227
_olex2_submission_special_instructions 'No special instructions were received'