Nitride-incorporated W-Fe-S double cubane clusters: terminal ligand substitutions and redox behaviors.
Xue, Lian; Xu, Gan; Wang, Zheng; Chen, Xu-Dong; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6840–6847; doi:10.1039/d1dt00414j

data_7707285
_publ_section_title
;
 Nitride-incorporated W-Fe-S double cubane clusters: terminal ligand
 substitutions and redox behaviors.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6840
_journal_page_last               6847
_journal_paper_doi               10.1039/d1dt00414j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C58 H72 B2 Fe6 N14 S10 W2, C3 H7 N O, 2(C8 H20 N)'
_chemical_formula_sum            'C77 H119 B2 Fe6 N17 O S10 W2'
_chemical_formula_weight         2343.90
_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             2021-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-05 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                76.250(2)
_cell_angle_beta                 89.471(2)
_cell_angle_gamma                88.082(2)
_cell_formula_units_Z            4
_cell_length_a                   14.222(3)
_cell_length_b                   25.989(5)
_cell_length_c                   28.267(5)
_cell_measurement_reflns_used    9326
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      24.908
_cell_measurement_theta_min      2.225
_cell_volume                     10143(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            196670
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.219
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.344
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0581 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.9329. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2216
_refine_ls_number_reflns         39770
_refine_ls_number_restraints     3054
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0412P)^2^+25.2431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27933
_reflns_number_total             39770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00414j2.cif
_cod_data_source_block           mo_222_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7707281--7707285.cif.'
_cod_original_cell_volume        10142(3)
_cod_database_code               7707285
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.554
_shelx_estimated_absorpt_t_min   0.348
_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. Uiso/Uaniso restraints and constraints
O2 \\sim C159 \\sim N33 \\sim C157 \\sim C158: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C30 \\sim C29 \\sim C28 \\sim
C27 \\sim C26 \\sim C20 \\sim C19 \\sim C18 \\sim C17 \\sim C16 \\sim C10 \\sim
C9 \\sim C8 \\sim C7 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1
\\sim C15 \\sim C14 \\sim C13 \\sim C12 \\sim C11 \\sim C45 \\sim C46 \\sim C47
\\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C53 \\sim C54 \\sim C55 \\sim C56
\\sim C57 \\sim C52 \\sim C58 \\sim C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33
\\sim C32 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43
\\sim C44 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C160 \\sim C161
\\sim C162 \\sim C157 \\sim C158 \\sim C159 \\sim C120 \\sim C123 \\sim C163
\\sim C167 \\sim C117 \\sim C118 \\sim C119 \\sim C121 \\sim C122 \\sim C124
\\sim C165 \\sim C166 \\sim C137 \\sim C138 \\sim C139 \\sim C140 \\sim C141
\\sim C144 \\sim C145 \\sim C148 \\sim C142 \\sim C143 \\sim C146 \\sim C147
\\sim C149 \\sim C150 \\sim C151 \\sim C152 \\sim C153 \\sim C154 \\sim C155
\\sim C156 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C132
\\sim C133 \\sim C136 \\sim C130 \\sim C131 \\sim C134 \\sim C135: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(H12J)=Sof(H12K)=Sof(H12L)=Sof(H16G)=
 Sof(H16H)=Sof(H16I)=Sof(H16M)=Sof(H16N)=Sof(H16O)=Sof(C122)=Sof(H12O)=
 Sof(H12P)=Sof(C124)=Sof(H12Q)=Sof(H12R)=Sof(C165)=Sof(H16P)=Sof(H16Q)=
 Sof(C166)=Sof(H16R)=Sof(H16S)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(H13J)=
 Sof(H13K)=Sof(H13L)=Sof(H13P)=Sof(H13Q)=Sof(H13R)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C142)=Sof(H14O)=Sof(H14P)=Sof(C143)=Sof(H14Q)=Sof(H14R)=
 Sof(C146)=Sof(H14S)=Sof(H14T)=Sof(C147)=Sof(H14U)=Sof(H14V)=Sof(H12V)=
 Sof(H12W)=Sof(H12X)=Sof(HC)=Sof(HD)=Sof(HE)=Sof(HH)=Sof(HI)=Sof(HJ)=Sof(HM)=
 Sof(HN)=Sof(HO)=Sof(C130)=Sof(H13Y)=Sof(HQ)=Sof(C131)=Sof(H13Z)=Sof(HR)=
 Sof(C134)=Sof(H1AA)=Sof(HS)=Sof(C135)=Sof(H2AA)=Sof(HT)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(H12G)=Sof(H12H)=Sof(H12I)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(H16J)=Sof(H16K)=Sof(H16L)=Sof(C117)=Sof(H11G)=
 Sof(H11H)=Sof(C118)=Sof(H11I)=Sof(H11J)=Sof(C119)=Sof(H11K)=Sof(H11L)=
 Sof(C121)=Sof(H12M)=Sof(H12N)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(H13G)=
 Sof(H13H)=Sof(H13I)=Sof(H13M)=Sof(H13N)=Sof(H13O)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C141)=Sof(H14G)=Sof(H14H)=Sof(C144)=Sof(H14I)=Sof(H14J)=
 Sof(C145)=Sof(H14K)=Sof(H14L)=Sof(C148)=Sof(H14M)=Sof(H14N)=Sof(H12S)=
 Sof(H12T)=Sof(H12U)=Sof(H12Y)=Sof(HA)=Sof(HB)=Sof(H12Z)=Sof(HF)=Sof(HG)=
 Sof(H12)=Sof(HK)=Sof(HL)=Sof(C129)=Sof(H0AA)=Sof(HP)=Sof(C132)=Sof(H13S)=
 Sof(H13T)=Sof(C133)=Sof(H13U)=Sof(H13V)=Sof(C136)=Sof(H13W)=Sof(H13X)=FVAR(1)
4.a Riding coordinates:
 C58(H58A,H58B,H58C), C44(H44A,H44B,H44C), C163(H16D,H16E,H16F), C163(H16G,
 H16H,H16I), C137(H13D,H13E,H13F), C138(H13G,H13H,H13I), C138(H13J,H13K,H13L),
 C139(H13P,H13Q,H13R), C125(H12V,H12W,H12X), C126(HC,HD,HE), C128(HM,HN,HO)
4.b Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3A), B4(H4)
4.c Secondary CH2 refined with riding coordinates:
 C117(H11G,H11H), C118(H11I,H11J), C119(H11K,H11L), C121(H12M,H12N), C122(H12O,
 H12P), C124(H12Q,H12R), C165(H16P,H16Q), C166(H16R,H16S), C141(H14G,H14H),
 C144(H14I,H14J), C145(H14K,H14L), C148(H14M,H14N), C142(H14O,H14P), C143(H14Q,
 H14R), C146(H14S,H14T), C147(H14U,H14V), C150(H15D,H15E), C152(H15I,H15J),
 C153(H15K,H15L), C155(H15P,H15Q), C129(H0AA,HP), C132(H13S,H13T), C133(H13U,
 H13V), C136(H13W,H13X), C130(H13Y,HQ), C131(H13Z,HR), C134(H1AA,HS), C135(H2AA,
 HT)
4.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C28(H28), C18(H18), C8(H8), C3(H3), C13(H13), C46(H46), C47(H47),
 C49(H49), C50(H50), C53(H53), C54(H54), C56(H56), C57(H57), C36(H36), C35(H35),
  C33(H33), C32(H32), C39(H39), C40(H40), C42(H42), C43(H43), C61(H61),
 C66(H66), C71(H71), C76(H76), C81(H81), C86(H86), C90(H90), C91(H91), C93(H93),
  C94(H94), C97(H97), C98(H98), C100(H100), C101(H101), C104(H104), C105(H105),
 C107(H107), C108(H108), C111(H111), C112(H112), C114(H114), C115(H115),
 C162(H162), C159(H159)
4.e Fitted hexagon refined as free rotating group:
 C53(C54,C55,C56,C57,C52)
4.f Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C26(H26A,H26B,
 H26C), C20(H20A,H20B,H20C), C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C6(H6A,
 H6B,H6C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C11(H11A,H11B,
 H11C), C51(H51A,H51B,H51C), C37(H37A,H37B,H37C), C59(H59A,H59B,H59C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C),
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C88(H88A,H88B,H88C), C95(H95A,
 H95B,H95C), C102(H10D,H10E,H10F), C109(H10G,H10H,H10I), C116(H11D,H11E,H11F),
 C160(H16T,H16U,H16V), C161(H16W,H16X,H16Y), C157(H15U,H15V,H15W), C158(H15X,
 H15Y,H), C120(H12A,H12B,H12C), C120(H12D,H12E,H12F), C123(H12G,H12H,H12I),
 C123(H12J,H12K,H12L), C167(H16J,H16K,H16L), C167(H16M,H16N,H16O), C137(H13A,
 H13B,H13C), C139(H13M,H13N,H13O), C140(H14A,H14B,H14C), C140(H14D,H14E,H14F),
 C149(H14W,H14X,H14Y), C151(H15F,H15G,H15H), C154(H15M,H15N,H15O), C156(H15R,
 H15S,H15T), C125(H12S,H12T,H12U), C126(H12Y,HA,HB), C127(H12Z,HF,HG), C127(HH,
 HI,HJ), C128(H12,HK,HL)
;
_shelx_res_checksum              9
_shelx_hkl_checksum              81574
_shelx_fab_checksum              48031
_olex2_submission_special_instructions 'No special instructions were received'