Synthesis and crystal structure of the cluster (Et4N)[(Tp*)MoFe3S3(μ3-NSiMe3)(N3)3]
Li, Yue; Wei, Jia; Han, Jie; Chen, Xu-Dong; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 691–694; doi:10.1107/S2056989024004833

data_2023149
_publ_section_title
;
 Synthesis and crystal structure of the cluster
 (Et4N)[(Tp*)MoFe3S3(\m3-NSiMe3)(N3)3]
;
_journal_coeditor_code           OI2008
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              691
_journal_page_last               694
_journal_paper_doi               10.1107/S2056989024004833
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'(C8 H20 N) [Fe3 Mo S3 (C15 H22 B N6) (C3 H9 N Si) (N3)3]'
_chemical_formula_moiety
'C8 H20 N +, C18 H31 B Fe3 Mo N16 S3 Si -, [+ solvents]'
_chemical_formula_sum            'C26 H51 B Fe3 Mo N17 S3 Si'
_chemical_formula_weight         1000.40
_chemical_name_systematic
;Tetraethylammonium
triazidotri-\m~3~-sulfido-[\m~3~-(trimethylsilyl)azanediido][tris(3,5-dimethylpyrazol-1-yl)hydroborato]triiron(+2.33)molybdenum(VI)
;
_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   geom
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_cell_angle_alpha                75.306(7)
_cell_angle_beta                 84.362(7)
_cell_angle_gamma                86.829(7)
_cell_formula_units_Z            2
_cell_length_a                   10.689(6)
_cell_length_b                   11.321(6)
_cell_length_c                   19.030(11)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.529
_cell_measurement_theta_min      2.296
_cell_volume                     2216(2)
_computing_cell_refinement
;
SAINT V8.40B (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT V8.40B (Bruker, 2016)
;
_computing_molecular_graphics
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Olex2 1.5-alpha (Dolomanov <i>et al.</i>,  2009)
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Olex2 1.5-alpha (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31083
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.680
_diffrn_reflns_theta_min         1.861
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            'dark black'
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       needle
_exptl_crystal_F_000             1026
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         10181
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0361P)^2^+0.6048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0709
_reflns_number_gt                8508
_reflns_number_total             10181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oi2008.cif
_cod_data_source_block           I
_cod_database_code               2023149
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.986
_shelx_hkl_checksum              9995
_shelx_res_checksum              42292
_shelx_fab_checksum              9511