Chemistry of group 5 metallaboranes with heterocyclic thiol ligands: a combined experimental and theoretical study.
Prakash, Rini; Haridas, Anagha; Bakthavachalam, K.; Roisnel, Thierry; Halet, Jean-François; Ghosh, Sundargopal; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4036–4044; doi:10.1039/d0dt04362a

data_7706618
_publ_section_title
;
 Chemistry of group 5 metallaboranes with heterocyclic thiol ligands: a
 combined experimental and theoretical study.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4036
_journal_page_last               4044
_journal_paper_doi               10.1039/d0dt04362a
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H38 B4 N Nb2 O S'
_chemical_formula_sum            'C27 H38 B4 N Nb2 O S'
_chemical_formula_weight         653.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2020-01-21 deposited with the CCDC.	2021-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.009(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3639(14)
_cell_length_b                   9.6186(9)
_cell_length_c                   13.6552(14)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.4734
_cell_measurement_theta_min      2.6100
_cell_measurement_wavelength     0.71073
_cell_volume                     1560.9(3)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15028
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         2.117
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plate
_exptl_crystal_F_000             666
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.140
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.175
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         6903
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0686
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+8.4148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1876
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.919
_reflns_number_gt                6300
_reflns_number_total             6903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0dt04362a2.cif
_cod_data_source_block           SGGR3
_cod_depositor_comments
'Adding full bibliography for 7706618--7706622.cif.'
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7706618
_shelx_res_checksum              75650
_shelx_hkl_checksum              92382