Chalcogen stabilized trimetallic clusters: synthesis, structures, and bonding of [(Cp*M)<sub>3</sub>(E)<sub>6+m</sub>(BH)<sub>n</sub>] (M = Nb or Ta; E = S or Se; m = 0 or 1 or 2; n = 0 or 1).
Kar, Sourav; Bairagi, Subhash; Saha, Koushik; Raghavendra, Beesam; Ghosh, Sundargopal; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4203–4210; doi:10.1039/c8dt05061a

data_7049163
_publ_section_title
;
 Chalcogen stabilized trimetallic clusters: synthesis, structures, and
 bonding of [(Cp*M)<sub>3</sub>(E)<sub>6+m</sub>(BH)<sub>n</sub>] (M = Nb
 or Ta; E = S or Se; m = 0 or 1 or 2; n = 0 or 1).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4203
_journal_page_last               4210
_journal_paper_doi               10.1039/c8dt05061a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '(C30 H45 B Nb3 S7) + 0.5(CH2Cl2)'
_chemical_formula_sum            'C30.5 H46 B Cl Nb3 S7'
_chemical_formula_weight         962.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-02-05 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7274(5)
_cell_length_b                   16.7472(5)
_cell_length_c                   15.8653(4)
_cell_measurement_reflns_used    6788
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.8
_cell_volume                     4178.8(2)
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex3 CMOS Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17535
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.771
_diffrn_reflns_theta_min         1.776
_diffrn_source                   'Sealed tube'
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2006)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 1772 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0516P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                4151
_reflns_number_total             4459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05061a2.cif
_cod_data_source_block           NBSH
_cod_depositor_comments
'Adding full bibliography for 7049161--7049163.cif.'
_cod_original_formula_sum        'C30.50 H46 B Cl Nb3 S7'
_cod_database_code               7049163
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.826
_shelx_res_checksum              67296