Hypoelectronic Dimetallaheteroboranes of Group 6 Transition Metals Containing Heavier Chalcogen Elements
Kiran Kumarvarma Chakrahari; Arunabha Thakur; Bijan Mondal; V. Ramkumar; Sundargopal Ghosh; Inorganic Chemistry 52 (2013) 7923–7932; doi:10.1021/ic400432v

data_4335445
_publ_section_title
;
 Hypoelectronic Dimetallaheteroboranes of Group 6 Transition Metals
 Containing Heavier Chalcogen Elements
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7923
_journal_page_last               7932
_journal_paper_doi               10.1021/ic400432v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety
'0.5(C20 H37 B5 S1 Mo2) + 0.5(C20 H36 B4 S1 MO2)'
_chemical_formula_sum            'C20 H36.5 B4.5 Mo2 S'
_chemical_formula_weight         549.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.2242(9)
_cell_length_b                   24.2242(9)
_cell_length_c                   8.3666(6)
_cell_measurement_reflns_used    2245
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.75
_cell_volume                     4909.6(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14823
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         4319
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0149P)^2^+19.9580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3457
_reflns_number_total             4319
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400432v_si_002_1.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-P4bc '
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C20 H36.50 B4.50 Mo2 S'
_cod_database_code               4335445