Chemistry of Molybdaboranes: Synthesis, Structures, and Characterization of a New Class of Open-Cage Dimolybdaheteroborane Clusters
Rajendra Singh Dhayal; Kiran Kumar Varma Chakrahari; Babu Varghese; Shaikh M. Mobin; Sundargopal Ghosh; Inorganic Chemistry 49 (2010) 7741–7747; doi:10.1021/ic100520k

data_4316351
_publ_section_title
;
 Chemistry of Molybdaboranes: Synthesis, Structures, and Characterization
 of a New Class of Open-Cage Dimolybdaheteroborane Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7741
_journal_page_last               7747
_journal_paper_doi               10.1021/ic100520k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '(C38 H47 B1 S4 Mo2) . 0.5(C H2 Cl2)'
_chemical_formula_sum            'C38.5 H48 B Cl Mo2 S4'
_chemical_formula_weight         877.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.821(2)
_cell_angle_beta                 82.061(2)
_cell_angle_gamma                65.939(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6733(3)
_cell_length_b                   11.8836(4)
_cell_length_c                   17.4329(6)
_cell_measurement_reflns_used    6274
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      2.45
_cell_volume                     1918.09(11)
_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, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractomter'
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27013
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.23
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker,1999)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9255
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0441P)^2^+3.9432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                6697
_reflns_number_total             9255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100520k_si_001_1.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C38.50 H48 B Cl Mo2 S4'
_cod_database_code               4316351