Synthesis and Characterization of Hypoelectronic Tantalaboranes: Comparison of the Geometric and Electronic Structures of [(Cp*TaX)2B5H11] (X = Cl, Br, and I)
K. Geetharani; Bellie Sundaram Krishnamoorthy; Samia Kahlal; Shaikh M. Mobin; Jean-François Halet; Sundargopal Ghosh; Inorganic Chemistry 51 (2012) 10176–10184; doi:10.1021/ic300848f

data_4330452
_publ_section_title
;
 Synthesis and Characterization of Hypoelectronic Tantalaboranes:
 Comparison of the Geometric and Electronic Structures of [(Cp*TaX)2B5H11]
 (X = Cl, Br, and I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10176
_journal_page_last               10184
_journal_paper_doi               10.1021/ic300848f
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C20 H34 B5 I Ta2'
_chemical_formula_weight         817.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 92.579(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.456(3)
_cell_length_b                   13.8228(19)
_cell_length_c                   10.2642(14)
_cell_measurement_reflns_used    3445
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.5
_cell_volume                     2615.9(7)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15055
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.544
_exptl_absorpt_correction_T_max  0.363
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         5.348
_refine_diff_density_min         -4.484
_refine_diff_density_rms         0.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0723
_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^)+(0.1347P)^2^+19.8339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2167
_reflns_number_gt                3326
_reflns_number_total             4601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300848f_si_002_3.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2615.9(6)
_cod_database_code               4330452