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_4330451
_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 H32 B5 I2 Ta2'
_chemical_formula_weight         942.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.4050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0832(2)
_cell_length_b                   15.5579(2)
_cell_length_c                   22.0241(3)
_cell_measurement_reflns_used    18854
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7545
_cell_measurement_theta_min      3.2288
_cell_volume                     5360.75(12)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39696
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    10.468
_exptl_absorpt_correction_T_max  0.1576
_exptl_absorpt_correction_T_min  0.1166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_description       block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.556
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0264P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                7315
_reflns_number_total             9427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300848f_si_002_2.cif
_cod_data_source_block           iitm098
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4330451