Low-Valent Ditantalum Complex Ta2(μ-BH3)(μ-dmpm)3(η2-BH4)2: First Dinuclear Compound Containing a Bridging BH3 Group with Direct Ta-B Bonds
F. Albert Cotton; Carlos A. Murillo; Xiaoping Wang; Journal of the American Chemical Society 120 (1998) 9594–9599; doi:10.1021/ja9817242

data_4116840
_publ_section_title
;
 Low-Valent Ditantalum Complex Ta2(\m-BH3)(\m-dmpm)3(\h2-BH4)2: First
 Dinuclear Compound Containing a Bridging BH3 Group with Direct Ta-B Bonds
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9594
_journal_page_last               9599
_journal_paper_doi               10.1021/ja9817242
_journal_volume                  120
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         Ta2(BH3)(dmpm)3(BH4)2.C7H8
_chemical_formula_sum            'C22 H61 B3 P6 Ta2'
_chemical_formula_weight         905.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3080(10)
_cell_length_b                   16.0860(10)
_cell_length_c                   13.8755(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.0
_cell_measurement_theta_min      17.0
_cell_volume                     3640.0(4)
_computing_cell_refinement       'CAD4 V5'
_computing_data_collection       'CAD4 V5'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       'Omega-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_refln_scan_mode_backgd   mo
_diffrn_refln_scan_width         0.70
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2700
_diffrn_reflns_theta_max         22.37
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.283
_exptl_absorpt_correction_T_max  0.9988
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.990
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2438
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.099
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_obs          0.0259
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+9.3405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0721
_refine_ls_wR_factor_obs         0.0674
_reflns_number_observed          2033
_reflns_number_total             2438
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9817242_3.cif
_cod_data_source_block           (1toluene)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_refln_scan_mode_backgd' value 'MO' changed to 'mo' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+9.3405P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+9.3405P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C22 H11 H50 B3 P6 Ta2'
_cod_database_code               4116840