Insertion and cleavage reactions of [closo-3,1,2-Ta(NMe2)3(C2B9H11)] with nitriles, phenols and thiols; structural characterisation of N,N-dimethylamidinate ligands †
Broder, Charlotte K.; Goeta, Andrés E.; Howard, Judith A. K.; Hughes, Andrew K.; Johnson, Andrew L.; Malget, John M.; Wade, Ken; Journal of the Chemical Society, Dalton Transactions  (2000) 3526–; doi:10.1039/b004862n

data_7009969
_publ_section_title
;
 Insertion and cleavage reactions of [closo-3,1,2-Ta(NMe2)3(C2B9H11)]
 with nitriles, phenols and thiols; structural characterisation of
 N,N-dimethylamidinate ligands&#x200A;&#x2020;
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3526
_journal_paper_doi               10.1039/b004862n
_journal_year                    2000
_chemical_formula_sum            'C31.5 H37 B9 N S4 Ta'
_chemical_formula_weight         836.10
_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                110.016(3)
_cell_angle_beta                 96.548(2)
_cell_angle_gamma                102.996(2)
_cell_formula_units_Z            2
_cell_length_a                   11.236(1)
_cell_length_b                   11.950(1)
_cell_length_c                   15.081(2)
_cell_measurement_reflns_used    700
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.92
_cell_measurement_theta_min      10.23
_cell_volume                     1813.1(3)
_computing_cell_refinement       'SMART-NT V5.0 (Bruker, 1998a)'
_computing_data_collection       'SMART-NT V5.0 (Bruker, 1998a)'
_computing_data_reduction        'SAINT-NT V5.0 (Bruker, 1998b)'
_computing_molecular_graphics    'SHELXTL-NT V5.1 (Bruker, 1998c)'
_computing_publication_material  'SHELXTL-NT V5.1 (Bruker, 1998c)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.901
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Bruker SMART-CCD'
_diffrn_measurement_method       \w
_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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.1763
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21823
_diffrn_reflns_theta_full        30.33
_diffrn_reflns_theta_max         30.33
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.286
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL-NT V5.1 (Bruker, 1998c)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.564
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9807
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                6099
_reflns_number_total             9807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004862n.txt
_cod_data_source_block           8
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C31.50 H37 B9 N S4 Ta'
_cod_database_code               7009969