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_7009968
_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            'C26 H38 B9 O3 Ta'
_chemical_formula_weight         676.80
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.108(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.732(3)
_cell_length_b                   19.920(3)
_cell_length_c                   15.986(3)
_cell_measurement_reflns_used    673
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.25
_cell_measurement_theta_min      13.69
_cell_volume                     5941.3(17)
_computing_cell_refinement       'SMART-NT V5.0 (Bruker, 1998)'
_computing_data_collection       'SMART-NT V5.0 (Bruker, 1998)'
_computing_data_reduction        'SAINT-NT V5.0 (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL-NT V5.1 (Bruker, 1998)'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71190
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.727
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.252
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL-NT V5.1 (Bruker, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         16897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+6.8731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0575
_reflns_number_gt                12834
_reflns_number_total             16897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004862n.txt
_cod_data_source_block           7
_cod_original_cell_volume        5941.4(17)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009968