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_7009966
_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            'C32 H44 B9 F3 N6 Ta'
_chemical_formula_weight         847.97
_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                 90.976(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.104(3)
_cell_length_b                   18.420(4)
_cell_length_c                   15.495(4)
_cell_measurement_reflns_used    870
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      13.70
_cell_volume                     3739.6(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42691
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         9287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0184
_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^)+(0.0222P)^2^+2.4514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0466
_reflns_number_gt                8380
_reflns_number_total             9287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004862n.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009966