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_7009965
_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            'C14 H38 B9 N6 Ta'
_chemical_formula_weight         568.74
_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                78.3220(10)
_cell_angle_beta                 83.6740(10)
_cell_angle_gamma                75.0130(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3136(5)
_cell_length_b                   10.4888(6)
_cell_length_c                   13.2061(7)
_cell_measurement_reflns_used    980
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.91
_cell_measurement_theta_min      5.13
_cell_volume                     1218.12(12)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13888
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.525
_exptl_absorpt_correction_T_max  0.7730
_exptl_absorpt_correction_T_min  0.2647
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXTL-NT V5.1 (Bruker, 1998c)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       Plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0459P)^2^+0.2102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                5000
_reflns_number_total             5565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004862n.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009965