Unexpected formation of a trinuclear complex containing a Ta(IV)-Ta(IV) bond in the reactions of ButN[double bond, length as m-dash]Ta(NMe2)3 with silanes
Shu-Jian Chen; Juan Li; B.Dougan; C.Steren; Xiaoping Wang; Xue-Tai Chen; Zhenyang Lin; Ziling Xue; Chem.Commun. 47 (2011) 8685–; doi:10.1039/c1cc12837j

data_7106705
_publ_section_title
;
 Unexpected formation of a trinuclear complex containing a Ta(IV)-Ta(IV)
 bond in the reactions of ButN[double bond, length as m-dash]Ta(NMe2)3
 with silanes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8685
_journal_paper_doi               10.1039/c1cc12837j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         C24H64N9OTa3
_chemical_formula_sum            'C24 H64 N9 O Ta3'
_chemical_formula_weight         1037.69
_chemical_name_common            'Tantalum oxo hydride'
_chemical_name_systematic
;
Tantalum oxo hydride
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.289(4)
_cell_length_b                   17.389(7)
_cell_length_c                   23.143(9)
_cell_measurement_temperature    173(2)
_cell_volume                     3738(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       multi-scan
_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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38925
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    8.787
_exptl_absorpt_correction_T_max  0.2724
_exptl_absorpt_correction_T_min  0.1269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         6.897
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.20(2)
_refine_ls_extinction_coef       0.00023(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         8559
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.416
_refine_ls_shift/su_mean         0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+18.8072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1082
_reflns_number_gt                8314
_reflns_number_total             8559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12837j.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorhomic' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3738(2)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_original_formula_sum        C24H64N9OTa3
_cod_database_code               7106705