Carbon Dioxide Reduction by Terminal Tantalum Hydrides: Formation and Isolation of Bridging Methylene Diolate Complexes
Matthew A. Rankin; Christopher C. Cummins; Journal of the American Chemical Society 132 (2010) 10021–10023; doi:10.1021/ja104761n

data_4102720
_publ_section_title
;
 Carbon Dioxide Reduction by Terminal Tantalum Hydrides: Formation and
 Isolation of Bridging Methylene Diolate Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10021
_journal_page_last               10023
_journal_paper_doi               10.1021/ja104761n
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C39 H60 N3 Ta'
_chemical_formula_weight         751.85
_chemical_name_common            (Ar[Np]N)2(eta2-tBuC(H)NAr)TaH
_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                79.0900(10)
_cell_angle_beta                 85.1270(10)
_cell_angle_gamma                66.3400(10)
_cell_formula_units_Z            2
_cell_length_a                   11.0320(8)
_cell_length_b                   11.1702(8)
_cell_length_c                   17.1210(12)
_cell_measurement_reflns_used    9374
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.34
_cell_measurement_theta_min      2.70
_cell_volume                     1897.4(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43632
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    2.924
_exptl_absorpt_correction_T_max  0.7586
_exptl_absorpt_correction_T_min  0.5284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         10987
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0192
_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^)+(0.0228P)^2^+0.9605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                10458
_reflns_number_total             10987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104761n_si_003.cif
_cod_data_source_block           09026mrb
_cod_database_code               4102720