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_4102721
_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            'C88.5 H145 N6 O2 Ta Ti'
_chemical_formula_weight         1553.95
_chemical_name_common            (Ar[Np]N)2(tBuC(H)NAr)TaOCH2OTi(N[tBu]Ar)3
_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                 104.3540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7446(14)
_cell_length_b                   38.429(3)
_cell_length_c                   12.6441(9)
_cell_measurement_reflns_used    9581
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.29
_cell_volume                     8823.7(11)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            180703
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.8099
_exptl_absorpt_correction_T_min  0.6159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3316
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_platon_squeeze_details
; The unit cell contains 8 molecules of n-pentane which have been treated 
as a diffuse contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         1.508
_refine_diff_density_min         -3.845
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         20563
_refine_ls_number_restraints     413
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+28.4041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                17747
_reflns_number_total             20563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104761n_si_004.cif
_cod_data_source_block           09393_5p
_cod_original_cell_volume        8823.6(11)
_cod_original_formula_sum        'C88.50 H145 N6 O2 Ta Ti'
_cod_database_code               4102721