N-N Bond Cleavage of Mid-Valent Ta(IV) Hydrazido and Hydrazidium Complexes Relevant to the Schrock Cycle for Dinitrogen Fixation
Andrew J. Keane; Peter Y. Zavalij; Lawrence R. Sita; Journal of the American Chemical Society 135 (2013) 9580–9583; doi:10.1021/ja402804k

data_4120013
_publ_section_title
;
 N-N Bond Cleavage of Mid-Valent Ta(IV) Hydrazido and Hydrazidium
 Complexes Relevant to the Schrock Cycle for Dinitrogen Fixation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9580
_journal_page_last               9583
_journal_paper_doi               10.1021/ja402804k
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C22 H44 Cl N5 Ta, 1.5(C6 H6), C F3 O3 S'
_chemical_formula_sum            'C32 H53 Cl F3 N5 O3 S Ta'
_chemical_formula_weight         861.25
_chemical_name_common            Ta-complex
_chemical_name_systematic
;
Ta-complex AK-505
;
_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 & ZCIF'
_cell_angle_alpha                110.2117(13)
_cell_angle_beta                 92.9333(14)
_cell_angle_gamma                107.0979(14)
_cell_formula_units_Z            2
_cell_length_a                   8.9354(9)
_cell_length_b                   13.3297(13)
_cell_length_c                   17.8137(17)
_cell_measurement_reflns_used    23834
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3
_cell_measurement_theta_min      2.4
_cell_volume                     1875.3(3)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0980086
_diffrn_orient_matrix_UB_12      -0.0218794
_diffrn_orient_matrix_UB_13      -0.0014082
_diffrn_orient_matrix_UB_21      -0.0245984
_diffrn_orient_matrix_UB_22      -0.0340030
_diffrn_orient_matrix_UB_23      -0.0606572
_diffrn_orient_matrix_UB_31      0.0625183
_diffrn_orient_matrix_UB_32      0.0745033
_diffrn_orient_matrix_UB_33      -0.0020090
_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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29057
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.110
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       needle
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         10872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0171
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+1.78P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0378
_refine_ls_wR_factor_ref         0.0381
_reflns_number_gt                10377
_reflns_number_total             10872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402804k_si_005.cif
_cod_data_source_block           2297
_cod_database_code               4120013