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_4120016
_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         'C38 H70 N8 Ta2'
_chemical_formula_sum            'C38 H70 N8 Ta2'
_chemical_formula_weight         1000.92
_chemical_name_common            ?Ta2-complex
_chemical_name_systematic
;
Ta2-complex
;
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 90.4380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1501(7)
_cell_length_b                   11.8403(8)
_cell_length_c                   14.9152(10)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.4
_cell_measurement_theta_min      2.2
_cell_volume                     1969.1(2)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
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_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
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_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      610,610,610
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTEGen loop'
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_diffrn_orient_matrix_UB_22      0.0630457
_diffrn_orient_matrix_UB_23      -0.0393879
_diffrn_orient_matrix_UB_31      0.0849631
_diffrn_orient_matrix_UB_32      0.0238444
_diffrn_orient_matrix_UB_33      -0.0097048
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
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_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22594
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.20
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.590
_exptl_absorpt_correction_T_max  0.366
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_id
'Sita/Yonke BY-6-034A (light yellow/brown xtals) @100K'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         5734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0158
_refine_ls_R_factor_gt           0.0148
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.015P)^2^+2.41P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0346
_refine_ls_wR_factor_ref         0.0350
_reflns_number_gt                5513
_reflns_number_total             5734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402804k_si_008.cif
_cod_data_source_block           cmpdtrans7
_cod_database_code               4120016
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 1830
_diffrn_measurement_frame_time-ccd 5
_diffrn_measurement_total_time-ccd 5.6
_diffrn_detector_distance-ccd    5.0000
_diffrn_measurement_frame_size-ccd 512