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_4120011
_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         'C21 H42 N5 Ta'
_chemical_formula_sum            'C21 H42 N5 Ta'
_chemical_formula_weight         545.55
_chemical_name_common            cmpd3
_chemical_name_systematic
;
Ta-complex
;
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_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 115.0620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6584(5)
_cell_length_b                   32.0742(19)
_cell_length_c                   9.6122(6)
_cell_measurement_reflns_used    14547
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.4
_cell_volume                     2418.1(3)
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_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
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_diffrn_detector                 'CCD area detector'
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_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
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_diffrn_orient_matrix_UB_11      0.0587953
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_diffrn_orient_matrix_UB_21      -0.0496216
_diffrn_orient_matrix_UB_22      0.0275295
_diffrn_orient_matrix_UB_23      -0.0462200
_diffrn_orient_matrix_UB_31      0.1016658
_diffrn_orient_matrix_UB_32      0.0145150
_diffrn_orient_matrix_UB_33      0.0787370
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30018
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
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_exptl_absorpt_correction_T_max  0.663
_exptl_absorpt_correction_T_min  0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.997
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0237
_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^)+(0.01P)^2^+4.955P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0452
_reflns_number_gt                6506
_reflns_number_total             7056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402804k_si_003.cif
_cod_data_source_block           cmpd3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4120011