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_4120014
_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 N5 Ta, C F3 O3 S'
_chemical_formula_sum            'C23 H44 F3 N5 O3 S Ta'
_chemical_formula_weight         708.64
_chemical_name_common            Ta-complex
_chemical_name_systematic
;
Ta-complex
;
_space_group_IT_number           14
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7149(7)
_cell_length_b                   16.1159(11)
_cell_length_c                   17.1925(12)
_cell_measurement_reflns_used    12994
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.3
_cell_volume                     2955.7(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
crystal id        'Sita-Keane AK-470 150K'
frame size         512
frame width      -0.30
total frames      3030
frame time          30
total time        27.8
detector_distance-CCD         5.000
;
_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      0.0025459
_diffrn_orient_matrix_UB_12      0.0477443
_diffrn_orient_matrix_UB_13      -0.0369696
_diffrn_orient_matrix_UB_21      -0.0202866
_diffrn_orient_matrix_UB_22      -0.0383889
_diffrn_orient_matrix_UB_23      -0.0451126
_diffrn_orient_matrix_UB_31      -0.0914851
_diffrn_orient_matrix_UB_32      0.0098543
_diffrn_orient_matrix_UB_33      0.0033637
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39953
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.840
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       prism
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.417
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_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^+7.41P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                6934
_reflns_number_total             8606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402804k_si_006.cif
_cod_data_source_block           cmpd6
_cod_database_code               4120014