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_4120009
_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 H41 Cl N5 Ta'
_chemical_formula_sum            'C21 H41 Cl N5 Ta'
_chemical_formula_weight         579.99
_chemical_name_common            cmpd1
_chemical_name_systematic
;
cmpd1
;
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 79.502(2)
_cell_angle_gamma                84.438(2)
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_cell_length_a                   8.4097(12)
_cell_length_b                   9.3623(14)
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_cell_measurement_temperature    150(2)
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_cell_volume                     1232.2(3)
_computing_cell_refinement       Apex2
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_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 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
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_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
sample ID : 'Sita-Keane AK-394 150K'
no. frames:  3030
time/frame:    15
total time:    17.7
detec.dist.     5.0
frame size:   512
;
_diffrn_measurement_device_type  'three-circle diffractometer'
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_diffrn_orient_matrix_UB_12      -0.0573169
_diffrn_orient_matrix_UB_13      0.0571466
_diffrn_orient_matrix_UB_21      0.0203968
_diffrn_orient_matrix_UB_22      0.0840823
_diffrn_orient_matrix_UB_23      0.0277665
_diffrn_orient_matrix_UB_31      -0.1163575
_diffrn_orient_matrix_UB_32      0.0365536
_diffrn_orient_matrix_UB_33      0.0027702
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20540
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_T_max  0.632
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            ligght-yellow
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0155
_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^)+(0.01P)^2^+1.135P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0339
_reflns_number_gt                6875
_reflns_number_total             7090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402804k_si_001.cif
_cod_data_source_block           cmpd1
_cod_database_code               4120009