Hydroalumination of a Dinuclear Tantalum Dinitrogen Complex: N−N Bond Cleavage and Ancillary Ligand Rearrangement
MacKay, Bruce A.; Patrick, Brian O.; Fryzuk, Michael D.; Organometallics 24 (2005) 3836–; doi:10.1021/om050208z

data_4075856
_publ_section_title
;
 Hydroalumination of a Dinuclear Tantalum Dinitrogen Complex:
 N&#x2212;N Bond Cleavage and Ancillary Ligand Rearrangement
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3836
_journal_paper_doi               10.1021/om050208z
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C52 H73 Al N6 P2 Si4 Ta2'
_chemical_formula_weight         1345.34
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4244(5)
_cell_length_b                   19.9666(5)
_cell_length_c                   29.2898(8)
_cell_measurement_reflns_used    35665
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.12
_cell_measurement_theta_min      2.35
_cell_volume                     11944.6(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            83972
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             5376
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.023
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.833
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         14991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.833
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0870
_reflns_number_gt                9395
_reflns_number_total             14991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050208zsi20050317_122159.cif
_cod_data_source_block           mf457Cpd5
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               4075856