Tantalum−Benzylidene Complexes Supported by C5Me5and Diazadiene Ligands: Synthesis, Kinetic Analysis of the Formation, and Reactive Studies
Tsurugi, Hayato; Ohno, Takashi; Kanayama, Tsuyoshi; Arteaga-Müller, Rocío A.; Mashima, Kazushi; Organometallics 28 (2009) 1950–; doi:10.1021/om8012019

data_4069011
_publ_section_title
;
 Tantalum&#x2212;Benzylidene Complexes Supported by C5Me5and Diazadiene
 Ligands: Synthesis, Kinetic Analysis of the Formation, and Reactive
 Studies
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1950
_journal_paper_doi               10.1021/om8012019
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C33 H37 N2 O2 Ta'
_chemical_formula_sum            'C33 H37 N2 O2 Ta'
_chemical_formula_weight         674.60
_chemical_name_common            3a
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 152.1360(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.5968(10)
_cell_length_b                   8.2103(3)
_cell_length_c                   27.1892(10)
_cell_measurement_reflns_used    183439
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      3.1
_cell_volume                     2879.2(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_molecular_graphics    ORTEP-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            144667
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    3.849
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.936
_refine_diff_density_min         -1.622
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         10456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+2.2508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                8388
_reflns_number_total             10456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8012019_si_002.cif
_cod_data_source_block           3a
_cod_original_cell_volume        2879.24(18)
_cod_original_sg_symbol_H-M      'P 21/a       '
_cod_database_code               4069011