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_4069010
_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_iupac          ' ? '
_chemical_formula_moiety         'C24 H25 Cl2 F2 N2 Ta'
_chemical_formula_structural     ' ? '
_chemical_formula_sum            'C24 H25 Cl2 F2 N2 Ta'
_chemical_formula_weight         631.31
_chemical_name_common            1a
_chemical_properties_physical    ' air-unstable '
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.1810(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.4000(8)
_cell_length_b                   8.9530(4)
_cell_length_c                   25.0747(10)
_cell_measurement_reflns_used    73333
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.02
_cell_volume                     4543.8(3)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'teXan (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997) and modified'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Maria et al., 2005)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_details
;
RAPID: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_collimation    ' 0.8 mm double pinhole '
_diffrn_radiation_detector       'imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            103153
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_diffrn_source_current           40
_diffrn_source_power             50
_exptl_absorpt_coefficient_mu    5.104
_exptl_absorpt_correction_T_max  0.4284
_exptl_absorpt_correction_T_min  0.1846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2464
_exptl_crystal_preparation
'mounted on the CryoLoop with mineral oil and placed in N2 stream at 120(1) K'
_exptl_crystal_recrystallization_method
'crystallization from a solution of **** at ambient temperature'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.138
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0192P)^2^+4.1169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                8988
_reflns_number_total             10382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8012019_si_002.cif
_cod_data_source_block           complex1a
_cod_original_cell_volume        4543.7(3)
_cod_original_sg_symbol_Hall     ' -P 2ybc '
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4069010