Synthesis, Structure, and Reactivity of Tantalum and Tungsten Homoenolate Complexes
Tsurugi, Hayato; Ohno, Takashi; Yamagata, Tsuneaki; Mashima, Kazushi; Organometallics 25 (2006) 3179–; doi:10.1021/om060264f

data_4075395
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Tantalum and Tungsten Homoenolate
 Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3179
_journal_paper_doi               10.1021/om060264f
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C49 H39 Al F15 N2 O4 Ta'
_chemical_formula_sum            'C49 H39 Al F15 N2 O4 Ta'
_chemical_formula_weight         1212.75
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.847(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6461(10)
_cell_length_b                   30.716(3)
_cell_length_c                   14.1092(8)
_cell_measurement_reflns_used    111001
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      3.0
_cell_volume                     4747.4(7)
_computing_cell_refinement       'Rigaku/RAPID Diffractometer Control'
_computing_data_collection       'Rigaku/RAPID Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_molecular_graphics    'Ortep-3 (Louis J. Farrugia, 1999)'
_computing_publication_material  'SHELXL-97 and modified'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (A. Altomare, et al., 1994)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            84125
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.725
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.725
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0229
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+3.1334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                9819
_reflns_number_total             10864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060264fsi20060323_094217.cif
_cod_data_source_block           complex6
_cod_original_cell_volume        4747.4(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4075395