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_4075394
_publ_section_title
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 Synthesis, Structure, and Reactivity of Tantalum and Tungsten Homoenolate
 Complexes
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_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         'C42 H51 Cl3 N3 O2 Ta'
_chemical_formula_sum            'C42 H51 Cl3 N3 O2 Ta'
_chemical_formula_weight         917.16
_chemical_temperature_decomposition 454(4)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Thu Feb  9 00:46:58 2006'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.47(3)
_cell_angle_beta                 76.69(3)
_cell_angle_gamma                80.30(3)
_cell_formula_units_Z            2
_cell_length_a                   9.436(4)
_cell_length_b                   11.148(4)
_cell_length_c                   20.172(8)
_cell_measurement_reflns_used    39014
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1992.8(14)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0774
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34100
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.785
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         8987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                7327
_reflns_number_total             8987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060264fsi20060323_094217.cif
_cod_data_source_block           complex3a
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been given
as '450-458(dec.)'. The value was changed to '454(4)' - the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1992(1)
_cod_database_code               4075394