Alkyne Exchange Reactions of Silylalkyne Complexes of Tantalum: Mechanistic Investigation and Its Application in the Preparation of New Tantalum Complexes Having Functional Alkynes (PhC⋮CR (R = COOMe, CONMe2))
Oshiki, Toshiyuki; Yamada, Atsushi; Kawai, Kimio; Arimitsu, Hirotaka; Takai, Kazuhiko; Organometallics 26 (2007) 173–; doi:10.1021/om060659z

data_4072476
_publ_section_title
;
 Alkyne Exchange Reactions of Silylalkyne Complexes of Tantalum:&#x00A0;
 Mechanistic Investigation and Its Application in the Preparation of New
 Tantalum Complexes Having Functional Alkynes (PhC&#x22EE;CR (R = COOMe,
 CONMe2))
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              173
_journal_paper_doi               10.1021/om060659z
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C14 H18 Cl3 O4 Ta '
_chemical_formula_sum            'C14 H18 Cl3 O4 Ta'
_chemical_formula_weight         537.60
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_cell_angle_alpha                90
_cell_angle_beta                 90.54(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.838(2)
_cell_length_b                   19.349(2)
_cell_length_c                   10.576(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      24.9
_cell_volume                     1808.5(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_measured_fraction_theta_full 1.0479
_diffrn_measured_fraction_theta_max 1.0479
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       w-2q
_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2286
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        0.29
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.523
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.66
_refine_diff_density_min         -4.71
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.923
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2187
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.0128
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[&#x00B4;s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                2145
_reflns_number_total             2187
_reflns_threshold_expression     F^2^>2.0&#x00B4;s(F^2^)
_cod_data_source_file            om060659zsi20060721_085422.cif
_cod_data_source_block           TaPhCCCO2MeCl3DME
_cod_original_cell_volume        1808.4(5)
_cod_original_formula_sum        'C14 H18 Cl3 O4 Ta '
_cod_database_code               4072476