Isolation and Crystal Structures of Both Enol and Keto Tautomer Intermediates in a Hydration of an Alkyne-Carboxylic Acid Ester Catalyzed by Iridium Complexes in Water
Hironobu Kanemitsu; Keiji Uehara; Shunichi Fukuzumi; Seiji Ogo; Journal of the American Chemical Society 130 (2008) 17141–17147; doi:10.1021/ja807254d

data_4108844
_publ_section_title
;
 Isolation and Crystal Structures of Both Enol and Keto Tautomer
 Intermediates in a Hydration of an Alkyne-Carboxylic Acid Ester Catalyzed
 by Iridium Complexes in Water
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17141
_journal_page_last               17147
_journal_paper_doi               10.1021/ja807254d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C27 H32 F3 Ir N2 O6 S'
_chemical_formula_weight         761.83
_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'
_cell_angle_alpha                110.076(4)
_cell_angle_beta                 103.100(2)
_cell_angle_gamma                98.843(2)
_cell_formula_units_Z            2
_cell_length_a                   10.566(3)
_cell_length_b                   11.450(3)
_cell_length_c                   13.400(3)
_cell_measurement_reflns_used    4586
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.5
_cell_volume                     1434.7(6)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  'teXsan Ver. 2.0'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_detector_area_resol_mean 28.57
_diffrn_measured_fraction_theta_full 0.9500
_diffrn_measured_fraction_theta_max 0.9500
_diffrn_measurement_device_type  'Rigaku/MSC Saturn CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11343
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    4.801
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       Prism
_exptl_crystal_F_000             752.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6240
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                5551
_reflns_number_total             6240
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja807254d_si_001.cif
_cod_data_source_block           '_Ir(CpMe5)(bpy)(TET)CF3SO3'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C27 H32 F3 Ir N2 O6 S '
_cod_database_code               4108844