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_4108845
_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 H36 F6 Ir N2 O4 P'
_chemical_formula_weight         789.78
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.899(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7539(9)
_cell_length_b                   12.9194(5)
_cell_length_c                   16.236(1)
_cell_measurement_reflns_used    10140
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2976.4(3)
_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    SIR92
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.9675
_diffrn_measured_fraction_theta_max 0.9675
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23657
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    4.625
_exptl_absorpt_correction_T_max  0.482
_exptl_absorpt_correction_T_min  0.273
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       Block
_exptl_crystal_F_000             1560.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.67
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6611
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.0027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.04100(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                6139
_reflns_number_total             6611
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja807254d_si_002.cif
_cod_data_source_block           '_CpMeIrbpy(acetoacetateEth'
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C27 H36 F6 Ir N2 O4 P '
_cod_database_code               4108845