Regio- and Stereoselective Multisubstituted Enol Ester Synthesis
Noriko Okamoto; Yoshihisa Miwa; Hideki Minami; Kei Takeda; Reiko Yanada; Journal of Organic Chemistry 76 (2011) 9133–9138; doi:10.1021/jo201609r

data_4026705
_publ_section_title
;
 Regio- and Stereoselective Multisubstituted Enol Ester Synthesis
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9133
_journal_page_last               9138
_journal_paper_doi               10.1021/jo201609r
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C17 H15 I O3'
_chemical_formula_sum            'C17 H15 I O3'
_chemical_formula_weight         394.21
_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
_cell_angle_alpha                99.63(3)
_cell_angle_beta                 94.03(4)
_cell_angle_gamma                89.28(3)
_cell_formula_units_Z            4
_cell_length_a                   9.079(8)
_cell_length_b                   10.357(8)
_cell_length_c                   17.832(18)
_cell_measurement_reflns_used    11263
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.00
_cell_volume                     1649(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15114
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             776.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.520
_refine_diff_density_min         -0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4620
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.044
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    474.2430    654.6550    196.2010
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0472
_reflns_number_gt                4620
_reflns_number_total             7135
_reflns_threshold_expression     F>2.0\s(F)
_cod_data_source_file            jo201609r_si_003.cif
_cod_data_source_block           100826
_cod_database_code               4026705