In Situ Evaluation of Kinetic Resolution Catalysts for Nitroaldol by Rationally Designed Fluorescence Probe
Takuya Matsumoto; Yasuteru Urano; Yoshinori Takahashi; Yusuke Mori; Takuya Terai; Tetsuo Nagano; Journal of Organic Chemistry 76 (2011) 3616–3625; doi:10.1021/jo1020344

data_4026273
_publ_section_title
;
 In Situ Evaluation of Kinetic Resolution Catalysts for Nitroaldol by
 Rationally Designed Fluorescence Probe
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3616
_journal_page_last               3625
_journal_paper_doi               10.1021/jo1020344
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C21 H21 B F2 I N3 O3 '
_chemical_formula_sum            'C21 H21 B F2 I N3 O3'
_chemical_formula_weight         539.13
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 105.365(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7711(4)
_cell_length_b                   11.8146(4)
_cell_length_c                   13.9067(4)
_cell_measurement_reflns_used    18541
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2181.75(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SAPI91
_diffrn_detector_area_resol_mean 10.00
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21478
_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.950
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.07
_refine_diff_density_min         -1.70
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8396
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.1340
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                8396
_reflns_number_total             9774
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            jo1020344_si_001.cif
_cod_data_source_block           Tokyo_BI20100217_Mo
_cod_original_cell_volume        2181.8(1)
_cod_original_formula_sum        'C21 H21 B F2 I N3 O3 '
_cod_database_code               4026273