Spontaneous resolution of Julia-Kocienski intermediates facilitates phase separation to produce Z- and E-monofluoroalkenes.
Zhao, Yanchuan; Jiang, Fanzhou; Hu, Jinbo; Journal of the American Chemical Society 137 (2015) 5199–5203; doi:10.1021/jacs.5b02112

data_4129409
_publ_section_title
;
 Spontaneous resolution of Julia-Kocienski intermediates facilitates phase
 separation to produce Z- and E-monofluoroalkenes.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5199
_journal_page_last               5203
_journal_paper_doi               10.1021/jacs.5b02112
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C24 H20 F N O3 S'
_chemical_formula_sum            'C24 H20 F N O3 S'
_chemical_formula_weight         421.47
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0153(12)
_cell_length_b                   9.3357(19)
_cell_length_c                   36.705(7)
_cell_measurement_reflns_used    2835
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.15
_cell_measurement_theta_min      2.41
_cell_volume                     2057.0(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.854
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            9517
_diffrn_reflns_theta_full        67.15
_diffrn_reflns_theta_max         67.15
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.8487
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+0.4264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                2835
_reflns_number_total             3147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b02112_si_003.cif
_cod_data_source_block           033
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4129409