(1<i>S</i>,4<i>S</i>)-2-(2,4-Difluorophenyl)-5-[(4-methylphenyl)sulfonyl]-2,5-diazabicyclo[2.2.1]heptane
Wu, Chunli; Zhang, Jingyu; Li, Pan; Zhang, Junxia; Wu, Jizhou; Acta Crystallographica Section E 67 (2011) o272–; doi:10.1107/S1600536810054541

data_2229007
_publ_section_title
;
 (1<i>S</i>,4<i>S</i>)-2-(2,4-Difluorophenyl)-5-[(4-methylphenyl)sulfonyl]-2,5-diazabicyclo[2.2.1]heptane
;
_journal_coeditor_code           CV5024
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o272
_journal_paper_doi               10.1107/S1600536810054541
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C18 H18 F2 N2 O2 S'
_chemical_formula_moiety         'C18 H18 F2 N2 O2 S'
_chemical_formula_sum            'C18 H18 F2 N2 O2 S'
_chemical_formula_weight         364.40
_chemical_melting_point_gt       460
_chemical_melting_point_lt       465
_chemical_name_systematic
;
(1<i>S</i>,4<i>S</i>)-2-(2,4-Difluorophenyl)-5-[(4-methylphenyl)sulfonyl]-
2,5-diazabicyclo[2.2.1]heptane
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.9790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9615(11)
_cell_length_b                   7.6586(8)
_cell_length_c                   11.3461(14)
_cell_measurement_reflns_used    1315
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.6585
_cell_measurement_theta_min      2.9605
_cell_volume                     855.00(17)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4425
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_correction_T_min  0.9197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.280
_refine_ls_abs_structure_details 'Flack (1983), 1569 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                2045
_reflns_number_total             2891
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2229007
_cod_database_fobs_code          2229007