Crystal structure analysis and sublimation thermodynamics of bicyclo derivatives of a neuroprotector family
Surov, Artem O.; Proshin, Alexey N.; Perlovich, German L.; Acta Crystallographica Section B 70 (2014) 47–53; doi:10.1107/S2052520613024384

data_2105731
_publ_section_title
;
 Crystal structure analysis and sublimation thermodynamics of bicyclo
 derivatives of a neuroprotector family
;
_journal_coeditor_code           BI5003
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              47
_journal_page_last               53
_journal_paper_doi               10.1107/S2052520613024384
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         'C14 H15 F3 N2 S'
_chemical_formula_sum            'C14 H15 F3 N2 S'
_chemical_formula_weight         300.34
_chemical_melting_point          364
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 109.33(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.074(8)
_cell_length_b                   9.185(5)
_cell_length_c                   12.652(8)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     1433.7(16)
_computing_cell_refinement       CAD-4
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1993)'
_computing_data_reduction        CAD-4
_computing_publication_material  SHELXL97
_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  'Nonius CAD-4'
_diffrn_measurement_method       '\w-\2q 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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.1951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2627
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2514
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.2773
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1222P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2209
_reflns_number_gt                852
_reflns_number_total             2514
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi5003sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        1433.7(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105731
_cod_database_fobs_code          2105731