A high-pressure polymorph of chlorpropamide formed on hydrostatic compression of the α-form in saturated ethanol solution
Seryotkin, Yury V.; Drebushchak, Tatiana N.; Boldyreva, Elena V.; Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials 69 (2013) 77–; doi:10.1107/S2052519212051147

data_2021882
_publ_section_title
;
 A high-pressure polymorph of chlorpropamide formed on hydrostatic
 compression of the \a-form in saturated ethanol solution
;
_journal_issue                   1
_journal_name_full
'Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials'
_journal_page_first              77
_journal_paper_doi               10.1107/S2052519212051147
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C10 H13 Cl N2 O3 S'
_chemical_formula_sum            'C10 H13 Cl N2 O3 S'
_chemical_formula_weight         276.73
_chemical_melting_point          'phase transition'
_chemical_name_common            'chlorpropamide, \a^II^-form'
_chemical_name_systematic
;
 4-chloro-N-((propylaminocarbonyl)benzenesulfonamide
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2xa'
_space_group_name_H-M_alt        'P 21 1 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2xa'
_symmetry_space_group_name_H-M   'P 21 1 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.109(4)
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.602(3)
_cell_length_b                   4.6340(2)
_cell_length_c                   8.8525(4)
_cell_measurement_pressure       29100000
_cell_measurement_reflns_used    3109
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1731
_cell_measurement_theta_min      2.3240
_cell_volume                     1037.01(14)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.279
_diffrn_measured_fraction_theta_max 0.279
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_sigmaI/netI    0.1548
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10171
_diffrn_reflns_theta_full        31.26
_diffrn_reflns_theta_max         31.26
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.331
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Absorb6.1 (R. J. Angel, 2006)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1745
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0681
_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^)+(0.0756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1444
_reflns_number_gt                1083
_reflns_number_total             1745
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            gp5058sup1.cif
_cod_data_source_block           acpa_2.91GPa
_cod_database_code               2021882