A conformational polymorphic transition in the high-temperature ε-form of chlorpropamide on cooling: a new ε'-form
Drebushchak, Tatiana N.; Chesalov, Yury A.; Boldyreva, Elena V.; Acta Crystallographica Section B 65 (2009) 770–781; doi:10.1107/S010876810903290X

data_2104623
_publ_section_title
;
 A conformational polymorphic transition in the high-temperature
 \e-form of chlorpropamide on cooling: a new \e'-form
;
_journal_coeditor_code           GP5033
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              770
_journal_page_last               781
_journal_paper_doi               10.1107/S010876810903290X
_journal_volume                  65
_journal_year                    2009
_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          'Kinetic phase transition'
_chemical_name_common            'chlorpropamide, \e`-form'
_chemical_name_systematic
;
 4-chloro-N-((propylaminocarbonyl)benzenesulfonamide
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.4353(19)
_cell_length_b                   5.1398(4)
_cell_length_c                   9.0845(6)
_cell_measurement_reflns_used    1973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1183
_cell_measurement_theta_min      3.0764
_cell_volume                     1234.33(15)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2008)'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction KM4 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0984
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4372
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.8004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.312
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.17(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1995
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0357P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                1399
_reflns_number_total             1995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gp5033.cif
_cod_data_source_block           enewcpa100
_cod_database_code               2104623
_cod_database_fobs_code          2104623