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_2104626
_publ_section_title
;
 A conformational polymorphic transition in the high-temperature
 \e-form of chlorpropamide on cooling: a new \e'-form
;
_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, \a-form'
_chemical_name_systematic
;
 4-chloro-N-((propylaminocarbonyl)benzenesulfonamide
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   26.657(6)
_cell_length_b                   5.0938(16)
_cell_length_c                   8.9941(18)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10.2
_cell_volume                     1221.3(5)
_computing_cell_refinement       'STADI4 (STOE & Cie, 1997)'
_computing_data_collection       'STADI4 (STOE & Cie, 1997)'
_computing_data_reduction        'X-RED (STOE & Cie, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer D094'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2875
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.8858
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 X-RED (STOE & Cie, 1997)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.448
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.09(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0440P)^2^+4.5034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1361
_reflns_number_gt                2041
_reflns_number_total             2397
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            gp5033.cif
_cod_data_source_block           acpa105
_cod_database_code               2104626
_cod_database_fobs_code          2104626