Solid-state transformations in the β-form of chlorpropamide on cooling to 100K
Drebushchak, Tatiana N.; Drebushchak, Valeri A.; Boldyreva, Elena V.; Acta Crystallographica Section B 67 (2011) 163–176; doi:10.1107/S0108768111004290

data_2104909
_publ_section_title
;
 Solid-state transformations in the \b-form of chlorpropamide on
 cooling to 100K
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              163
_journal_page_last               176
_journal_paper_doi               10.1107/S0108768111004290
_journal_volume                  67
_journal_year                    2011
_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, \b^III^-form'
_chemical_name_systematic
;
 4-chloro-N-((propylaminocarbonyl)benzenesulfonamide
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 95.562(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   28.4475(12)
_cell_length_b                   9.2322(3)
_cell_length_c                   19.2298(7)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3054
_cell_measurement_theta_min      3.0710
_cell_volume                     5026.6(3)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction,2008b)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction,2008a)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction,2008b)'
_computing_structure_refinement  'SHELXL-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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.087
_diffrn_reflns_av_sigmaI/netI    0.1754
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42040
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.468
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_correction_T_min  0.9458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED (Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         14436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.809
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                6814
_reflns_number_total             14436
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            gp5041.cif
_cod_data_source_block           bIIICPA100K
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2104909