Completing the picture of tolazamide polymorphism under extreme conditions: a low-temperature study
Fedorov, Alexey Yu.; Rychkov, Denis A.; Losev, Evgeniy A.; Drebushchak, Tatiana N.; Boldyreva, Elena V.; Acta Crystallographica Section C 75 (2019) 598–608; doi:10.1107/S2053229619005217

data_2021609
_publ_section_title
;
 Completing the picture of tolazamide polymorphism under extreme
 conditions: a low-temperature study
;
_journal_coeditor_code           KU3243
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              598
_journal_page_last               608
_journal_paper_doi               10.1107/S2053229619005217
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C14 H21 N3 O3 S'
_chemical_formula_moiety         'C14 H21 N3 O3 S'
_chemical_formula_sum            'C14 H21 N3 O3 S'
_chemical_formula_weight         311.40
_chemical_melting_point          444
_chemical_name_common            tolazamide
_chemical_name_systematic
;
1-[(Azepan-1-ylamino)carbonyl]-4-methylbenzenesulfonamide
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                81.882(16)
_cell_angle_beta                 86.073(16)
_cell_angle_gamma                85.167(13)
_cell_formula_units_Z            2
_cell_length_a                   6.3091(10)
_cell_length_b                   8.9270(15)
_cell_length_c                   13.576(3)
_cell_measurement_reflns_used    1573
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.5590
_cell_measurement_theta_min      3.4860
_cell_volume                     753.0(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.1053
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10088
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.504
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.629
_refine_ls_extinction_coef       0.054(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.2853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                2081
_reflns_number_total             3057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ku3243sup1.cif
_cod_data_source_block           TZA_II_100
_cod_depositor_comments
'Adding full bibliography for 2021596--2021609.cif.'
_cod_database_code               2021609
_cod_database_fobs_code          2021609
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.989
_shelx_hkl_checksum              72249
_shelx_res_checksum              60732