Effect of pressure on two polymorphs of tolazamide: why no interconversion?
Fedorov, A. Yu.; Rychkov, D. A.; Losev, E. A.; Zakharov, B. A.; Stare, J.; Boldyreva, E. V.; CrystEngComm 19 (2017) 2243–; doi:10.1039/C6CE02527G

data_7228019
_publ_section_title
;
 Effect of pressure on two polymorphs of tolazamide: why no
 interconversion?
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2243
_journal_paper_doi               10.1039/C6CE02527G
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C14 H21 N3 O3 S'
_chemical_formula_sum            'C14 H21 N3 O3 S'
_chemical_formula_weight         311.40
_chemical_name_common            tolazamide
_chemical_name_systematic
;
 N-[(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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-21 deposited with the CCDC.
2017-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                80.81(2)
_cell_angle_beta                 85.069(6)
_cell_angle_gamma                85.606(14)
_cell_formula_units_Z            2
_cell_length_a                   5.8202(3)
_cell_length_b                   8.536(5)
_cell_length_c                   12.7885(14)
_cell_measurement_pressure       4030000
_cell_measurement_reflns_used    799
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6070
_cell_measurement_theta_min      1.6460
_cell_volume                     623.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_pressure         4030000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3457
_diffrn_measured_fraction_theta_full 0.335
_diffrn_measured_fraction_theta_max 0.329
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_unetI/netI     0.1098
_diffrn_reflns_Laue_measured_fraction_full 0.335
_diffrn_reflns_Laue_measured_fraction_max 0.329
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3065
_diffrn_reflns_point_group_measured_fraction_full 0.335
_diffrn_reflns_point_group_measured_fraction_max 0.329
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.236
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.277
_exptl_absorpt_correction_T_max  0.480
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Absorb-7 (Angel, 2013)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         839
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0477P)^2^+0.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                552
_reflns_number_total             839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02527g2.cif
_cod_data_source_block           403GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7228012--7228029.cif.
;
_cod_database_code               7228019
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.927
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C11 \\sim C11-C10 \\sim C10-C9
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.08
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C9(H9A,H9B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A,H11B),
 C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C3(H3), C6(H6), C5(H5), C2(H2A)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              33742
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'