Solvatomorph and polymorph screening of clopamide drug and its copper(ii) complex crystals
Gál, G. Tamás; May, Nóra V.; Trif, László; Mihály, Judith; Bombicz, Petra; CrystEngComm 23 (2021) 7425–7441; doi:10.1039/D1CE00995H

data_7243712
_publ_section_title
;
 Solvatomorph and polymorph screening of clopamide drug and its copper(ii)
 complex crystals
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              7425
_journal_page_last               7441
_journal_paper_doi               10.1039/D1CE00995H
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C14 H20 Cl N3 O3 S'
_chemical_formula_sum            'C14 H20 Cl N3 O3 S'
_chemical_formula_weight         345.84
_chemical_name_common            'Clopamide anhydrate'
_chemical_name_systematic
;
4-chloro-N-(2,6-dimethylpiperidin-1-yl)-3-sulfamoylbenzamide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.32
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7914(4)
_cell_length_b                   9.2921(4)
_cell_length_c                   19.0621(4)
_cell_measurement_reflns_used    33523
_cell_measurement_temperature    128(2)
_cell_measurement_theta_max      68.255
_cell_measurement_theta_min      3.065
_cell_volume                     3284.52(17)
_computing_cell_refinement       'Crystal Clear (Rigaku/MSC, 2005)'
_computing_data_collection       'Crystal Clear (Rigaku/MSC, 2005)'
_computing_data_reduction        'Crystal Clear (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material
;
MERCURY (Macrae et al., 2006); Platon (Spek,
 2009
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      128(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  R-AXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42764
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.225
_diffrn_reflns_theta_min         3.063
_diffrn_source                   'NORMAL-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.389
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
NUMABS; Higashi, 2002
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0998
_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^)+(0.0389P)^2^+27.7443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5038
_reflns_number_total             5936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00995h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7243712--7243721.cif.'
_cod_original_cell_volume        3284.51(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7243712
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.282
_shelx_estimated_absorpt_t_max   0.728
_shelx_res_checksum              23314