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_7243721
_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         '2(C14 H20 Cl N3 O3 S), O'
_chemical_formula_sum            'C28 H40 Cl2 N6 O7 S2'
_chemical_formula_weight         707.68
_chemical_name_common            'Clopamide hemihydrate'
_chemical_name_systematic
;
4-chloro-N-(2,6-dimethylpiperidin-1-yl)-3-sulfamoylbenzamide hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_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                 100.965(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5166(8)
_cell_length_b                   9.3747(7)
_cell_length_c                   24.7064(17)
_cell_measurement_reflns_used    32344
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      3.03
_cell_volume                     3300.9(4)
_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      103(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  R-AXIS-RAPID
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       RX
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.028
_diffrn_source                   'NORMAL-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.9450
_exptl_absorpt_correction_T_min  0.8179
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
NUMABS; Higashi, 2002
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0495P)^2^+6.3890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1109
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3253
_reflns_number_total             3762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00995h2.cif
_cod_data_source_block           shelx_CCDC9
_cod_depositor_comments
'Adding full bibliography for 7243712--7243721.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7243721
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.963
_shelx_res_checksum              42689