Preparation and characterization for multicomponent crystals of the antidiabetic drug gliquidone based on crystal engineering
Jia, Lina; Yu, Yang; Wang, Mengwei; Ouyang, Hanzhi; Gong, Junbo; CrystEngComm 21 (2019) 1617–; doi:10.1039/C8CE01848K

data_7232232
_publ_section_title
;
 Preparation and characterization for multicomponent crystals of the
 antidiabetic drug gliquidone based on crystal engineering
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1617
_journal_paper_doi               10.1039/C8CE01848K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C27 H32 N3 O6 S, C2 H6 N, C H4 O'
_chemical_formula_sum            'C30 H42 N4 O7 S'
_chemical_formula_weight         602.73
_chemical_name_systematic        gliquidone
_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
_audit_creation_date             2018-10-27
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-10-29 deposited with the CCDC.
2019-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                102.55(3)
_cell_angle_beta                 92.36(3)
_cell_angle_gamma                92.73(3)
_cell_formula_units_Z            2
_cell_length_a                   6.5899(13)
_cell_length_b                   15.349(3)
_cell_length_c                   15.887(3)
_cell_measurement_reflns_used    3829
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9384
_cell_measurement_theta_min      1.3614
_cell_volume                     1564.6(6)
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18842
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.802
_diffrn_reflns_theta_min         1.315
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0184(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4651
_reflns_number_total             7376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01848k2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7232232--7232235.cif.'
_cod_database_code               7232232
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.970
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C24(H24A,H24B), C23(H23A,
 H23B), C14(H14A,H14B), C13(H13A,H13B), C1P(H1PA,H1PB), C2P(H2PA,H2PB)
2.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C20(H20), C16(H16), C17(H17), C4(H4), C3(H3A), C0AA(H0AA)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C1S(H1SA,H1SB,
 H1SC)
2.e Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              60792
_shelx_hkl_checksum              31111
_olex2_submission_special_instructions 'No special instructions were received'