Supramolecular synthesis based on piperidone derivatives and pharmaceutically acceptable co-formers
Sandhu, Bhupinder; Draguta, Sergiu; Kinnibrugh, Tiffany L.; Khrustalev, Victor N.; Timofeeva, Tatiana V.; Acta Crystallographica Section C 69 (2013) 421–427; doi:10.1107/S0108270113006185

data_2018924
_publ_section_title
;
 Supramolecular synthesis based on piperidone derivatives and
 pharmaceutically acceptable co-formers
;
_journal_coeditor_code           QS3023
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              421
_journal_page_last               427
_journal_paper_doi               10.1107/S0108270113006185
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '2C27 H36 N3 O + , C4 H4 O4 2-'
_chemical_formula_moiety         '2(C27 H36 N3 O +), C4 H4 O4 2-'
_chemical_formula_sum            'C58 H76 N6 O6'
_chemical_formula_weight         953.27
_chemical_name_systematic
;
Bis{(<i>E</i>,<i>E</i>)-3,5-bis[4-(diethylamino)benzylidene]-4-oxopiperidinium}
butanedioate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL97
_cell_angle_alpha                96.320(3)
_cell_angle_beta                 92.211(3)
_cell_angle_gamma                95.861(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1075(15)
_cell_length_b                   12.9650(18)
_cell_length_c                   17.899(3)
_cell_measurement_reflns_used    4344
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.21
_cell_volume                     2545.3(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16330
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9952
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0897P)^2^+1.4P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1846
_reflns_number_gt                6795
_reflns_number_total             9952
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            qs3023.cif
_cod_data_source_block           II
_cod_database_code               2018924
_cod_database_fobs_code          2018924