Crystal structures of four organic salts of trihexyphenidyl at 90 K
Vinaya,; Basavaraju, Yeriyur B.; Yathirajan, Hemmige S.; Parkin, Sean; Acta Crystallographica Section E Crystallographic Communications 79 (2023) –; doi:10.1107/S2056989023005960

data_2022819
_publ_section_title
;
 Crystal structures of four organic salts of trihexyphenidyl at
 90&#x2005;K
;
_journal_coeditor_code           VM2286
_journal_issue                   8
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989023005960
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '2C20 H32 N O +, 2C5 H3 O2 S -, H2 O'
_chemical_formula_moiety         '2(C20 H32 N O +), 2(C5 H3 O2 S -), H2 O'
_chemical_formula_sum            'C50 H72 N2 O7 S2'
_chemical_formula_weight         877.21
_chemical_name_common
;
Trihexyphenidylium thiophene-2-carboxylate hemihydrate
;
_chemical_name_systematic
;
1-(3-Cyclohexyl-3-hydroxy-3-phenylpropyl)piperidin-1-ium
thiophene-2-carboxylate hemihydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-2019/2 and CIFFIX'
_cell_angle_alpha                89.710(2)
_cell_angle_beta                 81.600(2)
_cell_angle_gamma                88.977(2)
_cell_formula_units_Z            2
_cell_length_a                   6.2765(3)
_cell_length_b                   18.5390(13)
_cell_length_c                   20.6383(14)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.20
_cell_volume                     2375.3(3)
_computing_cell_refinement
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>XP</i> in <i>SHELXTL</i> (Sheldrick, 2008) and
<i>Mercury</i> (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
<i>SHELX</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip,
2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/2</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78578
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         1.995
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       'cut block'
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.302
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL-2019/2 (Sheldrick 2008)
;
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10922
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0315P)^2^+1.4676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                8540
_reflns_number_total             10922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2286sup1.cif
_cod_data_source_block           IV
_cod_database_code               2022819
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.982
_shelx_hkl_checksum              57591
_shelx_res_checksum              79360
_cod_database_fobs_code 2022819