Crystal structures of three 4-methylpiperidinium salts (one as three polymorphs) with tetrahalogenidoaurate(III), halide and (in one case) dichloroiodate(I) counter-anions
Döring, Cindy; Jones, Peter G.; Acta Crystallographica Section E Crystallographic Communications 81 (2025) –; doi:10.1107/S2056989025004918

data_2023538
_publ_section_title
;
 Crystal structures of three 4-methylpiperidinium salts (one as three
 polymorphs) with tetrahalogenidoaurate(III), halide and (in one case)
 dichloroiodate(I) counter-anions
;
_journal_coeditor_code           YZ2066
_journal_issue                   7
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989025004918
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          '(C6 H14 N) [Au Cl4]4 (Cl2 I) Cl'
_chemical_formula_moiety         '6(C6 H14 N +), 4(Au Cl4 -), Cl2 I -, Cl -'
_chemical_formula_sum            'C36 H84 Au4 Cl19 I N6'
_chemical_formula_weight         2189.40
_chemical_name_systematic
;
Hexakis(4-methylpiperidinium) tetrakis{tetrachloridoaurate(III)}
dichloroiodate(I) chloride
;
_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-2019/3
_cell_angle_alpha                98.422(4)
_cell_angle_beta                 108.961(5)
_cell_angle_gamma                96.954(4)
_cell_formula_units_Z            1
_cell_length_a                   9.5362(5)
_cell_length_b                   13.4772(6)
_cell_length_c                   13.7179(7)
_cell_measurement_reflns_used    17356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7630
_cell_measurement_theta_min      2.4420
_cell_volume                     1622.37(15)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2013)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2013)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.36.28 (Rigaku OD, 2013)
;
_computing_molecular_graphics
;
Bruker XP, Version 5.1 (Bruker, 1998)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            97738
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.884
_diffrn_reflns_theta_min         2.296
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2013)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.962
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         9693
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.4353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0433
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                8260
_reflns_number_total             9693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2066.cif
_cod_data_source_block           3
_cod_original_cell_volume        1622.36(15)
_cod_database_code               2023538
_shelx_estimated_absorpt_t_min   0.426
_shelx_estimated_absorpt_t_max   0.683
_shelx_hkl_checksum              88195
_shelx_res_checksum              70582