Crystal structures of anhydrous and hydrated <i>N</i>-benzylcinchonidinium bromide
Janzen, Daron E.; Butler, Maya S.; Reinheimer, Eric W.; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022005096

data_2244097
_publ_section_title
;
 Crystal structures of anhydrous and hydrated
 <i>N</i>-benzylcinchonidinium bromide
;
_journal_coeditor_code           PK2664
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022005096
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C26 H29 N2 O +, Br -, 1.5H2 O1'
_chemical_formula_moiety         'C26 H29 N2 O +, Br -, 1.5(H2 O)'
_chemical_formula_sum            'C26 H32 Br N2 O2.5'
_chemical_formula_weight         492.44
_chemical_name_common
;
<i>N</i>-Benzylcinchonidinium bromide sesquihydrate
;
_chemical_name_systematic
;(<i>R</i>)-[(2<i>S</i>,4<i>S</i>,5<i>R</i>)-1-Benzyl-5-ethenyl-1-azoniabicyclo[2.2.2]octan-2-yl](quinolin-4-yl)methanol bromide
sesquihydrate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.9254(2)
_cell_length_b                   9.9254(2)
_cell_length_c                   47.1267(14)
_cell_measurement_reflns_used    19124
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      28.5610
_cell_measurement_theta_min      1.7220
_cell_volume                     4642.62(19)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2020)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  XtaLABmini
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            36339
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         1.728
_exptl_absorpt_coefficient_mu    1.799
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.404
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1347 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0509
_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^)+19.0784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                3919
_reflns_number_total             4154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2664sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
;

2023-01-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C52 H64 Br2 N4 O5'
_cod_original_formula_weight         984.89
_cod_original_formula_moiety         '2(C26 H29 N2 O +), 2(Br -), 3(H2 O)'
_cod_original_formula_iupac          '2C26 H29 N2 O +, 2Br -, 3H2 O1'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        4642.6(2)
_cod_database_code               2244097
_shelx_estimated_absorpt_t_min   0.455
_shelx_estimated_absorpt_t_max   0.564
_cod_database_fobs_code 2244097