Redetermination of bis{(1<i>S</i>,2<i>S</i>,4<i>S</i>,5<i>R</i>)-2-[(<i>R</i>)-hydroxy(6-methoxy-4-quinolyl)methyl]-5-vinylquinuclidinium} sulfate dihydrate
Mangwala Kimpende, Peter; Van Meervelt, Luc; Acta Crystallographica Section E 66 (2010) o2443–o2444; doi:10.1107/S1600536810034288

data_2227811
_publ_section_title
;
 Redetermination of
 bis{(1<i>S</i>,2<i>S</i>,4<i>S</i>,5<i>R</i>)-2-[(<i>R</i>)-hydroxy(6-methoxy-4-quinolyl)methyl]-5-vinylquinuclidinium}
 sulfate dihydrate
;
_journal_coeditor_code           LX2164
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2443
_journal_page_last               o2444
_journal_paper_doi               10.1107/S1600536810034288
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '2C20 H25 N2 O2 +, S O4 2-, 2H2 O'
_chemical_formula_moiety         '2(C20 H25 N2 O2 +), O4 S 2-, 2(H2 O)'
_chemical_formula_sum            'C40 H54 N4 O10 S'
_chemical_formula_weight         782.94
_chemical_name_common            'Quinine sulfate dihydrate'
_chemical_name_systematic
;
bis{(1<i>S</i>,2<i>S</i>,4<i>S</i>,5<i>R</i>)-2-[(<i>R</i>)-hydroxy(6-methoxy-
4-quinolyl)methyl]-5-vinylquinuclidinium} sulfate dihydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.288(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   20.180(7)
_cell_length_b                   6.637(2)
_cell_length_c                   15.316(6)
_cell_measurement_reflns_used    3041
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.749
_cell_measurement_theta_min      3.142
_cell_volume                     1884.2(11)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
'PLUTON (Spek, 2009) and DIAMOND (Brandenburg, 2010)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_monochromator  'crossed Globel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9588
_diffrn_reflns_theta_full        67.70
_diffrn_reflns_theta_max         70.67
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.291
_refine_ls_abs_structure_details 'Flack (1983), 1339 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3319
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0484P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                3112
_reflns_number_total             3319
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            lx2164.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2227811
_cod_database_fobs_code          2227811