Quininium (<i>R</i>)-mandelate, a structure with large <i>Z</i>' described as an incommensurately modulated structure in (3+1)-dimensional superspace
Schönleber, Andreas; Chapuis, Gervais; Acta Crystallographica Section B 60 (2004) 108–120; doi:10.1107/S0108768103027605

data_2102241
_publ_section_title
;
 Quininium (<i>R</i>)-mandelate, a structure with large <i>Z</i>'
 described as an incommensurately modulated structure in
 (3+1)-dimensional superspace
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              108
_journal_page_last               120
_journal_paper_doi               10.1107/S0108768103027605
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C20 H25 N2 O2+ , C8 H7 O3-'
_chemical_formula_sum            'C28 H32 N2 O5'
_chemical_formula_weight         476.57
_chemical_name_common            'quininium (R)-mandelate'
_chemical_name_systematic
;
6'-methoxy (8,9R)-cinchonan-9-ol
;
_symmetry_cell_setting           monoclinic
_cell_angle_alpha                90
_cell_angle_beta                 107.47(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.614(3)
_cell_length_b                   18.552(7)
_cell_length_c                   10.377(4)
_cell_measurement_reflns_used    7295
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      49.17
_cell_measurement_theta_min      4.04
_cell_volume                     1214.6(9)
_computing_cell_refinement       '(NADA; Sch\"onleber et al., 2001)'
_computing_data_collection       '(X-Area, Stoe & Cie, 2002)'
_computing_data_reduction        '(X-Area, Stoe & Cie, 2002)'
_computing_publication_material  '(Jana2000; Petricek and Dusek, 2000)'
_computing_structure_refinement  '(Jana2000; Petricek and Dusek, 2000)'
_computing_structure_solution    '(DIRDIF, Beurskens et al., 1996)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.1094
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            204354
_diffrn_reflns_theta_full        24.59
_diffrn_reflns_theta_max         24.59
_diffrn_reflns_theta_min         1.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.09
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.3027(9)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.81
_refine_ls_extinction_coef       1.22(14)
_refine_ls_extinction_method
'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_ref   1.25
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     1636
_refine_ls_number_reflns         26261
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.1604
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0004F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                11584
_reflns_number_total             26261
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sn5002.cif
_cod_data_source_block           QuiRMa
_cod_database_code               2102241