A Study of Diastereomeric Mandelate Salts of Cinchonidine and the Relation to Their Quasidiastereomeric Analogues
Gjerløv, A.; Larsen, S.; Acta Crystallographica Section B 53 (1997) 708–718; doi:10.1107/S0108768197003480

data_2101872
_publ_section_title
;
 A Study of Diastereomeric Mandelate Salts of Cinchonidine and the
 Relation to Their Quasidiastereomeric Analogues
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              708
_journal_page_last               718
_journal_paper_doi               10.1107/S0108768197003480
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety
;
C~19~H~23~N~2~O^+^C~8~H~7~O~3~^-^
;
_chemical_formula_sum            'C27 H30 N2 O4'
_chemical_formula_weight         446.53
_chemical_name_systematic
;
cinchonidinium (S)-mandelate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.304(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.400(2)
_cell_length_b                   6.2777(6)
_cell_length_c                   17.853(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      45.19
_cell_measurement_theta_min      37.91
_cell_volume                     2263.6(4)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'DREADD (Blessing, 1987)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
;
SHELXL-93 (Sheldrick, 1995) and local programs
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1995)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0124
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3022
_diffrn_reflns_theta_max         74.94
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        4.2
_diffrn_standards_interval_time  166.7
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.201
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(15)
_refine_ls_extinction_coef       0.0034(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.944
_refine_ls_goodness_of_fit_obs   0.946
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         2707
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.944
_refine_ls_restrained_S_obs      0.946
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_obs          0.0259
_refine_ls_shift/esd_max         0.030
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.7316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0723
_refine_ls_wR_factor_obs         0.0721
_reflns_number_observed          2684
_reflns_number_total             2707
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab0369.cif
_cod_data_source_block           S
_cod_depositor_comments
;
 Changing the space group from 'P 2y' to 'C 2y' after consulting the original
 publication. All related space group information was changed accordingly.

 Antanas Vaitkus,
 2017-07-05

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.7316P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.7316P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2101872