Non-Polar to Polar Phase Transition of a Chiral Ionic Plastic Crystal and the Switch of Rotation Symmetry.
Matsuki, Masaya; Yamada, Teppei; Yasuda, Nobuhiro; Dekura, Shun; Kitagawa, Hiroshi; Kimizuka, Nobuo; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10249

data_4126870
_publ_section_title
;
 Non-Polar to Polar Phase Transition of a Chiral Ionic Plastic Crystal and
 the Switch of Rotation Symmetry.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10249
_journal_year                    2017
_chemical_formula_sum            'C18 H35 N O4 S'
_chemical_formula_weight         361.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90.025(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5107(12)
_cell_length_b                   9.5076(12)
_cell_length_c                   11.6475(15)
_cell_measurement_reflns_used    6640
_cell_measurement_temperature    354(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     1053.2(2)
_computing_cell_refinement       'Crystal Clear 1.4.0 SP1'
_computing_data_collection       'Rigaku Saturn 70/31K'
_computing_data_reduction        'Crystal Clear 1.4.0 SP1'
_computing_molecular_graphics    'Crystal Maker'
_computing_publication_material
'Yadokari-XG 2014 (Wakita, Nemoto et al., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS 97 '
_diffrn_ambient_temperature      354(2)
_diffrn_detector_area_resol_mean 28.5
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Rigaku Saturn 724 plus'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.78203
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6640
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        27.984
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         5.095
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7355
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       platelet
_exptl_crystal_F_000             396
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 726 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         3068
_refine_ls_number_restraints     265
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.442
_refine_ls_shift/su_mean         0.062
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2530
_refine_ls_wR_factor_ref         0.2850
_reflns_Friedel_coverage         0.627
_reflns_Friedel_fraction_full    0.666
_reflns_Friedel_fraction_max     0.696
_reflns_number_gt                2229
_reflns_number_total             3068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10249_si_004.cif
_cod_data_source_block           d2D_354K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4126870
_shelxl_version_number           2013-4
_shelx_res_checksum              66331
_shelx_hkl_checksum              81854