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_4126869
_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      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3219(8)
_cell_length_b                   13.3283(8)
_cell_length_c                   11.5783(8)
_cell_measurement_reflns_used    5343
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.378
_cell_volume                     2055.8(2)
_computing_molecular_graphics    'Crystal Maker'
_computing_publication_material
'Yadokari-XG 2014 (Wakita, Nemoto et al., 2014)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS 97'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Rigaku Saturn 724'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_radiation_source         'Synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.78203
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.893
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5343
_diffrn_reflns_point_group_measured_fraction_full 0.834
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        27.984
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.378
_exptl_absorpt_coefficient_mu    0.225
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 727 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_coef       0.25(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   2.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         3105
_refine_ls_number_restraints     247
_refine_ls_restrained_S_all      2.031
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0955
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2392
_refine_ls_wR_factor_ref         0.2898
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.756
_reflns_Friedel_fraction_max     0.795
_reflns_number_gt                2091
_reflns_number_total             3105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10249_si_003.cif
_cod_data_source_block           293K
_cod_database_code               4126869
_shelxl_version_number           2013-4
_shelx_res_checksum              62180
_shelx_hkl_checksum              60169