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_4126868
_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
_chemical_name_systematic
;
 ?
;
_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                   13.0612(5)
_cell_length_b                   13.1299(5)
_cell_length_c                   11.4816(5)
_cell_measurement_reflns_used    5221
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3
_cell_volume                     1969.01(14)
_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      100(2)
_diffrn_detector_area_resol_mean 29
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.950
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0935
_diffrn_reflns_Laue_measured_fraction_full 0.909
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5221
_diffrn_reflns_point_group_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        27.984
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         2.420
_exptl_absorpt_coefficient_mu    0.235
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.220
_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          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 693 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.10(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         3033
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0802P)^2^+3.6120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.2248
_reflns_Friedel_coverage         0.634
_reflns_Friedel_fraction_full    0.771
_reflns_Friedel_fraction_max     0.811
_reflns_number_gt                2085
_reflns_number_total             3033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10249_si_002.cif
_cod_data_source_block           ydkr
_cod_database_code               4126868
_shelxl_version_number           2013-4
_shelx_res_checksum              38974
_shelx_hkl_checksum              53789