Enhancing switchable dielectric property for crystalline supramolecular rotor compounds by adding polar components.
Huang, Rui-Kang; Chen, Xiao-Xian; Xiao, Zhi-Feng; Liu, De-Xuan; Zhang, Wei-Xiong; Chen, Xiao-Ming; Chemical communications (Cambridge, England) 56 (2020) 4114–4117; doi:10.1039/d0cc01026j

data_7126154
_publ_section_title
;
 Enhancing switchable dielectric property for crystalline supramolecular
 rotor compounds by adding polar components.
;
_journal_issue                   29
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4114
_journal_page_last               4117
_journal_paper_doi               10.1039/d0cc01026j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C F3 O3 S, C7 H9 N2 O3, C12 H24 O6'
_chemical_formula_sum            'C20 H33 F3 N2 O12 S'
_chemical_formula_weight         582.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-07 deposited with the CCDC.	2020-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 96.2561(8)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   20.31807(19)
_cell_length_b                   17.85897(16)
_cell_length_c                   14.64020(12)
_cell_measurement_reflns_used    12230
_cell_measurement_temperature    212.99(10)
_cell_measurement_theta_max      73.9240
_cell_measurement_theta_min      4.2870
_cell_volume                     5280.70(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      212.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -109.00 -20.00   1.00    3.00    --  -41.24 -38.00 -90.00   89
  2  \w    -92.00  -2.00   1.00    3.00    --  -41.24 125.00  60.00   90
  3  \w      5.00  34.00   1.00    3.00    --   41.24 -99.00-180.00   29
  4  \w     37.00 137.00   1.00   12.00    --  107.79 -77.00  60.00  100
  5  \w     82.00 174.00   1.00   12.00    --  107.79  45.00-150.00   92
  6  \w     55.00  96.00   1.00   12.00    --  107.79 -94.00   0.00   41
  7  \w     38.00 106.00   1.00   12.00    --  107.79-125.00 -30.00   68
  8  \w    109.00 137.00   1.00   12.00    --  107.79  94.00  45.00   28
  9  \w     44.00 114.00   1.00   12.00    --  107.79-125.00-120.00   70
 10  \w    110.00 166.00   1.00   12.00    --  107.79 125.00   0.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0309402000
_diffrn_orient_matrix_UB_12      -0.0788333000
_diffrn_orient_matrix_UB_13      0.0079107000
_diffrn_orient_matrix_UB_21      0.0325185000
_diffrn_orient_matrix_UB_22      0.0137960000
_diffrn_orient_matrix_UB_23      -0.0887891000
_diffrn_orient_matrix_UB_31      0.0616361000
_diffrn_orient_matrix_UB_32      0.0322673000
_diffrn_orient_matrix_UB_33      0.0570967000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20583
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.127
_diffrn_reflns_theta_min         3.918
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_description       plate
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         10415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0722P)^2^+1.8016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1235
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9222
_reflns_number_total             10415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01026j2.cif
_cod_data_source_block           25mna18c6so3cf3_lt
_cod_depositor_comments
'Adding full bibliography for 7126151--7126154.cif.'
_cod_database_code               7126154
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CHNFO
_chemical_oxdiff_usercomment     HRK-213K
_cell_oxdiff_angle_alpha         89.9623(14)
_cell_oxdiff_angle_beta          96.2355(13)
_cell_oxdiff_angle_gamma         89.9898(14)
_cell_oxdiff_length_a            20.3249(3)
_cell_oxdiff_length_b            17.8530(3)
_cell_oxdiff_length_c            14.6396(2)
_cell_oxdiff_measurement_reflns_used 12230
_cell_oxdiff_volume              5280.70(16)
_shelx_estimated_absorpt_t_max   0.836
_shelx_estimated_absorpt_t_min   0.653
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C1A(H1AA,H1AB), C12A(H12A,H12B), C11A(H11A,H11B), C7A(H7AA,
 H7AB), C3A(H3AA,H3AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B),
 C5A(H5AA,H5AB), C6A(H6AA,H6AB), C4A(H4AA,H4AB), C8B(H8BA,H8BB), C12B(H12C,
 H12D), C11B(H11C,H11D), C9B(H9BA,H9BB), C1B(H1BA,H1BB), C5B(H5BA,H5BB),
 C6B(H6BA,H6BB), C10B(H10C,H10D), C2B(H2BA,H2BB), C4B(H4BA,H4BB), C7B(H7BA,
 H7BB), C3B(H3BA,H3BB)
2.b Aromatic/amide H refined with riding coordinates:
 C18B(H18B), C16A(H16A), C18A(H18A), C15B(H15B), C15A(H15A), C16B(H16B)
2.c Idealised Me refined as rotating group:
 N1B(H1BC,H1BD,H1BE), N1A(H1AC,H1AD,H1AE), C19A(H19A,H19B,H19C), C19B(H19D,
 H19E,H19F)
;
_shelx_res_checksum              27110
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.698