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_7126151
_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         '2(F3 P0.5), C7 H9 N2 O3, C12 H24 O6'
_chemical_formula_sum            'C19 H33 F6 N2 O9 P'
_chemical_formula_weight         578.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-01
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7788(4)
_cell_length_b                   19.7210(3)
_cell_length_c                   15.0786(2)
_cell_measurement_reflns_used    10535
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.7890
_cell_measurement_theta_min      3.3150
_cell_volume                     5286.79(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -72.00  43.00   1.00   10.00    --  -32.00   0.00-108.00  115
  2  \w    -78.00 -18.00   1.00   10.00    --  -32.00 -72.00-180.00   60
  3  \w   -200.00 -38.00   1.00   50.00    -- -110.00   0.00 -36.00  162
  4  \w   -125.00 -60.00   1.00   50.00    -- -110.00  72.00 -36.00   65
  5  \w   -200.00-125.00   1.00   50.00    -- -110.00 -72.00 108.00   75
  6  \w    -80.00 -20.00   1.00   50.00    -- -110.00  72.00  36.00   60
  7  \w   -106.00 -20.00   1.00   50.00    -- -110.00  72.00 108.00   86
  8  \w    -80.00 -20.00   1.00   50.00    -- -110.00  72.00-180.00   60
  9  \w    -98.00 -38.00   1.00   50.00    -- -110.00  72.00-108.00   60
 10  \w   -200.00-130.00   1.00   50.00    -- -110.00 -72.00-180.00   70
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26161
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.992
_diffrn_reflns_theta_min         3.347
_exptl_absorpt_coefficient_mu    1.767
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         4998
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0867
_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^)+(0.3000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2941
_refine_ls_wR_factor_ref         0.3198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4136
_reflns_number_total             4998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc01026j2.cif
_cod_data_source_block           25mna18c6pf6_ht
_cod_depositor_comments
'Adding full bibliography for 7126151--7126154.cif.'
_cod_database_code               7126151
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.719
_shelx_estimated_absorpt_t_min   0.619
_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. Restrained distances
 F7-F10 \\sim F7-F11 \\sim F7-F8 \\sim F8-F9 \\sim F11-F8 \\sim F10-F11 \\sim
F7-F9 \\sim F9-F10
 with sigma of 0.02
 F3-F4 \\sim F5-F3 \\sim F1-F5 \\sim F4-F1 \\sim F2-F4 \\sim F2-F3 \\sim F2-F5
\\sim F2-F1 \\sim F6-F1 \\sim F6-F3
 \\sim F6-F5 \\sim F6-F4
 with sigma of 0.02
 P1-F2 \\sim P1-F6 \\sim P1-F4 \\sim P1-F5 \\sim P1-F1 \\sim P1-F3 \\sim P2-F7
\\sim P2-F8 \\sim P2-F9 \\sim P2-
 F10 \\sim P2-F11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C11A \\sim C10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
F3 \\sim F2 \\sim F4 \\sim F5 \\sim F6 \\sim F1: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
F8 \\sim F9 \\sim F10 \\sim F7 \\sim F11: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F6) \\sim Ueq, Uanis(F5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C8A)=Sof(H8Aa)=Sof(H8Ab)=Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(O1A)=Sof(C2A)=
 Sof(H2Aa)=Sof(H2Ab)=Sof(C12A)=Sof(H12c)=Sof(H12d)=Sof(O2A)=Sof(C11A)=Sof(H11c)=
 Sof(H11d)=Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(O6A)=Sof(C10A)=Sof(H10c)=Sof(H10d)=
 Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C9A)=Sof(H9Aa)=Sof(H9Ab)=Sof(O3A)=Sof(O5A)=
 Sof(C5A)=Sof(H5Aa)=Sof(H5Ab)=Sof(C6A)=Sof(H6Aa)=Sof(H6Ab)=Sof(C7A)=Sof(H7Aa)=
 Sof(H7Ab)=Sof(O4A)=1-FVAR(1)
 Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(O1)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(O6)=Sof(O4)=
 Sof(C3)=Sof(H3a)=Sof(H3b)=Sof(C10)=Sof(H10a)=Sof(H10b)=Sof(C7)=Sof(H7a)=
 Sof(H7b)=Sof(O3)=Sof(O2)=Sof(O5)=Sof(C11)=Sof(H11a)=Sof(H11b)=Sof(C8)=Sof(H8a)=
 Sof(H8b)=Sof(C6)=Sof(H6a)=Sof(H6b)=Sof(C9)=Sof(H9a)=Sof(H9b)=Sof(C5)=Sof(H5a)=
 Sof(H5b)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(C2)=Sof(H2a)=Sof(H2b)=FVAR(1)
 Fixed Sof: F9(0.5) F6(0.5) F11(0.5) F4(0.5) F5(0.5) F3(0.5) F2(0.5) F1(0.5)
 F10(0.5) F8(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C4(H4a,H4b), C3(H3a,H3b), C10(H10a,H10b), C7(H7a,H7b), C11(H11a,
 H11b), C8(H8a,H8b), C6(H6a,H6b), C9(H9a,H9b), C5(H5a,H5b), C12(H12a,H12b),
 C2(H2a,H2b), C8A(H8Aa,H8Ab), C1A(H1Aa,H1Ab), C2A(H2Aa,H2Ab), C12A(H12c,H12d),
 C11A(H11c,H11d), C3A(H3Aa,H3Ab), C10A(H10c,H10d), C4A(H4Aa,H4Ab), C9A(H9Aa,
 H9Ab), C5A(H5Aa,H5Ab), C6A(H6Aa,H6Ab), C7A(H7Aa,H7Ab)
5.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C15(H15), C16(H16)
5.c Idealised Me refined as rotating group:
 N1(H1c,H1d,H1e), C19(H19a,H19b,H19c)
;
_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
- Detector area scaling
;