Modulating the ferroelectric phases in cholesteryl-based organic compounds with perfluoroalkyl tail engineering.
Jiang, Huan-Huan; Zhang, Nan; Mao, Wei-Xin; Lan, Jin-Fei; Zhou, Long-Xing; Xu, Hua-Ming; Zhang, Han-Yue; Liao, Wei-Qiang; Chemical communications (Cambridge, England) 60 (2024) 4322–4325; doi:10.1039/d4cc00840e

data_7132861
_publ_section_title
;
 Modulating the ferroelectric phases in cholesteryl-based organic
 compounds with perfluoroalkyl tail engineering.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4322
_journal_page_last               4325
_journal_paper_doi               10.1039/d4cc00840e
_journal_volume                  60
_journal_year                    2024
_chemical_absolute_configuration a.d.
_chemical_formula_moiety         'C31 H45 F7 O2'
_chemical_formula_sum            'C31 H45 F7 O2'
_chemical_formula_weight         582.67
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-01-01 deposited with the CCDC.	2024-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.745(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7803(5)
_cell_length_b                   9.3254(4)
_cell_length_c                   13.7005(7)
_cell_measurement_reflns_used    9747
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      75.8380
_cell_measurement_theta_min      3.3170
_cell_volume                     1579.07(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22309
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.200
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.875
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: EA'
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1441 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(13)
_refine_ls_extinction_coef       0.012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6104
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0781
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2410
_refine_ls_wR_factor_ref         0.2740
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.931
_reflns_Friedel_fraction_max     0.857
_reflns_number_gt                3938
_reflns_number_total             6104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00840e2.cif
_cod_data_source_block           jhh-qfds-300k_auto
_cod_depositor_comments
'Adding full bibliography for 7132858--7132863.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7132861
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F3, C35, O00S, C3, C8, F9, C6, F00M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F21, F37, F48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C00Q, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F9) \\sim Ueq, Uanis(F3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(F00R) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F21) \\sim Ueq, Uanis(F37) \\sim Ueq, Uanis(F48) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F48) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: F00A(0.5) F00M(0.5) C00P(0.5) H00(0.5) H1(0.5) HB(0.5) HC(0.5)
 HD(0.5) F00R(0.5) O00S(0.5) F00V(0.5) C10(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) F9(0.5) F20(0.5) F21(0.5) F48(0.5)
 C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C2(0.5)
 H2A(0.5) O16(0.5)
5.a Ternary CH refined with riding coordinates:
 C004(H004), C006(H006), C00B(H00K), C00C(H00L), C00K(H00V), C00P(H00),
 C00W(H4), C2(H2A)
5.b Secondary CH2 refined with riding coordinates:
 C005(H00D,H00E), C007(H00F,H00G), C00D(H00M,H00N), C00E(H00O,H00P), C00F(H00Q,
 H00R), C00H(H00T,H00U), C00L(H00W,H00X), C00N(H00Y,H), C00O(H00Z,HA), C00Q(H1,
 HB), C00Q(HC,HD), C00U(H3,HG)
5.c Me refined with riding coordinates:
 C10(H10A,H10B,H10C)
5.d Aromatic/amide H refined with riding coordinates:
 C00G(H00S)
5.e Idealised Me refined as rotating group:
 C003(H00A,H00B,H00C), C009(H00H,H00I,H00J), C00T(H2,HE,HF), C16(H16A,H16B,
 H16C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              81161
_shelx_hkl_checksum              57785
_olex2_submission_special_instructions 'No special instructions were received'