Anionic modulation induces molecular polarity in a three-component crown ether system.
Liu, Feiyan; Chen, Guoyong; Liu, Xiao; Jiang, Ting; Guo, Wenjing; Li, Xiancai; Wei, Zhenhong; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2793–2798; doi:10.1039/d4dt03466j

data_7717762
_publ_section_title
;
 Anionic modulation induces molecular polarity in a three-component crown
 ether system.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2793
_journal_page_last               2798
_journal_paper_doi               10.1039/d4dt03466j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety
'C10 H18 O5, C10 H20 O5, 2(C7 H7 F3 N), 2(Cl O4)'
_chemical_formula_sum            'C34 H52 Cl2 F6 N2 O18'
_chemical_formula_weight         961.68
_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_block_doi                 10.5517/ccdc.csd.cc2lv8c3
_audit_creation_date             2024-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-12-09 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.882(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.5944(5)
_cell_length_b                   9.4697(2)
_cell_length_c                   17.1687(5)
_cell_measurement_reflns_used    23583
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      30.7840
_cell_measurement_theta_min      3.0070
_cell_volume                     2201.84(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37369
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.815
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.822
_diffrn_reflns_theta_min         3.008
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             1004.0
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 3534 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.23(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         11270
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.268
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0546
_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^)+(0.1044P)^2^+0.3145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1684
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.764
_reflns_number_gt                9075
_reflns_number_total             11270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03466j2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7717762--7717764.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7717762
_shelx_shelxl_version_number     2018/3
_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
2. Uiso/Uaniso restraints and constraints
Uanis(O7) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Cl1) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(O8) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(O7) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O8) \\sim
Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C12(H12), C13(H13), C15(H15), C16(H16), C29(H29), C30(H30),
 C32(H32), C33(H33)
3.c Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E), N2(H2C,H2D,H2E)
;
_shelx_res_checksum              30923
_olex2_submission_special_instructions 'No special instructions were received'