Proton conduction in two hydrogen-bonded supramolecular lanthanide complexes
Shi, Zhi-Qiang; Ji, Ning-Ning; Chen, Wan-Yao; Li, Gang; New Journal of Chemistry 44 (2020) 10562–10568; doi:10.1039/D0NJ02085K

data_7059648
_publ_section_title
;
 Proton conduction in two hydrogen-bonded supramolecular lanthanide
 complexes
;
_journal_issue                   25
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10562
_journal_page_last               10568
_journal_paper_doi               10.1039/D0NJ02085K
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C22 H24 Eu F2 N4 O14, C11 H6 F N2 O4, 6(H2 O)'
_chemical_formula_sum            'C33 H42 Eu F3 N6 O24'
_chemical_formula_weight         1115.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-25 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                96.834(3)
_cell_angle_beta                 108.861(4)
_cell_angle_gamma                96.387(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4389(5)
_cell_length_b                   12.4406(4)
_cell_length_c                   16.1101(7)
_cell_measurement_reflns_used    6662
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.7330
_cell_measurement_theta_min      4.1450
_cell_volume                     2126.54(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2312
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega -105.00   38.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000    0.0000  -30.0000 143

  2 omega  -45.00   25.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   57.0000   90.0000 70

  3 omega   21.00   60.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000  150.0000 39

  4 omega   -4.00   41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000 -180.0000 45

  5 omega   11.00  101.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000  -30.0000 90

  6 omega   57.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000    0.0000 40

  7 omega   42.00   76.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  -90.0000 34

  8 omega   14.00   46.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  150.0000 32

  9 omega    4.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   19.0000  150.0000 29

 10 omega   68.00  108.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000   90.0000 40

 11 omega   47.00   77.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000   90.0000 30

 12 omega   44.00  107.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734 -157.0000  -87.0000 63

 13 omega   63.00  105.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   19.0000  150.0000 42

 14 omega   77.00  109.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734  178.0000  -30.0000 32

 15 omega   23.00   59.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.4734   77.0000   30.0000 36

 16 omega   57.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 51

 17 omega   63.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 115

 18 omega   38.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 19 omega   83.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 26

 20 omega   42.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 54

 21 omega   42.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 46

 22 omega   42.00   68.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 26

 23 omega   59.00  125.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  120.0000 66

 24 omega   38.00   93.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 55

 25 omega   45.00   86.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 41

 26 omega  121.00  154.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 33

 27 omega   38.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 61

 28 omega   56.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 35

 29 omega   43.00  108.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 65

 30 omega  111.00  137.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  120.0000 26

 31 omega   38.00   64.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   90.0000 26

 32 omega   83.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 26

 33 omega  118.00  146.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 28

 34 omega   44.00  114.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000 -120.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1441210000
_diffrn_orient_matrix_UB_12      -0.0228738000
_diffrn_orient_matrix_UB_13      -0.0359701000
_diffrn_orient_matrix_UB_21      -0.0019804000
_diffrn_orient_matrix_UB_22      0.0324811000
_diffrn_orient_matrix_UB_23      0.0947907000
_diffrn_orient_matrix_UB_31      -0.0027560000
_diffrn_orient_matrix_UB_32      0.1199241000
_diffrn_orient_matrix_UB_33      -0.0147517000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.063
_diffrn_reflns_theta_max         67.063
_diffrn_reflns_theta_min         3.625
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.551
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.117
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.3202
_exptl_crystal_size_mid          0.1558
_exptl_crystal_size_min          0.0366
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         7583
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0730P)^2^+0.3101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6666
_reflns_number_total             7583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02085k2.cif
_cod_data_source_block           201807325
_cod_depositor_comments
;Adding full bibliography for 7059647--7059648.cif.

 Adding full bibliography for 7059647--7059648.cif.
;
_cod_database_code               7059648
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C33H33O24N6Eu1F3
_reflns_odcompleteness_completeness 99.83
_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 N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H10A-O10
 0.9 with sigma of 0.02
 F2A-C21
 1.35 with sigma of 0.02
 C8-F1
 1.35 with sigma of 0.02
 C10-F1A
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(O23) = Uanis(O23A)
Uanis(O20) = Uanis(O20A)
4. Others
 Sof(H8)=Sof(F1A)=1-FVAR(1)
 Sof(H10)=Sof(F1)=FVAR(1)
 Sof(H19)=Sof(F2A)=1-FVAR(2)
 Sof(H21)=Sof(F2)=FVAR(2)
 Sof(O23A)=Sof(H23C)=Sof(H23D)=1-FVAR(3)
 Sof(O23)=Sof(H23A)=Sof(H23B)=FVAR(3)
 Sof(O20A)=Sof(H20C)=Sof(H20D)=1-FVAR(4)
 Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(4)
5.a Riding coordinates:
 O15(H15A,H15B), O16(H16A,H16B), O19(H19A,H19B), O20A(H20C,H20D), O22(H22A,
 H22B), O23(H23A,H23B), O24(H24A,H24B)
5.b Free rotating group:
 O20(H20A,H20B), O21(H21A,H21B), O23A(H23C,H23D)
5.c Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O17(H17A,H17B), O18(H18A,H18B)
5.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), N1(H1), N4(H4), C29(H29), C31(H31), C32(H32), C33(H33),
 N6(H6)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7A)
;
_olex2_date_sample_data_collection 2018-07-11
_olex2_submission_special_instructions 'No special instructions were received'