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_7059647
_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 Dy F2 N4 O14, 13(H2 O), C11 H6 F N2 O4'
_chemical_formula_sum            'C33 H56 Dy F3 N6 O31'
_chemical_formula_weight         1252.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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
;
2018-12-14 deposited with the CCDC.	2020-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.5448(2)
_cell_length_b                   20.51697(19)
_cell_length_c                   23.3482(2)
_cell_measurement_reflns_used    10195
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.9190
_cell_measurement_theta_min      3.5730
_cell_volume                     9841.66(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -103.00  -60.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000   30.0000 86

  2 omega  -83.00  -22.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000   30.0000 122

  3 omega   19.00   61.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -90.0000 84

  4 omega   32.00  103.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   57.0000    0.0000 142

  5 omega   16.00   77.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734  -99.0000  120.0000 122

  6 omega   80.00  106.00   0.5000    8.7500
omega____ theta____ kappa____ phi______ frames
    -       36.4734   37.0000  -90.0000 52

  7 omega   87.00  112.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 50

  8 omega   39.00   82.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 86

  9 omega  106.00  157.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -150.0000 102

 10 omega  127.00  175.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 96

 11 omega   39.00   98.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 118

 12 omega   52.00   78.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 52

 13 omega   90.00  177.00   0.5000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0033411000
_diffrn_orient_matrix_UB_12      -0.0706168000
_diffrn_orient_matrix_UB_13      0.0221707000
_diffrn_orient_matrix_UB_21      0.0041475000
_diffrn_orient_matrix_UB_22      0.0250078000
_diffrn_orient_matrix_UB_23      0.0621124000
_diffrn_orient_matrix_UB_31      -0.0748063000
_diffrn_orient_matrix_UB_32      0.0046275000
_diffrn_orient_matrix_UB_33      0.0025496000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25165
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         3.585
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.158
_exptl_absorpt_correction_T_max  0.655
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_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    1.690
_exptl_crystal_description       needle
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.3191
_exptl_crystal_size_mid          0.1009
_exptl_crystal_size_min          0.0519
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
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_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+3.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7342
_reflns_number_total             8786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj02085k2.cif
_cod_data_source_block           201807328
_cod_depositor_comments
;Adding full bibliography for 7059647--7059648.cif.

 Adding full bibliography for 7059647--7059648.cif.
;
_cod_original_cell_volume        9841.66(17)
_cod_database_code               7059647
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C33H56O31N6Dy1F3
_reflns_odcompleteness_completeness 99.73
_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
 C21-F2A
 1.35 with sigma of 0.02
 C19-F2
 1.35 with sigma of 0.02
 C32-F3A
 1.35 with sigma of 0.02
 F1A-C10
 1.35 with sigma of 0.02
 H7A-O7
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
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(H30)=Sof(F3A)=1-FVAR(3)
 Sof(H32)=Sof(F3)=FVAR(3)
5.a Riding coordinates:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O30(H30A,
 H30B), O23(H23A,H23B), O29(H29A,H29B)
5.b Free rotating group:
 O19(H19A,H19B), O21(H21A,H21B), O22(H22A,H22B), O24(H24A,H24B), O26(H26A,
 H26B), O27(H27A,H27B), O28(H28A,H28B), O31(H31A,H31B)
5.c Rotating group:
 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), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
 N6(H6)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3A), O10(H10A)
;
_olex2_date_sample_data_collection 2018-07-12
_olex2_submission_special_instructions 'No special instructions were received'