Two novel lanthanide metal-organic frameworks based on tetraphenylethylene for ultra-high proton conduction.
Wu, Qi; Li, Qianxi; Zou, Wenkang; Zhang, Zheyu; Zhou, Yan; Zhao, Qihua; Chemical communications (Cambridge, England) 61 (2025) 1842–1845; doi:10.1039/d4cc06013j

data_7134124
_publ_section_title
;
 Two novel lanthanide metal-organic frameworks based on
 tetraphenylethylene for ultra-high proton conduction.
;
_journal_issue                   9
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1842
_journal_page_last               1845
_journal_paper_doi               10.1039/d4cc06013j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C58 H36 Dy F4 N O11, C3 H7 N O, C2 H8 N'
_chemical_formula_sum            'C63 H52 Dy F4 N3 O12'
_chemical_formula_weight         1281.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-09-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-23 deposited with the CCDC.	2024-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.096(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.9144(15)
_cell_length_b                   9.0765(6)
_cell_length_c                   39.7778(19)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      59
_cell_measurement_theta_min      5
_cell_volume                     7782.5(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54052
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.062
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       needle
_exptl_crystal_F_000             2596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.364
_refine_diff_density_min         -2.139
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         13677
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0659P)^2^+47.0163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11445
_reflns_number_total             13677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06013j2.cif
_cod_data_source_block           Dy-MOF
_cod_depositor_comments
'Adding full bibliography for 7134123--7134124.cif.'
_cod_database_code               7134124
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.862
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C60-N2
 1.5 with sigma of 0.01
3. Rigid bond restraints
 O2, N2, C59, C60, C61
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 F3, C36, C35, C39, C38, C56, C57', C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(F3) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57') \\sim Ueq,
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
5. Others
 Fixed Sof: N1(0.5) C55(0.5) H55(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5)
 C57'(0.5) H57D(0.5) H57E(0.5) H57F(0.5) N1'(0.5) C55'(0.5) H55'(0.5) C56(0.5)
 H56A(0.5) H56B(0.5) H56C(0.5) C56'(0.5) H56D(0.5) H56E(0.5) H56F(0.5)
6.a Fixed occupancy and ADP/Uiso:
 O2
6.b Riding coordinates:
 C57'(H57D,H57E,H57F), C56(H56A,H56B,H56C), C56'(H56D,H56E,H56F), N3(H3A,H3B),
 C63(H63A,H63B,H63C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C12(H12), C13(H13), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C26(H26), C29(H29), C30(H30),
  C32(H32), C33(H33), C35(H35), C38(H38), C39(H39), C43(H43), C44(H44),
 C46(H46), C47(H47), C49(H49), C50(H50), C53(H53), C58(H58), C55(H55),
 C55'(H55'), C61(H61)
6.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,
 H62C)
;
_shelx_res_checksum              37011
_shelx_fab_checksum              89580
_olex2_submission_special_instructions 'No special instructions were received'