Anionic lanthanide metal-organic frameworks with magnetism, fluorescence, proton conductivity and selective adsorption of cationic dye
Zhang, Xiao-Nuan; Chen, Bo-Chen; Zhang, Jia-Li; Zhang, Jialin; Liu, Sui-Jun; Wen, He-Rui; Dalton Transactions  (2022) –; doi:10.1039/D2DT02347D

data_7711302
_publ_section_title
;
 Anionic lanthanide metal-organic frameworks with magnetism, fluorescence,
 proton conductivity and selective adsorption of cationic dye
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02347D
_journal_year                    2022
_chemical_formula_moiety         'C16 H6 Dy O8, C2 H8 N'
_chemical_formula_sum            'C18 H14 Dy N O8'
_chemical_formula_weight         534.70
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-12 deposited with the CCDC.	2022-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.7063(4)
_cell_length_b                   13.7063(4)
_cell_length_c                   22.8201(17)
_cell_measurement_reflns_used    6467
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      2
_cell_measurement_theta_min      2.96
_cell_volume                     3712.7(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'phi and omega scans'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      180.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27375
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.972
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       rod
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 1620 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4369
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.471
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0196P)^2^+18.0915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3959
_reflns_number_total             4369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02347d2.cif
_cod_data_source_block           d_sq_s_sq_s
_cod_original_cell_volume        3712.7(4)
_cod_database_code               7711302
_shelx_shelxl_version_number     2017/1
_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
 H2C-C2
 0.85 with sigma of 0.01
 H2C-H2B
 2.5 with sigma of 0.02
 C2-N2
 1.54 with sigma of 0.01
3. Rigid bond restraints
 Dy1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O3, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Dy1, O3
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.2
4. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 N2(H2D,H2E)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              96901
_shelx_hkl_checksum              42922
_shelx_fab_checksum              68796
_olex2_submission_special_instructions 'No special instructions were received'