The gas-selective Zn-MOF exhibits selective sensing of Fe3+ ions by doping with Tb3+
Wang, Zhi Gang; Ding, Tao; Fei, Jie; Dalton Transactions  (2023) –; doi:10.1039/D3DT02721J

data_7713957
_publ_section_title
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 The gas-selective Zn-MOF exhibits selective sensing of Fe3+ ions by
 doping with Tb3+
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02721J
_journal_year                    2023
_chemical_formula_moiety         '0.13(C352 H184 N96 O128 Zn32), 2(C2 H8 N)'
_chemical_formula_sum            'C48 H39 N14 O16 Zn4'
_chemical_formula_weight         1329.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2023-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2346(5)
_cell_length_b                   24.4346(5)
_cell_length_c                   28.7280(8)
_cell_measurement_reflns_used    9101
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.906
_cell_measurement_theta_min      2.385
_cell_volume                     17011.7(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.1286
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31407
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        62.496
_diffrn_reflns_theta_max         62.496
_diffrn_reflns_theta_min         3.076
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5038
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1161 before and 0.0777 after correction.
The Ratio of minimum to maximum transmission is 0.6694.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             5384
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details          TITL
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6692
_refine_ls_number_restraints     1373
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1686P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3215
_reflns_number_total             6692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02721j2.cif
_cod_data_source_block           2017770-de-1_0m
_cod_database_code               7713957
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C4 = C13-C14 = C14A-C13A
 1.45 with sigma of 0.01
 C1-C2 = C2A-C1 = C5A-C8 = C5-C8 = C19A-C20 = C19-C20
 1.45 with sigma of 0.01
 C26-C25
 2.5 with sigma of 0.02
 C23-N8
 1.45 with sigma of 0.02
 N8-C24
 1.45 with sigma of 0.02
 N9-C25 = N9-C26
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C22 \\sim C20 \\sim C8 \\sim C19 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim
C18 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C2 \\sim C3 \\sim C1 \\sim C13
\\sim C12 \\sim C11 \\sim C10 \\sim C9 \\sim C13A \\sim C12A \\sim C11A \\sim
C10A \\sim C9A \\sim C19A \\sim C18A \\sim C17A \\sim C16A \\sim C15A \\sim
C14A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C2A \\sim C3A \\sim C21A
\\sim C21 \\sim C24 \\sim C23 \\sim C25 \\sim C26 \\sim N6 \\sim N3 \\sim N1
\\sim N4 \\sim N21 \\sim N7 \\sim N7A \\sim N5 \\sim N2 \\sim N22A \\sim N8
\\sim N9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O7) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C13A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C11A) \\sim Ueq,
Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C18A)
\\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C15A) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A)
\\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq,
Uanis(C21A) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(N6) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N21) \\sim
Ueq, Uanis(N7) \\sim Ueq, Uanis(N7A) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(N22A) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(N9) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) = Uanis(O2) = Uanis(O7)
4. Rigid body (RIGU) restrains
 C22, C20, C8, C19, C14, C15, C16, C17, C18, C4, C5, C6, C7, C2, C3, C1, C13,
 C12, C11, C10, C9, C13A, C12A, C11A, C10A, C9A, C19A, C18A, C17A, C16A, C15A,
 C14A, C4A, C5A, C6A, C7A, C2A, C3A, C21A, C21, C24, C23, C25, C26, N6, N3, N1,
 N4, N21, N7, N7A, N5, N2, N22A, N8, N9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(N7A)=Sof(C13A)=Sof(C12A)=Sof(H12A)=Sof(C11A)=Sof(H11A)=Sof(C10A)=
 Sof(H10A)=Sof(C9A)=Sof(C19A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=
 Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(C7A)=
 Sof(H7A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(C19)=Sof(C14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(C17)=Sof(H17)=Sof(C18)=
 Sof(H18)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C2)=Sof(C3)=
 Sof(H3)=Sof(N7)=Sof(C13)=Sof(C12)=Sof(H12)=Sof(C11)=Sof(H11)=Sof(C10)=Sof(H10)=
 Sof(C9)=FVAR(1)
 Fixed Sof: C22(0.5) N21(0.5) N5(0.5) H5A(0.5) H5B(0.5) N2(0.5) H2A(0.5)
 H2B(0.5) C21A(0.5) N22A(0.5) H22A(0.5) N8(0.5) H8A(0.5) H8B(0.5) N9(0.5)
 H9A(0.5) H9B(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C23(0.5) H23A(0.5)
 H23B(0.5) H23C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26(0.5) H26A(0.5)
 H26B(0.5) H26C(0.5)
 Fixed U11: N8(0.11732) N9(0.11732)
 Fixed U12: N8(0.00418) N9(0.00418)
 Fixed U13: N8(-0.01316) N9(-0.01316)
 Fixed U22: N8(0.10439) N9(0.10439)
 Fixed U23: N8(-0.01025) N9(-0.01025)
 Fixed U33: N8(0.08111) N9(0.08111)
6.a Riding coordinates:
 N5(H5A,H5B), N2(H2A,H2B), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C)
6.b Secondary CH2 refined with riding coordinates:
 N8(H8A,H8B), N9(H9A,H9B)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C18(H18), C6(H6), C7(H7), C3(H3), C12(H12), C11(H11),
 C10(H10), C12A(H12A), C11A(H11A), C10A(H10A), C18A(H18A), C17A(H17A),
 C15A(H15A), C4A(H4A), C7A(H7A), C3A(H3A), N22A(H22A)
6.d Fitted hexagon refined as free rotating group:
 C19(C14,C15,C16,C17,C18), C4(C5,C6,C7,C2,C3), N7(C13,C12,C11,C10,C9),
 N7A(C13A,C12A,C11A,C10A,C9A), C19A(C18A,C17A,C16A,C15A,C14A), C4A(C5A,C6A,C7A,
 C2A,C3A)
;
_olex2_submission_special_instructions 'No special instructions were received'