Anion-dependent dynamic structure and tunable luminescence of Zn-MOFs with carboxyphenyl-terpyridine ligands
Guo, Runzhong; Liu, Yuchen; Wang, Zhibin; Wang, Haiying; Liu, Huiyan; CrystEngComm 25 (2023) 4157–4166; doi:10.1039/D3CE00405H

data_7246895
_publ_section_title
;
 Anion-dependent dynamic structure and tunable luminescence of Zn-MOFs
 with carboxyphenyl-terpyridine ligands
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4157
_journal_page_last               4166
_journal_paper_doi               10.1039/D3CE00405H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C22 H18 N3 O4 Zn, C44 H32 N8 O11.598 Zn2, Cl O4, 3(C4 H9 N O), 0.5(H2 O)'
_chemical_formula_sum            'C78 H78 Cl N14 O23.11 Zn3'
_chemical_formula_weight         1812.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2023-06-14
_audit_creation_method
; 
Olex2 1.5 
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) 
;
_audit_update_record
;
2023-06-18 deposited with the CCDC.	2023-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3263(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5019(12)
_cell_length_b                   21.9566(17)
_cell_length_c                   23.6652(18)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.35
_cell_volume                     7898.0(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.277
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5473
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1295 before and 0.0385 after correction. 
The Ratio of minimum to maximum transmission is 0.7340. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.830
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         17982
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      14.101
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0738P)^2^+13.6372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12969
_reflns_number_total             17982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00405h2.cif
_cod_data_source_block           compound1-ClO4
_cod_depositor_comments
'Adding full bibliography for 7246892--7246895.cif.'
_cod_database_code               7246895
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.806
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups, All O(H,H) groups 
2. Restrained distances 
 H7B-H25 
 2.2 with sigma of 0.01 
 Zn1-H18A \\sim Zn1-H18B 
 with sigma of 0.02 
 Zn3-H10A \\sim Zn3-H10B 
 with sigma of 0.02 
 O19-O28 \\sim O19A-O28A 
 with sigma of 0.04 
 O8-O28 \\sim O8A-O28A 
 with sigma of 0.04 
 O8-O19 \\sim O8A-O19A 
 with sigma of 0.04 
 Zn2-N25 \\sim Zn2-N25A 
 with sigma of 0.04 
 N25-O28 \\sim N25A-O28A 
 with sigma of 0.02 
 O19-N25 \\sim O19A-N25A 
 with sigma of 0.02 
 O8-N25 \\sim O8A-N25A 
 with sigma of 0.02 
 Zn2-O28 \\sim Zn2-O28A 
 with sigma of 0.02 
3. Rigid bond restraints 
 C73A 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 
4. Uiso/Uaniso restraints and constraints 
Uanis(O17) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 
0.005 and sigma for terminal atoms of 0.01 
Uanis(O8A) \\sim Ueq, Uanis(O15A) \\sim Ueq, Uanis(O19A) \\sim Ueq: with sigma 
of 0.01 and sigma for terminal atoms of 0.02 
5. Rigid body (RIGU) restrains 
 O16, C76, C77, C78, C75, N13 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O16A, C76A, C77A, C78A, C75A, N13A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O13, O12, O11 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O15, C71, C72, C73, N12, C9 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O15A, C71A, C72A, C73A, N12A, C9A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
6. Others 
 Sof(N25A)=Sof(O8A)=Sof(O19A)=Sof(O28A)=1-FVAR(1) 
 Sof(N25)=Sof(O8)=Sof(O19)=Sof(O28)=FVAR(1) 
 Sof(O16A)=Sof(C75A)=Sof(C76A)=Sof(H76D)=Sof(H76E)=Sof(H76F)=Sof(N13A)= 
 Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=Sof(C78A)=Sof(H78D)=Sof(H78E)= 
 Sof(H78F)=1-FVAR(2) 
 Sof(O16)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C77)=Sof(H77A)=Sof(H77B)= 
 Sof(H77C)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C75)=Sof(N13)=FVAR(2) 
 Sof(O13)=Sof(O12)=Sof(O11)=FVAR(3) 
 Sof(O15A)=Sof(C9A)=Sof(C71A)=Sof(H71D)=Sof(H71E)=Sof(H71F)=Sof(N12A)= 
 Sof(C72A)=Sof(H72D)=Sof(H72E)=Sof(H72F)=Sof(C73A)=Sof(H73D)=Sof(H73E)= 
 Sof(H73F)=1-FVAR(4) 
 Sof(O15)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C72)=Sof(H72A)=Sof(H72B)= 
 Sof(H72C)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(N12)=Sof(C9)=FVAR(4) 
 Fixed Sof: O17(0.5) H17A(0.5) H17B(0.5) 
7.a Free rotating group: 
 O10(H10A,H10B), O18(H18A,H18B), O17(H17A,H17B) 
7.b Rotating group: 
 O7(H7A,H7B), O9(H9A,H9B) 
7.c Aromatic/amide H refined with riding coordinates: 
 C37(H37), C64(H64), C12(H12), C56(H56), C34(H34), C53(H53), C47(H47), 
 C31(H31), C6(H6), C7(H7), C19(H19), C50(H50), C25(H25), C48(H48), C51(H51), 
 C28(H28), C65(H65), C14(H14), C21(H21), C22(H22), C43(H43), C26(H26), C17(H17), 
  C3(H3), C4(H4), C16(H16), C59(H59), C15(H15), C39(H39), C44(H44), C41(H41), 
 C63(H63), C38(H38), C29(H29), C66(H66), C42(H42), C20(H20), C58(H58), C36(H36), 
  C60(H60), C61(H61) 
7.d Idealised Me refined as rotating group: 
 C70(H70A,H70B,H70C), C69(H69A,H69B,H69C), C68(H68A,H68B,H68C), C76(H76A,H76B, 
 H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C76A(H76D,H76E,H76F), 
 C77A(H77D,H77E,H77F), C78A(H78D,H78E,H78F), C71(H71A,H71B,H71C), C72(H72A,H72B, 
 H72C), C73(H73A,H73B,H73C), C71A(H71D,H71E,H71F), C72A(H72D,H72E,H72F), 
 C73A(H73D,H73E,H73F) 
;
_shelx_res_checksum              96280
_shelx_hkl_checksum              34848
_olex2_submission_special_instructions 'No special instructions were received'