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_7246894
_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 O11.5 Zn2, B F4, 1.943(C4 H9 N O), C2.113 H4.755 N0.473 O0.528, 0.472(C4 H6 N1 O1), 0.5(H2 O)'
_chemical_formula_sum            'C77.78 H76.08 B F4 N13.89 O18.94 Zn3'
_chemical_formula_weight         1791.37
_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
_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                 101.131(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.521(7)
_cell_length_b                   21.920(11)
_cell_length_c                   23.657(11)
_cell_measurement_reflns_used    7546
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.36
_cell_volume                     7897(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42663
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.488
_diffrn_reflns_theta_min         1.278
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6242
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0555 before and 0.0446 after correction. 
The Ratio of minimum to maximum transmission is 0.8374. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             3690
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1257
_refine_ls_number_reflns         16098
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+0.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10101
_reflns_number_total             16098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00405h2.cif
_cod_data_source_block           compound1-bf4
_cod_depositor_comments
'Adding full bibliography for 7246892--7246895.cif.'
_cod_original_cell_volume        7897(7)
_cod_database_code               7246894
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.826
_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. Rigid bond restraints 
 O19 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005 
 O22, N24 
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 
3. Uiso/Uaniso restraints and constraints 
Uanis(F3) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of 
0.005 and sigma for terminal atoms of 0.01 
Uanis(F4) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(O11A) 
\\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(O18A) \\sim Ueq: with sigma of 0.01 and 
sigma for terminal atoms of 0.02 
Uanis(O22) \\sim Ueq, Uanis(N24) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(O14A) 
\\sim Ueq, Uanis(C69A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C74A) \\sim Ueq: 
with sigma of 0.01 and sigma for terminal atoms of 0.02 
4. Rigid body (RIGU) restrains 
 O16, C77, C78, N12, C76, C75 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O16A, C77A, C78A, N12A, C76A, C75A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O14 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 N12 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O11 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O11A, N14A, O18, O17A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O14, C68, C69, N10, C74, C67 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
 O14A, C68A, C69A, N10A, C74A, C67A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
5. Others 
 Sof(O16A)=Sof(C75A)=Sof(C76A)=Sof(N12A)=Sof(C78A)=Sof(H78D)=Sof(H78E)= 
 Sof(H78F)=Sof(C77A)=Sof(H77D)=Sof(H77E)=Sof(H77F)=1-FVAR(1) 
 Sof(O16)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=Sof(C78)=Sof(H78A)=Sof(H78B)= 
 Sof(H78C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C75)=FVAR(1) 
 Sof(O11A)=Sof(O18A)=1-FVAR(2) 
 Sof(O11)=Sof(O18)=FVAR(2) 
 Sof(O14)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)= 
 Sof(H69C)=Sof(N10)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C67)=FVAR(3) 
 Fixed Sof: O22(0.5) O14A(0.3294) C67A(0.3294) C68A(0.3294) H68D(0.3294) 
 H68E(0.3294) H68F(0.3294) N10A(0.3294) C69A(0.3294) H69D(0.3294) H69E(0.3294) 
 H69F(0.3294) C74A(0.3294) H74D(0.3294) H74E(0.3294) H74F(0.3294) O19(0.5) 
 H19A(0.5) H19B(0.5) 
6.a Free rotating group: 
 O7(H7A,H7B,O8,H8A,H8B,O9,H9A,H9B), O19(H19A,H19B) 
6.b Rotating group: 
 O10(H10A,H10B) 
6.c Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C12(H12), C14(H14), C15(H15), 
 C16(H16), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26), C29(H29), C31(H31), 
  C34(H34), C36(H36), C39(H39), C42(H42), C43(H43), C44(H44), C47(H47), 
 C48(H48), C50(H50), C51(H51), C53(H53), C56(H56), C58(H58), C59(H59), C60(H60), 
  C61(H61), C63(H63), C64(H64) 
6.d Idealised Me refined as rotating group: 
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C71(H71A,H71B,H71C), C77(H77A,H77B, 
 H77C), C78(H78A,H78B,H78C), C76(H76A,H76B,H76C), C78A(H78D,H78E,H78F), 
 C77A(H77D,H77E,H77F), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C74(H74A,H74B, 
 H74C), C68A(H68D,H68E,H68F), C69A(H69D,H69E,H69F), C74A(H74D,H74E,H74F) 
;
_shelx_res_checksum              90008
_shelx_hkl_checksum              17951
_olex2_submission_special_instructions 'No special instructions were received'