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_7246893
_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 H33 Cl1.5 N6 O6.5 Zn2, N O2.705, 3(C4 H9 N O), 0.5(H2 O)'
_chemical_formula_sum            'C78 H79 Cl1.5 N13 O16.7 Zn3'
_chemical_formula_weight         1715.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-06-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-19 deposited with the CCDC.	2023-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.952(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8121(19)
_cell_length_b                   21.163(3)
_cell_length_c                   15.335(2)
_cell_measurement_reflns_used    6730
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.41
_cell_volume                     3799.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 0.996
_diffrn_measured_fraction_theta_max 0.944
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22937
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.150
_diffrn_reflns_theta_min         2.594
_exptl_absorpt_coefficient_mu    1.071
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1774
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.574
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         9024
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.237
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0868P)^2^+4.6081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6546
_reflns_number_total             9024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00405h2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7246892--7246895.cif.'
_cod_original_formula_sum        'C78 H79 Cl1.50 N13 O16.70 Zn3'
_cod_database_code               7246893
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.814
_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
 N47-C50
 1.229 with sigma of 0.001
 O10-N10 = O11-N10
 2.1 with sigma of 0.02
 Zn2-Cl1 \\sim Zn2A-Cl1
 with sigma of 0.02
 Zn2-O1 \\sim Zn2A-O1
 with sigma of 0.02
 N47-C51 \\sim N47-C52 \\sim O53-C50
 with sigma of 0.001
 N47-O53 \\sim O53-C9
 with sigma of 0.02
 C9-C50 \\sim C9A-C50A
 with sigma of 0.02
 C51-N47 \\sim C51A-N47A
 with sigma of 0.02
 C52-N47 \\sim C52A-N47A
 with sigma of 0.02
 C50-O53 \\sim C50A-O53A
 with sigma of 0.02
 C9-N47 \\sim C9A-N47A
 with sigma of 0.04
 C9-O53 \\sim C9A-O53A
 with sigma of 0.04
 C50-C50A \\sim C51-C52
 with sigma of 0.04
3. Restrained planarity
 C9, C51, C52, N47, C50, O53
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Cl1 \\sim O3: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.008 within 2A
C51A \\sim C52: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C51 \\sim C9A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
Uanis(Zn2) \\sim Ueq, Uanis(Zn2A) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O4A)
\\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C9A) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C51A) \\sim Ueq, Uanis(C52A)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(Zn2) = Uanis(Zn2A)
5. Rigid body (RIGU) restrains
 C46, O8, C45, N7, C49, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50, C9, N47, O53, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C50A, C9A, N47A, O53A, C51A, C52A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Zn2(0.25) Cl1(0.75) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5)
 H43(0.5) C44(0.5) H44(0.5) C9(0.25) H9A(0.25) H9B(0.25) H9C(0.25) C51(0.25)
 H51A(0.25) H51B(0.25) H51C(0.25) C52(0.25) H52A(0.25) H52B(0.25) H52C(0.25)
 N47(0.25) C50(0.25) O53(0.25) C50A(0.25) C9A(0.25) H9AA(0.25) H9AB(0.25)
 H9AC(0.25) N47A(0.25) O53A(0.25) C51A(0.25) H51D(0.25) H51E(0.25) H51F(0.25)
 C52A(0.25) H52D(0.25) H52E(0.25) H52F(0.25) O9(0.25) H9D(0.25) H9E(0.25)
 Zn2A(0.75) O3(0.25) H3A(0.25) H3B(0.25)
7.a Riding coordinates:
 C51(H51A,H51B,H51C), C9A(H9AA,H9AB,H9AC), O9(H9D,H9E), O3(H3A,H3B)
7.b Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C47(H47), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
  C28(H28), C29(H29), C31(H31), C34(H34), C36(H36), C37(H37), C38(H38),
 C39(H39), C41(H41), C42(H42), C43(H43), C44(H44)
7.d Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C9(H9A,H9B,
 H9C), C52(H52A,H52B,H52C), C51A(H51D,H51E,H51F), C52A(H52D,H52E,H52F)
;
_shelx_res_checksum              91163
_shelx_hkl_checksum              42091
_olex2_submission_special_instructions 'No special instructions were received'