Assembly of metal‒organic frameworks based on 4-connected 3,3′,5,5′-azobenzenetetracarboxylic acid: structures, magnetic properties, and sensing of Fe3+ ions
Di, Min; Shen, Jingwen; Cui, Zheng; Zhang, Xiaoying; Zhang, Jingping; New Journal of Chemistry 43 (2019) 4226–; doi:10.1039/C8NJ05139A

data_7058152
_publ_section_title
;
 Assembly of metal--organic frameworks based on 4-connected
 3,3&#x2032;,5,5&#x2032;-azobenzenetetracarboxylic acid: structures,
 magnetic properties, and sensing of Fe3+ ions
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4226
_journal_paper_doi               10.1039/C8NJ05139A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '0.33(C156 H111 N21 O90 Zn18)'
_chemical_formula_sum            'C52 H37 N7 O30 Zn6'
_chemical_formula_weight         1632.10
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.8480(10)
_cell_length_b                   22.8480(10)
_cell_length_c                   20.330(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      25.862
_cell_measurement_theta_min      2.682
_cell_volume                     9191.0(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       SAINT
_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 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.055
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.7658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.885
_exptl_crystal_description       block
_exptl_crystal_F_000             2454
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
A solvent mask was calculated and 1724 electrons were 
found in a volume of 5674\%A^3 in 3 voids. 
This is consistent with the presence of 
ten N,N-dimethylacetamide and four methanol per formula unit 
which account for 1656 electrons.
;
_refine_diff_density_max         0.792
_refine_diff_density_min         -2.530
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         12112
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0889P)^2^+20.9271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9667
_reflns_number_total             12112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05139a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7058150--7058152.cif.'
_cod_original_cell_volume        9191.0(12)
_cod_database_code               7058152
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.49(3)
2. 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
3. Restrained distances
 C20-N3 = N3A-C30
 1.4 with sigma of 0.02
 N3-N3A
 1.2 with sigma of 0.02
 O6-C9 = C9-O5
 1.2 with sigma of 0.02
 C9-C8
 1.4 with sigma of 0.02
 O6A-C9A = C9A-O5A
 1.2 with sigma of 0.02
 C9A-C8
 1.4 with sigma of 0.02
 C25-C22
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim
Ueq, Uanis(O6A) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C20, C30, N3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, C8, C9, C9A, O6A, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C15, C16, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C22, O15, N4, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.5) O6(0.5) O7(0.5) H7A(0.5) H7B(0.5) H15A(0.5) H15B(0.5)
 N3(0.5) N4(0.5) C9(0.5) C22(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 N3A(0.5) C9A(0.5) O6A(0.5) O5A(0.5) O7A(0.5) H7AA(0.5) H7AB(0.5)
7.a Riding coordinates:
 O7(H7A,H7B), O13(H13A,H13B), O15(H15A,H15B), O7A(H7AA,H7AB)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C13(H13), C14(H14), C17(H17), C19(H19), C21(H21),
 C28(H28), C29(H29)
7.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              15666
_shelx_hkl_checksum              89797
_shelx_fab_checksum              96990
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'