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_7058150
_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         'C25 H27 Co2 N5 O11.34'
_chemical_formula_sum            'C25 H27 Co2 N5 O11.34'
_chemical_formula_weight         696.88
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-06 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.880
_cell_length_b                   13.880
_cell_length_c                   45.438
_cell_measurement_reflns_used    2448
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.1368
_cell_measurement_theta_min      3.0629
_cell_volume                     8753.831
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.2375
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -78.00   10.50   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.6627  -38.0000 -120.0000 118
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0263610000
_diffrn_orient_matrix_UB_12      0.0156057000
_diffrn_orient_matrix_UB_13      -0.0124914000
_diffrn_orient_matrix_UB_21      0.0176907000
_diffrn_orient_matrix_UB_22      0.0398892000
_diffrn_orient_matrix_UB_23      0.0081332000
_diffrn_orient_matrix_UB_31      0.0400394000
_diffrn_orient_matrix_UB_32      -0.0278970000
_diffrn_orient_matrix_UB_33      0.0046218000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            18407
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.069
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_description       cone-shaped
_exptl_crystal_F_000             2854
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0913P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1765
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5842
_reflns_number_total             8258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05139a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7058150--7058152.cif.'
_cod_original_cell_volume        8753.8
_cod_database_code               7058150
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(4)
 0.47(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C20-C21
 2.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Co1, O9, O10, O11, N3, N4, N5, C17, C18, C19, C20, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, N1, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C22(H22A,H22B,H22C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11), C13(H13), C16(H16), C17(H17), C20(H20),
 C23(H23)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              45636
_shelx_hkl_checksum              36820
_shelx_fab_checksum              8740
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'