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_7058151
_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
'0.5(C240 H212 Mn24 N36 O128), H8 Mn1 O4, 2(C2 H8 N)+, 36H2O'
_chemical_formula_sum            'C124 H202 Mn13 N20 O104'
_chemical_formula_weight         4351.24
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-17
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2019.01.14 svn.r3558 for OlexSys, GUI svn.r5646)
;
_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                90
_cell_formula_units_Z            2
_cell_length_a                   22.5444(4)
_cell_length_b                   22.5444(4)
_cell_length_c                   22.5444(4)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.2539
_cell_measurement_theta_min      2.8514
_cell_volume                     11458.2(4)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 10.2375
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -32.00   55.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.6627   57.0000  -30.0000 87
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21484
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.985
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         2.857
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94449
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             4450
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0643P)^2^+4.8241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2803
_reflns_number_total             3364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj05139a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7058150--7058152.cif.'
_cod_original_cell_volume        11458.2(6)
_cod_database_code               7058151
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.89(5)
 0.11(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O1W \\sim O1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O1, N2, C1, C2, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Mn2, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O1(0.5) O1W(0.5) N2(0.5) C1(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 O7(0.3333) H7A(0.3333) H7B(0.3333) O12(0.5)
 Fixed Uiso: C3(0.1) O12(0.1)
6.a Rotating group:
 O7(H7A,H7B)
6.b Ternary CH refined with riding coordinates:
 O2(H2)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 679 electrons were 
found in a volume of 3967\%A^3 in 2 voids. 
This is consistent with the presence of 
2[(CH3)2NH2]+, 30[H2O] per formula unit 
which account for 704 electrons.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78338
_shelx_hkl_checksum              44773
_shelx_fab_checksum              30483
_olex2_submission_special_instructions 'No special instructions were received'