Two porous three-dimensional (3D) metal–organic frameworks based on diverse metal clusters: selective sensing of Fe3+ and Cr2O72−
Yan, Yang-Tian; Wu, Yun-long; Zheng, Li-Na; Wei-Cai,; Tang, Peng-Fei; Wu, Wei-Ping; Zhang, Wen-Yan; Wang, Yao-Yu; New Journal of Chemistry 46 (2022) 4292–4299; doi:10.1039/D1NJ06217D

data_7061205
_publ_section_title
;
 Two porous three-dimensional (3D) metal--organic frameworks based on
 diverse metal clusters: selective sensing of Fe3+ and Cr2O72&#x2212;
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4292
_journal_page_last               4299
_journal_paper_doi               10.1039/D1NJ06217D
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety
'C46 H20 O22 Zn5, 2(C2 H8 N), 3[C3H7NO], 4[H2O]'
_chemical_formula_sum            'C59 H65 N5 O29 Zn5'
_chemical_formula_weight         1635.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-15
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-16 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                84.243(3)
_cell_angle_beta                 85.337(3)
_cell_angle_gamma                78.012(3)
_cell_formula_units_Z            1
_cell_length_a                   12.153(2)
_cell_length_b                   12.643(3)
_cell_length_c                   12.690(3)
_cell_measurement_reflns_used    5468
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.373
_cell_measurement_theta_min      3.23
_cell_volume                     1894.0(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.912
_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_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8710
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.454
_diffrn_reflns_theta_min         1.616
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.640
_exptl_absorpt_correction_T_max  0.8217
_exptl_absorpt_correction_T_min  0.7044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0576 before and 0.0398 after correction. The Ratio of minimum to maximum transmission is 0.8568. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         8710
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+2.5149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1774
_refine_ls_wR_factor_ref         0.1913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7272
_reflns_number_total             8710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj06217d2.cif
_cod_data_source_block           1_tw_sq
_cod_depositor_comments
'Adding full bibliography for 7061204--7061205.cif.'
_cod_original_cell_volume        1894.1(7)
_cod_database_code               7061205
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.828
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.867(2)
 0.133(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Restrained distances
 H3-O3
 0.82 with sigma of 0.02
 C25-N1 = N1-C24
 1.4 with sigma of 0.02
 C25-C24
 2.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N1, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O3(H3), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C15(H15), C16(H16),
 C23(H23)
;
_shelx_res_checksum              68240
_shelx_fab_checksum              13002
_platon_squeeze_special_details
;
A solvent mask was calculated and 82 electrons were 
found in a volume of 776\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[H2O], 1.5[C3H7NO], per Asymmetric Unit 
which account for 160 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'