Construction of ZnII/CdII-based MOFs containing a tripodal aromatic carboxylate ligand with unequal arms and their fluorescence detection for Cu2+ and Fe3+ cations
Huang, Gui-Mei; Li, Shuang; Ma, Meng-Xia; Li, Shi-Ming; Li, Wen-Qiang; Ni, Qing-Ling; Gui, Liu-Cheng; Wang, Xiu-Jian; CrystEngComm 25 (2023) 1232–1239; doi:10.1039/D3CE00007A

data_7246261
_publ_section_title
;
 Construction of ZnII/CdII-based MOFs containing a tripodal aromatic
 carboxylate ligand with unequal arms and their fluorescence detection for
 Cu2+ and Fe3+ cations
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1232
_journal_page_last               1239
_journal_paper_doi               10.1039/D3CE00007A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C88 H80 Cd3 N8 O14'
_chemical_formula_sum            'C88 H82 Cd3 N8 O15'
_chemical_formula_weight         1828.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-02 deposited with the CCDC.	2023-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 132.196(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.9381(7)
_cell_length_b                   9.43740(10)
_cell_length_c                   29.5532(5)
_cell_measurement_reflns_used    8071
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.886
_cell_measurement_theta_min      3.011
_cell_volume                     8045.7(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -36.00   1.00   0.50    1.00    --   43.18 -19.00-120.00   74
  2  \w     38.00  70.00   0.50    3.00    --  109.26 -61.00 -30.00   64
  3  \w     66.00 101.00   0.50    3.00    --  109.26 -77.00  30.00   70
  4  \w     44.00  70.00   0.50    3.00    --  109.26 -61.00  90.00   52
  5  \w     35.00  73.00   0.50    3.00    --  109.26 -62.00  24.00   76
  6  \w     35.00  60.00   0.50    3.00    --  109.26 -61.00  60.00   50
  7  \w     38.00  70.00   0.50    3.00    --  109.26 -61.00 120.00   64
  8  \w     37.00 111.00   0.50    3.00    --  109.26-125.00  30.00  148
  9  \w     88.00 174.00   0.50    3.00    --  109.26  45.00 120.00  172
 10  \w    125.00 175.00   0.50    3.00    --  109.26 125.00   0.00  100
 11  \w     96.00 175.00   0.50    3.00    --  109.26  62.00 161.00  158
 12  \w     95.00 120.00   0.50    3.00    --  109.26 125.00   0.00   50
 13  \w     88.00 138.00   0.50    3.00    --  109.26  61.00 -90.00  100
 14  \w     87.00 172.00   0.50    3.00    --  109.26  61.00  90.00  170
 15  \w    -51.00 -14.00   0.50    3.00    --  -90.25  45.00   0.00   74
 16  \w    -51.00 -22.00   0.50    3.00    --  -90.25  45.00 -60.00   58
 17  \w   -109.00 -20.00   0.50    1.00    --  -43.18 -62.00  24.00  178
 18  \w    -63.00  31.00   0.50    1.00    --  -43.18  62.00 161.00  188
 19  \w   -119.00 -92.00   0.50    3.00    --  -90.25 -94.00 120.00   54
 20  \w   -140.00-115.00   0.50    3.00    --  -90.25 -62.00  24.00   50
 21  \w   -158.00-132.00   0.50    3.00    --  -90.25 -94.00 120.00   52
 22  \w    -73.00 -48.00   0.50    3.00    --  -90.25  62.00 161.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0387652000
_diffrn_orient_matrix_UB_12      -0.0063514000
_diffrn_orient_matrix_UB_13      -0.0014981000
_diffrn_orient_matrix_UB_21      0.0262209000
_diffrn_orient_matrix_UB_22      0.1188866000
_diffrn_orient_matrix_UB_23      0.0481249000
_diffrn_orient_matrix_UB_31      0.0257360000
_diffrn_orient_matrix_UB_32      -0.1116858000
_diffrn_orient_matrix_UB_33      0.0513018000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            24756
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.886
_diffrn_reflns_theta_min         3.011
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21297
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   0.409
_exptl_transmission_factor_min   0.333
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         8071
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+4.1238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7518
_reflns_number_total             8071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00007a3.cif
_cod_data_source_block           20210409-wxj-ls-557-cd-bib
_cod_depositor_comments
'Adding full bibliography for 7246258--7246261.cif.'
_cod_database_code               7246261
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C360 H312 Cd12 N40 O48 '
_shelx_estimated_absorpt_t_max   1.00000
_shelx_estimated_absorpt_t_min   0.21297
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C3
 1.23 with sigma of 0.02
 C7-N5
 1.459 with sigma of 0.005
 C6-N5
 1.459 with sigma of 0.005
 N5-C6 = N5-C7
 1.46 with sigma of 0.02
 C3-O2
 1.22 with sigma of 0.005
 C3-C4
 1.497 with sigma of 0.005
 C3-N5
 1.322 with sigma of 0.005
 O2-N5
 2.22 with sigma of 0.04
 O2-C4
 2.37 with sigma of 0.04
 C3-C6 = C3-C7
 2.45 with sigma of 0.04
 Cd01-O2 \\sim Cd01-O2A
 with sigma of 0.02
 C3-C6 \\sim C3A-C6A
 with sigma of 0.04
 O2-C3 \\sim O2A-C3A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.04
 C4-N5 \\sim C4A-N5A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 O2-N5 \\sim O2A-N5A
 with sigma of 0.04
 C3-C7 \\sim C3A-C7A
 with sigma of 0.04
 N5-C6 \\sim N5A-C6A
 with sigma of 0.02
 N5-C7 \\sim N5A-C7A
 with sigma of 0.02
 C3-N5 \\sim C3A-N5A
 with sigma of 0.02
 Cd01-C3 \\sim Cd01-C3A
 with sigma of 0.04
 O2-C4 \\sim O2A-C4A
 with sigma of 0.04
3. Restrained planarity
 O2, C3, C4, N5, C6, C7
 with sigma of 0.1
4. Others
 Sof(N5A)=Sof(C6A)=Sof(H6Aa)=Sof(H6Ab)=Sof(H6Ac)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=
 Sof(H4Ac)=Sof(C3A)=Sof(O2A)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=Sof(H7Ac)=1-FVAR(1)
 Sof(O2)=Sof(C3)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(H4c)=Sof(N5)=Sof(C6)=Sof(H6a)=
 Sof(H6b)=Sof(H6c)=Sof(C7)=Sof(H7a)=Sof(H7b)=Sof(H7c)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C00W(H00a,H00b), C011(H01a,H01b), C01E(H01g,H01h), C01F(H01i,H01j)
5.b Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00K(H00K), C00L(H00L), C00M(H00M), C00O(H00O), C00P(H00P),
 C00S(H00S), C00V(H00V), C00Y(H00Y), C00Z(H00Z), C010(H010), C012(H012),
 C013(H013), C014(H014), C015(H015), C016(H016), C017(H017), C018(H018),
 C01A(H01c), C01B(H01d), C01C(H01e), C01D(H01f), C01G(H01k)
5.c Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C6A(H6Aa,H6Ab,H6Ac),
 C4A(H4Aa,H4Ab,H4Ac), C7A(H7Aa,H7Ab,H7Ac)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 36 electrons were 
found in a volume of 280\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.9[H2O] per Asymmetric Unit 
which account for 40 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.991
_oxdiff_exptl_absorpt_empirical_full_min 0.562