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_7246260
_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         'C94 H68 Cd3 N6 O12'
_chemical_formula_sum            'C94 H68 Cd3 N6 O12'
_chemical_formula_weight         1810.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-12-20
_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                 91.899(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.0745(5)
_cell_length_b                   9.7503(2)
_cell_length_c                   29.6517(5)
_cell_measurement_reflns_used    8835
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1590
_cell_measurement_theta_min      4.0040
_cell_volume                     7823.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.872
_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    -42.00  48.00   1.00    5.00    --   17.69 -77.00 120.00   90
  2  \w     -4.00  86.00   1.00    5.00    --   17.69  57.00  60.00   90
  3  \w    -51.00  39.00   1.00    5.00    --   17.69 -57.00 -60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0056806000
_diffrn_orient_matrix_UB_12      -0.0074865000
_diffrn_orient_matrix_UB_13      0.0233898000
_diffrn_orient_matrix_UB_21      0.0253143000
_diffrn_orient_matrix_UB_22      -0.0091407000
_diffrn_orient_matrix_UB_23      -0.0047155000
_diffrn_orient_matrix_UB_31      0.0038163000
_diffrn_orient_matrix_UB_32      0.0717569000
_diffrn_orient_matrix_UB_33      0.0018494000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            20974
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.706
_diffrn_reflns_theta_min         3.330
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         8820
_refine_ls_number_restraints     948
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0249P)^2^+4.2186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6947
_reflns_number_total             8820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00007a3.cif
_cod_data_source_block           557-cd-yixi-dmf-1_auto
_cod_depositor_comments
'Adding full bibliography for 7246258--7246261.cif.'
_cod_database_code               7246260
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C41A-C38A = C43-C42 = C43A-C42A = C41-C38
 1.5 with sigma of 0.01
 C42-C41 = C42A-C41A
 1.34 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 N2, C40, C42, N1, C37, C45, C36, C46, C38, C44, C39, C43, C41, C47, Cd1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C42A, C38A, C40A, C46A, N1A, C39A, C44A, C45A, N2A, C37A, C47A, C43A, C41A,
 C36A, Cd1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C42A)=Sof(H42A)=Sof(N2A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=
 Sof(C43A)=Sof(C44A)=Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(N1A)=Sof(C36A)=Sof(H36A)=
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=
 Sof(C41A)=Sof(H41A)=1-FVAR(1)
 Sof(N2)=Sof(C45)=Sof(H45)=Sof(C44)=Sof(H44)=Sof(C43)=Sof(C47)=Sof(H47)=
 Sof(C46)=Sof(H46)=Sof(N1)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C42)=Sof(H42)=Sof(C41)=Sof(H41)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C8(H8A,H8B)
6.b Aromatic/amide H refined with riding coordinates:
 C45(H45), C44(H44), C47(H47), C46(H46), C36(H36), C37(H37), C39(H39),
 C40(H40), C25(H25), C7(H7), C24(H24), C3(H3), C6(H6), C27(H27), C5(H5),
 C13(H13), C14(H14), C30(H30), C11(H11), C10(H10), C33(H33), C31(H31), C28(H28),
  C16(H16), C19(H19), C32(H32), C17(H17), C18(H18), C42(H42), C41(H41),
 C42A(H42A), C46A(H46A), C47A(H47A), C44A(H44A), C45A(H45A), C36A(H36A),
 C37A(H37A), C39A(H39A), C40A(H40A), C41A(H41A)
;
_shelx_res_checksum              65558
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.863