Metal–organic frameworks constructed using acid–base mixed ligands, carboxylic acids and N-containing chalcone, and their catalytic performance for Knoevenagel condensation
Cheng, Limin; Zhang, Junyong; Zhan, Caihong; Xu, Hao; Gong, Chunhua; Xie, Jingli; New Journal of Chemistry 48 (2024) 8597–8602; doi:10.1039/D3NJ05164A

data_7063120
_publ_section_title
;
 Metal--organic frameworks constructed using acid--base mixed ligands,
 carboxylic acids and N-containing chalcone, and their catalytic
 performance for Knoevenagel condensation
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8597
_journal_page_last               8602
_journal_paper_doi               10.1039/D3NJ05164A
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C42 H29 Cd N5 O7, 1(C3 H7 N O)'
_chemical_formula_sum            'C45 H36 Cd N6 O8'
_chemical_formula_weight         901.20
_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     iterative
_audit_creation_date             2023-09-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-13 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                114.157(10)
_cell_angle_beta                 95.733(9)
_cell_angle_gamma                94.009(9)
_cell_formula_units_Z            2
_cell_length_a                   8.7214(9)
_cell_length_b                   15.1141(14)
_cell_length_c                   17.2898(19)
_cell_measurement_reflns_used    1150
_cell_measurement_temperature    300
_cell_measurement_theta_max      71.5110
_cell_measurement_theta_min      5.2060
_cell_volume                     2053.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.959
_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    -30.00  64.00   1.00    2.50    --   36.83 -77.00-180.00   94
  2  \w      9.00 100.00   1.00    2.50    --   36.83  19.00 120.00   91
  3  \w      1.00  76.00   1.00    2.50    --   36.83 -99.00 120.00   75
  4  \w     10.00 104.00   1.00    2.50    --   36.83  77.00 -60.00   94
  5  \w     57.00 103.00   1.00    2.50    --   36.83 178.00 120.00   46
  6  \w     50.00 102.00   1.00   10.00    --  108.00-111.00  30.00   52
  7  \w     87.00 173.00   1.00   10.00    --  108.00  30.00-120.00   86
  8  \w     38.00 110.00   1.00   10.00    --  108.00 -99.00-122.00   72
  9  \w     40.00 124.00   1.00   10.00    --  108.00 -30.00-180.00   84
 10  \w     41.00 126.00   1.00   10.00    --  108.00 -61.00  90.00   85
 11  \w     38.00 115.00   1.00   10.00    --  108.00 -30.00 -90.00   77
 12  \w     39.00  95.00   1.00   10.00    --  108.00 -95.00 -60.00   56
 13  \w     38.00 113.00   1.00   10.00    --  108.00-111.00 120.00   75
 14  \w    120.00 173.00   1.00   10.00    --  108.00 111.00-180.00   53
 15  \w     47.00 146.00   1.00   10.00    --  108.00 -15.00  30.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180428000
_diffrn_orient_matrix_UB_12      0.0803839000
_diffrn_orient_matrix_UB_13      -0.0326896000
_diffrn_orient_matrix_UB_21      -0.0301555000
_diffrn_orient_matrix_UB_22      0.0764835000
_diffrn_orient_matrix_UB_23      0.0871871000
_diffrn_orient_matrix_UB_31      0.1753808000
_diffrn_orient_matrix_UB_32      0.0188892000
_diffrn_orient_matrix_UB_33      0.0325578000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.1450
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11681
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.179
_diffrn_reflns_theta_min         5.112
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         7754
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5157
_reflns_number_total             7754
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj05164a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7063120--7063122.cif.'
_cod_database_code               7063120
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.576
_shelx_estimated_absorpt_t_min   0.480
_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, All O(H) groups
2. Restrained distances
 O8-C41
 1.2164 with sigma of 0.01
 N6-C42 = N6-C43
 1.45 with sigma of 0.01
 N6-C41
 1.3625 with sigma of 0.01
 C41-C43
 2.45 with sigma of 0.02
 O8-C42
 2.828 with sigma of 0.02
 C42-C41
 2.45 with sigma of 0.02
 N6-O8
 2.2984 with sigma of 0.02
 C41-C43 \\sim C41A-C43A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 N6-C43 \\sim N6A-C43A
 with sigma of 0.02
 N6A-C42A \\sim N6-C42
 with sigma of 0.02
 O8-N6 \\sim O8A-N6A
 with sigma of 0.02
 O8-C41 \\sim O8A-C41A
 with sigma of 0.02
 N6-C41 \\sim N6A-C41A
 with sigma of 0.02
3. Restrained planarity
 C41, N6, C43, C42
 with sigma of 0.1
 C41A, N6A, C42A, C43A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O8 \\sim C41 \\sim N6 \\sim C43 \\sim C42 \\sim N6A \\sim O8A \\sim C41A \\sim
C43A \\sim C42A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O8) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(N6A) \\sim Ueq, Uanis(O8A) \\sim Ueq,
Uanis(C41A) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(C42A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 O8, C41, N6, C43, C42, N6A, O8A, C41A, C43A, C42A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(N6A)=Sof(O8A)=Sof(C41A)=Sof(H41A)=Sof(C43A)=Sof(H43d)=Sof(H43e)=Sof(H43f)=
 Sof(C42A)=Sof(H42d)=Sof(H42e)=Sof(H42f)=1-FVAR(1)
 Sof(O8)=Sof(C41)=Sof(H41)=Sof(N6)=Sof(C43)=Sof(H43a)=Sof(H43b)=Sof(H43c)=
 Sof(C42)=Sof(H42a)=Sof(H42b)=Sof(H42c)=FVAR(1)
7.a Riding coordinates:
 C43(H43a,H43b,H43c), C42(H42a,H42b,H42c)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C12(H12a,H12b), C11(H11a,H11b)
7.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C15(H15), C30(H30), C22(H22), C29(H29), C6(H6), C33(H33), C5(H5),
 C1(H1), C16(H16), C34(H34), C25(H25), C18(H18), C46(H46), C13(H13), C17(H17),
 C45(H45), C3(H3), C24(H24), C38(H38), C2(H2), C37(H37), C41(H41), C41A(H41A)
7.d Idealised Me refined as rotating group:
 C43A(H43d,H43e,H43f), C42A(H42d,H42e,H42f)
7.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              98786
_shelx_hkl_checksum              92615
_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 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.757