Friedländer, Knoevenagel, and Michael Reactions Employing the Same MOF: Synthesis, Structure, and Heterogeneous Catalytic Studies of ([Zn(1,4-NDCA)(3-BPDB)0.5]·(DMF)(MeOH) and [Cd4(1,4-NDCA)4(3-BPDB)4]·2(DMF)
Sarkar, Anupam; Mistry, Subhradeep; Natarajan, Srinivasan; The Journal of Physical Chemistry C 125 (2021) 27230–27240; doi:10.1021/acs.jpcc.1c08474

data_1565902
_publ_section_title
;
 Friedl\"ander, Knoevenagel, and Michael Reactions Employing the Same MOF:
 Synthesis, Structure, and Heterogeneous Catalytic Studies of
 ([Zn(1,4-NDCA)(3-BPDB)0.5]&#x00B7;(DMF)(MeOH) and
 [Cd4(1,4-NDCA)4(3-BPDB)4]&#x00B7;2(DMF)
;
_journal_issue                   49
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              27230
_journal_page_last               27240
_journal_paper_doi               10.1021/acs.jpcc.1c08474
_journal_volume                  125
_journal_year                    2021
_chemical_formula_moiety         'C18 H9 N2 O4 Zn'
_chemical_formula_sum            'C18 H9 N2 O4 Zn'
_chemical_formula_weight         382.66
_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   geom
_audit_creation_date             2015-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                93.653(3)
_cell_angle_beta                 109.577(4)
_cell_angle_gamma                97.147(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2597(4)
_cell_length_b                   10.8766(4)
_cell_length_c                   10.9289(5)
_cell_measurement_reflns_used    4852
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.5580
_cell_measurement_theta_min      3.0740
_cell_volume                     1132.87(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -46.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5962  -57.0000  -60.0000 81

  2 omega  -19.00   18.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2212  -99.0000  -30.0000 37

  3 omega  -19.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2212  -99.0000 -150.0000 38

  4 omega  -48.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5962  -57.0000 -180.0000 83

  5 omega  -49.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5962  -57.0000   60.0000 84

  6 omega  -18.00   19.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2212  -99.0000   90.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0007668000
_diffrn_orient_matrix_UB_12      0.0619067000
_diffrn_orient_matrix_UB_13      -0.0167699000
_diffrn_orient_matrix_UB_21      -0.0508758000
_diffrn_orient_matrix_UB_22      -0.0224671000
_diffrn_orient_matrix_UB_23      -0.0621561000
_diffrn_orient_matrix_UB_31      -0.0541082000
_diffrn_orient_matrix_UB_32      0.0061719000
_diffrn_orient_matrix_UB_33      0.0257175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.592
_diffrn_source                   'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.705
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0618
_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^)+(0.1287P)^2^+3.5105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.1924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3757
_reflns_number_total             3983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp1c08474_si_002.cif
_cod_data_source_block           I_Zn
_cod_database_code               1565902
_chemical_oxdiff_formula         'C12 H12 N2 O4 Zn2'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C4(0.5) H4(0.5) C7(0.5) H7(0.5) C5(0.5) H5(0.5) C8(0.5) H8(0.5)
 C20(0.5) H20(0.5) C18(0.5) H18(0.5) C21(0.5) H21(0.5) C22(0.5) H22(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C10(H10), C11(H11), C14(H14), C9(H9), C4(H4), C7(H7), C5(H5),
 C8(H8), C20(H20), C18(H18), C21(H21), C22(H22)
;
_shelx_res_checksum              18865
_shelx_hkl_checksum              72598
_shelx_fab_checksum              43959
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'