Synthesis and structural analysis of a ZIF-9/GO composite for green catalytic C–C bond formation and N-formylation: a spectroscopic study
Kumari, Lalita; Mittal, Rupali; Khurana, Mehak; Awasthi, Satish Kumar; RSC Advances 15 (2025) 19500–19514; doi:10.1039/D5RA02165K

data_7250535
_publ_section_title
;
 Synthesis and structural analysis of a ZIF-9/GO composite for green
 catalytic C--C bond formation and N-formylation: a spectroscopic study
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              19500
_journal_page_last               19514
_journal_paper_doi               10.1039/D5RA02165K
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C8 H5 N2 S'
_chemical_formula_sum            'C8 H5 N2 S'
_chemical_formula_weight         161.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2025-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.589(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6969(2)
_cell_length_b                   18.5921(8)
_cell_length_c                   7.4729(3)
_cell_measurement_reflns_used    7742
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2860
_cell_measurement_theta_min      3.5040
_cell_volume                     784.58(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.69a (Rigaku OD, 2022)'
_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_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.884
_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    -17.00  79.00   0.50    1.14    --    5.83  77.00  30.00  192
  2  \w    -23.00  38.00   0.50    1.14    --    5.83 -99.00-150.00  122
  3  \w    -23.00  38.00   0.50    1.14    --    5.83 -99.00-120.00  122
  4  \w    -23.00  38.00   0.50    1.14    --    5.83 -99.00  30.00  122
  5  \w    -23.00  38.00   0.50    1.14    --    5.83 -99.00 -30.00  122
  6  \w    -67.00 -36.00   0.50    1.14    --    5.83 -38.00 -90.00   62
  7  \w     -6.00  79.00   0.50    1.14    --    5.83  38.00 -30.00  170
  8  \w    -18.00  70.00   0.50    1.14    --   -5.68  19.00  60.00  176
  9  \w    -78.00   9.00   0.50    1.14    --   -5.68 -57.00 120.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1009513000
_diffrn_orient_matrix_UB_12      -0.0152858000
_diffrn_orient_matrix_UB_13      -0.0315752000
_diffrn_orient_matrix_UB_21      0.0007000000
_diffrn_orient_matrix_UB_22      0.0283649000
_diffrn_orient_matrix_UB_23      -0.0633444000
_diffrn_orient_matrix_UB_31      0.0747043000
_diffrn_orient_matrix_UB_32      0.0204192000
_diffrn_orient_matrix_UB_33      0.0645304000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17520
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.051
_diffrn_reflns_theta_min         3.517
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.69a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       needle
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0562
_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^)+(0.1292P)^2^+0.1258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1955
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1610
_reflns_number_total             2221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra02165k2.cif
_cod_data_source_block           ly-27_auto
_cod_database_code               7250535
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N S'
_chemical_oxdiff_usercomment     27.12.2022
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C8(H8)
;
_shelx_res_checksum              49253
_shelx_hkl_checksum              18571
_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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.619