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_7250534
_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         'C7 H5 F2 N O'
_chemical_formula_sum            'C7 H5 F2 N O'
_chemical_formula_weight         157.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2025-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.654(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.7817(3)
_cell_length_b                   13.1946(8)
_cell_length_c                   6.9708(5)
_cell_measurement_reflns_used    1227
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      29.5660
_cell_measurement_theta_min      4.6460
_cell_volume                     338.00(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.106a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.788
_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      8.00  40.00   0.50    1.51    --    5.69  83.00 -53.00   64
  2  \w     -3.00  76.00   0.50    1.51    --    5.69  38.00-180.00  158
  3  \w     -6.00  19.00   0.50    1.51    --    5.69 -83.00-174.00   50
  4  \w    -18.00  27.00   0.50    1.51    --   -5.53 -99.00  30.00   90
  5  \w     -3.00  24.00   0.50    1.51    --    5.69 -99.00  60.00   54
;
_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      -0.0759714000
_diffrn_orient_matrix_UB_12      0.0195548000
_diffrn_orient_matrix_UB_13      -0.0957645000
_diffrn_orient_matrix_UB_21      -0.0661487000
_diffrn_orient_matrix_UB_22      0.0426838000
_diffrn_orient_matrix_UB_23      0.0424756000
_diffrn_orient_matrix_UB_31      0.1646241000
_diffrn_orient_matrix_UB_32      0.0261301000
_diffrn_orient_matrix_UB_33      0.0019121000
_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  0.0235
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.788
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2166
_diffrn_reflns_point_group_measured_fraction_full 0.733
_diffrn_reflns_point_group_measured_fraction_max 0.547
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.895
_diffrn_reflns_theta_min         3.381
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.106a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       needle
_exptl_crystal_F_000             160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 273 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1169
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0410
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1191
_reflns_Friedel_coverage         0.375
_reflns_Friedel_fraction_full    0.470
_reflns_Friedel_fraction_max     0.301
_reflns_number_gt                1049
_reflns_number_total             1169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra02165k2.cif
_cod_data_source_block           la-15_auto
_cod_database_code               7250534
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 98.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N004(H004), C00A(H00A), C00B(H00B), C006(H006), C009(H009)
;
_shelx_res_checksum              21036
_shelx_hkl_checksum              93336
_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 1.527
_oxdiff_exptl_absorpt_empirical_full_min 0.533