Pd@BTL-Cd core-shell nanoparticles as plasmonic photocatalysts for the reductive amination of furfural in water.
Rohilla, Jyoti; Thakur, Sahil; Sharma, Sahil; Singh, Raghubir; Kaur, Varinder; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3645–3658; doi:10.1039/d4dt03058c

data_7717838
_publ_section_title
;
 Pd@BTL-Cd core-shell nanoparticles as plasmonic photocatalysts for the
 reductive amination of furfural in water.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3645
_journal_page_last               3658
_journal_paper_doi               10.1039/d4dt03058c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C27 H34 Cd2 Cl2 N4 O3, [+ solvents]'
_chemical_formula_sum            'C27 H34 Cd2 Cl2 N4 O3'
_chemical_formula_weight         758.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-26 deposited with the CCDC.	2025-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.9155(6)
_cell_length_b                   15.7883(3)
_cell_length_c                   8.7097(2)
_cell_measurement_reflns_used    18462
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5920
_cell_measurement_theta_min      3.4780
_cell_volume                     3701.19(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.31d (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.944
_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      9.00  35.00   0.50    8.00    --   -9.95  44.00 -33.00   52
  2  \w    -72.00 -25.00   0.50    8.00    --   -9.95 -44.00 175.00   94
  3  \w     25.00  52.00   0.50    8.00    --   10.22  44.00 -33.00   54
  4  \w    -14.00  11.00   0.50    8.00    --   10.22 -44.00 175.00   50
  5  \w    -28.00  53.00   0.50    8.00    --   -9.95  57.00  30.00  162
  6  \w    -42.00  -4.00   0.50    8.00    --   -9.95 125.00 -90.00   76
  7  \w    -21.00  60.00   0.50    8.00    --   -9.95  19.00 120.00  162
  8  \w     15.00  44.00   0.50    8.00    --   10.22-125.00 150.00   58
  9  \w    -43.00 -17.00   0.50    8.00    --   10.22 -77.00 150.00   52
 10  \w     11.00  36.00   0.50    8.00    --   10.22 -77.00 150.00   50
 11  \w     -3.00  43.00   0.50    8.00    --   10.22 -99.00  60.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0202908000
_diffrn_orient_matrix_UB_12      -0.0080307000
_diffrn_orient_matrix_UB_13      -0.0499053000
_diffrn_orient_matrix_UB_21      0.0158908000
_diffrn_orient_matrix_UB_22      -0.0233430000
_diffrn_orient_matrix_UB_23      -0.0493137000
_diffrn_orient_matrix_UB_31      -0.0055282000
_diffrn_orient_matrix_UB_32      -0.0375271000
_diffrn_orient_matrix_UB_33      0.0413372000
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31122
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.442
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.31d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 2121 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         7869
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0311P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                6156
_reflns_number_total             7869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03058c2.cif
_cod_data_source_block           vk-cd
_cod_depositor_comments
'Adding full bibliography for 7717838--7717839.cif.'
_cod_database_code               7717838
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Cd'
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.458
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C13, C12
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C8(H8A,H8B), C19(H19A,H19B), C7(H7A,H7B), C11(H11A,H11B),
 C12(H12A,H12B), C20(H20A,H20B), C9(H9A,H9B), C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C27(H27), C26(H26), C25(H25), C16(H16), C15(H15), C14(H14),
 C17(H17), C2(H2A), C3(H3A), C29(H29), C5(H5)
3.d Fitted hexagon refined as free rotating group:
 C24(C23,C22,C27,C26,C25), C16(C15,C14,C13,C18,C17), C1(C2,C3,C29,C5,C6)
3.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30198
_shelx_hkl_checksum              59169
_shelx_fab_checksum              73678
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.492