A Pd4L2 Cage Containing Brønsted-Base Active Sites for One-Pot Photooxidation/Knoevenagel Condensation Reaction
Zhou, Yan-Fang; Yan, Dan-Ni; Hu, Shao-Jun; Zhou, Lipeng; Cai, Li-Xuan; Sun, Qing-Fu; Dalton Transactions  (2023) –; doi:10.1039/D3DT00815K

data_7713039
_publ_section_title
;
 A Pd4L2 Cage Containing Br\/onsted-Base Active Sites for One-Pot
 Photooxidation/Knoevenagel Condensation Reaction
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00815K
_journal_year                    2023
_chemical_formula_moiety
'2(C112 H128 N32 Pd4), 5(F6 Si), 2(N O3) [+ solvent]'
_chemical_formula_sum            'C224 H256 F30 N66 O6 Pd8 Si5'
_chemical_formula_weight         5530.58
_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
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-05-08 deposited with the CCDC.	2023-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.463(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.7341(8)
_cell_length_b                   58.059(2)
_cell_length_c                   18.5454(7)
_cell_measurement_reflns_used    19204
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.3470
_cell_measurement_theta_min      2.2610
_cell_volume                     19340.8(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       72
_diffrn_reflns_limit_k_min       -72
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            129923
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.910
_diffrn_reflns_theta_min         2.138
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.950
_exptl_crystal_description       block
_exptl_crystal_F_000             5636
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.006
_refine_diff_density_max         2.078
_refine_diff_density_min         -2.652
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.482
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1528
_refine_ls_number_reflns         39474
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.485
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.1543
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3959
_refine_ls_wR_factor_ref         0.4092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26022
_reflns_number_total             39474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00815k2.cif
_cod_data_source_block           ydn597_sq_s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7713039
_shelx_shelxl_version_number     2019/3
_oxdiff_exptl_absorpt_empirical_full_min 0.310
_oxdiff_exptl_absorpt_empirical_full_max 3.555
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              27786
_shelx_hkl_checksum              66594
_shelx_fab_checksum              69252