Post-synthetic modification of amine-functionalized permanently porous coordination cages.
Hoq, Jahidul; Dworzak, Michael R.; Dissanayake, Duleeka; Skalla, Rebecca X.; Yamamoto, Nobuyuki; Yap, Glenn P. A.; Bloch, Eric D.; Chemical communications (Cambridge, England) 61 (2025) 1641–1644; doi:10.1039/d4cc04370g

data_7134034
_publ_section_title
;
 Post-synthetic modification of amine-functionalized permanently porous
 coordination cages.
;
_journal_issue                   8
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1641
_journal_page_last               1644
_journal_paper_doi               10.1039/d4cc04370g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C16 H14 Cl2 N2 O4 Pd'
_chemical_formula_sum            'C16 H14 Cl2 N2 O4 Pd'
_chemical_formula_weight         475.59
_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             2022-09-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-08-23 deposited with the CCDC.	2024-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.597(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1543(12)
_cell_length_b                   8.5115(8)
_cell_length_c                   16.4253(15)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      66.66
_cell_measurement_theta_min      3.59
_cell_volume                     1721.5(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Venture Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17566
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        66.651
_diffrn_reflns_theta_max         66.651
_diffrn_reflns_theta_min         3.589
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.778
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4010
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1257 before and 0.0757 after correction.
The Ratio of minimum to maximum transmission is 0.5327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0193P)^2^+5.7849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2686
_reflns_number_total             2935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04370g2.cif
_cod_data_source_block           eric685
_cod_depositor_comments
'Adding full bibliography for 7134033--7134034.cif.'
_cod_database_code               7134034
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.608
_shelx_estimated_absorpt_t_min   0.289
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1C,H1B), C10(H10A,H10C,H10B)
;
_shelx_res_checksum              32379
_shelx_hkl_checksum              8938
_olex2_submission_special_instructions 'No special instructions were received'