A metal-organic cage-based nanoagent for enhanced photodynamic antitumor therapy.
Li, Wen-Yan; Zhao, Chao-Wei; Zhang, Yue-Feng; Guan, Qun; Wan, Jing-Jing; Ma, Jian-Ping; Li, Yan-An; Dong, Yu-Bin; Chemical communications (Cambridge, England) 57 (2021) 7954–7957; doi:10.1039/d1cc02629a

data_7128634
_publ_section_title
;
 A metal-organic cage-based nanoagent for enhanced photodynamic antitumor
 therapy.
;
_journal_issue                   64
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7954
_journal_page_last               7957
_journal_paper_doi               10.1039/d1cc02629a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C264 H224 N72 O24 Pd6, 4(N O3)'
_chemical_formula_sum            'C264 H224 N76 O36 Pd6'
_chemical_formula_weight         5675.58
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.5568(17)
_cell_length_b                   28.5568(17)
_cell_length_c                   28.6245(15)
_cell_measurement_reflns_used    6413
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      56.8590
_cell_measurement_theta_min      3.7820
_cell_volume                     23343(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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     33.00  69.00   1.00   10.00    --    0.00  57.00   0.00   36
  2  \w    -32.00  19.00   1.00   10.00    --    0.00  99.00 129.00   51
  3  \w     -2.00  51.00   1.00   10.00    --    0.00  57.00 -90.00   53
  4  \w     -1.00  28.00   1.00   10.00    --    0.00  57.00   0.00   29
  5  \w     25.00  95.00   1.00   12.50    --   54.00  77.00  60.00   70
  6  \w      1.00  96.00   1.00   12.50    --   54.00 -99.00 150.00   95
  7  \w     46.00 108.00   1.00   12.50    --   54.00  57.00-150.00   62
  8  \w     64.00  91.00   1.00   12.50    --   54.00  37.00-180.00   27
  9  \w     37.00 124.00   1.00   12.50    --   54.00  37.00 -60.00   87
 10  \w     39.00 107.00   1.00   12.50    --   54.00  57.00   0.00   68
 11  \w     39.00 106.00   1.00   12.50    --   54.00-125.00 -30.00   67
 12  \w     38.00 130.00   1.00   12.50    --  108.00 -50.00 120.00   92
 13  \w    152.00 178.00   1.00   12.50    --  108.00  25.00 -60.00   26
 14  \w     75.00 147.00   1.00   12.50    --  108.00  25.00 -60.00   72
 15  \w     39.00 113.00   1.00   12.50    --  108.00-111.00  90.00   74
 16  \w     47.00 141.00   1.00   12.50    --  108.00 -91.00 120.00   94
 17  \w     89.00 139.00   1.00   12.50    --  108.00  77.00 -30.00   50
 18  \w    125.00 152.00   1.00   12.50    --  108.00  25.00  90.00   27
 19  \w     78.00 105.00   1.00   12.50    --  108.00  25.00  90.00   27
 20  \w     81.00 115.00   1.00   12.50    --  108.00-111.00 -30.00   34
 21  \w    104.00 177.00   1.00   12.50    --  108.00 111.00 150.00   73
 22  \w     81.00 114.00   1.00   12.50    --  108.00-111.00-120.00   33
 23  \w     36.00  63.00   1.00   12.50    --  108.00-111.00 -30.00   27
 24  \w     43.00 122.00   1.00   12.50    --  108.00 -63.00-120.00   79
 25  \w     41.00 111.00   1.00   12.50    --  108.00 -37.00  30.00   70
 26  \w     91.00 178.00   1.00   12.50    --  108.00  37.00-150.00   87
 27  \w    100.00 141.00   1.00   12.50    --  108.00 111.00  90.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0153065000
_diffrn_orient_matrix_UB_12      -0.0068128000
_diffrn_orient_matrix_UB_13      0.0423317000
_diffrn_orient_matrix_UB_21      0.0101109500
_diffrn_orient_matrix_UB_22      0.0249019500
_diffrn_orient_matrix_UB_23      0.0014020000
_diffrn_orient_matrix_UB_31      -0.0197841000
_diffrn_orient_matrix_UB_32      0.0075991000
_diffrn_orient_matrix_UB_33      0.0334305000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1256
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            76610
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.298
_diffrn_reflns_theta_min         3.785
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.807
_exptl_crystal_description       block
_exptl_crystal_F_000             5808
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
TITL 1_a.res in C2/m New: P4/m New: I4/m
CELL   28.5568   28.5568   28.6245     90.00     90.00     90.00
SPGR I4/m
C101 0.698 0.195 0.002 !       9.26 eA-3
C102 0.500 0.500 0.000 !       8.14 eA-3
C103 0.878 0.754 0.044 !       6.47 eA-3
C104 0.375 0.453-0.001 !       6.40 eA-3
C105 0.304 0.383 0.002 !       6.25 eA-3
C106 0.175 0.430 0.002 !       5.67 eA-3
C107 0.500 0.496 0.250 !       5.40 eA-3
C108 0.859 0.211 0.001 !       4.93 eA-3
C109 0.181 0.117 0.002 !       4.11 eA-3
C110 0.961 0.391-0.001 !       3.78 eA-3
Q111 0.507 0.150 0.070 !       3.65 eA-3
C112 0.571 0.350 0.123 !       3.38 eA-3
C113 0.328 0.441 0.089 !       3.32 eA-3
C114 0.454 0.484-0.001 !       3.30 eA-3
C115 0.874 0.141 0.003 !       3.26 eA-3
C116 0.884 0.477 0.001 !       3.25 eA-3
C117 0.997 0.445 0.088 !       2.66 eA-3
C118 0.878 0.491 0.040 !       2.56 eA-3
C119 0.157 0.250 0.002 !       2.55 eA-3
C120 0.922 0.195 0.001 !       2.52 eA-3
C121 0.906 0.785 0.176 !       2.46 eA-3
C122 0.730 0.548 0.092 !       2.45 eA-3
C123 0.686 0.016-0.001 !       2.36 eA-3
C124 0.640 0.336 0.227 !       2.32 eA-3
C125 0.883 0.014 0.213 !       2.15 eA-3
C126 0.945 0.767 0.148 !       2.15 eA-3
C127 0.829 0.888 0.125 !       2.11 eA-3
C128 0.143 0.824 0.125 !       2.06 eA-3
C129 0.895 0.032 0.184 !       1.95 eA-3
C130 0.327 0.663 0.211 !       1.87 eA-3
C131 0.025 0.351-0.002 !       1.85 eA-3
C132 0.655 0.593 0.246 !       1.82 eA-3
C133 0.028 0.244 0.115 !       1.75 eA-3
C134 0.991 0.367 0.000 !       1.73 eA-3
C135 0.055 0.187 0.001 !       1.53 eA-3
C136 0.062 0.398 0.002 !       1.53 eA-3
C137 0.509 0.164 0.000 !       1.50 eA-3
C138 0.841 0.500 0.026 !       1.41 eA-3
C139 0.014 0.510 0.151 !       1.36 eA-3
C140 0.564 0.328 0.001 !       1.30 eA-3
C141 0.059 0.981 0.073 !       1.28 eA-3
C142 0.500 0.998 0.023 !       1.25 eA-3
C143 0.439 0.673 0.033 !       1.23 eA-3
C144 0.107 0.970 0.145 !       1.22 eA-3
C145 0.031 0.501 0.171 !       1.21 eA-3
C146 0.200 0.106 0.150 !       1.18 eA-3
C147 0.956 0.078 0.000 !       1.16 eA-3
C148 0.077 0.242 0.001 !       1.15 eA-3
Q149 0.226 0.999 0.204 !       1.15 eA-3
C150 1.000 0.499 0.172 !       1.14 eA-3
C151 0.942 0.157 0.107 !       1.11 eA-3
Q152 0.751 0.336 0.002 !       1.11 eA-3
Q153 0.328 0.219-0.004 !       1.10 eA-3
Q154 0.515 0.529 0.137 !       1.09 eA-3
Q155 0.431 0.297-0.001 !       1.08 eA-3
C156 0.477 0.030 0.128 !       1.08 eA-3
C157 0.870 0.141 0.126 !       1.05 eA-3
C158 0.936 0.039 0.165 !       1.04 eA-3
C159 0.062 0.928 0.014 !       1.03 eA-3
Q160 0.361 0.344 0.002 !       1.03 eA-3
C161 0.056 0.979 0.174 !       1.02 eA-3
Q162 0.998 0.373 0.122 !       1.01 eA-3
C163 0.028 0.170 0.016 !       0.99 eA-3
Q164 0.312 0.148-0.001 !       0.98 eA-3
C165 0.030 0.250 0.000 !       0.98 eA-3
C166 1.000 0.500 0.203 !       0.97 eA-3
C167 0.182 0.899 0.097 !       0.95 eA-3
C168 0.986 0.250-0.003 !       0.94 eA-3
C169 0.494 0.055 0.000 !       0.94 eA-3
Q170 0.695 0.598 0.172 !       0.93 eA-3
C171 0.928 0.046 0.180 !       0.93 eA-3
C172 0.932 0.188 0.151 !       0.93 eA-3
C173 0.021 0.998 0.185 !       0.90 eA-3
C174 0.944 0.936 0.201 !       0.89 eA-3
C175 0.887 0.800 0.158 !       0.87 eA-3
C176 0.135 0.287 0.012 !       0.87 eA-3
C177 0.943 0.952 0.169 !       0.87 eA-3
Q178 0.344 0.172 0.000 !       0.86 eA-3
C179 0.804 0.910 0.178 !       0.86 eA-3
C180 0.802 0.064 0.148 !       0.82 eA-3
C181 0.568 0.990 0.028 !       0.81 eA-3
Q182 0.817 0.313 0.116 !       0.80 eA-3
C183 0.905 0.219 0.163 !       0.80 eA-3
C184 0.222 0.992 0.003 !       0.79 eA-3
Q185 0.679 0.289 0.001 !       0.79 eA-3
C186 0.761 0.006 0.053 !       0.77 eA-3
Q187 0.383 0.109 0.001 !       0.77 eA-3
C188 0.345 0.431 0.177 !       0.77 eA-3
Q189 0.503 0.195 0.000 !       0.76 eA-3
C190 0.074 0.063 0.165 !       0.76 eA-3
C191 0.517 0.063-0.002 !       0.75 eA-3
C192 0.889 0.813 0.131 !       0.74 eA-3
Q193 0.390 0.305 0.003 !       0.74 eA-3
C194 0.788 0.542 0.086 !       0.73 eA-3
Q195 0.424 0.211 0.002 !       0.73 eA-3
C196 0.548 0.978 0.018 !       0.73 eA-3
C197 0.407 0.492 0.002 !       0.72 eA-3
Q198 0.209 0.043 0.204 !       0.72 eA-3
C199 0.906 0.979 0.225 !       0.71 eA-3
;
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         11419
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.1005
_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^)+(0.1628P)^2^+83.6397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2901
_refine_ls_wR_factor_ref         0.3516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6166
_reflns_number_total             11419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02629a2.cif
_cod_data_source_block           5_sq
_cod_depositor_comments          'Adding full bibliography for 7128634.cif.'
_cod_original_cell_volume        23343(3)
_cod_database_code               7128634
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.607
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C15A, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C14(H14C,H14D), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B)
4.b Me refined with riding coordinates:
 C15A(H15A,H15B,H15C), C15(H15D,H15E,H15F)
4.c Aromatic/amide H refined with riding coordinates:
 N7(H7), C1(H1), C2(H2), C4(H4), C5(H5), C23(H23), C24(H24), C25(H25),
 C26(H26), C30(H30), C31(H31), C32(H32), C33(H33)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.822
_oxdiff_exptl_absorpt_empirical_full_min 0.606