 
data_Pd6L8
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C264 H192 N24 O16 P4 Pd3'
_chemical_formula_sum
 'C264 H192 N24 O16 P4 Pd3' 
_chemical_formula_weight          4399.50

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0137   0.0067
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'F'  'F'   0.0583   0.0400
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0241   0.0134
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0389   0.0241
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2543   0.3332
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd'  'Pd'   0.0375   3.1039
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B'  'B'   0.0070   0.0029
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       cubic
_space_group_IT_number            225
_space_group_name_H-M_alt         'F m -3 m'
_space_group_name_Hall            '-F 4 2 3'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'y, x, -z'
 '-y, -x, -z'
 'y, -x, z'
 '-y, x, z'
 'x, z, -y'
 '-x, z, y'
 '-x, -z, -y'
 'x, -z, y'
 'z, y, -x'
 'z, -y, x'
 '-z, y, x'
 '-z, -y, -x'
 'x, y+1/2, z+1/2'
 '-x, -y+1/2, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x, -y+1/2, -z+1/2'
 'z, x+1/2, y+1/2'
 'z, -x+1/2, -y+1/2'
 '-z, -x+1/2, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z+1/2, x+1/2'
 '-y, z+1/2, -x+1/2'
 'y, -z+1/2, -x+1/2'
 '-y, -z+1/2, x+1/2'
 'y, x+1/2, -z+1/2'
 '-y, -x+1/2, -z+1/2'
 'y, -x+1/2, z+1/2'
 '-y, x+1/2, z+1/2'
 'x, z+1/2, -y+1/2'
 '-x, z+1/2, y+1/2'
 '-x, -z+1/2, -y+1/2'
 'x, -z+1/2, y+1/2'
 'z, y+1/2, -x+1/2'
 'z, -y+1/2, x+1/2'
 '-z, y+1/2, x+1/2'
 '-z, -y+1/2, -x+1/2'
 'x+1/2, y, z+1/2'
 '-x+1/2, -y, z+1/2'
 '-x+1/2, y, -z+1/2'
 'x+1/2, -y, -z+1/2'
 'z+1/2, x, y+1/2'
 'z+1/2, -x, -y+1/2'
 '-z+1/2, -x, y+1/2'
 '-z+1/2, x, -y+1/2'
 'y+1/2, z, x+1/2'
 '-y+1/2, z, -x+1/2'
 'y+1/2, -z, -x+1/2'
 '-y+1/2, -z, x+1/2'
 'y+1/2, x, -z+1/2'
 '-y+1/2, -x, -z+1/2'
 'y+1/2, -x, z+1/2'
 '-y+1/2, x, z+1/2'
 'x+1/2, z, -y+1/2'
 '-x+1/2, z, y+1/2'
 '-x+1/2, -z, -y+1/2'
 'x+1/2, -z, y+1/2'
 'z+1/2, y, -x+1/2'
 'z+1/2, -y, x+1/2'
 '-z+1/2, y, x+1/2'
 '-z+1/2, -y, -x+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, -z'
 'z+1/2, x+1/2, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x+1/2, y'
 '-z+1/2, x+1/2, -y'
 'y+1/2, z+1/2, x'
 '-y+1/2, z+1/2, -x'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z+1/2, x'
 'y+1/2, x+1/2, -z'
 '-y+1/2, -x+1/2, -z'
 'y+1/2, -x+1/2, z'
 '-y+1/2, x+1/2, z'
 'x+1/2, z+1/2, -y'
 '-x+1/2, z+1/2, y'
 '-x+1/2, -z+1/2, -y'
 'x+1/2, -z+1/2, y'
 'z+1/2, y+1/2, -x'
 'z+1/2, -y+1/2, x'
 '-z+1/2, y+1/2, x'
 '-z+1/2, -y+1/2, -x'
 '-x, -y, -z'
 'x, y, -z'
 'x, -y, z'
 '-x, y, z'
 '-z, -x, -y'
 '-z, x, y'
 'z, x, -y'
 'z, -x, y'
 '-y, -z, -x'
 'y, -z, x'
 '-y, z, x'
 'y, z, -x'
 '-y, -x, z'
 'y, x, z'
 '-y, x, -z'
 'y, -x, -z'
 '-x, -z, y'
 'x, -z, -y'
 'x, z, y'
 '-x, z, -y'
 '-z, -y, x'
 '-z, y, -x'
 'z, -y, -x'
 'z, y, x'
 '-x, -y+1/2, -z+1/2'
 'x, y+1/2, -z+1/2'
 'x, -y+1/2, z+1/2'
 '-x, y+1/2, z+1/2'
 '-z, -x+1/2, -y+1/2'
 '-z, x+1/2, y+1/2'
 'z, x+1/2, -y+1/2'
 'z, -x+1/2, y+1/2'
 '-y, -z+1/2, -x+1/2'
 'y, -z+1/2, x+1/2'
 '-y, z+1/2, x+1/2'
 'y, z+1/2, -x+1/2'
 '-y, -x+1/2, z+1/2'
 'y, x+1/2, z+1/2'
 '-y, x+1/2, -z+1/2'
 'y, -x+1/2, -z+1/2'
 '-x, -z+1/2, y+1/2'
 'x, -z+1/2, -y+1/2'
 'x, z+1/2, y+1/2'
 '-x, z+1/2, -y+1/2'
 '-z, -y+1/2, x+1/2'
 '-z, y+1/2, -x+1/2'
 'z, -y+1/2, -x+1/2'
 'z, y+1/2, x+1/2'
 '-x+1/2, -y, -z+1/2'
 'x+1/2, y, -z+1/2'
 'x+1/2, -y, z+1/2'
 '-x+1/2, y, z+1/2'
 '-z+1/2, -x, -y+1/2'
 '-z+1/2, x, y+1/2'
 'z+1/2, x, -y+1/2'
 'z+1/2, -x, y+1/2'
 '-y+1/2, -z, -x+1/2'
 'y+1/2, -z, x+1/2'
 '-y+1/2, z, x+1/2'
 'y+1/2, z, -x+1/2'
 '-y+1/2, -x, z+1/2'
 'y+1/2, x, z+1/2'
 '-y+1/2, x, -z+1/2'
 'y+1/2, -x, -z+1/2'
 '-x+1/2, -z, y+1/2'
 'x+1/2, -z, -y+1/2'
 'x+1/2, z, y+1/2'
 '-x+1/2, z, -y+1/2'
 '-z+1/2, -y, x+1/2'
 '-z+1/2, y, -x+1/2'
 'z+1/2, -y, -x+1/2'
 'z+1/2, y, x+1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, y+1/2, -z'
 'x+1/2, -y+1/2, z'
 '-x+1/2, y+1/2, z'
 '-z+1/2, -x+1/2, -y'
 '-z+1/2, x+1/2, y'
 'z+1/2, x+1/2, -y'
 'z+1/2, -x+1/2, y'
 '-y+1/2, -z+1/2, -x'
 'y+1/2, -z+1/2, x'
 '-y+1/2, z+1/2, x'
 'y+1/2, z+1/2, -x'
 '-y+1/2, -x+1/2, z'
 'y+1/2, x+1/2, z'
 '-y+1/2, x+1/2, -z'
 'y+1/2, -x+1/2, -z'
 '-x+1/2, -z+1/2, y'
 'x+1/2, -z+1/2, -y'
 'x+1/2, z+1/2, y'
 '-x+1/2, z+1/2, -y'
 '-z+1/2, -y+1/2, x'
 '-z+1/2, y+1/2, -x'
 'z+1/2, -y+1/2, -x'
 'z+1/2, y+1/2, x'
 
_cell_length_a                    36.6353(5)
_cell_length_b                    36.6353(5)
_cell_length_c                    36.6353(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      49170(2)
_cell_formula_units_Z             8
_cell_measurement_temperature     253(2)
_cell_measurement_reflns_used     17580
_cell_measurement_theta_min       1.8820
_cell_measurement_theta_max       42.4290
 
_exptl_crystal_description        block
_exptl_crystal_colour             colorless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.189          
_exptl_crystal_F_000              18160
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.32
_exptl_crystal_size_min           0.24
_exptl_absorpt_coefficient_mu     1.677
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.38357
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       253(2)
_diffrn_radiation_wavelength      1.3405
_diffrn_radiation_type            GaK\a
_diffrn_source                    'micro-focus metaljet'
_diffrn_measurement_device_type   'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             21746
_diffrn_reflns_av_unetI/netI      0.0107
_diffrn_reflns_av_R_equivalents   0.0327
_diffrn_reflns_limit_h_min        -36
_diffrn_reflns_limit_h_max        28
_diffrn_reflns_limit_k_min        -36
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        36
_diffrn_reflns_theta_min          1.816
_diffrn_reflns_theta_max          42.796
_diffrn_reflns_theta_full         42.796
_diffrn_measured_fraction_theta_max   0.979
_diffrn_measured_fraction_theta_full  0.979
_diffrn_reflns_Laue_measured_fraction_max    0.979
_diffrn_reflns_Laue_measured_fraction_full   0.979
_diffrn_reflns_point_group_measured_fraction_max   0.979
_diffrn_reflns_point_group_measured_fraction_full  0.979
_reflns_number_total              1369
_reflns_number_gt                 1222
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection        'CrysAlisPro system (CCD 43.116a 64-bit (release 22-03-2024))'
_computing_cell_refinement        'CrysAlisPro 1.171.43.116a (Rigaku OD, 2024)'
_computing_data_reduction         'CrysAlisPro 1.171.43.116a (Rigaku OD, 2024)'
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.00012(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          1369
_refine_ls_number_parameters      113
_refine_ls_number_restraints      123
_refine_ls_R_factor_all           0.1437
_refine_ls_R_factor_gt            0.1406
_refine_ls_wR_factor_ref          0.3848
_refine_ls_wR_factor_gt           0.3770
_refine_ls_goodness_of_fit_ref    1.878
_refine_ls_restrained_S_all       1.895
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pd1 Pd 0.74131(4) 0.500000 0.500000 0.1063(11) Uani 1 8 d S T P . .
O1 O 0.93398(17) 0.56602(17) 0.56602(17) 0.099(3) Uani 1 6 d S T P . .
P2 P 0.91094(7) 0.58906(7) 0.58906(7) 0.0856(14) Uani 1 6 d S T P . .
N1_1 N 0.7413(2) 0.5488(2) 0.5261(3) 0.189(4) Uani 1 1 d G U . A -1
C2_1 C 0.70878(16) 0.5646(3) 0.5376(3) 0.204(5) Uani 1 1 d G U . A -1
H2_1 H 0.686743 0.552606 0.533787 0.244 Uiso 1 1 calc R U . A -1
C3_1 C 0.7092(2) 0.5985(3) 0.5547(3) 0.228(6) Uani 1 1 d G U . A -1
H3_1 H 0.687487 0.609070 0.562448 0.273 Uiso 1 1 calc R U . A -1
C4_1 C 0.7422(3) 0.6164(2) 0.5604(3) 0.222(6) Uani 1 1 d G U . A -1
H4_1 H 0.742455 0.639063 0.571896 0.267 Uiso 1 1 calc R U . A -1
C5_1 C 0.7746(2) 0.6006(2) 0.5489(3) 0.188(4) Uani 1 1 d G U . A -1
C6_1 C 0.77420(16) 0.5667(2) 0.5317(3) 0.181(4) Uani 1 1 d G U . A -1
H6_1 H 0.795938 0.556123 0.524025 0.217 Uiso 1 1 calc R U . A -1
C8_1 C 0.81050(18) 0.6176(2) 0.5563(2) 0.161(4) Uani 1 1 d G U . A -1
C9_1 C 0.8399(2) 0.59770(19) 0.5699(2) 0.123(4) Uani 1 1 d G U . A -1
C10_1 C 0.87418(19) 0.6137(2) 0.5721(2) 0.108(4) Uani 0.5 1 d G U P A -1
C11_1 C 0.8792(2) 0.6496(2) 0.5608(3) 0.144(4) Uani 1 1 d DG U . A -1
C12_1 C 0.8498(3) 0.66945(19) 0.5473(2) 0.142(5) Uani 0.5 1 d DG U P A -1
C13_1 C 0.8155(2) 0.6534(2) 0.5450(2) 0.169(4) Uani 1 1 d DG U . A -1
H13_1 H 0.795833 0.666739 0.535978 0.203 Uiso 1 1 calc R U . A -1
O14_1 O 0.8324(4) 0.5612(4) 0.5821(4) 0.120(5) Uani 0.5 1 d . U P A -1
C1_3 C 0.8540(6) 0.7110(5) 0.5377(8) 0.41(3) Uani 1 1 d D . . A -1
H1A_3 H 0.831156 0.720240 0.528793 0.620 Uiso 1 1 calc R U . A -1
H1B_3 H 0.860980 0.724225 0.559220 0.620 Uiso 1 1 calc R U . A -1
H1C_3 H 0.872395 0.713898 0.519293 0.620 Uiso 1 1 calc R U . A -1
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pd1 N1_1 2.026(7) . ?
O1 P2 1.462(12) . ?
P2 C10_1 1.736(8) . ?
N1_1 C2_1 1.3900 . ?
N1_1 C6_1 1.3900 . ?
C2_1 C3_1 1.3900 . ?
C3_1 C4_1 1.3900 . ?
C4_1 C5_1 1.3900 . ?
C5_1 C6_1 1.3900 . ?
C5_1 C8_1 1.479(10) . ?
C8_1 C9_1 1.3900 . ?
C8_1 C13_1 1.3900 . ?
C9_1 C10_1 1.3900 . ?
C9_1 O14_1 1.437(14) . ?
C10_1 C11_1 1.3900 . ?
C11_1 C12_1 1.3900 . ?
C12_1 C13_1 1.3900 . ?
C12_1 C1_3 1.569(16) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O1 P2 C10_1 122.8(3) . . ?
C2_1 N1_1 C6_1 120.0 . . ?
C2_1 N1_1 Pd1 120.8(5) . . ?
C6_1 N1_1 Pd1 119.2(5) . . ?
N1_1 C2_1 C3_1 120.0 . . ?
C4_1 C3_1 C2_1 120.0 . . ?
C5_1 C4_1 C3_1 120.0 . . ?
C4_1 C5_1 C6_1 120.0 . . ?
C4_1 C5_1 C8_1 121.9(7) . . ?
C6_1 C5_1 C8_1 118.0(7) . . ?
C5_1 C6_1 N1_1 120.0 . . ?
C9_1 C8_1 C13_1 120.0 . . ?
C9_1 C8_1 C5_1 122.2(6) . . ?
C13_1 C8_1 C5_1 117.4(7) . . ?
C8_1 C9_1 C10_1 120.0 . . ?
C8_1 C9_1 O14_1 116.8(8) . . ?
C10_1 C9_1 O14_1 123.1(8) . . ?
C11_1 C10_1 C9_1 120.0 . . ?
C11_1 C10_1 P2 119.8(5) . . ?
C9_1 C10_1 P2 120.2(5) . . ?
C10_1 C11_1 C12_1 120.0 . . ?
C11_1 C12_1 C13_1 120.0 . . ?
C11_1 C12_1 C1_3 120.8(7) . . ?
C13_1 C12_1 C1_3 119.0(7) . . ?
C12_1 C13_1 C8_1 120.0 . . ?
 
_refine_diff_density_max    3.083
_refine_diff_density_min   -1.005
_refine_diff_density_rms    0.163




# start Validation Reply Form
_vrf_THETM01_Pd6L8
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Author Response: The crystals of this giant supramolecular assembly 
diffract very weekly in nature, possibly due to a large amount of amorphous 
solvents and highly-disordered counterions existing in the unit cell, which 
occupy as much as 55.4% of the unit cell based on PLATON calculation.
;
_vrf_PLAT973_Pd6L8
;
PROBLEM: Check Calcd Positive Resid. Density on       Pd1       3.10 eA-3  
RESPONSE: The positive residual electron density peak is located near the 
Pd1 atom and arises from residual Fourier features commonly observed 
around heavy metal centers. Palladium is a strong scatterer, and minor 
absorption and truncation effects can lead to such residual density. The 
coordination environment of Pd1 is chemically reasonable and well defined, 
and no chemically meaningful disorder could be identified.
;
# end Validation Reply Form