# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PdBF4
_database_code_depnum_ccdc_archive 'CCDC 2025726'
loop_
_audit_author_name
_audit_author_address
'Dongwon Kim'
;Pusan National University
South Korea
;
_audit_update_record             
;
2020-08-27 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C128 H192 B8 F32 N16 Pd4 Si16'
_chemical_formula_weight         3524.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0047 0.0022 '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'
B B 0.0021 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0089 0.0045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0231 0.0138 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.1026 0.0917 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.7364 1.2670 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

_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+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   16.927(3)
_cell_length_b                   20.121(4)
_cell_length_c                   55.331(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18845(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    52116
_cell_measurement_theta_min      0.458
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             7232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.750
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.800
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27032
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_av_R_equivalents  0.1256
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_theta_min         1.817
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_full        28.685
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.953
_reflns_number_total             4193
_reflns_number_gt                2152
_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.
 
 _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       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  SHELXL
_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)+(0.1000P)²+188.0000P] 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       0.00030(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4193
_refine_ls_number_parameters     295
_refine_ls_number_restraints     285
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.1026
_refine_ls_wR_factor_ref         0.2861
_refine_ls_wR_factor_gt          0.2550
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.190
_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 0.875000 0.375000 0.45169(2) 0.0810(5) Uani 1 2 d S TU P . .
C1 C 0.7184(7) 0.3253(5) 0.4665(2) 0.100(2) Uani 1 1 d . U . . .
H1 H 0.746759 0.303081 0.478423 0.120 Uiso 1 1 calc R U . . .
N1 N 0.8872(5) 0.2748(4) 0.45146(14) 0.0889(19) Uani 1 1 d . U . . .
Si1 Si 0.57927(18) 0.43920(15) 0.40723(6) 0.1012(10) Uani 1 1 d . U . . .
Si2 Si 0.7970(2) 0.12674(18) 0.40879(7) 0.1187(11) Uani 1 1 d D U . . .
C2 C 0.6363(7) 0.3174(6) 0.4650(2) 0.110(3) Uani 1 1 d . U . . .
H2 H 0.610399 0.288944 0.475656 0.132 Uiso 1 1 calc R U . . .
N2 N 0.7562(5) 0.3644(4) 0.45084(13) 0.0862(19) Uani 1 1 d . U . . .
C6 C 0.4705(7) 0.4193(7) 0.4088(3) 0.143(4) Uani 1 1 d . U . . .
H6A H 0.443019 0.443172 0.396356 0.215 Uiso 1 1 calc R U . . .
H6B H 0.450198 0.432115 0.424316 0.215 Uiso 1 1 calc R U . . .
H6C H 0.462902 0.372410 0.406533 0.215 Uiso 1 1 calc R U . . .
C5 C 0.7125(6) 0.3939(4) 0.43351(17) 0.084(2) Uani 1 1 d . U . . .
H5 H 0.739570 0.418337 0.421876 0.100 Uiso 1 1 calc R U . . .
C4 C 0.6324(6) 0.3912(5) 0.43151(19) 0.091(2) Uani 1 1 d . U . . .
C3 C 0.5942(7) 0.3518(6) 0.4479(2) 0.102(2) Uani 1 1 d . U . . .
H3 H 0.539468 0.348316 0.447437 0.122 Uiso 1 1 calc R U . . .
C8 C 0.6157(7) 0.4130(5) 0.3772(2) 0.108(3) Uani 1 1 d . U . . .
H8A H 0.583186 0.433883 0.364905 0.129 Uiso 1 1 calc R U . . .
H8AB H 0.669159 0.429407 0.375171 0.129 Uiso 1 1 calc R U . . .
C7 C 0.5979(8) 0.5283(6) 0.4112(2) 0.133(4) Uani 1 1 d . U . . .
H7A H 0.653382 0.536924 0.409385 0.199 Uiso 1 1 calc R U . . .
H7B H 0.581186 0.541666 0.427048 0.199 Uiso 1 1 calc R U . . .
H7C H 0.568981 0.552851 0.399259 0.199 Uiso 1 1 calc R U . . .
C9 C 0.9311(7) 0.2422(5) 0.4680(2) 0.110(3) Uani 1 1 d . U . . .
H9 H 0.956298 0.265994 0.480170 0.132 Uiso 1 1 calc R U . . .
C10 C 0.9390(8) 0.1750(6) 0.4671(2) 0.126(3) Uani 1 1 d . U . . .
H10 H 0.972410 0.153556 0.477969 0.151 Uiso 1 1 calc R U . . .
C11 C 0.8986(8) 0.1390(6) 0.4505(2) 0.121(3) Uani 1 1 d . U . . .
H11 H 0.900779 0.092806 0.450837 0.145 Uiso 1 1 calc R U . . .
C12 C 0.8542(7) 0.1709(5) 0.4331(2) 0.101(2) Uani 1 1 d . U . . .
C13 C 0.8526(6) 0.2384(5) 0.43407(18) 0.088(2) Uani 1 1 d . U . . .
H13 H 0.825813 0.260843 0.421877 0.105 Uiso 1 1 calc R U . . .
C14 C 0.7687(8) 0.0437(6) 0.4187(3) 0.150(4) Uani 1 1 d . U . . .
H14A H 0.722172 0.029845 0.410219 0.224 Uiso 1 1 calc R U . . .
H14B H 0.758122 0.044380 0.435789 0.224 Uiso 1 1 calc R U . . .
H14C H 0.811004 0.013211 0.415478 0.224 Uiso 1 1 calc R U . . .
C15 C 0.7180(7) 0.1752(6) 0.4006(2) 0.144(4) Uani 1 1 d D U . . .
H15A H 0.678850 0.174032 0.413165 0.216 Uiso 1 1 calc R U . . .
H15B H 0.695526 0.158435 0.385879 0.216 Uiso 1 1 calc R U . . .
H15C H 0.735289 0.220104 0.398200 0.216 Uiso 1 1 calc R U . . .
C16 C 0.8745(7) 0.1076(8) 0.38832(9) 0.170(4) Uani 1 1 d D U . . .
H16A H 0.917368 0.136991 0.392927 0.204 Uiso 1 1 calc R U . . .
H16B H 0.891426 0.063292 0.392830 0.204 Uiso 1 1 calc R U . . .
B2 B 0.8675(19) 0.3870(9) 0.5209(4) 0.126(5) Uani 0.25 1 d D U P A 1
F2 F 0.8433(10) 0.3265(7) 0.5100(2) 0.144(5) Uani 0.5 1 d D U P A 1
F3 F 0.7932(18) 0.4173(12) 0.5165(4) 0.123(6) Uani 0.25 1 d D U P A 1
F4 F 0.865(2) 0.3564(12) 0.5439(3) 0.120(6) Uani 0.25 1 d D U P A 1
B1 B 0.875000 0.375000 0.3721(4) 0.205(8) Uani 0.5 2 d DS TU P B 2
F1 F 0.8207(11) 0.3206(9) 0.3717(3) 0.214(7) Uani 0.5 1 d D U P B 2
F10 F 0.9063(12) 0.3827(13) 0.3957(3) 0.212(7) Uani 0.5 1 d D U P B 2
F4A F 1.0865(16) 0.209(2) 0.5190(7) 0.412(14) Uani 0.5 1 d D U P . .
F3A F 1.188(2) 0.1413(13) 0.5058(8) 0.418(15) Uani 0.5 1 d D U P . .
F2A F 1.2172(18) 0.2420(17) 0.5240(7) 0.421(14) Uani 0.5 1 d D U P . .
F1A F 1.161(3) 0.2404(19) 0.4859(5) 0.436(15) Uani 0.5 1 d D U P . .
B1A B 1.1632(15) 0.2082(13) 0.5087(5) 0.419(14) Uani 0.5 1 d D U P . .


_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 N2 2.022(9) 2_655 ?
Pd1 N2 2.022(9) . ?
Pd1 N1 2.028(8) 2_655 ?
Pd1 N1 2.028(8) . ?
C1 N2 1.334(11) . ?
C1 C2 1.401(14) . ?
C1 H1 0.9300 . ?
N1 C13 1.344(12) . ?
N1 C9 1.349(12) . ?
Si1 C7 1.833(12) . ?
Si1 C8 1.849(12) . ?
Si1 C4 1.883(11) . ?
Si1 C6 1.886(12) . ?
Si2 C15 1.716(11) . ?
Si2 C16 1.775(7) . ?
Si2 C14 1.823(13) . ?
Si2 C12 1.881(12) . ?
C2 C3 1.374(14) . ?
C2 H2 0.9300 . ?
N2 C5 1.349(11) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C5 C4 1.363(13) . ?
C5 H5 0.9300 . ?
C4 C3 1.366(13) . ?
C3 H3 0.9300 . ?
C8 C8 1.55(2) 4 ?
C8 H8A 0.9700 . ?
C8 H8AB 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 C10 1.360(14) . ?
C9 H9 0.9300 . ?
C10 C11 1.355(16) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(15) . ?
C11 H11 0.9300 . ?
C12 C13 1.358(13) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C16 1.474(10) 3_655 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
B2 B2 0.54(5) 2_655 ?
B2 F2 1.16(3) 2_655 ?
B2 F4 1.313(18) 2_655 ?
B2 F4 1.415(10) . ?
B2 F2 1.418(10) . ?
B2 F3 1.420(10) . ?
B2 F3 1.88(6) 2_655 ?
F4 F4 0.82(5) 2_655 ?
B1 B1 0.33(4) 3_655 ?
B1 F10 1.13(3) 3_655 ?
B1 F10 1.13(3) 4 ?
B1 F10 1.418(10) 2_655 ?
B1 F10 1.418(10) . ?
B1 F1 1.429(9) 2_655 ?
B1 F1 1.429(9) . ?
B1 F1 1.470(12) 4 ?
B1 F1 1.470(12) 3_655 ?
F1 F10 1.62(3) 3_655 ?
F1 F10 1.67(3) 2_655 ?
F10 F10 1.10(3) 2_655 ?
F4A B1A 1.418(9) . ?
F3A B1A 1.421(9) . ?
F2A B1A 1.417(9) . ?
F1A B1A 1.418(9) . ?

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
N2 Pd1 N2 177.3(4) 2_655 . ?
N2 Pd1 N1 89.8(3) 2_655 2_655 ?
N2 Pd1 N1 90.2(3) . 2_655 ?
N2 Pd1 N1 90.2(3) 2_655 . ?
N2 Pd1 N1 89.8(3) . . ?
N1 Pd1 N1 179.3(4) 2_655 . ?
N2 C1 C2 120.4(10) . . ?
N2 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
C13 N1 C9 117.5(10) . . ?
C13 N1 Pd1 120.1(6) . . ?
C9 N1 Pd1 122.4(7) . . ?
C7 Si1 C8 109.2(5) . . ?
C7 Si1 C4 109.5(6) . . ?
C8 Si1 C4 109.6(5) . . ?
C7 Si1 C6 111.7(6) . . ?
C8 Si1 C6 107.8(6) . . ?
C4 Si1 C6 108.9(5) . . ?
C15 Si2 C16 122.1(5) . . ?
C15 Si2 C14 113.3(7) . . ?
C16 Si2 C14 100.9(7) . . ?
C15 Si2 C12 108.8(6) . . ?
C16 Si2 C12 100.3(6) . . ?
C14 Si2 C12 110.6(6) . . ?
C3 C2 C1 119.8(10) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C1 N2 C5 117.3(9) . . ?
C1 N2 Pd1 121.6(7) . . ?
C5 N2 Pd1 121.0(6) . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C5 C4 125.9(9) . . ?
N2 C5 H5 117.1 . . ?
C4 C5 H5 117.1 . . ?
C5 C4 C3 116.1(10) . . ?
C5 C4 Si1 120.8(7) . . ?
C3 C4 Si1 123.0(9) . . ?
C4 C3 C2 120.4(11) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C8 C8 Si1 115.0(9) 4 . ?
C8 C8 H8A 108.5 4 . ?
Si1 C8 H8A 108.5 . . ?
C8 C8 H8AB 108.5 4 . ?
Si1 C8 H8AB 108.5 . . ?
H8A C8 H8AB 107.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C9 C10 120.9(11) . . ?
N1 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 120.4(12) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.0(12) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 116.7(11) . . ?
C13 C12 Si2 119.3(9) . . ?
C11 C12 Si2 124.0(9) . . ?
N1 C13 C12 124.3(10) . . ?
N1 C13 H13 117.8 . . ?
C12 C13 H13 117.8 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C16 Si2 130.3(11) 3_655 . ?
C16 C16 H16A 104.7 3_655 . ?
Si2 C16 H16A 104.7 . . ?
C16 C16 H16B 104.7 3_655 . ?
Si2 C16 H16B 104.7 . . ?
H16A C16 H16B 105.7 . . ?
B2 B2 F2 107(6) 2_655 2_655 ?
B2 B2 F4 89(3) 2_655 2_655 ?
F2 B2 F4 108(2) 2_655 2_655 ?
B2 B2 F4 68.1(17) 2_655 . ?
F2 B2 F4 139(3) 2_655 . ?
F4 B2 F4 35(2) 2_655 . ?
B2 B2 F2 51(4) 2_655 . ?
F2 B2 F2 119(2) 2_655 . ?
F4 B2 F2 124(2) 2_655 . ?
F4 B2 F2 90.2(14) . . ?
B2 B2 F3 142(6) 2_655 . ?
F2 B2 F3 98(2) 2_655 . ?
F4 B2 F3 109(3) 2_655 . ?
F4 B2 F3 109(3) . . ?
F2 B2 F3 92.2(19) . . ?
B2 B2 F3 27(5) 2_655 2_655 ?
F2 B2 F3 81(2) 2_655 2_655 ?
F4 B2 F3 90(2) 2_655 2_655 ?
F4 B2 F3 83(2) . 2_655 ?
F2 B2 F3 71.3(14) . 2_655 ?
F3 B2 F3 160.0(19) . 2_655 ?
B2 F2 B2 22(3) 2_655 . ?
B2 F3 B2 10.1(14) . 2_655 ?
F4 F4 B2 79.6(18) 2_655 2_655 ?
F4 F4 B2 65.9(13) 2_655 . ?
B2 F4 B2 23(2) 2_655 . ?
B1 B1 F10 150.6(12) 3_655 4 ?
F10 B1 F10 59(2) 3_655 4 ?
B1 B1 F10 22.9(7) 3_655 . ?
F10 B1 F10 165(2) 3_655 . ?
F10 B1 F10 130(2) 4 . ?
F10 B1 F10 45.8(14) 2_655 . ?
B1 B1 F1 90.9(9) 3_655 . ?
F10 B1 F1 77.8(17) 3_655 . ?
F10 B1 F1 100.6(16) 4 . ?
F10 B1 F1 72.0(13) 2_655 . ?
F10 B1 F1 109.7(10) . . ?
F1 B1 F1 178.2(18) 2_655 . ?
F10 F10 B1 67.1(7) 2_655 . ?
B1 F10 B1 6.5(10) 3_655 . ?
F2A B1A F4A 110.2(9) . . ?
F2A B1A F1A 109.0(9) . . ?
F4A B1A F1A 109.3(9) . . ?
F2A B1A F3A 109.4(9) . . ?
F4A B1A F3A 109.1(9) . . ?
F1A B1A F3A 109.8(9) . . ?

_refine_diff_density_max         1.249
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.139

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PdReO4_a
_database_code_depnum_ccdc_archive 'CCDC 2025728'
loop_
_audit_author_name
_audit_author_address
'Dongwon Kim'
;Pusan National University
South Korea
;
_audit_update_record             
;
2020-08-27 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H100 N8 O13 Pd2 Re3 Si8'
_chemical_formula_weight         2197.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0064 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0816 0.0698 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -1.0218 0.9968 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -0.8872 7.1331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.087(4)
_cell_length_b                   16.899(3)
_cell_length_c                   29.527(6)
_cell_angle_alpha                90
_cell_angle_beta                 109.40(3)
_cell_angle_gamma                90
_cell_volume                     9453(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    79039
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_F_000             4316
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    4.151
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30732
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.590
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             8395
_reflns_number_gt                5962
_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.
 
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8395
_refine_ls_number_parameters     537
_refine_ls_number_restraints     515
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.1213
_refine_ls_wR_factor_ref         0.3429
_refine_ls_wR_factor_gt          0.3244
_refine_ls_goodness_of_fit_ref   2.121
_refine_ls_restrained_S_all      2.185
_refine_ls_shift/su_max          0.001
_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 0.43353(7) 0.60578(7) 0.59708(4) 0.0579(4) Uani 1 1 d . U . . .
Si1 Si 0.2270(5) 0.7075(5) 0.6764(3) 0.134(3) Uani 1 1 d D U . . .
Si2 Si 0.4056(3) 0.3087(3) 0.68459(19) 0.0719(13) Uani 1 1 d . U . . .
Si3 Si 0.5249(3) 0.9114(4) 0.6804(3) 0.0996(19) Uani 1 1 d D U . . .
Si4 Si 0.7272(3) 0.5459(3) 0.6958(2) 0.0819(14) Uani 1 1 d . U . . .
N1 N 0.3310(7) 0.5957(8) 0.5965(5) 0.067(3) Uani 1 1 d . U . . .
N2 N 0.4458(7) 0.4861(7) 0.6012(4) 0.060(3) Uani 1 1 d . U . . .
N3 N 0.4228(6) 0.7267(7) 0.5948(4) 0.060(3) Uani 1 1 d . U . . .
N4 N 0.5346(8) 0.6184(7) 0.6005(5) 0.063(2) Uani 1 1 d . U . . .
C1 C 0.3110(9) 0.6377(9) 0.6264(6) 0.065(3) Uani 1 1 d . U . . .
H1 H 0.345234 0.671417 0.647566 0.078 Uiso 1 1 calc R U . . .
C2 C 0.2447(11) 0.6379(11) 0.6301(8) 0.094(4) Uani 1 1 d D U . . .
C3 C 0.1963(12) 0.5885(15) 0.5963(10) 0.123(5) Uani 1 1 d D U . . .
H3 H 0.148040 0.589137 0.594195 0.147 Uiso 1 1 calc R U . . .
C4 C 0.2182(13) 0.5373(16) 0.5653(11) 0.120(5) Uani 1 1 d . U . . .
H4 H 0.187498 0.498963 0.545528 0.144 Uiso 1 1 calc R U . . .
C5 C 0.2868(10) 0.5471(12) 0.5657(8) 0.087(4) Uani 1 1 d . U . . .
H5 H 0.302558 0.518340 0.543538 0.104 Uiso 1 1 calc R U . . .
C6 C 0.2779(18) 0.7915(16) 0.6827(9) 0.137(7) Uani 1 1 d . U . . .
H6A H 0.326997 0.776474 0.688010 0.206 Uiso 1 1 calc R U . . .
H6B H 0.275232 0.822306 0.710167 0.206 Uiso 1 1 calc R U . . .
H6C H 0.260276 0.823526 0.653447 0.206 Uiso 1 1 calc R U . . .
C7 C 0.1306(17) 0.7303(16) 0.6544(13) 0.161(9) Uani 1 1 d . U . . .
H7A H 0.121274 0.775344 0.672257 0.242 Uiso 1 1 calc R U . . .
H7B H 0.104186 0.684029 0.659119 0.242 Uiso 1 1 calc R U . . .
H7C H 0.115627 0.743345 0.620097 0.242 Uiso 1 1 calc R U . . .
C8 C 0.4679(8) 0.4480(9) 0.5680(5) 0.060(3) Uani 1 1 d . U . . .
H8 H 0.481695 0.477768 0.545334 0.072 Uiso 1 1 calc R U . . .
C9 C 0.4702(10) 0.3682(10) 0.5673(6) 0.067(3) Uani 1 1 d . U . . .
H9 H 0.482288 0.342298 0.542571 0.081 Uiso 1 1 calc R U . . .
C10 C 0.4546(10) 0.3213(10) 0.6036(6) 0.069(3) Uani 1 1 d . U . . .
H10 H 0.458729 0.265276 0.604079 0.083 Uiso 1 1 calc R U . . .
C11 C 0.4325(10) 0.3621(9) 0.6390(6) 0.068(3) Uani 1 1 d . U . . .
C12 C 0.4294(9) 0.4443(9) 0.6345(6) 0.062(3) Uani 1 1 d . U . . .
H12 H 0.414305 0.473071 0.656955 0.075 Uiso 1 1 calc R U . . .
C13 C 0.3110(11) 0.3221(15) 0.6748(8) 0.103(6) Uani 1 1 d . U . . .
H13A H 0.296150 0.284796 0.694960 0.154 Uiso 1 1 calc R U . . .
H13B H 0.284020 0.312167 0.640919 0.154 Uiso 1 1 calc R U . . .
H13C H 0.302490 0.376348 0.683144 0.154 Uiso 1 1 calc R U . . .
C14 C 0.4216(16) 0.1986(11) 0.6794(10) 0.118(7) Uani 1 1 d . U . . .
H14A H 0.406109 0.169424 0.702796 0.177 Uiso 1 1 calc R U . . .
H14B H 0.471997 0.189270 0.685732 0.177 Uiso 1 1 calc R U . . .
H14C H 0.394784 0.180420 0.646896 0.177 Uiso 1 1 calc R U . . .
C15 C 0.4588(10) 0.3481(10) 0.7459(7) 0.069(3) Uani 1 1 d . U . . .
H15A H 0.443386 0.402719 0.749336 0.083 Uiso 1 1 calc R U . . .
H15B H 0.449591 0.315043 0.770888 0.083 Uiso 1 1 calc R U . . .
C16 C 0.3687(10) 0.7588(10) 0.5594(7) 0.083(5) Uani 1 1 d . U . . .
H16 H 0.336495 0.726942 0.535454 0.099 Uiso 1 1 calc R U . . .
C17 C 0.3622(12) 0.8430(11) 0.5594(9) 0.094(5) Uani 1 1 d . U . . .
H17 H 0.326043 0.867951 0.534129 0.113 Uiso 1 1 calc R U . . .
C18 C 0.4044(10) 0.8860(10) 0.5931(8) 0.080(4) Uani 1 1 d . U . . .
H18 H 0.397514 0.941634 0.592122 0.095 Uiso 1 1 calc R U . . .
C19 C 0.4611(8) 0.8526(9) 0.6318(7) 0.067(3) Uani 1 1 d . U . . .
C20 C 0.4650(7) 0.7733(8) 0.6282(5) 0.055(3) Uani 1 1 d . U . . .
H20 H 0.502391 0.747916 0.652451 0.066 Uiso 1 1 calc R U . . .
C21 C 0.7775(12) 0.6129(13) 0.7472(9) 0.108(5) Uani 1 1 d D U . . .
H21A H 0.803050 0.580309 0.775437 0.129 Uiso 1 1 calc R U . . .
H21B H 0.812778 0.643710 0.737797 0.129 Uiso 1 1 calc R U . . .
C22 C 0.6109(12) 0.8750(15) 0.6937(12) 0.128(7) Uani 1 1 d . U . . .
H22A H 0.613382 0.821171 0.706580 0.192 Uiso 1 1 calc R U . . .
H22B H 0.643765 0.909227 0.717649 0.192 Uiso 1 1 calc R U . . .
H22C H 0.623608 0.874133 0.664442 0.192 Uiso 1 1 calc R U . . .
C23 C 0.5547(11) 0.6644(10) 0.5699(7) 0.072(3) Uani 1 1 d . U . . .
H23 H 0.519218 0.690590 0.544802 0.086 Uiso 1 1 calc R U . . .
C24 C 0.6248(10) 0.6752(10) 0.5733(7) 0.073(4) Uani 1 1 d . U . . .
H24 H 0.637000 0.707193 0.550739 0.087 Uiso 1 1 calc R U . . .
C25 C 0.6729(11) 0.6404(10) 0.6081(6) 0.074(4) Uani 1 1 d . U . . .
H25 H 0.720797 0.645329 0.609922 0.089 Uiso 1 1 calc R U . . .
C26 C 0.6567(10) 0.5945(8) 0.6441(6) 0.063(3) Uani 1 1 d . U . . .
C27 C 0.5882(9) 0.5847(8) 0.6370(6) 0.063(3) Uani 1 1 d . U . . .
H27 H 0.575633 0.551721 0.658957 0.075 Uiso 1 1 calc R U . . .
C28 C 0.6861(10) 0.4627(11) 0.7186(7) 0.083(5) Uani 1 1 d . U . . .
H28A H 0.634730 0.464667 0.703322 0.125 Uiso 1 1 calc R U . . .
H28B H 0.698078 0.467511 0.753456 0.125 Uiso 1 1 calc R U . . .
H28C H 0.703940 0.412220 0.710939 0.125 Uiso 1 1 calc R U . . .
C29 C 0.8014(10) 0.5069(14) 0.6777(8) 0.097(5) Uani 1 1 d . U . . .
H29A H 0.830470 0.471461 0.702790 0.146 Uiso 1 1 calc R U . . .
H29B H 0.830285 0.551074 0.673398 0.146 Uiso 1 1 calc R U . . .
H29C H 0.782404 0.477642 0.647497 0.146 Uiso 1 1 calc R U . . .
C31 C 0.5160(17) 1.0167(14) 0.6619(13) 0.175(12) Uani 1 1 d . U . . .
H31A H 0.541020 1.050003 0.689455 0.263 Uiso 1 1 calc R U . . .
H31B H 0.465931 1.031319 0.650081 0.263 Uiso 1 1 calc R U . . .
H31C H 0.536309 1.024603 0.636264 0.263 Uiso 1 1 calc R U . . .
C32 C 0.7276(11) 0.6701(15) 0.7607(6) 0.121(7) Uani 1 1 d D U . . .
H32A H 0.683375 0.642435 0.758969 0.145 Uiso 1 1 calc R U . . .
H32B H 0.715471 0.715102 0.737914 0.145 Uiso 1 1 calc R U . . .
C33 C 0.5333(6) 0.8780(18) 0.7425(6) 0.153(7) Uani 1 1 d D U . . .
H33A H 0.552451 0.823464 0.746598 0.184 Uiso 1 1 calc R U . . .
H33B H 0.568987 0.912008 0.765457 0.184 Uiso 1 1 calc R U . . .
Re2 Re 0.46356(12) 0.10237(11) 0.50083(9) 0.0693(9) Uani 0.311(2) 1 d D U P A 1
O9 O 0.4059(17) 0.047(2) 0.5247(13) 0.080(8) Uani 0.311(2) 1 d D U P A 1
O10 O 0.535(3) 0.050(3) 0.548(2) 0.133(14) Uani 0.311(2) 1 d . U P A 1
O1 O 0.457(2) 0.2085(16) 0.5167(11) 0.073(9) Uani 0.311(2) 1 d . U P A 1
O2 O 0.425(3) 0.105(2) 0.4426(15) 0.093(10) Uani 0.311(2) 1 d . U P A 1
Re3 Re 0.34188(5) 0.59146(6) 0.44925(3) 0.0648(4) Uani 0.689(2) 1 d D U P A 2
O3 O 0.3562(11) 0.5826(9) 0.3924(4) 0.083(5) Uani 0.689(2) 1 d D U P A 2
O4 O 0.3023(12) 0.6843(10) 0.4514(9) 0.125(8) Uani 0.689(2) 1 d D U P A 2
O5 O 0.4243(10) 0.5892(12) 0.4916(6) 0.083(5) Uani 0.689(2) 1 d . U P A 2
O6 O 0.2896(14) 0.5146(15) 0.4552(8) 0.118(7) Uani 0.689(2) 1 d . U P A 2
Re1 Re 0.500000 0.6177(5) 0.750000 0.286(6) Uani 0.659(12) 2 d DS TU P B 3
O7 O 0.514(2) 0.5604(11) 0.8033(3) 0.223(10) Uani 0.659(12) 1 d D U P B 3
O8 O 0.5687(15) 0.6892(18) 0.7555(14) 0.225(11) Uani 0.659(12) 1 d D U P B 3
Re1B Re 0.500000 0.62084(16) 0.750000 0.0501(18) Uani 0.341(12) 2 d DS TU P B 4
O1B O 0.5736(19) 0.554(3) 0.7684(17) 0.130(11) Uani 0.341(12) 1 d D U P B 4
O2B O 0.481(3) 0.666(3) 0.7994(12) 0.158(12) Uani 0.341(12) 1 d D U P B 4
O1A O 0.7659(12) 0.7503(15) 0.5509(9) 0.079(7) Uani 0.5 1 d D U P C 5
H1A H 0.786293 0.742867 0.580405 0.119 Uiso 0.5 1 calc R U P C 5
C1A C 0.784(2) 0.6884(19) 0.5245(13) 0.084(9) Uani 0.5 1 d D U P C 5
H1AA H 0.831677 0.696992 0.523675 0.127 Uiso 0.5 1 calc R U P C 5
H1AB H 0.750336 0.687884 0.491640 0.127 Uiso 0.5 1 calc R U P C 5
H1AC H 0.781887 0.637537 0.539971 0.127 Uiso 0.5 1 calc R U P C 5


_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 N4 2.009(14) . ?
Pd1 N2 2.037(12) . ?
Pd1 N3 2.054(12) . ?
Pd1 N1 2.062(14) . ?
Si1 C6 1.72(3) . ?
Si1 C7 1.87(3) . ?
Si1 C32 1.885(10) 2_656 ?
Si1 C2 1.93(2) . ?
Si2 C13 1.84(2) . ?
Si2 C11 1.845(16) . ?
Si2 C15 1.89(2) . ?
Si2 C14 1.90(2) . ?
Si3 C22 1.75(3) . ?
Si3 C31 1.85(3) . ?
Si3 C19 1.861(18) . ?
Si3 C33 1.874(10) . ?
Si4 C29 1.86(2) . ?
Si4 C28 1.865(17) . ?
Si4 C26 1.890(19) . ?
Si4 C21 1.89(2) . ?
N1 C1 1.29(2) . ?
N1 C5 1.32(2) . ?
N2 C12 1.338(18) . ?
N2 C8 1.362(18) . ?
N3 C20 1.326(18) . ?
N3 C16 1.35(2) . ?
N4 C23 1.35(2) . ?
N4 C27 1.37(2) . ?
C1 C2 1.37(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.411(10) . ?
C3 C4 1.43(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.38(3) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.35(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.45(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.44(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.40(2) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C15 1.59(3) 2_656 ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.43(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.29(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.44(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.35(2) . ?
C20 H20 0.9500 . ?
C21 C32 1.537(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.39(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.30(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.44(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.33(2) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C33 1.542(10) 2_656 ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
Re2 O2 1.63(4) . ?
Re2 O9 1.800(10) . ?
Re2 O10 1.85(4) . ?
Re2 O1 1.87(3) . ?
Re3 O5 1.711(18) . ?
Re3 O6 1.71(2) . ?
Re3 O4 1.770(9) . ?
Re3 O3 1.799(9) . ?
Re1 O7 1.788(9) 2_656 ?
Re1 O7 1.788(9) . ?
Re1 O8 1.802(10) 2_656 ?
Re1 O8 1.802(10) . ?
Re1B O2B 1.793(10) . ?
Re1B O2B 1.793(10) 2_656 ?
Re1B O1B 1.794(10) . ?
Re1B O1B 1.794(10) 2_656 ?
O1A C1A 1.421(10) . ?
O1A H1A 0.8400 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?

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
N4 Pd1 N2 90.1(5) . . ?
N4 Pd1 N3 89.4(5) . . ?
N2 Pd1 N3 178.5(5) . . ?
N4 Pd1 N1 177.3(5) . . ?
N2 Pd1 N1 91.1(5) . . ?
N3 Pd1 N1 89.3(5) . . ?
C6 Si1 C7 112.1(14) . . ?
C6 Si1 C32 95.4(13) . 2_656 ?
C7 Si1 C32 121.3(13) . 2_656 ?
C6 Si1 C2 109.7(11) . . ?
C7 Si1 C2 107.0(14) . . ?
C32 Si1 C2 110.6(11) 2_656 . ?
C13 Si2 C11 111.3(11) . . ?
C13 Si2 C15 109.5(9) . . ?
C11 Si2 C15 108.5(7) . . ?
C13 Si2 C14 107.5(12) . . ?
C11 Si2 C14 108.7(9) . . ?
C15 Si2 C14 111.4(11) . . ?
C22 Si3 C31 113.3(15) . . ?
C22 Si3 C19 111.2(11) . . ?
C31 Si3 C19 108.2(11) . . ?
C22 Si3 C33 85.0(12) . . ?
C31 Si3 C33 123.1(16) . . ?
C19 Si3 C33 114.1(11) . . ?
C29 Si4 C28 109.2(10) . . ?
C29 Si4 C26 112.2(8) . . ?
C28 Si4 C26 108.5(8) . . ?
C29 Si4 C21 100.2(10) . . ?
C28 Si4 C21 110.1(10) . . ?
C26 Si4 C21 116.3(9) . . ?
C1 N1 C5 121.3(16) . . ?
C1 N1 Pd1 119.0(11) . . ?
C5 N1 Pd1 119.7(13) . . ?
C12 N2 C8 119.8(12) . . ?
C12 N2 Pd1 120.8(9) . . ?
C8 N2 Pd1 119.2(10) . . ?
C20 N3 C16 119.4(13) . . ?
C20 N3 Pd1 122.2(9) . . ?
C16 N3 Pd1 118.3(11) . . ?
C23 N4 C27 115.7(15) . . ?
C23 N4 Pd1 123.3(12) . . ?
C27 N4 Pd1 120.9(10) . . ?
N1 C1 C2 125.7(18) . . ?
N1 C1 H1 117.2 . . ?
C2 C1 H1 117.2 . . ?
C1 C2 C3 113.7(19) . . ?
C1 C2 Si1 118.1(16) . . ?
C3 C2 Si1 128.1(18) . . ?
C2 C3 C4 121(2) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 116(2) . . ?
C5 C4 H4 122.0 . . ?
C3 C4 H4 122.0 . . ?
N1 C5 C4 121(2) . . ?
N1 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 N2 120.3(14) . . ?
C9 C8 H8 119.9 . . ?
N2 C8 H8 119.9 . . ?
C8 C9 C10 121.2(14) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 H9 119.4 . . ?
C11 C10 C9 118.0(14) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C12 C11 C10 115.0(14) . . ?
C12 C11 Si2 122.8(11) . . ?
C10 C11 Si2 122.1(12) . . ?
N2 C12 C11 125.5(13) . . ?
N2 C12 H12 117.2 . . ?
C11 C12 H12 117.2 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 C15 Si2 112.0(14) 2_656 . ?
C15 C15 H15A 109.2 2_656 . ?
Si2 C15 H15A 109.2 . . ?
C15 C15 H15B 109.2 2_656 . ?
Si2 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N3 C16 C17 116.8(17) . . ?
N3 C16 H16 121.6 . . ?
C17 C16 H16 121.6 . . ?
C18 C17 C16 121.5(19) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 122.4(16) . . ?
C17 C18 H18 118.8 . . ?
C19 C18 H18 118.8 . . ?
C20 C19 C18 112.3(15) . . ?
C20 C19 Si3 123.2(13) . . ?
C18 C19 Si3 124.4(12) . . ?
N3 C20 C19 127.6(14) . . ?
N3 C20 H20 116.2 . . ?
C19 C20 H20 116.2 . . ?
C32 C21 Si4 111.4(14) . . ?
C32 C21 H21A 109.4 . . ?
Si4 C21 H21A 109.4 . . ?
C32 C21 H21B 109.4 . . ?
Si4 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 C24 123.3(18) . . ?
N4 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C25 C24 C23 117.8(17) . . ?
C25 C24 H24 121.1 . . ?
C23 C24 H24 121.1 . . ?
C24 C25 C26 122.7(19) . . ?
C24 C25 H25 118.6 . . ?
C26 C25 H25 118.6 . . ?
C27 C26 C25 115.3(17) . . ?
C27 C26 Si4 122.0(12) . . ?
C25 C26 Si4 122.7(14) . . ?
C26 C27 N4 125.0(15) . . ?
C26 C27 H27 117.5 . . ?
N4 C27 H27 117.5 . . ?
Si4 C28 H28A 109.5 . . ?
Si4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si4 C29 H29A 109.5 . . ?
Si4 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si4 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si3 C31 H31A 109.5 . . ?
Si3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
Si3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C21 C32 Si1 108.8(14) . 2_656 ?
C21 C32 H32A 109.9 . . ?
Si1 C32 H32A 109.9 2_656 . ?
C21 C32 H32B 109.9 . . ?
Si1 C32 H32B 109.9 2_656 . ?
H32A C32 H32B 108.3 . . ?
C33 C33 Si3 118.4(14) 2_656 . ?
C33 C33 H33A 107.7 2_656 . ?
Si3 C33 H33A 107.7 . . ?
C33 C33 H33B 107.7 2_656 . ?
Si3 C33 H33B 107.7 . . ?
H33A C33 H33B 107.1 . . ?
O2 Re2 O9 107(2) . . ?
O2 Re2 O10 141(3) . . ?
O9 Re2 O10 85(2) . . ?
O2 Re2 O1 101.0(18) . . ?
O9 Re2 O1 106.9(18) . . ?
O10 Re2 O1 111.7(18) . . ?
O5 Re3 O6 112.6(12) . . ?
O5 Re3 O4 109.3(9) . . ?
O6 Re3 O4 111.7(14) . . ?
O5 Re3 O3 105.4(9) . . ?
O6 Re3 O3 108.9(9) . . ?
O4 Re3 O3 108.7(11) . . ?
O7 Re1 O7 114.4(10) 2_656 . ?
O7 Re1 O8 109.6(15) 2_656 . ?
O7 Re1 O8 113.1(8) . . ?
O8 Re1 O8 96(3) 2_656 . ?
O2B Re1B O2B 130(4) . 2_656 ?
O2B Re1B O1B 113.3(9) . . ?
O2B Re1B O1B 98(3) 2_656 . ?
C1A O1A H1A 109.5 . . ?
O1A C1A H1AA 109.5 . . ?
O1A C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
O1A C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 0(3) . . . . ?
Pd1 N1 C1 C2 179.6(14) . . . . ?
N1 C1 C2 C3 -2(3) . . . . ?
N1 C1 C2 Si1 -178.6(13) . . . . ?
C1 C2 C3 C4 6(4) . . . . ?
Si1 C2 C3 C4 -177(2) . . . . ?
C2 C3 C4 C5 -8(4) . . . . ?
C1 N1 C5 C4 -2(3) . . . . ?
Pd1 N1 C5 C4 178.2(18) . . . . ?
C3 C4 C5 N1 6(4) . . . . ?
C12 N2 C8 C9 3(2) . . . . ?
Pd1 N2 C8 C9 -173.9(13) . . . . ?
N2 C8 C9 C10 -5(3) . . . . ?
C8 C9 C10 C11 3(3) . . . . ?
C9 C10 C11 C12 -1(3) . . . . ?
C9 C10 C11 Si2 175.9(14) . . . . ?
C13 Si2 C11 C12 63.8(18) . . . . ?
C15 Si2 C11 C12 -56.8(18) . . . . ?
C14 Si2 C11 C12 -178.0(17) . . . . ?
C13 Si2 C11 C10 -112.5(17) . . . . ?
C15 Si2 C11 C10 126.9(16) . . . . ?
C14 Si2 C11 C10 6(2) . . . . ?
C8 N2 C12 C11 0(3) . . . . ?
Pd1 N2 C12 C11 176.8(14) . . . . ?
C10 C11 C12 N2 -1(3) . . . . ?
Si2 C11 C12 N2 -177.5(14) . . . . ?
C13 Si2 C15 C15 -172.9(10) . . . 2_656 ?
C11 Si2 C15 C15 -51.2(9) . . . 2_656 ?
C14 Si2 C15 C15 68.3(11) . . . 2_656 ?
C20 N3 C16 C17 2(3) . . . . ?
Pd1 N3 C16 C17 179.0(16) . . . . ?
N3 C16 C17 C18 -3(4) . . . . ?
C16 C17 C18 C19 1(4) . . . . ?
C17 C18 C19 C20 1(3) . . . . ?
C17 C18 C19 Si3 178.3(19) . . . . ?
C22 Si3 C19 C20 39(2) . . . . ?
C31 Si3 C19 C20 163.7(19) . . . . ?
C33 Si3 C19 C20 -55.3(18) . . . . ?
C22 Si3 C19 C18 -138.5(19) . . . . ?
C31 Si3 C19 C18 -14(2) . . . . ?
C33 Si3 C19 C18 127.4(16) . . . . ?
C16 N3 C20 C19 0(3) . . . . ?
Pd1 N3 C20 C19 -176.6(14) . . . . ?
C18 C19 C20 N3 -2(3) . . . . ?
Si3 C19 C20 N3 -179.1(13) . . . . ?
C29 Si4 C21 C32 164.9(18) . . . . ?
C28 Si4 C21 C32 -80.1(19) . . . . ?
C26 Si4 C21 C32 44(2) . . . . ?
C27 N4 C23 C24 2(2) . . . . ?
Pd1 N4 C23 C24 177.8(13) . . . . ?
N4 C23 C24 C25 -1(3) . . . . ?
C23 C24 C25 C26 -3(3) . . . . ?
C24 C25 C26 C27 5(2) . . . . ?
C24 C25 C26 Si4 -178.4(15) . . . . ?
C29 Si4 C26 C27 139.2(14) . . . . ?
C28 Si4 C26 C27 18.4(16) . . . . ?
C21 Si4 C26 C27 -106.3(15) . . . . ?
C29 Si4 C26 C25 -36.8(16) . . . . ?
C28 Si4 C26 C25 -157.6(14) . . . . ?
C21 Si4 C26 C25 77.7(16) . . . . ?
C25 C26 C27 N4 -4(2) . . . . ?
Si4 C26 C27 N4 179.6(11) . . . . ?
C23 N4 C27 C26 0(2) . . . . ?
Pd1 N4 C27 C26 -175.0(12) . . . . ?
Si4 C21 C32 Si1 159.7(13) . . . 2_656 ?
C22 Si3 C33 C33 -169.8(13) . . . 2_656 ?
C31 Si3 C33 C33 75.5(17) . . . 2_656 ?
C19 Si3 C33 C33 -58.9(13) . . . 2_656 ?

_refine_diff_density_max         2.270
_refine_diff_density_min         -2.505
_refine_diff_density_rms         0.244

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PdPF6
_database_code_depnum_ccdc_archive 'CCDC 2025729'
loop_
_audit_author_name
_audit_author_address
'Dongwon Kim'
;Pusan National University
South Korea
;
_audit_update_record             
;
2020-08-27 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H96 F24 N8 P4 Pd2 Si8'
_chemical_formula_weight         1994.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0026 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0052 0.0028 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0147 0.0087 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0715 0.0599 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0892 0.0801 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -1.2241 0.8719 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

_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+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   16.586(3)
_cell_length_b                   19.950(4)
_cell_length_c                   57.908(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19161(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    121648
_cell_measurement_theta_min      0.372
_cell_measurement_theta_max      33.425

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             8128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.047
_exptl_absorpt_coefficient_mu    0.486
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.650
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42394
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_theta_min         1.495
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        22.955
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6158
_reflns_number_gt                5483
_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.
 
 _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       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  SHELXL
_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)+(0.1961P)²+152.1437P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6158
_refine_ls_number_parameters     316
_refine_ls_number_restraints     287
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0949
_refine_ls_wR_factor_ref         0.2974
_refine_ls_wR_factor_gt          0.2909
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.204
_refine_ls_shift/su_max          0.003
_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
C1 C 0.6711(4) 0.7583(3) 0.72008(11) 0.0549(14) Uani 1 1 d . U . . .
H1 H 0.694731 0.733689 0.731921 0.066 Uiso 1 1 calc R U . . .
N1 N 0.6334(2) 0.7259(2) 0.70281(6) 0.0351(8) Uani 1 1 d . U . . .
Si1 Si 0.55493(9) 0.87571(7) 0.65936(2) 0.0388(3) Uani 1 1 d . . . . .
P1 P 0.625000 0.625000 0.625000 0.101(2) Uani 1 4 d DS TU P . .
F1 F 0.5771(4) 0.6996(3) 0.61149(10) 0.0520(14) Uani 0.5 1 d D U P . .
Pd1 Pd 0.625000 0.625000 0.70259(2) 0.0313(2) Uani 1 2 d S T P . .
C2 C 0.6756(5) 0.8273(4) 0.72060(13) 0.073(2) Uani 1 1 d . U . . .
H2 H 0.702543 0.848755 0.732609 0.087 Uiso 1 1 calc R U . . .
P2 P 0.625000 0.625000 0.77577(4) 0.0510(5) Uani 1 2 d S TU P . .
Si2 Si 0.32998(8) 0.55910(8) 0.65552(3) 0.0490(4) Uani 1 1 d . . . . .
N2 N 0.5025(3) 0.63187(19) 0.70122(6) 0.0342(8) Uani 1 1 d . U . . .
F3 F 0.5652(3) 0.6488(3) 0.64397(9) 0.0971(18) Uani 1 1 d D U . . .
C3 C 0.6399(5) 0.8648(4) 0.70315(13) 0.0648(18) Uani 1 1 d . U . . .
H3 H 0.641641 0.911406 0.703579 0.078 Uiso 1 1 calc R U . . .
F4 F 0.5475(3) 0.5772(3) 0.77547(10) 0.0831(13) Uani 1 1 d . U . . .
C4 C 0.5998(2) 0.7621(2) 0.68568(8) 0.0332(8) Uani 1 1 d . U . . .
H4 H 0.574390 0.739220 0.673741 0.040 Uiso 1 1 calc R U . . .
F5 F 0.5861(4) 0.6706(3) 0.79498(11) 0.108(2) Uani 1 1 d . U . . .
C5 C 0.6010(3) 0.8316(2) 0.68482(9) 0.0385(9) Uani 1 1 d . U . . .
F6 F 0.5858(4) 0.6725(4) 0.75675(12) 0.127(3) Uani 1 1 d . U . . .
C6 C 0.5198(4) 0.9609(3) 0.66781(12) 0.0556(13) Uani 1 1 d . . . . .
H6A H 0.491834 0.981133 0.655074 0.083 Uiso 1 1 calc R U . . .
H6B H 0.565351 0.988030 0.671922 0.083 Uiso 1 1 calc R U . . .
H6C H 0.483993 0.957403 0.680784 0.083 Uiso 1 1 calc R U . . .
C7 C 0.4707(3) 0.8234(3) 0.64876(9) 0.0436(10) Uani 1 1 d . . . . .
H7A H 0.444291 0.845805 0.636181 0.065 Uiso 1 1 calc R U . . .
H7B H 0.432774 0.816188 0.661039 0.065 Uiso 1 1 calc R U . . .
H7C H 0.491199 0.781018 0.643545 0.065 Uiso 1 1 calc R U . . .
C8 C 0.6383(4) 0.8794(3) 0.63738(11) 0.0514(14) Uani 1 1 d . . . . .
H8A H 0.669703 0.919676 0.640142 0.062 Uiso 1 1 calc R U . . .
H8AB H 0.673653 0.841349 0.639793 0.062 Uiso 1 1 calc R U . . .
C9 C 0.4607(3) 0.6699(3) 0.71591(9) 0.0438(10) Uani 1 1 d . U . . .
H9 H 0.487778 0.691985 0.727727 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3777(3) 0.6773(3) 0.71402(11) 0.0513(13) Uani 1 1 d . U . . .
H10 H 0.349414 0.703381 0.724584 0.062 Uiso 1 1 calc R U . . .
C11 C 0.3378(3) 0.6454(3) 0.69618(10) 0.0451(11) Uani 1 1 d . U . . .
H11 H 0.282262 0.650010 0.694765 0.054 Uiso 1 1 calc R U . . .
C12 C 0.3804(3) 0.6060(3) 0.68016(10) 0.0399(10) Uani 1 1 d . U . . .
C13 C 0.4633(3) 0.6010(2) 0.68371(9) 0.0373(9) Uani 1 1 d . U . . .
H13 H 0.493253 0.575114 0.673481 0.045 Uiso 1 1 calc R U . . .
C14 C 0.3538(5) 0.4680(3) 0.65903(14) 0.0673(17) Uani 1 1 d . . . . .
H14A H 0.318432 0.442015 0.649450 0.101 Uiso 1 1 calc R U . . .
H14B H 0.346521 0.455367 0.674886 0.101 Uiso 1 1 calc R U . . .
H14C H 0.408695 0.460001 0.654558 0.101 Uiso 1 1 calc R U . . .
C15 C 0.2206(3) 0.5758(4) 0.65710(13) 0.0625(17) Uani 1 1 d . . . . .
H15A H 0.192610 0.546466 0.646676 0.094 Uiso 1 1 calc R U . . .
H15B H 0.210282 0.621540 0.652868 0.094 Uiso 1 1 calc R U . . .
H15C H 0.201944 0.568082 0.672566 0.094 Uiso 1 1 calc R U . . .
C16 C 0.3706(4) 0.5881(4) 0.62685(11) 0.0544(15) Uani 1 1 d . . . . .
H16A H 0.425522 0.571956 0.625294 0.065 Uiso 1 1 calc R U . . .
H16B H 0.338964 0.567487 0.614689 0.065 Uiso 1 1 calc R U . . .
F1A F 0.3036(9) 0.3686(8) 0.7621(3) 0.121(7) Uani 0.294(8) 1 d D U P A -1
F2A F 0.2894(12) 0.4743(10) 0.7790(4) 0.134(7) Uani 0.294(8) 1 d D U P A -1
F3A F 0.3406(17) 0.4647(12) 0.7417(3) 0.163(8) Uani 0.294(8) 1 d D U P A -1
P3 P 0.3631(5) 0.4323(8) 0.7670(2) 0.064(4) Uani 0.147(4) 1 d D U P A -1
P1C P 0.3167(15) 0.5290(12) 0.7615(5) 0.146(8) Uani 0.103(4) 1 d D U P A -2
F1C F 0.2487(13) 0.5080(16) 0.7810(5) 0.122(8) Uani 0.206(8) 1 d D U P A -2
F2C F 0.3746(8) 0.4662(12) 0.7697(3) 0.051(4) Uani 0.206(8) 1 d D U P A -2
F3C F 0.2716(19) 0.481(2) 0.7425(5) 0.171(11) Uani 0.206(8) 1 d D U P A -2


_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
C1 N1 1.346(6) . ?
C1 C2 1.379(9) . ?
C1 H1 0.9300 . ?
N1 C4 1.348(6) . ?
N1 Pd1 2.017(5) . ?
Si1 C7 1.849(5) . ?
Si1 C6 1.862(6) . ?
Si1 C5 1.880(5) . ?
Si1 C8 1.881(6) . ?
P1 F3 1.554(5) . ?
P1 F3 1.555(5) 8 ?
P1 F3 1.555(5) 14 ?
P1 F3 1.555(5) 11 ?
P1 F1 1.859(5) . ?
P1 F1 1.859(5) 11 ?
P1 F1 1.859(5) 8 ?
P1 F1 1.859(5) 14 ?
Pd1 N2 2.037(4) . ?
Pd1 N2 2.037(4) 14 ?
C2 C3 1.390(10) . ?
C2 H2 0.9300 . ?
P2 F5 1.575(5) 14 ?
P2 F5 1.575(5) . ?
P2 F6 1.591(5) . ?
P2 F6 1.592(5) 14 ?
P2 F4 1.600(5) . ?
P2 F4 1.600(5) 14 ?
Si2 C15 1.847(6) . ?
Si2 C14 1.870(7) . ?
Si2 C16 1.883(7) . ?
Si2 C12 1.900(6) . ?
N2 C9 1.335(6) . ?
N2 C13 1.353(6) . ?
C3 C5 1.408(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.386(6) . ?
C4 H4 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C8 1.500(13) 11 ?
C8 H8A 0.9700 . ?
C8 H8AB 0.9700 . ?
C9 C10 1.388(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.382(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.406(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.394(6) . ?
C13 H13 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C16 1.487(15) 8 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
F1A P3 1.635(9) . ?
F2A P3 1.636(9) . ?
F3A P3 1.646(10) . ?
P1C F3C 1.644(10) . ?
P1C F2C 1.648(10) . ?
P1C F1C 1.652(10) . ?

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
N1 C1 C2 121.4(5) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 N1 C4 118.7(5) . . ?
C1 N1 Pd1 121.1(4) . . ?
C4 N1 Pd1 120.1(3) . . ?
C7 Si1 C6 111.4(3) . . ?
C7 Si1 C5 107.6(2) . . ?
C6 Si1 C5 110.4(3) . . ?
C7 Si1 C8 110.7(3) . . ?
C6 Si1 C8 111.8(3) . . ?
C5 Si1 C8 104.5(3) . . ?
F3 P1 F3 100.7(3) . 8 ?
F3 P1 F3 90.0(4) . 14 ?
F3 P1 F3 144.5(5) 8 14 ?
F3 P1 F3 144.5(5) . 11 ?
F3 P1 F3 90.0(4) 8 11 ?
F3 P1 F3 100.7(3) 14 11 ?
F3 P1 F1 77.3(3) . . ?
F3 P1 F1 71.0(3) 8 . ?
F3 P1 F1 144.5(3) 14 . ?
F3 P1 F1 74.4(3) 11 . ?
F3 P1 F1 74.4(3) . 11 ?
F3 P1 F1 144.5(3) 8 11 ?
F3 P1 F1 71.0(3) 14 11 ?
F3 P1 F1 77.3(3) 11 11 ?
F1 P1 F1 73.7(4) . 11 ?
F3 P1 F1 71.0(3) . 8 ?
F3 P1 F1 77.3(3) 8 8 ?
F3 P1 F1 74.4(3) 14 8 ?
F3 P1 F1 144.5(3) 11 8 ?
F1 P1 F1 129.4(4) . 8 ?
F1 P1 F1 130.2(4) 11 8 ?
F3 P1 F1 144.5(3) . 14 ?
F3 P1 F1 74.4(3) 8 14 ?
F3 P1 F1 77.3(3) 14 14 ?
F3 P1 F1 71.0(3) 11 14 ?
F1 P1 F1 130.2(4) . 14 ?
F1 P1 F1 129.4(4) 11 14 ?
F1 P1 F1 73.7(4) 8 14 ?
N1 Pd1 N1 179.3(2) . 14 ?
N1 Pd1 N2 90.10(15) . . ?
N1 Pd1 N2 89.93(15) 14 . ?
N1 Pd1 N2 89.93(15) . 14 ?
N1 Pd1 N2 90.10(15) 14 14 ?
N2 Pd1 N2 175.5(2) . 14 ?
C1 C2 C3 119.9(6) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
F5 P2 F5 90.1(6) 14 . ?
F5 P2 F6 178.7(4) 14 . ?
F5 P2 F6 88.7(4) . . ?
F5 P2 F6 88.7(4) 14 14 ?
F5 P2 F6 178.7(4) . 14 ?
F6 P2 F6 92.4(7) . 14 ?
F5 P2 F4 89.6(3) 14 . ?
F5 P2 F4 91.3(3) . . ?
F6 P2 F4 91.1(3) . . ?
F6 P2 F4 88.0(3) 14 . ?
F5 P2 F4 91.3(3) 14 14 ?
F5 P2 F4 89.6(3) . 14 ?
F6 P2 F4 88.0(3) . 14 ?
F6 P2 F4 91.1(3) 14 14 ?
F4 P2 F4 178.7(4) . 14 ?
C15 Si2 C14 112.2(4) . . ?
C15 Si2 C16 109.9(3) . . ?
C14 Si2 C16 108.6(3) . . ?
C15 Si2 C12 107.8(3) . . ?
C14 Si2 C12 107.7(3) . . ?
C16 Si2 C12 110.7(3) . . ?
C9 N2 C13 119.1(4) . . ?
C9 N2 Pd1 122.1(3) . . ?
C13 N2 Pd1 118.6(3) . . ?
C2 C3 C5 119.3(6) . . ?
C2 C3 H3 120.3 . . ?
C5 C3 H3 120.3 . . ?
N1 C4 C5 123.8(4) . . ?
N1 C4 H4 118.1 . . ?
C5 C4 H4 118.1 . . ?
C4 C5 C3 116.8(5) . . ?
C4 C5 Si1 119.4(4) . . ?
C3 C5 Si1 123.8(5) . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C8 Si1 115.5(6) 11 . ?
C8 C8 H8A 108.4 11 . ?
Si1 C8 H8A 108.4 . . ?
C8 C8 H8AB 108.4 11 . ?
Si1 C8 H8AB 108.4 . . ?
H8A C8 H8AB 107.5 . . ?
N2 C9 C10 121.7(5) . . ?
N2 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 120.7(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 116.0(5) . . ?
C13 C12 Si2 120.6(4) . . ?
C11 C12 Si2 123.4(4) . . ?
N2 C13 C12 123.6(4) . . ?
N2 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C16 Si2 115.5(5) 8 . ?
C16 C16 H16A 108.4 8 . ?
Si2 C16 H16A 108.4 . . ?
C16 C16 H16B 108.4 8 . ?
Si2 C16 H16B 108.4 . . ?
H16A C16 H16B 107.5 . . ?
F1A P3 F2A 91.2(6) . . ?
F1A P3 F3A 90.9(7) . . ?
F2A P3 F3A 90.5(7) . . ?
F3C P1C F2C 90.6(7) . . ?
F3C P1C F1C 89.9(7) . . ?
F2C P1C F1C 90.4(7) . . ?

_refine_diff_density_max         3.266
_refine_diff_density_min         -2.928
_refine_diff_density_rms         0.195

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PdSiF6
_database_code_depnum_ccdc_archive 'CCDC 2025730'
loop_
_audit_author_name
_audit_author_address
'Dongwon Kim'
;Pusan National University
South Korea
;
_audit_update_record             
;
2020-08-27 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C80 H144 F12 N8 O8 Pd2 S8 Si10'
_chemical_formula_weight         2324.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_H-M_alt        'P 4/n'
_space_group_name_Hall           '-P 4a'

_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+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'

_cell_length_a                   17.554(3)
_cell_length_b                   17.554(3)
_cell_length_c                   18.597(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5730(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9989
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.40

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_F_000             2424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.632
_shelx_estimated_absorpt_T_min   0.873
_shelx_estimated_absorpt_T_max   0.895
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6980
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            158013
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.190
_diffrn_reflns_theta_max         27.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6920
_reflns_number_gt                4977
_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.
 
 _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       'Bruker APEX software'
_computing_cell_refinement       'Bruker APEX software'
_computing_data_reduction        'Bruker APEX software'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.0711P)²+12.4338P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6920
_refine_ls_number_parameters     303
_refine_ls_number_restraints     279
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1646
_refine_ls_wR_factor_gt          0.1341
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_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
S1 S 0.67446(9) 0.41917(9) 0.86627(10) 0.0814(5) Uani 1 1 d . U . . .
Pd1 Pd 0.250000 0.250000 0.69728(3) 0.03220(15) Uani 1 4 d S TU P . .
Si1 Si 0.52595(6) 0.28974(6) 0.54367(6) 0.0390(2) Uani 1 1 d . U . . .
F1 F 0.250000 0.250000 0.5180(7) 0.256(8) Uani 1 4 d S TU P . .
O1 O 0.5903(2) 0.4157(3) 0.8585(3) 0.1061(17) Uani 1 1 d . U . . .
N1 N 0.35726(17) 0.29005(17) 0.69642(14) 0.0331(6) Uani 1 1 d . U . . .
C1 C 0.3910(2) 0.3148(2) 0.75750(19) 0.0402(8) Uani 1 1 d . U . . .
H1 H 0.362294 0.317365 0.800721 0.048 Uiso 1 1 calc R U . . .
S2 S 0.17121(7) -0.01836(7) 0.88791(7) 0.0594(3) Uani 1 1 d . U . . .
Pd2 Pd 0.250000 0.250000 0.18224(3) 0.03077(14) Uani 1 4 d S TU P . .
Si2 Si 0.49281(7) 0.40888(7) 0.32716(6) 0.0435(3) Uani 1 1 d . U . . .
F2 F 0.1859(4) 0.1872(4) 0.4375(6) 0.246(4) Uani 1 1 d . U . . .
O2 O 0.1615(2) -0.1028(2) 0.8950(3) 0.0816(13) Uani 1 1 d . U . . .
N2 N 0.35193(17) 0.30269(17) 0.18056(15) 0.0320(6) Uani 1 1 d . U . . .
C2 C 0.4660(3) 0.3361(3) 0.7578(2) 0.0480(10) Uani 1 1 d . U . . .
H2 H 0.489049 0.354321 0.800747 0.058 Uiso 1 1 calc R U . . .
Si3 Si 0.250000 0.250000 0.43380(10) 0.0380(4) Uani 1 4 d S TU P . .
F3 F 0.250000 0.250000 0.3471(7) 0.229(7) Uani 1 4 d S TU P . .
C3 C 0.5081(2) 0.3308(2) 0.6947(2) 0.0428(9) Uani 1 1 d . U . . .
H3 H 0.560467 0.344386 0.695020 0.051 Uiso 1 1 calc R U . . .
F4 F 0.250000 0.250000 1.0251(2) 0.0554(13) Uani 1 4 d S TU P . .
Si4 Si 0.250000 0.250000 0.93554(8) 0.0225(3) Uani 1 4 d S TU P . .
C4 C 0.4744(2) 0.3056(2) 0.63071(19) 0.0367(8) Uani 1 1 d . U . . .
F5 F 0.18012(14) 0.18472(13) 0.93523(15) 0.0518(6) Uani 1 1 d . U . . .
C5 C 0.3977(2) 0.2867(2) 0.63508(18) 0.0360(8) Uani 1 1 d . U . . .
H5 H 0.372557 0.270567 0.592513 0.043 Uiso 1 1 calc R U . . .
F6 F 0.250000 0.250000 0.8463(2) 0.0659(15) Uani 1 4 d S TU P . .
C6 C 0.4969(3) 0.1941(3) 0.5112(2) 0.0540(11) Uani 1 1 d . U . . .
H6A H 0.528986 0.179271 0.470433 0.081 Uiso 1 1 calc R U . . .
H6B H 0.443459 0.195529 0.495981 0.081 Uiso 1 1 calc R U . . .
H6C H 0.502855 0.156878 0.550120 0.081 Uiso 1 1 calc R U . . .
C7 C 0.6301(2) 0.2931(3) 0.5634(2) 0.0538(11) Uani 1 1 d . U . . .
H7A H 0.658815 0.286523 0.518647 0.081 Uiso 1 1 calc R U . . .
H7B H 0.643259 0.252120 0.596975 0.081 Uiso 1 1 calc R U . . .
H7C H 0.642904 0.342396 0.584967 0.081 Uiso 1 1 calc R U . . .
C8 C 0.4996(3) 0.3628(3) 0.4754(2) 0.0455(9) Uani 1 1 d . U . . .
H8A H 0.446788 0.379933 0.484566 0.055 Uiso 1 1 calc R U . . .
H8AB H 0.533512 0.407531 0.481134 0.055 Uiso 1 1 calc R U . . .
C9 C 0.5053(3) 0.3342(3) 0.3977(2) 0.0526(11) Uani 1 1 d . U . . .
H9A H 0.466188 0.294309 0.390293 0.063 Uiso 1 1 calc R U . . .
H9AB H 0.555792 0.310017 0.390959 0.063 Uiso 1 1 calc R U . . .
C10 C 0.4203(3) 0.4797(3) 0.3542(3) 0.0624(13) Uani 1 1 d . U . . .
H10A H 0.411536 0.515355 0.314530 0.094 Uiso 1 1 calc R U . . .
H10B H 0.438399 0.507731 0.396448 0.094 Uiso 1 1 calc R U . . .
H10C H 0.372635 0.453475 0.365963 0.094 Uiso 1 1 calc R U . . .
C11 C 0.5842(3) 0.4571(4) 0.3051(3) 0.0760(17) Uani 1 1 d . U . . .
H11A H 0.576312 0.492420 0.264994 0.114 Uiso 1 1 calc R U . . .
H11B H 0.622286 0.418884 0.291532 0.114 Uiso 1 1 calc R U . . .
H11C H 0.602247 0.485429 0.347228 0.114 Uiso 1 1 calc R U . . .
C12 C 0.3855(2) 0.3270(2) 0.24146(18) 0.0339(7) Uani 1 1 d . U . . .
H12 H 0.360969 0.317225 0.286052 0.041 Uiso 1 1 calc R U . . .
C13 C 0.4547(2) 0.3660(2) 0.24184(19) 0.0354(8) Uani 1 1 d . U . . .
C14 C 0.4891(2) 0.3774(2) 0.1753(2) 0.0420(9) Uani 1 1 d . U . . .
H14 H 0.536895 0.402751 0.172790 0.050 Uiso 1 1 calc R U . . .
C15 C 0.4547(2) 0.3523(2) 0.1130(2) 0.0452(9) Uani 1 1 d . U . . .
H15 H 0.478524 0.360366 0.067700 0.054 Uiso 1 1 calc R U . . .
C16 C 0.3863(2) 0.3159(2) 0.11694(19) 0.0381(8) Uani 1 1 d . U . . .
H16 H 0.362267 0.299435 0.073889 0.046 Uiso 1 1 calc R U . . .
C17 C 0.7003(4) 0.3434(4) 0.9228(4) 0.0819(17) Uani 1 1 d . U . . .
H17A H 0.755938 0.339553 0.924973 0.123 Uiso 1 1 calc R U . . .
H17B H 0.679185 0.295730 0.903860 0.123 Uiso 1 1 calc R U . . .
H17C H 0.680145 0.352456 0.971221 0.123 Uiso 1 1 calc R U . . .
C18 C 0.7157(5) 0.3805(6) 0.7861(5) 0.125(3) Uani 1 1 d . U . . .
H18A H 0.771246 0.378493 0.791375 0.187 Uiso 1 1 calc R U . . .
H18B H 0.702566 0.412955 0.745065 0.187 Uiso 1 1 calc R U . . .
H18C H 0.695973 0.329022 0.778082 0.187 Uiso 1 1 calc R U . . .
C19 C 0.0978(3) 0.0243(3) 0.9411(3) 0.0718(16) Uani 1 1 d . U . . .
H19A H 0.110055 0.078032 0.949605 0.108 Uiso 1 1 calc R U . . .
H19B H 0.093969 -0.002345 0.987271 0.108 Uiso 1 1 calc R U . . .
H19C H 0.049056 0.020649 0.915598 0.108 Uiso 1 1 calc R U . . .
C20 C 0.2492(3) 0.0065(3) 0.9436(3) 0.0532(11) Uani 1 1 d . U . . .
H20A H 0.255900 0.061972 0.943133 0.080 Uiso 1 1 calc R U . . .
H20B H 0.295554 -0.017970 0.925511 0.080 Uiso 1 1 calc R U . . .
H20C H 0.239259 -0.010567 0.992838 0.080 Uiso 1 1 calc R U . . .


_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
S1 O1 1.486(4) . ?
S1 C17 1.756(6) . ?
S1 C18 1.791(9) . ?
Pd1 N1 2.010(3) 2 ?
Pd1 N1 2.010(3) 4 ?
Pd1 N1 2.010(3) 3 ?
Pd1 N1 2.010(3) . ?
Si1 C6 1.856(5) . ?
Si1 C8 1.864(4) . ?
Si1 C7 1.866(4) . ?
Si1 C4 1.875(4) . ?
F1 Si3 1.567(14) . ?
N1 C5 1.345(4) . ?
N1 C1 1.353(4) . ?
C1 C2 1.369(6) . ?
C1 H1 0.9500 . ?
S2 O2 1.498(4) . ?
S2 C20 1.771(4) . ?
S2 C19 1.789(6) . ?
Pd2 N2 2.014(3) 2 ?
Pd2 N2 2.014(3) 4 ?
Pd2 N2 2.014(3) 3 ?
Pd2 N2 2.014(3) . ?
Si2 C10 1.848(5) . ?
Si2 C11 1.860(5) . ?
Si2 C9 1.868(5) . ?
Si2 C13 1.879(4) . ?
F2 Si3 1.576(5) . ?
N2 C12 1.346(4) . ?
N2 C16 1.348(4) . ?
C2 C3 1.390(6) . ?
C2 H2 0.9500 . ?
Si3 F3 1.612(13) . ?
C3 C4 1.401(5) . ?
C3 H3 0.9500 . ?
F4 Si4 1.666(5) . ?
Si4 F6 1.659(5) . ?
Si4 F5 1.679(2) . ?
Si4 F5 1.679(2) 2 ?
Si4 F5 1.679(2) 4 ?
Si4 F5 1.679(2) 3 ?
C4 C5 1.389(5) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.534(6) . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.394(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(5) . ?
C14 C15 1.379(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.363(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

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 S1 C17 106.5(3) . . ?
O1 S1 C18 107.8(4) . . ?
C17 S1 C18 96.1(4) . . ?
N1 Pd1 N1 89.996(2) 2 4 ?
N1 Pd1 N1 89.996(2) 2 3 ?
N1 Pd1 N1 179.10(15) 4 3 ?
N1 Pd1 N1 179.10(15) 2 . ?
N1 Pd1 N1 89.995(2) 4 . ?
N1 Pd1 N1 89.997(2) 3 . ?
C6 Si1 C8 109.5(2) . . ?
C6 Si1 C7 111.2(2) . . ?
C8 Si1 C7 110.8(2) . . ?
C6 Si1 C4 106.41(19) . . ?
C8 Si1 C4 111.51(18) . . ?
C7 Si1 C4 107.34(19) . . ?
C5 N1 C1 119.6(3) . . ?
C5 N1 Pd1 119.1(2) . . ?
C1 N1 Pd1 121.1(2) . . ?
N1 C1 C2 120.9(3) . . ?
N1 C1 H1 119.6 . . ?
C2 C1 H1 119.6 . . ?
O2 S2 C20 106.3(2) . . ?
O2 S2 C19 106.5(3) . . ?
C20 S2 C19 97.5(3) . . ?
N2 Pd2 N2 89.986(3) 2 4 ?
N2 Pd2 N2 89.986(3) 2 3 ?
N2 Pd2 N2 178.22(16) 4 3 ?
N2 Pd2 N2 178.22(16) 2 . ?
N2 Pd2 N2 89.986(3) 4 . ?
N2 Pd2 N2 89.986(3) 3 . ?
C10 Si2 C11 110.4(3) . . ?
C10 Si2 C9 111.2(2) . . ?
C11 Si2 C9 111.9(3) . . ?
C10 Si2 C13 104.7(2) . . ?
C11 Si2 C13 107.7(2) . . ?
C9 Si2 C13 110.70(19) . . ?
C12 N2 C16 119.2(3) . . ?
C12 N2 Pd2 121.4(2) . . ?
C16 N2 Pd2 119.3(2) . . ?
C1 C2 C3 119.3(4) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
F1 Si3 F2 87.5(4) . . ?
F1 Si3 F2 87.5(4) . 2 ?
F2 Si3 F2 175.0(8) . 2 ?
F1 Si3 F2 87.5(4) . 4 ?
F2 Si3 F2 89.89(4) . 4 ?
F2 Si3 F2 89.89(4) 2 4 ?
F1 Si3 F2 87.5(4) . 3 ?
F2 Si3 F2 89.89(3) . 3 ?
F2 Si3 F2 89.89(4) 2 3 ?
F2 Si3 F2 175.0(8) 4 3 ?
F1 Si3 F3 180.0 . . ?
F2 Si3 F3 92.5(4) . . ?
F2 Si3 F3 92.5(4) 2 . ?
F2 Si3 F3 92.5(4) 4 . ?
F2 Si3 F3 92.5(4) 3 . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
F6 Si4 F4 180.0 . . ?
F6 Si4 F5 89.80(11) . . ?
F4 Si4 F5 90.20(11) . . ?
F6 Si4 F5 89.80(11) . 2 ?
F4 Si4 F5 90.20(11) . 2 ?
F5 Si4 F5 179.6(2) . 2 ?
F6 Si4 F5 89.80(11) . 4 ?
F4 Si4 F5 90.20(11) . 4 ?
F5 Si4 F5 90.000(1) . 4 ?
F5 Si4 F5 89.999(1) 2 4 ?
F6 Si4 F5 89.80(11) . 3 ?
F4 Si4 F5 90.20(11) . 3 ?
F5 Si4 F5 89.998(1) . 3 ?
F5 Si4 F5 89.999(1) 2 3 ?
F5 Si4 F5 179.6(2) 4 3 ?
C5 C4 C3 115.8(3) . . ?
C5 C4 Si1 118.9(3) . . ?
C3 C4 Si1 125.3(3) . . ?
N1 C5 C4 123.5(3) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 Si1 113.6(3) . . ?
C9 C8 H8A 108.9 . . ?
Si1 C8 H8A 108.9 . . ?
C9 C8 H8AB 108.9 . . ?
Si1 C8 H8AB 108.9 . . ?
H8A C8 H8AB 107.7 . . ?
C8 C9 Si2 115.1(3) . . ?
C8 C9 H9A 108.5 . . ?
Si2 C9 H9A 108.5 . . ?
C8 C9 H9AB 108.5 . . ?
Si2 C9 H9AB 108.5 . . ?
H9A C9 H9AB 107.5 . . ?
Si2 C10 H10A 109.5 . . ?
Si2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C13 122.8(3) . . ?
N2 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C14 C13 C12 116.4(3) . . ?
C14 C13 Si2 122.5(3) . . ?
C12 C13 Si2 120.8(3) . . ?
C15 C14 C13 120.7(4) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C16 C15 C14 119.3(4) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
N2 C16 C15 121.5(3) . . ?
N2 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
S1 C17 H17A 109.5 . . ?
S1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
S1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S1 C18 H18A 109.5 . . ?
S1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
S1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
S2 C19 H19A 109.5 . . ?
S2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
S2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S2 C20 H20A 109.5 . . ?
S2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
S2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -0.3(6) . . . . ?
Pd1 N1 C1 C2 174.6(3) . . . . ?
N1 C1 C2 C3 -1.2(6) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C2 C3 C4 Si1 -175.8(3) . . . . ?
C6 Si1 C4 C5 -44.4(4) . . . . ?
C8 Si1 C4 C5 74.9(3) . . . . ?
C7 Si1 C4 C5 -163.6(3) . . . . ?
C6 Si1 C4 C3 131.1(4) . . . . ?
C8 Si1 C4 C3 -109.6(4) . . . . ?
C7 Si1 C4 C3 11.9(4) . . . . ?
C1 N1 C5 C4 1.8(6) . . . . ?
Pd1 N1 C5 C4 -173.2(3) . . . . ?
C3 C4 C5 N1 -1.5(6) . . . . ?
Si1 C4 C5 N1 174.4(3) . . . . ?
C6 Si1 C8 C9 -33.7(4) . . . . ?
C7 Si1 C8 C9 89.3(4) . . . . ?
C4 Si1 C8 C9 -151.2(3) . . . . ?
Si1 C8 C9 Si2 -171.8(2) . . . . ?
C10 Si2 C9 C8 -36.9(4) . . . . ?
C11 Si2 C9 C8 87.0(4) . . . . ?
C13 Si2 C9 C8 -152.9(3) . . . . ?
C16 N2 C12 C13 0.3(5) . . . . ?
Pd2 N2 C12 C13 -177.7(3) . . . . ?
N2 C12 C13 C14 -1.4(6) . . . . ?
N2 C12 C13 Si2 172.5(3) . . . . ?
C10 Si2 C13 C14 112.2(4) . . . . ?
C11 Si2 C13 C14 -5.2(4) . . . . ?
C9 Si2 C13 C14 -127.8(4) . . . . ?
C10 Si2 C13 C12 -61.4(4) . . . . ?
C11 Si2 C13 C12 -178.9(4) . . . . ?
C9 Si2 C13 C12 58.5(4) . . . . ?
C12 C13 C14 C15 1.3(6) . . . . ?
Si2 C13 C14 C15 -172.6(3) . . . . ?
C13 C14 C15 C16 -0.1(7) . . . . ?
C12 N2 C16 C15 1.0(6) . . . . ?
Pd2 N2 C16 C15 179.0(3) . . . . ?
C14 C15 C16 N2 -1.1(6) . . . . ?

_refine_diff_density_max         1.681
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.096

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ClO4_sq
_database_code_depnum_ccdc_archive 'CCDC 2025727'
loop_
_audit_author_name
_audit_author_address
'Dongwon Kim'
;Pusan National University
South Korea
;
_audit_update_record             
;
2020-08-27 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H94 Cl4 N8 O16 Pd2 Si8'
_chemical_formula_weight         1810.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   16.8262(16)
_cell_length_b                   20.1636(16)
_cell_length_c                   55.633(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18875(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9878
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      23.06

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             7472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    0.652
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.6978
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            80848
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_theta_min         1.921
_diffrn_reflns_theta_max         27.677
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11015
_reflns_number_gt                8450
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX software'
_computing_cell_refinement       'Bruker APEX software'
_computing_data_reduction        'Bruker APEX software'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1267P)²+52.0965P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3637 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.523(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11015
_refine_ls_number_parameters     530
_refine_ls_number_restraints     559
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1996
_refine_ls_wR_factor_gt          0.1780
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001

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 0.250000 0.750000 0.41324(2) 0.0455(3) Uani 1 2 d S TU P . .
C1 C 0.1960(10) 0.6165(7) 0.5821(3) 0.090(5) Uani 1 1 d . U . . .
H1 H 0.169782 0.641724 0.594191 0.108 Uiso 1 1 calc R U . . .
N1 N 0.2626(6) 0.6509(5) 0.4140(3) 0.055(2) Uani 1 1 d . U . . .
Pd2 Pd 0.250000 0.750000 0.56681(2) 0.0447(3) Uani 1 2 d S TU P . .
C2 C 0.1849(12) 0.5502(9) 0.5825(4) 0.114(6) Uani 1 1 d . U . . .
H2 H 0.149864 0.529343 0.593566 0.137 Uiso 1 1 calc R U . . .
N2 N 0.2390(6) 0.6489(5) 0.5668(2) 0.052(2) Uani 1 1 d . U . . .
C3 C 0.2261(12) 0.5162(7) 0.5665(4) 0.096(5) Uani 1 1 d . U . . .
H3 H 0.224927 0.469104 0.567210 0.116 Uiso 1 1 calc R U . . .
N3 N 0.3714(6) 0.7410(4) 0.5663(2) 0.049(2) Uani 1 1 d . U . . .
Si04 Si 0.5460(2) 0.68480(18) 0.45787(8) 0.0653(10) Uani 1 1 d . U . . .
C4 C 0.2709(8) 0.5465(6) 0.5487(3) 0.065(3) Uani 1 1 d . U . . .
N4 N 0.3692(5) 0.7596(4) 0.4146(2) 0.048(2) Uani 1 1 d . U . . .
Si05 Si 0.54712(18) 0.81473(16) 0.52177(8) 0.0584(9) Uani 1 1 d . U . . .
C5 C 0.2740(7) 0.6144(6) 0.5494(2) 0.052(3) Uani 1 1 d . U . . .
H5 H 0.301664 0.637443 0.537042 0.063 Uiso 1 1 calc R U . . .
Si06 Si 0.3311(3) 0.5039(2) 0.52311(10) 0.0848(16) Uani 1 1 d D U . . .
C6 C 0.3647(11) 0.4209(7) 0.5344(4) 0.106(5) Uani 1 1 d . U . . .
H6A H 0.394308 0.397976 0.521649 0.160 Uiso 1 1 calc R U . . .
H6B H 0.318322 0.394328 0.538898 0.160 Uiso 1 1 calc R U . . .
H6C H 0.399164 0.426912 0.548394 0.160 Uiso 1 1 calc R U . . .
Si07 Si 0.1773(3) 0.50099(17) 0.45582(10) 0.0708(12) Uani 1 1 d D U . . .
C7 C 0.4167(9) 0.5578(7) 0.5174(3) 0.098(5) Uani 1 1 d . U . . .
H7A H 0.455202 0.534386 0.507272 0.146 Uiso 1 1 calc R U . . .
H7B H 0.441779 0.569728 0.532706 0.146 Uiso 1 1 calc R U . . .
H7C H 0.398916 0.598145 0.509183 0.146 Uiso 1 1 calc R U . . .
C10 C 0.1505(10) 0.4176(7) 0.4473(4) 0.114(6) Uani 1 1 d . U . . .
H10A H 0.163356 0.401602 0.431718 0.136 Uiso 1 1 calc R U . . .
H10B H 0.123519 0.389765 0.458386 0.136 Uiso 1 1 calc R U . . .
C11 C 0.0956(9) 0.5505(8) 0.4663(3) 0.089(4) Uani 1 1 d . U . . .
H11A H 0.064312 0.565817 0.452496 0.134 Uiso 1 1 calc R U . . .
H11B H 0.116031 0.588881 0.475143 0.134 Uiso 1 1 calc R U . . .
H11C H 0.061878 0.523813 0.476892 0.134 Uiso 1 1 calc R U . . .
C13 C 0.2275(6) 0.5452(6) 0.4326(3) 0.057(3) Uani 1 1 d . U . . .
C12 C 0.2258(6) 0.6153(5) 0.4304(2) 0.047(2) Uani 1 1 d . U . . .
H12 H 0.195229 0.638838 0.441983 0.056 Uiso 1 1 calc R U . . .
C14 C 0.2768(13) 0.5140(8) 0.4159(4) 0.101(5) Uani 1 1 d . U . . .
H14 H 0.288057 0.467972 0.417355 0.121 Uiso 1 1 calc R U . . .
C15 C 0.3094(11) 0.5505(8) 0.3972(4) 0.112(6) Uani 1 1 d . U . . .
H15 H 0.335746 0.527240 0.384662 0.134 Uiso 1 1 calc R U . . .
C16 C 0.3056(8) 0.6208(7) 0.3957(3) 0.080(4) Uani 1 1 d . U . . .
H16 H 0.330587 0.645295 0.383251 0.096 Uiso 1 1 calc R U . . .
C19 C 0.5293(9) 0.7299(7) 0.5647(3) 0.071(3) Uani 1 1 d . U . . .
H19 H 0.585539 0.732597 0.566092 0.085 Uiso 1 1 calc R U . . .
C18 C 0.4926(8) 0.6945(9) 0.5787(3) 0.079(4) Uani 1 1 d . U . . .
H18 H 0.519109 0.660508 0.587383 0.094 Uiso 1 1 calc R U . . .
C17 C 0.4124(8) 0.7045(7) 0.5816(2) 0.067(3) Uani 1 1 d . U . . .
H17 H 0.385919 0.684703 0.594877 0.081 Uiso 1 1 calc R U . . .
C20 C 0.4911(6) 0.7665(6) 0.5469(2) 0.045(2) Uani 1 1 d . U . . .
C21 C 0.4148(6) 0.7704(5) 0.54801(19) 0.044(2) Uani 1 1 d . U . . .
H21 H 0.387384 0.794278 0.535848 0.052 Uiso 1 1 calc R U . . .
C22 C 0.6545(8) 0.7920(11) 0.5254(4) 0.112(6) Uani 1 1 d . U . . .
H22A H 0.677796 0.818494 0.538428 0.167 Uiso 1 1 calc R U . . .
H22B H 0.682934 0.800936 0.510418 0.167 Uiso 1 1 calc R U . . .
H22C H 0.658800 0.744818 0.529405 0.167 Uiso 1 1 calc R U . . .
C23 C 0.5203(12) 0.9072(7) 0.5262(4) 0.099(5) Uani 1 1 d . U . . .
H23A H 0.547876 0.934014 0.514084 0.149 Uiso 1 1 calc R U . . .
H23B H 0.536590 0.921500 0.542284 0.149 Uiso 1 1 calc R U . . .
H23C H 0.462742 0.913056 0.524416 0.149 Uiso 1 1 calc R U . . .
C24 C 0.5105(7) 0.7856(8) 0.4922(3) 0.067(3) Uani 1 1 d . U . . .
H24A H 0.456094 0.803146 0.489888 0.081 Uiso 1 1 calc R U . . .
H24B H 0.544482 0.805450 0.479579 0.081 Uiso 1 1 calc R U . . .
C25 C 0.5082(7) 0.7114(7) 0.4882(3) 0.072(3) Uani 1 1 d . U . . .
H25A H 0.452798 0.695788 0.490124 0.087 Uiso 1 1 calc R U . . .
H25B H 0.540647 0.689570 0.500828 0.087 Uiso 1 1 calc R U . . .
C26 C 0.6544(8) 0.7000(7) 0.4581(4) 0.096(5) Uani 1 1 d . U . . .
H26A H 0.675160 0.696614 0.441681 0.144 Uiso 1 1 calc R U . . .
H26B H 0.680538 0.666979 0.468316 0.144 Uiso 1 1 calc R U . . .
H26C H 0.664993 0.744532 0.464405 0.144 Uiso 1 1 calc R U . . .
C27 C 0.5304(10) 0.5981(7) 0.4532(3) 0.091(4) Uani 1 1 d . U . . .
H27A H 0.536520 0.587812 0.436082 0.137 Uiso 1 1 calc R U . . .
H27B H 0.476593 0.586177 0.458411 0.137 Uiso 1 1 calc R U . . .
H27C H 0.569353 0.572818 0.462526 0.137 Uiso 1 1 calc R U . . .
C28 C 0.4077(7) 0.7297(5) 0.4309(2) 0.049(2) Uani 1 1 d . U . . .
H28 H 0.377841 0.703646 0.441934 0.058 Uiso 1 1 calc R U . . .
C29 C 0.4959(7) 0.7317(7) 0.4346(3) 0.056(3) Uani 1 1 d . U . . .
C30 C 0.5349(7) 0.7751(7) 0.4186(3) 0.062(3) Uani 1 1 d . U . . .
H30 H 0.589326 0.785840 0.420822 0.074 Uiso 1 1 calc R U . . .
C31 C 0.4887(8) 0.8040(9) 0.3980(3) 0.080(4) Uani 1 1 d . U . . .
H31 H 0.515389 0.825468 0.385178 0.096 Uiso 1 1 calc R U . . .
C32 C 0.4065(8) 0.7988(6) 0.3981(2) 0.068(3) Uani 1 1 d . U . . .
H32 H 0.376120 0.822731 0.386580 0.081 Uiso 1 1 calc R U . . .
Cl3 Cl 0.250000 0.750000 0.63694(15) 0.155(5) Uani 1 2 d DS TU P . .
O6 O 0.2900(11) 0.6978(8) 0.6241(4) 0.192(7) Uani 1 1 d D U . . .
O7 O 0.250000 0.750000 0.6632(3) 0.214(14) Uani 1 2 d DS TU P . .
O3 O 0.3212(16) 0.7926(14) 0.6276(5) 0.196(12) Uani 0.5 1 d D U P . .
Cl2 Cl 0.250000 0.750000 0.34291(15) 0.173(5) Uani 1 2 d DS TU P . .
O1 O 0.2601(18) 0.8085(10) 0.3587(5) 0.180(10) Uani 0.5 1 d D U P . .
O8 O 0.3290(10) 0.7108(11) 0.3455(3) 0.161(8) Uani 0.5 1 d D U P . .
O4 O 0.2620(14) 0.7836(9) 0.3197(2) 0.202(8) Uani 1 1 d D U . . .
Cl1 Cl 0.250000 0.750000 0.49012(16) 0.0629(6) Uani 1 2 d DS TU P . .
O5 O 0.250000 0.750000 0.4666(2) 0.164(9) Uani 1 2 d DS TU P . .
O2 O 0.3050(11) 0.6971(8) 0.5003(4) 0.124(7) Uani 0.5 1 d D U P . .
O9 O 0.2968(15) 0.8149(8) 0.4995(3) 0.226(8) Uani 1 1 d D U . . .
C8 C 0.2590(9) 0.4695(7) 0.4996(2) 0.065(4) Uani 0.653(16) 1 d D U P A 1
H8A H 0.270120 0.421809 0.497165 0.078 Uiso 0.653(16) 1 calc R U P A 1
H8B H 0.203989 0.473593 0.505802 0.078 Uiso 0.653(16) 1 calc R U P A 1
C9 C 0.2645(12) 0.5040(10) 0.4764(3) 0.081(4) Uani 0.653(16) 1 d D U P A 1
H9A H 0.310757 0.485497 0.467675 0.097 Uiso 0.653(16) 1 calc R U P A 1
H9B H 0.276437 0.551180 0.479721 0.097 Uiso 0.653(16) 1 calc R U P A 1
C1B C 0.2906(17) 0.5317(16) 0.4919(4) 0.071(6) Uani 0.347(16) 1 d D U P A 2
H1B1 H 0.301911 0.579455 0.489595 0.085 Uiso 0.347(16) 1 calc R U P A 2
H1B2 H 0.318511 0.506822 0.479115 0.085 Uiso 0.347(16) 1 calc R U P A 2
C2B C 0.1999(18) 0.5198(18) 0.4896(3) 0.074(6) Uani 0.347(16) 1 d D U P A 2
H2B1 H 0.170255 0.559655 0.494885 0.089 Uiso 0.347(16) 1 calc R U P A 2
H2B2 H 0.183527 0.481896 0.499767 0.089 Uiso 0.347(16) 1 calc R U P A 2
Cl4 Cl -0.0134(6) 0.5821(9) 0.6253(3) 0.218(8) Uani 0.5 1 d D U P B 3
O10 O 0.0608(10) 0.5559(19) 0.6355(6) 0.244(15) Uani 0.5 1 d D U P B 3
O14 O -0.0566(18) 0.5266(16) 0.6122(6) 0.282(18) Uani 0.5 1 d D U P B 3
O11 O -0.0691(14) 0.6063(13) 0.6446(5) 0.209(14) Uani 0.5 1 d D U P B 3
O13 O -0.0032(16) 0.6376(16) 0.6072(6) 0.262(16) Uani 0.5 1 d D U P B 3


_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 2.010(10) 14_565 ?
Pd1 N1 2.010(10) . ?
Pd1 N4 2.016(9) 14_565 ?
Pd1 N4 2.016(9) . ?
C1 N2 1.294(17) . ?
C1 C2 1.35(2) . ?
C1 H1 0.9500 . ?
N1 C12 1.317(17) . ?
N1 C16 1.386(17) . ?
Pd2 N2 2.048(10) 14_565 ?
Pd2 N2 2.048(10) . ?
Pd2 N3 2.050(9) 14_565 ?
Pd2 N3 2.050(9) . ?
C2 C3 1.32(3) . ?
C2 H2 0.9500 . ?
N2 C5 1.332(17) . ?
C3 C4 1.39(2) . ?
C3 H3 0.9500 . ?
N3 C17 1.320(15) . ?
N3 C21 1.387(13) . ?
Si04 C27 1.787(17) . ?
Si04 C29 1.814(15) . ?
Si04 C26 1.850(13) . ?
Si04 C25 1.883(18) . ?
C4 C5 1.371(18) . ?
C4 Si06 1.947(17) . ?
N4 C28 1.271(15) . ?
N4 C32 1.365(14) . ?
Si05 C24 1.852(16) . ?
Si05 C22 1.874(14) . ?
Si05 C23 1.935(16) . ?
Si05 C20 1.948(13) . ?
C5 H5 0.9500 . ?
Si06 C7 1.832(15) . ?
Si06 C6 1.874(16) . ?
Si06 C8 1.914(11) . ?
Si06 C1B 1.947(13) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Si07 C13 1.783(14) . ?
Si07 C11 1.796(15) . ?
Si07 C10 1.804(16) . ?
Si07 C9 1.86(2) . ?
Si07 C2B 1.954(14) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C13 C14 1.39(2) . ?
C13 C12 1.420(16) . ?
C12 H12 0.9500 . ?
C14 C15 1.39(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.42(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C19 C18 1.22(2) . ?
C19 C20 1.392(18) . ?
C19 H19 0.9500 . ?
C18 C17 1.374(18) . ?
C18 H18 0.9500 . ?
C17 H17 0.9500 . ?
C20 C21 1.287(14) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.514(12) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.497(16) . ?
C28 H28 0.9500 . ?
C29 C30 1.41(2) . ?
C30 C31 1.50(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(18) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
Cl3 O6 1.440(12) 14_565 ?
Cl3 O6 1.440(12) . ?
Cl3 O7 1.459(13) . ?
Cl3 O3 1.565(14) 14_565 ?
Cl3 O3 1.565(14) . ?
Cl2 O4 1.473(12) . ?
Cl2 O4 1.473(12) 14_565 ?
Cl2 O1 1.480(12) . ?
Cl2 O1 1.480(12) 14_565 ?
Cl2 O8 1.554(13) 14_565 ?
Cl2 O8 1.554(13) . ?
O1 O8 1.71(3) 14_565 ?
O4 O4 1.41(4) 14_565 ?
Cl1 O5 1.310(14) . ?
Cl1 O2 1.522(10) . ?
Cl1 O2 1.522(10) 14_565 ?
Cl1 O9 1.614(16) . ?
Cl1 O9 1.614(16) 14_565 ?
O2 O9 1.73(3) 14_565 ?
C8 C9 1.469(13) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C1B C2B 1.550(14) . ?
C1B H1B1 0.9900 . ?
C1B H1B2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
Cl4 O10 1.469(14) . ?
Cl4 O11 1.505(11) . ?
Cl4 O13 1.515(14) . ?
Cl4 O14 1.522(12) . ?

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
N1 Pd1 N1 177.6(8) 14_565 . ?
N1 Pd1 N4 89.4(4) 14_565 14_565 ?
N1 Pd1 N4 90.5(4) . 14_565 ?
N1 Pd1 N4 90.5(4) 14_565 . ?
N1 Pd1 N4 89.4(4) . . ?
N4 Pd1 N4 175.8(7) 14_565 . ?
N2 C1 C2 125.9(16) . . ?
N2 C1 H1 117.0 . . ?
C2 C1 H1 117.0 . . ?
C12 N1 C16 121.1(10) . . ?
C12 N1 Pd1 120.4(8) . . ?
C16 N1 Pd1 118.3(10) . . ?
N2 Pd2 N2 179.9(7) 14_565 . ?
N2 Pd2 N3 90.1(3) 14_565 14_565 ?
N2 Pd2 N3 89.9(4) . 14_565 ?
N2 Pd2 N3 89.9(4) 14_565 . ?
N2 Pd2 N3 90.1(3) . . ?
N3 Pd2 N3 178.4(6) 14_565 . ?
C3 C2 C1 115.6(16) . . ?
C3 C2 H2 122.2 . . ?
C1 C2 H2 122.2 . . ?
C1 N2 C5 117.7(11) . . ?
C1 N2 Pd2 123.6(10) . . ?
C5 N2 Pd2 118.6(9) . . ?
C2 C3 C4 122.6(14) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 H3 118.7 . . ?
C17 N3 C21 115.9(10) . . ?
C17 N3 Pd2 124.1(8) . . ?
C21 N3 Pd2 119.8(8) . . ?
C27 Si04 C29 109.7(7) . . ?
C27 Si04 C26 108.0(7) . . ?
C29 Si04 C26 112.2(7) . . ?
C27 Si04 C25 111.1(8) . . ?
C29 Si04 C25 109.7(6) . . ?
C26 Si04 C25 106.2(8) . . ?
C5 C4 C3 116.2(14) . . ?
C5 C4 Si06 116.1(11) . . ?
C3 C4 Si06 127.7(11) . . ?
C28 N4 C32 121.5(10) . . ?
C28 N4 Pd1 119.2(8) . . ?
C32 N4 Pd1 119.3(9) . . ?
C24 Si05 C22 109.9(8) . . ?
C24 Si05 C23 109.9(7) . . ?
C22 Si05 C23 116.5(9) . . ?
C24 Si05 C20 108.6(6) . . ?
C22 Si05 C20 105.4(6) . . ?
C23 Si05 C20 106.1(8) . . ?
N2 C5 C4 121.6(13) . . ?
N2 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C7 Si06 C6 110.5(7) . . ?
C7 Si06 C8 126.5(8) . . ?
C6 Si06 C8 95.5(7) . . ?
C7 Si06 C4 105.9(7) . . ?
C6 Si06 C4 107.9(8) . . ?
C8 Si06 C4 109.2(7) . . ?
C7 Si06 C1B 87.1(12) . . ?
C6 Si06 C1B 131.3(12) . . ?
C4 Si06 C1B 110.0(11) . . ?
Si06 C6 H6A 109.5 . . ?
Si06 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si06 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C13 Si07 C11 108.6(6) . . ?
C13 Si07 C10 113.1(9) . . ?
C11 Si07 C10 114.3(8) . . ?
C13 Si07 C9 93.3(7) . . ?
C11 Si07 C9 112.7(8) . . ?
C10 Si07 C9 112.9(9) . . ?
C13 Si07 C2B 120.6(11) . . ?
C11 Si07 C2B 74.3(12) . . ?
C10 Si07 C2B 118.8(13) . . ?
Si06 C7 H7A 109.5 . . ?
Si06 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si06 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si07 C10 H10A 120.0 . . ?
Si07 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
Si07 C11 H11A 109.5 . . ?
Si07 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si07 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C13 C12 114.0(12) . . ?
C14 C13 Si07 122.6(11) . . ?
C12 C13 Si07 123.3(9) . . ?
N1 C12 C13 126.2(10) . . ?
N1 C12 H12 116.9 . . ?
C13 C12 H12 116.9 . . ?
C15 C14 C13 119.6(14) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 123.7(15) . . ?
C14 C15 H15 118.2 . . ?
C16 C15 H15 118.2 . . ?
N1 C16 C15 114.7(15) . . ?
N1 C16 H16 122.6 . . ?
C15 C16 H16 122.6 . . ?
C18 C19 C20 121.8(13) . . ?
C18 C19 H19 119.1 . . ?
C20 C19 H19 119.1 . . ?
C19 C18 C17 119.1(13) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
N3 C17 C18 121.3(12) . . ?
N3 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C21 C20 C19 117.4(12) . . ?
C21 C20 Si05 119.0(9) . . ?
C19 C20 Si05 123.5(9) . . ?
C20 C21 N3 122.2(11) . . ?
C20 C21 H21 118.9 . . ?
N3 C21 H21 118.9 . . ?
Si05 C22 H22A 109.5 . . ?
Si05 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si05 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si05 C23 H23A 109.5 . . ?
Si05 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si05 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 Si05 116.8(7) . . ?
C25 C24 H24A 108.1 . . ?
Si05 C24 H24A 108.1 . . ?
C25 C24 H24B 108.1 . . ?
Si05 C24 H24B 108.1 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 Si04 113.8(8) . . ?
C24 C25 H25A 108.8 . . ?
Si04 C25 H25A 108.8 . . ?
C24 C25 H25B 108.8 . . ?
Si04 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
Si04 C26 H26A 109.5 . . ?
Si04 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si04 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si04 C27 H27A 109.5 . . ?
Si04 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si04 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N4 C28 C29 126.1(10) . . ?
N4 C28 H28 117.0 . . ?
C29 C28 H28 117.0 . . ?
C30 C29 C28 113.2(12) . . ?
C30 C29 Si04 123.9(9) . . ?
C28 C29 Si04 122.9(10) . . ?
C29 C30 C31 118.7(11) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C32 C31 C30 119.1(12) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
N4 C32 C31 120.2(12) . . ?
N4 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
O6 Cl3 O6 120(2) 14_565 . ?
O6 Cl3 O7 119.8(10) 14_565 . ?
O6 Cl3 O7 119.8(10) . . ?
O6 Cl3 O3 83.0(14) 14_565 14_565 ?
O6 Cl3 O3 78.0(15) . 14_565 ?
O7 Cl3 O3 109.5(12) . 14_565 ?
O6 Cl3 O3 78.0(15) 14_565 . ?
O6 Cl3 O3 83.0(14) . . ?
O7 Cl3 O3 109.5(12) . . ?
O3 Cl3 O3 141(2) 14_565 . ?
O4 Cl2 O4 57.4(14) . 14_565 ?
O4 Cl2 O1 97.9(14) . . ?
O4 Cl2 O1 154.5(14) 14_565 . ?
O4 Cl2 O1 154.5(14) . 14_565 ?
O4 Cl2 O1 97.9(14) 14_565 14_565 ?
O1 Cl2 O1 107(2) . 14_565 ?
O4 Cl2 O8 88.1(12) . 14_565 ?
O4 Cl2 O8 101.5(12) 14_565 14_565 ?
O1 Cl2 O8 68.7(11) . 14_565 ?
O1 Cl2 O8 104.5(10) 14_565 14_565 ?
O4 Cl2 O8 101.5(12) . . ?
O4 Cl2 O8 88.1(12) 14_565 . ?
O1 Cl2 O8 104.5(10) . . ?
O1 Cl2 O8 68.7(11) 14_565 . ?
O8 Cl2 O8 169.2(16) 14_565 . ?
Cl2 O1 O8 57.7(8) . 14_565 ?
Cl2 O8 O1 53.6(8) . 14_565 ?
O4 O4 Cl2 61.3(7) 14_565 . ?
O5 Cl1 O2 111.9(9) . . ?
O5 Cl1 O2 111.9(9) . 14_565 ?
O2 Cl1 O2 136.3(18) . 14_565 ?
O5 Cl1 O9 108.8(9) . . ?
O2 Cl1 O9 98.7(8) . . ?
O2 Cl1 O9 66.9(11) 14_565 . ?
O5 Cl1 O9 108.8(9) . 14_565 ?
O2 Cl1 O9 66.9(11) . 14_565 ?
O2 Cl1 O9 98.7(8) 14_565 14_565 ?
O9 Cl1 O9 142.3(17) . 14_565 ?
Cl1 O2 O9 59.1(7) . 14_565 ?
Cl1 O9 O2 54.0(8) . 14_565 ?
C9 C8 Si06 112.9(12) . . ?
C9 C8 H8A 109.0 . . ?
Si06 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
Si06 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 Si07 118.4(14) . . ?
C8 C9 H9A 107.7 . . ?
Si07 C9 H9A 107.7 . . ?
C8 C9 H9B 107.7 . . ?
Si07 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
C2B C1B Si06 112.0(16) . . ?
C2B C1B H1B1 109.2 . . ?
Si06 C1B H1B1 109.2 . . ?
C2B C1B H1B2 109.2 . . ?
Si06 C1B H1B2 109.2 . . ?
H1B1 C1B H1B2 107.9 . . ?
C1B C2B Si07 107.5(13) . . ?
C1B C2B H2B1 110.2 . . ?
Si07 C2B H2B1 110.2 . . ?
C1B C2B H2B2 110.2 . . ?
Si07 C2B H2B2 110.2 . . ?
H2B1 C2B H2B2 108.5 . . ?
O10 Cl4 O11 111.7(12) . . ?
O10 Cl4 O13 115.2(19) . . ?
O11 Cl4 O13 107.8(11) . . ?
O10 Cl4 O14 109.0(12) . . ?
O11 Cl4 O14 106.5(10) . . ?
O13 Cl4 O14 106.2(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 C3 4(3) . . . . ?
C2 C1 N2 C5 2(3) . . . . ?
C2 C1 N2 Pd2 178.0(16) . . . . ?
C1 C2 C3 C4 -7(3) . . . . ?
C2 C3 C4 C5 4(3) . . . . ?
C2 C3 C4 Si06 -177.4(17) . . . . ?
C1 N2 C5 C4 -6(2) . . . . ?
Pd2 N2 C5 C4 178.1(9) . . . . ?
C3 C4 C5 N2 3(2) . . . . ?
Si06 C4 C5 N2 -176.0(9) . . . . ?
C11 Si07 C13 C14 -159.9(16) . . . . ?
C10 Si07 C13 C14 -31.9(18) . . . . ?
C9 Si07 C13 C14 84.7(17) . . . . ?
C2B Si07 C13 C14 118(2) . . . . ?
C11 Si07 C13 C12 25.1(14) . . . . ?
C10 Si07 C13 C12 153.2(12) . . . . ?
C9 Si07 C13 C12 -90.2(12) . . . . ?
C2B Si07 C13 C12 -57.3(17) . . . . ?
C16 N1 C12 C13 3(2) . . . . ?
Pd1 N1 C12 C13 177.9(10) . . . . ?
C14 C13 C12 N1 3(2) . . . . ?
Si07 C13 C12 N1 178.7(11) . . . . ?
C12 C13 C14 C15 -9(3) . . . . ?
Si07 C13 C14 C15 175.3(15) . . . . ?
C13 C14 C15 C16 10(3) . . . . ?
C12 N1 C16 C15 -3(2) . . . . ?
Pd1 N1 C16 C15 -178.0(12) . . . . ?
C14 C15 C16 N1 -3(3) . . . . ?
C20 C19 C18 C17 -19(3) . . . . ?
C21 N3 C17 C18 -3(2) . . . . ?
Pd2 N3 C17 C18 172.6(12) . . . . ?
C19 C18 C17 N3 15(3) . . . . ?
C18 C19 C20 C21 11(2) . . . . ?
C18 C19 C20 Si05 -172.0(15) . . . . ?
C19 C20 C21 N3 1(2) . . . . ?
Si05 C20 C21 N3 -175.8(9) . . . . ?
C17 N3 C21 C20 -4.9(18) . . . . ?
Pd2 N3 C21 C20 179.6(10) . . . . ?
C22 Si05 C24 C25 65.0(12) . . . . ?
C23 Si05 C24 C25 -165.5(11) . . . . ?
C20 Si05 C24 C25 -49.8(12) . . . . ?
Si05 C24 C25 Si04 -136.6(5) . . . . ?
C27 Si04 C25 C24 -173.0(10) . . . . ?
C29 Si04 C25 C24 -51.6(12) . . . . ?
C26 Si04 C25 C24 69.8(11) . . . . ?
C32 N4 C28 C29 -1(2) . . . . ?
Pd1 N4 C28 C29 -179.7(10) . . . . ?
N4 C28 C29 C30 4(2) . . . . ?
N4 C28 C29 Si04 -177.7(10) . . . . ?
C27 Si04 C29 C30 -120.5(15) . . . . ?
C26 Si04 C29 C30 -0.5(17) . . . . ?
C25 Si04 C29 C30 117.3(14) . . . . ?
C27 Si04 C29 C28 61.7(14) . . . . ?
C26 Si04 C29 C28 -178.3(12) . . . . ?
C25 Si04 C29 C28 -60.5(14) . . . . ?
C28 C29 C30 C31 -10(2) . . . . ?
Si04 C29 C30 C31 171.9(13) . . . . ?
C29 C30 C31 C32 13(2) . . . . ?
C28 N4 C32 C31 4(2) . . . . ?
Pd1 N4 C32 C31 -177.4(12) . . . . ?
C30 C31 C32 N4 -10(2) . . . . ?
O4 Cl2 O1 O8 84.8(13) . . . 14_565 ?
O4 Cl2 O1 O8 71(4) 14_565 . . 14_565 ?
O1 Cl2 O1 O8 -99.3(12) 14_565 . . 14_565 ?
O8 Cl2 O1 O8 -171.1(13) . . . 14_565 ?
O4 Cl2 O8 O1 -155.4(16) . . . 14_565 ?
O4 Cl2 O8 O1 -99.3(15) 14_565 . . 14_565 ?
O1 Cl2 O8 O1 103(3) . . . 14_565 ?
O8 Cl2 O8 O1 52.9(14) 14_565 . . 14_565 ?
O1 Cl2 O4 O4 -173(2) . . . 14_565 ?
O1 Cl2 O4 O4 16(5) 14_565 . . 14_565 ?
O8 Cl2 O4 O4 -105.0(19) 14_565 . . 14_565 ?
O8 Cl2 O4 O4 80(2) . . . 14_565 ?
O5 Cl1 O2 O9 -102.0(9) . . . 14_565 ?
O2 Cl1 O2 O9 78.0(9) 14_565 . . 14_565 ?
O9 Cl1 O2 O9 143.6(18) . . . 14_565 ?
O5 Cl1 O9 O2 106.4(11) . . . 14_565 ?
O2 Cl1 O9 O2 -136.8(18) . . . 14_565 ?
O9 Cl1 O9 O2 -73.6(11) 14_565 . . 14_565 ?
Si06 C8 C9 Si07 -157.1(11) . . . . ?
C13 Si07 C9 C8 -176.5(12) . . . . ?
C11 Si07 C9 C8 71.7(14) . . . . ?
C10 Si07 C9 C8 -59.6(15) . . . . ?
Si06 C1B C2B Si07 -148.8(15) . . . . ?

_refine_diff_density_max         0.909
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.103


