# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_clav003
_database_code_depnum_ccdc_archive 'CCDC 1034345'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-12-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H23 F6 O6 Pd Sb'
_chemical_formula_weight         629.47

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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.539(2)
_cell_length_b                   10.408(2)
_cell_length_c                   11.253(3)
_cell_angle_alpha                115.767(3)
_cell_angle_beta                 97.422(3)
_cell_angle_gamma                91.945(3)
_cell_volume                     992.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    1059
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      19.99

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.039
_exptl_absorpt_coefficient_mu    2.349
_shelx_estimated_absorpt_T_min   0.632
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6614
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'

_exptl_special_details           
; 
Data collection is performed with four batch runs at 
φ = 0.00 ° (600 frames), at φ = 90.00 ° 
(600 frames), at φ = 180 ° (600 frames) and 
at φ = 270 ° (600 frames). 
Frame width = 0.30 \& in ω. Data is 
merged, corrected for decay, and treated with 
multi-scan absorption corrections. 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            10777
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.916
_diffrn_reflns_theta_max         27.366
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4461
_reflns_number_gt                2891
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0146P)²] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4461
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0716
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
Pd Pd 0.16107(5) 1.24690(5) 0.31013(5) 0.02456(14) Uani 1 1 d . . . . .
Sb Sb 0.30023(5) 0.86185(5) 0.75494(5) 0.03088(14) Uani 1 1 d . . . . .
F1 F 0.4667(4) 0.8614(4) 0.8613(4) 0.0491(11) Uani 1 1 d . . . . .
F2 F 0.2183(5) 0.9619(5) 0.9062(4) 0.0657(14) Uani 1 1 d . . . . .
F3 F 0.3674(5) 1.0323(4) 0.7559(5) 0.0644(14) Uani 1 1 d . . . . .
F4 F 0.3777(4) 0.7580(4) 0.6033(4) 0.0535(12) Uani 1 1 d . . . . .
F5 F 0.2321(4) 0.6901(4) 0.7542(4) 0.0499(11) Uani 1 1 d . . . . .
F6 F 0.1294(4) 0.8556(5) 0.6490(4) 0.0599(13) Uani 1 1 d . . . . .
O1 O 0.2054(5) 0.5806(5) 0.2342(5) 0.0395(12) Uani 1 1 d . . . . .
O2 O 0.4427(5) 0.5990(4) 0.2523(4) 0.0352(12) Uani 1 1 d . . . . .
O3 O 0.0841(5) 0.6593(4) -0.0330(4) 0.0359(12) Uani 1 1 d . . . . .
O4 O 0.2960(5) 0.5799(4) -0.0117(4) 0.0331(11) Uani 1 1 d . . . . .
C1 C 0.3018(9) 1.3639(7) 0.4909(7) 0.037(2) Uani 1 1 d . . . . .
H1A H 0.296(7) 1.454(7) 0.509(6) 0.045 Uiso 1 1 d . U . . .
H1B H 0.388(7) 1.329(7) 0.479(6) 0.045 Uiso 1 1 d . U . . .
C2 C 0.1951(8) 1.2949(7) 0.5147(6) 0.0368(18) Uani 1 1 d . . . . .
H2A H 0.1272 1.3571 0.5692 0.044 Uiso 1 1 calc R U . . .
C3 C 0.2122(8) 1.1562(7) 0.5249(6) 0.043(2) Uani 1 1 d . . . . .
H3A H 0.1171 1.1087 0.5163 0.051 Uiso 1 1 calc R U . . .
H3B H 0.2651 1.1776 0.6142 0.051 Uiso 1 1 calc R U . . .
C4 C 0.2905(7) 1.0548(6) 0.4183(6) 0.0269(15) Uani 1 1 d . . . . .
H4 H 0.3950 1.0702 0.4520 0.032 Uiso 1 1 calc R U . . .
C5 C 0.2356(7) 0.8976(6) 0.3689(6) 0.0303(16) Uani 1 1 d . . . . .
H5 H 0.2230 0.8695 0.4416 0.036 Uiso 1 1 calc R U . . .
C6 C 0.3306(7) 0.8037(6) 0.2695(6) 0.0259(15) Uani 1 1 d . . . . .
H6 H 0.4318 0.8459 0.3032 0.031 Uiso 1 1 calc R U . . .
C7 C 0.3187(7) 0.6516(7) 0.2524(6) 0.0284(16) Uani 1 1 d . . . . .
C8 C 0.4413(8) 0.4502(7) 0.2228(7) 0.048(2) Uani 1 1 d . . . . .
H8A H 0.4083 0.4355 0.2954 0.071 Uiso 1 1 calc R U . . .
H8B H 0.5375 0.4210 0.2142 0.071 Uiso 1 1 calc R U . . .
H8C H 0.3772 0.3925 0.1388 0.071 Uiso 1 1 calc R U . . .
C9 C 0.2357(9) 0.4385(6) -0.1138(7) 0.050(2) Uani 1 1 d . . . . .
H9A H 0.1587 0.4031 -0.0825 0.076 Uiso 1 1 calc R U . . .
H9B H 0.3097 0.3725 -0.1312 0.076 Uiso 1 1 calc R U . . .
H9C H 0.1983 0.4447 -0.1962 0.076 Uiso 1 1 calc R U . . .
C10 C 0.2039(8) 0.6807(6) 0.0226(6) 0.0273(15) Uani 1 1 d . . . . .
C11 C 0.2776(7) 0.8178(6) 0.1386(6) 0.0236(14) Uani 1 1 d . . . . .
H11 H 0.3585 0.8558 0.1106 0.028 Uiso 1 1 calc R U . . .
C12 C 0.1716(6) 0.9313(6) 0.1866(6) 0.0228(14) Uani 1 1 d . . . . .
H12 H 0.1066 0.9390 0.1133 0.027 Uiso 1 1 calc R U . . .
C13 C 0.0972(7) 0.8851(7) 0.2758(6) 0.0287(15) Uani 1 1 d . . . . .
H13A H 0.0499 0.7860 0.2278 0.034 Uiso 1 1 calc R U . . .
H13B H 0.0294 0.9523 0.3222 0.034 Uiso 1 1 calc R U . . .
C14 C 0.2606(6) 1.0731(6) 0.2877(5) 0.0209(14) Uani 1 1 d . . . . .
H14 H 0.3527 1.0799 0.2563 0.025 Uiso 1 1 calc R U . . .
O5 O 0.1024(6) 1.1793(5) 0.1015(4) 0.0418(13) Uani 1 1 d G . . . .
H5A H 0.0488 1.2320 0.0802 0.050 Uiso 1 1 d G U . . .
H5B H 0.1430 1.1162 0.0429 0.050 Uiso 1 1 d G U . . .
O6 O 0.0503(5) 1.4409(5) 0.3352(4) 0.0324(11) Uani 1 1 d G . . . .
H6A H -0.0160 1.4168 0.2691 0.039 Uiso 1 1 d G U . . .
H6B H 0.0360 1.4290 0.4029 0.039 Uiso 1 1 d G 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
Pd C14 2.004(6) . ?
Pd C2 2.109(6) . ?
Pd C1 2.110(6) . ?
Pd O5 2.125(4) . ?
Pd O6 2.236(4) . ?
Sb F4 1.844(4) . ?
Sb F2 1.858(4) . ?
Sb F3 1.861(4) . ?
Sb F1 1.862(4) . ?
Sb F6 1.871(4) . ?
Sb F5 1.878(4) . ?
O1 C7 1.229(7) . ?
O2 C7 1.320(7) . ?
O2 C8 1.436(7) . ?
O3 C10 1.193(7) . ?
O4 C10 1.348(7) . ?
O4 C9 1.455(7) . ?
C1 C2 1.346(10) . ?
C2 C3 1.510(9) . ?
C3 C4 1.515(8) . ?
C4 C5 1.529(8) . ?
C4 C14 1.555(8) . ?
C5 C13 1.540(8) . ?
C5 C6 1.549(8) . ?
C6 C7 1.508(8) . ?
C6 C11 1.564(8) . ?
C10 C11 1.520(8) . ?
C11 C12 1.542(8) . ?
C12 C13 1.525(8) . ?
C12 C14 1.549(7) . ?

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
C14 Pd C2 84.3(2) . . ?
C14 Pd C1 88.2(2) . . ?
C2 Pd C1 37.2(3) . . ?
C14 Pd O5 94.45(19) . . ?
C2 Pd O5 172.1(3) . . ?
C1 Pd O5 150.6(3) . . ?
C14 Pd O6 179.9(2) . . ?
C2 Pd O6 95.7(2) . . ?
C1 Pd O6 91.7(2) . . ?
O5 Pd O6 85.57(16) . . ?
F4 Sb F2 178.3(2) . . ?
F4 Sb F3 90.4(2) . . ?
F2 Sb F3 91.1(2) . . ?
F4 Sb F1 90.20(18) . . ?
F2 Sb F1 90.5(2) . . ?
F3 Sb F1 91.62(18) . . ?
F4 Sb F6 90.19(19) . . ?
F2 Sb F6 89.0(2) . . ?
F3 Sb F6 90.86(19) . . ?
F1 Sb F6 177.48(19) . . ?
F4 Sb F5 89.74(19) . . ?
F2 Sb F5 88.76(19) . . ?
F3 Sb F5 179.9(2) . . ?
F1 Sb F5 88.45(17) . . ?
F6 Sb F5 89.06(18) . . ?
C7 O2 C8 117.2(5) . . ?
C10 O4 C9 115.2(5) . . ?
C2 C1 Pd 71.3(4) . . ?
C1 C2 C3 121.7(7) . . ?
C1 C2 Pd 71.5(4) . . ?
C3 C2 Pd 107.9(4) . . ?
C2 C3 C4 112.2(6) . . ?
C3 C4 C5 112.5(6) . . ?
C3 C4 C14 111.3(5) . . ?
C5 C4 C14 101.6(5) . . ?
C4 C5 C13 101.5(5) . . ?
C4 C5 C6 108.1(5) . . ?
C13 C5 C6 102.4(5) . . ?
C7 C6 C5 111.5(5) . . ?
C7 C6 C11 113.9(5) . . ?
C5 C6 C11 103.6(5) . . ?
O1 C7 O2 122.9(6) . . ?
O1 C7 C6 124.0(6) . . ?
O2 C7 C6 112.9(6) . . ?
O3 C10 O4 122.8(6) . . ?
O3 C10 C11 127.8(6) . . ?
O4 C10 C11 109.3(5) . . ?
C10 C11 C12 110.4(5) . . ?
C10 C11 C6 114.8(5) . . ?
C12 C11 C6 101.4(5) . . ?
C13 C12 C11 101.8(5) . . ?
C13 C12 C14 103.1(5) . . ?
C11 C12 C14 106.4(5) . . ?
C12 C13 C5 94.0(5) . . ?
C12 C14 C4 103.7(5) . . ?
C12 C14 Pd 112.8(4) . . ?
C4 C14 Pd 113.3(4) . . ?

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
Pd C1 C2 C3 100.0(6) . . . . ?
C1 C2 C3 C4 -42.6(9) . . . . ?
Pd C2 C3 C4 36.2(7) . . . . ?
C2 C3 C4 C5 -144.9(6) . . . . ?
C2 C3 C4 C14 -31.5(8) . . . . ?
C3 C4 C5 C13 77.2(6) . . . . ?
C14 C4 C5 C13 -41.9(6) . . . . ?
C3 C4 C5 C6 -175.5(5) . . . . ?
C14 C4 C5 C6 65.4(6) . . . . ?
C4 C5 C6 C7 160.3(5) . . . . ?
C13 C5 C6 C7 -93.0(6) . . . . ?
C4 C5 C6 C11 -76.8(6) . . . . ?
C13 C5 C6 C11 29.9(6) . . . . ?
C8 O2 C7 O1 3.1(9) . . . . ?
C8 O2 C7 C6 -173.7(5) . . . . ?
C5 C6 C7 O1 46.5(8) . . . . ?
C11 C6 C7 O1 -70.4(8) . . . . ?
C5 C6 C7 O2 -136.7(5) . . . . ?
C11 C6 C7 O2 106.4(6) . . . . ?
C9 O4 C10 O3 -5.4(9) . . . . ?
C9 O4 C10 C11 174.6(5) . . . . ?
O3 C10 C11 C12 4.1(9) . . . . ?
O4 C10 C11 C12 -175.9(5) . . . . ?
O3 C10 C11 C6 118.0(7) . . . . ?
O4 C10 C11 C6 -62.0(7) . . . . ?
C7 C6 C11 C10 8.5(8) . . . . ?
C5 C6 C11 C10 -112.9(6) . . . . ?
C7 C6 C11 C12 127.5(6) . . . . ?
C5 C6 C11 C12 6.2(6) . . . . ?
C10 C11 C12 C13 81.4(6) . . . . ?
C6 C11 C12 C13 -40.7(5) . . . . ?
C10 C11 C12 C14 -171.0(5) . . . . ?
C6 C11 C12 C14 66.9(5) . . . . ?
C11 C12 C13 C5 58.2(5) . . . . ?
C14 C12 C13 C5 -52.0(5) . . . . ?
C4 C5 C13 C12 58.2(5) . . . . ?
C6 C5 C13 C12 -53.5(5) . . . . ?
C13 C12 C14 C4 28.0(6) . . . . ?
C11 C12 C14 C4 -78.7(5) . . . . ?
C13 C12 C14 Pd -95.0(5) . . . . ?
C11 C12 C14 Pd 158.3(4) . . . . ?
C3 C4 C14 C12 -111.5(6) . . . . ?
C5 C4 C14 C12 8.5(6) . . . . ?
C3 C4 C14 Pd 11.1(7) . . . . ?
C5 C4 C14 Pd 131.1(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O3 0.85 1.90 2.749(6) 175.3 2_575
O5 H5B F2 0.85 1.92 2.765(6) 174.6 1_554
O6 H6A F5 0.85 2.24 2.826(6) 126.4 2_576
O6 H6A O3 0.85 2.41 3.161(6) 148.2 2_575

_refine_diff_density_max         1.095
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.165

_shelxl_version_number           2013-2



####################################################################### 
# 
# 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_clav009
_database_code_depnum_ccdc_archive 'CCDC 1034346'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-12-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H22 F6 N O6 Pd Sb'
_chemical_formula_weight         654.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   18.890(5)
_cell_length_b                   16.805(4)
_cell_length_c                   13.196(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4189.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9001
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      24.95

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_F_000             2544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.124
_exptl_absorpt_coefficient_mu    2.232
_shelx_estimated_absorpt_T_min   0.534
_shelx_estimated_absorpt_T_max   0.769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'

_exptl_special_details           
; 
Data collection is performed with four batch runs at 
φ = 0.00 ° (600 frames), at φ = 90.00 ° 
(600 frames), at φ = 180 ° (600 frames) and 
at φ = 270 ° (600 frames). 
Frame width = 0.30 \& in ω. Data is 
merged, corrected for decay, and treated with 
multi-scan absorption corrections. 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            52413
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.883
_diffrn_reflns_theta_max         27.647
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5031
_reflns_number_gt                4342
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0380P)²+6.0245P] 
 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         5031
_refine_ls_number_parameters     293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0711
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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
Pd Pd 0.33750(2) 0.03235(2) 0.72772(2) 0.02417(7) Uani 1 1 d . . . . .
Sb1 Sb 0.24082(2) 0.2500 0.35500(3) 0.03513(9) Uani 1 2 d S T P . .
Sb2 Sb 0.57885(2) 0.2500 0.50946(2) 0.03711(9) Uani 1 2 d S T P . .
F1 F 0.14301(18) 0.2500 0.3412(3) 0.0607(9) Uani 1 2 d S T P . .
F2 F 0.24909(15) 0.17036(14) 0.2565(2) 0.0610(7) Uani 1 1 d . . . . .
F3 F 0.23420(15) 0.17113(13) 0.45562(19) 0.0602(7) Uani 1 1 d . . . . .
F4 F 0.33862(19) 0.2500 0.3723(4) 0.0761(12) Uani 1 2 d S T P . .
F5 F 0.6605(2) 0.2500 0.5901(4) 0.0923(15) Uani 1 2 d S T P . .
F6 F 0.5284(3) 0.2500 0.6281(3) 0.0934(15) Uani 1 2 d S T P . .
F7 F 0.57940(16) 0.13856(17) 0.5094(3) 0.0783(9) Uani 1 1 d . . . . .
F8 F 0.4970(3) 0.2500 0.4353(4) 0.113(2) Uani 1 2 d S T P . .
F9 F 0.6350(4) 0.2500 0.3966(5) 0.155(3) Uani 1 2 d S T P . .
O1 O 0.26264(11) -0.08330(13) 1.19224(16) 0.0289(5) Uani 1 1 d . . . . .
O2 O 0.37366(12) -0.07286(15) 1.14178(19) 0.0414(6) Uani 1 1 d . . . . .
O3 O 0.14360(12) -0.04820(15) 1.06415(16) 0.0327(5) Uani 1 1 d . . . . .
O4 O 0.15838(11) -0.01678(14) 0.90270(16) 0.0302(5) Uani 1 1 d . . . . .
O5 O 0.5103(2) 0.1852(3) 0.0408(3) 0.0939(13) Uani 1 1 d . . . . .
O6 O 0.4040(3) 0.3132(2) 0.7478(3) 0.0917(14) Uani 1 1 d . . . . .
N1 N 0.5002(3) 0.2500 0.0795(4) 0.0571(13) Uani 1 2 d S T P . .
N2 N 0.3864(3) 0.2500 0.7108(3) 0.0511(12) Uani 1 2 d S T P . .
C1 C 0.41140(18) -0.0629(2) 0.7427(3) 0.0359(8) Uani 1 1 d . . . . .
H1A H 0.4007 -0.1032 0.7952 0.043 Uiso 1 1 calc R U . . .
H1B H 0.4298 -0.0860 0.6789 0.043 Uiso 1 1 calc R U . . .
C2 C 0.44316(16) 0.0060(2) 0.7755(2) 0.0314(7) Uani 1 1 d . . . . .
H2A H 0.4815 0.0271 0.7307 0.038 Uiso 1 1 calc R U . . .
C3 C 0.44714(16) 0.0315(2) 0.8852(2) 0.0306(7) Uani 1 1 d . . . . .
H3A H 0.4524 0.0900 0.8890 0.037 Uiso 1 1 calc R U . . .
H3B H 0.4892 0.0070 0.9175 0.037 Uiso 1 1 calc R U . . .
C4 C 0.37999(15) 0.00598(18) 0.9425(2) 0.0242(6) Uani 1 1 d . . . . .
H4A H 0.3847 -0.0499 0.9676 0.029 Uiso 1 1 calc R U . . .
C5 C 0.36303(16) 0.06315(18) 1.0312(2) 0.0244(6) Uani 1 1 d . . . . .
H5A H 0.4050 0.0778 1.0735 0.029 Uiso 1 1 calc R U . . .
C6 C 0.29862(15) 0.03166(17) 1.0931(2) 0.0217(6) Uani 1 1 d . . . . .
H6A H 0.2928 0.0705 1.1499 0.026 Uiso 1 1 calc R U . . .
C7 C 0.30808(16) -0.04744(18) 1.1441(2) 0.0248(6) Uani 1 1 d . . . . .
C8 C 0.3897(3) -0.1450(3) 1.1988(5) 0.0795(18) Uani 1 1 d . . . . .
H8A H 0.4406 -0.1563 1.1945 0.119 Uiso 1 1 calc R U . . .
H8B H 0.3631 -0.1898 1.1704 0.119 Uiso 1 1 calc R U . . .
H8C H 0.3764 -0.1375 1.2700 0.119 Uiso 1 1 calc R U . . .
C9 C 0.09600(19) -0.0648(3) 0.8806(3) 0.0418(9) Uani 1 1 d . . . . .
H9A H 0.0870 -0.0644 0.8075 0.063 Uiso 1 1 calc R U . . .
H9B H 0.0550 -0.0426 0.9163 0.063 Uiso 1 1 calc R U . . .
H9C H 0.1041 -0.1195 0.9034 0.063 Uiso 1 1 calc R U . . .
C10 C 0.17628(16) -0.01187(19) 0.9992(2) 0.0249(6) Uani 1 1 d . . . . .
C11 C 0.23379(15) 0.04893(18) 1.0189(2) 0.0225(6) Uani 1 1 d . . . . .
H11A H 0.2086 0.0953 1.0499 0.027 Uiso 1 1 calc R U . . .
C12 C 0.27135(15) 0.08346(17) 0.9239(2) 0.0229(6) Uani 1 1 d . . . . .
H12A H 0.2399 0.1136 0.8766 0.028 Uiso 1 1 calc R U . . .
C13 C 0.32919(17) 0.13347(18) 0.9751(2) 0.0279(6) Uani 1 1 d . . . . .
H13A H 0.3097 0.1741 1.0216 0.033 Uiso 1 1 calc R U . . .
H13B H 0.3618 0.1585 0.9257 0.033 Uiso 1 1 calc R U . . .
C14 C 0.31334(15) 0.01460(18) 0.8746(2) 0.0226(6) Uani 1 1 d . . . . .
H14A H 0.2847 -0.0352 0.8803 0.027 Uiso 1 1 calc R U . . .
C15 C 0.4756(4) 0.2500 0.1839(6) 0.077(2) Uani 1 2 d S T P . .
H15A H 0.4684 0.3049 0.2065 0.115 Uiso 0.5 1 calc R U P . .
H15B H 0.5110 0.2243 0.2271 0.115 Uiso 0.5 1 calc R U P . .
H15C H 0.4308 0.2208 0.1884 0.115 Uiso 0.5 1 calc R U P . .
C16 C 0.3508(4) 0.2500 0.6109(5) 0.0614(17) Uani 1 2 d S T P . .
H16A H 0.3436 0.1950 0.5884 0.092 Uiso 0.5 1 calc R U P . .
H16B H 0.3804 0.2782 0.5615 0.092 Uiso 0.5 1 calc R U P . .
H16C H 0.3049 0.2768 0.6166 0.092 Uiso 0.5 1 calc R 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
Pd C14 2.014(3) . ?
Pd O1 2.129(2) 4_554 ?
Pd C1 2.133(3) . ?
Pd C2 2.139(3) . ?
Pd O3 2.204(2) 4_554 ?
Sb1 F4 1.861(4) . ?
Sb1 F1 1.857(3) . ?
Sb1 F2 1.872(2) 7_565 ?
Sb1 F2 1.872(2) . ?
Sb1 F3 1.880(2) . ?
Sb1 F3 1.880(2) 7_565 ?
Sb2 F9 1.828(5) . ?
Sb2 F6 1.833(4) . ?
Sb2 F8 1.830(4) . ?
Sb2 F7 1.873(3) . ?
Sb2 F7 1.873(3) 7_565 ?
Sb2 F5 1.874(4) . ?
O1 C7 1.226(4) . ?
O1 Pd 2.129(2) 4 ?
O2 C7 1.311(4) . ?
O2 C8 1.460(4) . ?
O3 C10 1.220(4) . ?
O3 Pd 2.204(2) 4 ?
O4 C10 1.320(4) . ?
O4 C9 1.457(4) . ?
O5 N1 1.219(5) . ?
O6 N2 1.215(4) . ?
N1 O5 1.219(5) 7_565 ?
N1 C15 1.453(9) . ?
N2 O6 1.215(4) 7_565 ?
N2 C16 1.480(8) . ?
C1 C2 1.374(5) . ?
C2 C3 1.512(4) . ?
C3 C4 1.538(4) . ?
C4 C5 1.548(4) . ?
C4 C14 1.552(4) . ?
C5 C13 1.534(4) . ?
C5 C6 1.558(4) . ?
C6 C7 1.500(4) . ?
C6 C11 1.595(4) . ?
C10 C11 1.514(4) . ?
C11 C12 1.552(4) . ?
C12 C13 1.535(4) . ?
C12 C14 1.546(4) . ?

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
C14 Pd O1 94.01(10) . 4_554 ?
C14 Pd C1 87.03(13) . . ?
O1 Pd C1 154.66(12) 4_554 . ?
C14 Pd C2 84.11(12) . . ?
O1 Pd C2 167.73(11) 4_554 . ?
C1 Pd C2 37.53(14) . . ?
C14 Pd O3 175.87(10) . 4_554 ?
O1 Pd O3 83.10(8) 4_554 4_554 ?
C1 Pd O3 94.32(11) . 4_554 ?
C2 Pd O3 99.34(10) . 4_554 ?
F4 Sb1 F1 178.60(19) . . ?
F4 Sb1 F2 90.12(14) . 7_565 ?
F1 Sb1 F2 90.86(12) . 7_565 ?
F4 Sb1 F2 90.12(14) . . ?
F1 Sb1 F2 90.86(12) . . ?
F2 Sb1 F2 91.26(17) 7_565 . ?
F4 Sb1 F3 88.83(14) . . ?
F1 Sb1 F3 90.18(12) . . ?
F2 Sb1 F3 178.68(12) 7_565 . ?
F2 Sb1 F3 89.53(11) . . ?
F4 Sb1 F3 88.83(14) . 7_565 ?
F1 Sb1 F3 90.18(12) . 7_565 ?
F2 Sb1 F3 89.54(11) 7_565 7_565 ?
F2 Sb1 F3 178.68(12) . 7_565 ?
F3 Sb1 F3 89.65(15) . 7_565 ?
F9 Sb2 F6 175.9(3) . . ?
F9 Sb2 F8 93.1(3) . . ?
F6 Sb2 F8 91.0(3) . . ?
F9 Sb2 F7 89.81(10) . . ?
F6 Sb2 F7 90.17(10) . . ?
F8 Sb2 F7 90.27(9) . . ?
F9 Sb2 F7 89.81(10) . 7_565 ?
F6 Sb2 F7 90.17(10) . 7_565 ?
F8 Sb2 F7 90.27(9) . 7_565 ?
F7 Sb2 F7 179.37(19) . 7_565 ?
F9 Sb2 F5 89.1(3) . . ?
F6 Sb2 F5 86.8(3) . . ?
F8 Sb2 F5 177.7(3) . . ?
F7 Sb2 F5 89.74(9) . . ?
F7 Sb2 F5 89.74(9) 7_565 . ?
C7 O1 Pd 122.6(2) . 4 ?
C7 O2 C8 117.1(3) . . ?
C10 O3 Pd 123.1(2) . 4 ?
C10 O4 C9 115.7(3) . . ?
O5 N1 O5 126.8(7) 7_565 . ?
O5 N1 C15 116.6(4) 7_565 . ?
O5 N1 C15 116.6(4) . . ?
O6 N2 O6 121.8(6) 7_565 . ?
O6 N2 C16 118.8(3) 7_565 . ?
O6 N2 C16 118.8(3) . . ?
C2 C1 Pd 71.5(2) . . ?
C1 C2 C3 124.2(3) . . ?
C1 C2 Pd 70.99(19) . . ?
C3 C2 Pd 105.7(2) . . ?
C2 C3 C4 110.6(3) . . ?
C3 C4 C5 111.7(3) . . ?
C3 C4 C14 111.1(2) . . ?
C5 C4 C14 102.2(2) . . ?
C13 C5 C4 101.5(2) . . ?
C13 C5 C6 100.9(2) . . ?
C4 C5 C6 110.3(2) . . ?
C7 C6 C5 116.3(2) . . ?
C7 C6 C11 121.9(2) . . ?
C5 C6 C11 102.5(2) . . ?
O1 C7 O2 120.9(3) . . ?
O1 C7 C6 125.7(3) . . ?
O2 C7 C6 113.0(3) . . ?
O3 C10 O4 121.1(3) . . ?
O3 C10 C11 125.5(3) . . ?
O4 C10 C11 113.1(3) . . ?
C10 C11 C12 116.2(2) . . ?
C10 C11 C6 122.3(2) . . ?
C12 C11 C6 102.3(2) . . ?
C13 C12 C14 103.3(2) . . ?
C13 C12 C11 100.1(2) . . ?
C14 C12 C11 107.1(2) . . ?
C12 C13 C5 95.0(2) . . ?
C12 C14 C4 104.1(2) . . ?
C12 C14 Pd 114.23(19) . . ?
C4 C14 Pd 112.69(19) . . ?

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
Pd C1 C2 C3 96.4(3) . . . . ?
C1 C2 C3 C4 -34.6(4) . . . . ?
Pd C2 C3 C4 42.7(3) . . . . ?
C2 C3 C4 C5 -150.8(3) . . . . ?
C2 C3 C4 C14 -37.5(4) . . . . ?
C3 C4 C5 C13 78.5(3) . . . . ?
C14 C4 C5 C13 -40.3(3) . . . . ?
C3 C4 C5 C6 -175.2(2) . . . . ?
C14 C4 C5 C6 66.0(3) . . . . ?
C13 C5 C6 C7 169.1(2) . . . . ?
C4 C5 C6 C7 62.4(3) . . . . ?
C13 C5 C6 C11 33.7(3) . . . . ?
C4 C5 C6 C11 -73.0(3) . . . . ?
Pd O1 C7 O2 165.4(2) 4 . . . ?
Pd O1 C7 C6 -7.4(4) 4 . . . ?
C8 O2 C7 O1 -0.1(5) . . . . ?
C8 O2 C7 C6 173.5(4) . . . . ?
C5 C6 C7 O1 -176.7(3) . . . . ?
C11 C6 C7 O1 -50.6(4) . . . . ?
C5 C6 C7 O2 10.1(4) . . . . ?
C11 C6 C7 O2 136.2(3) . . . . ?
Pd O3 C10 O4 -172.8(2) 4 . . . ?
Pd O3 C10 C11 -0.2(4) 4 . . . ?
C9 O4 C10 O3 2.7(4) . . . . ?
C9 O4 C10 C11 -170.7(3) . . . . ?
O3 C10 C11 C12 176.1(3) . . . . ?
O4 C10 C11 C12 -10.7(4) . . . . ?
O3 C10 C11 C6 49.9(4) . . . . ?
O4 C10 C11 C6 -137.0(3) . . . . ?
C7 C6 C11 C10 2.9(4) . . . . ?
C5 C6 C11 C10 135.0(3) . . . . ?
C7 C6 C11 C12 -129.3(3) . . . . ?
C5 C6 C11 C12 2.8(3) . . . . ?
C10 C11 C12 C13 -174.1(2) . . . . ?
C6 C11 C12 C13 -38.4(3) . . . . ?
C10 C11 C12 C14 -66.7(3) . . . . ?
C6 C11 C12 C14 69.0(3) . . . . ?
C14 C12 C13 C5 -51.3(3) . . . . ?
C11 C12 C13 C5 59.2(2) . . . . ?
C4 C5 C13 C12 56.2(3) . . . . ?
C6 C5 C13 C12 -57.3(2) . . . . ?
C13 C12 C14 C4 27.7(3) . . . . ?
C11 C12 C14 C4 -77.4(3) . . . . ?
C13 C12 C14 Pd -95.6(2) . . . . ?
C11 C12 C14 Pd 159.27(18) . . . . ?
C3 C4 C14 C12 -111.7(3) . . . . ?
C5 C4 C14 C12 7.5(3) . . . . ?
C3 C4 C14 Pd 12.6(3) . . . . ?
C5 C4 C14 Pd 131.8(2) . . . . ?

_refine_diff_density_max         0.971
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.099

_shelxl_version_number           2013-2



####################################################################### 
# 
# 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_clav010a
_database_code_depnum_ccdc_archive 'CCDC 1034347'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-12-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H35 F6 O6 Pd Sb'
_chemical_formula_weight         737.65

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'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

_cell_length_a                   16.758(3)
_cell_length_b                   16.947(4)
_cell_length_c                   9.5046(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2699.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3837
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      24.68

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.119
_exptl_absorpt_coefficient_mu    1.743
_shelx_estimated_absorpt_T_min   0.527
_shelx_estimated_absorpt_T_max   0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6048
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'

_exptl_special_details           
; 
Data collection is performed with four batch runs at 
φ = 0.00 ° (600 frames), at φ = 90.00 ° 
(600 frames), at φ = 180 ° (600 frames) and 
at φ = 270 ° (600 frames). 
Frame width = 0.30 \& in ω. Data is 
merged, corrected for decay, and treated with 
multi-scan absorption corrections. 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            17478
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.709
_diffrn_reflns_theta_max         27.809
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             6048
_reflns_number_gt                5361
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_max     0.892
_reflns_Friedel_fraction_full    0.942

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0222P)²+1.3018P] 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 2133 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.031(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6048
_refine_ls_number_parameters     331
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0620
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.027
_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
Pd Pd 0.39194(2) 0.25776(2) 0.42063(5) 0.03091(12) Uani 1 1 d . . . . .
Sb Sb 0.35988(2) 0.85670(2) 0.39017(4) 0.03883(12) Uani 1 1 d . . . . .
F1 F 0.3296(4) 0.9439(3) 0.4946(6) 0.0926(18) Uani 1 1 d . . . . .
F2 F 0.3839(3) 0.9226(3) 0.2399(5) 0.0688(14) Uani 1 1 d . . . . .
F3 F 0.4639(3) 0.8677(3) 0.4549(7) 0.111(2) Uani 1 1 d . . . . .
F4 F 0.3376(3) 0.7910(3) 0.5436(6) 0.0750(16) Uani 1 1 d . . . . .
F5 F 0.2574(3) 0.8445(4) 0.3304(7) 0.112(2) Uani 1 1 d . . . . .
F6 F 0.3949(5) 0.7701(3) 0.2905(7) 0.113(3) Uani 1 1 d . . . . .
O1 O 0.5414(3) 0.5094(2) 0.2326(5) 0.0434(11) Uani 1 1 d . . . . .
O2 O 0.4602(3) 0.5577(2) 0.0662(5) 0.0420(11) Uani 1 1 d . . . . .
O3 O 0.6341(3) 0.3454(3) 0.2969(5) 0.0426(11) Uani 1 1 d . . . . .
O4 O 0.6687(3) 0.4199(3) 0.1113(5) 0.0478(12) Uani 1 1 d . . . . .
O5 O 0.4764(2) 0.16774(19) 0.3886(6) 0.0396(10) Uani 1 1 d . U . . .
O6 O 0.3401(3) 0.1755(3) 0.5802(5) 0.0482(12) Uani 1 1 d . U . . .
C1 C 0.3304(5) 0.3576(4) 0.5093(9) 0.0477(19) Uani 1 1 d . . . . .
H1A H 0.3665 0.4006 0.5021 0.057 Uiso 1 1 calc R U . . .
H1B H 0.3223 0.3323 0.5973 0.057 Uiso 1 1 calc R U . . .
C2 C 0.2898(4) 0.3320(3) 0.3923(10) 0.0458(16) Uani 1 1 d . . . . .
H2 H 0.2372 0.3063 0.4116 0.055 Uiso 1 1 calc R U . . .
C3 C 0.2983(4) 0.3677(4) 0.2489(9) 0.0493(19) Uani 1 1 d . . . . .
H3A H 0.2623 0.4138 0.2406 0.059 Uiso 1 1 calc R U . . .
H3B H 0.2824 0.3285 0.1768 0.059 Uiso 1 1 calc R U . . .
C4 C 0.3848(4) 0.3937(3) 0.2226(7) 0.0353(15) Uani 1 1 d . . . . .
H4 H 0.3941 0.4478 0.2615 0.042 Uiso 1 1 calc R U . . .
C5 C 0.4061(4) 0.3911(4) 0.0661(7) 0.0385(15) Uani 1 1 d . . . . .
H5 H 0.3650 0.4147 0.0025 0.046 Uiso 1 1 calc R U . . .
C6 C 0.4917(4) 0.4247(3) 0.0462(6) 0.0345(14) Uani 1 1 d . . . . .
H6 H 0.5014 0.4346 -0.0561 0.041 Uiso 1 1 calc R U . . .
C7 C 0.5452(4) 0.3549(3) 0.0962(6) 0.0324(14) Uani 1 1 d . . . . .
H7 H 0.5655 0.3296 0.0081 0.039 Uiso 1 1 calc R U . . .
C8 C 0.4846(4) 0.2960(3) 0.1578(7) 0.0346(14) Uani 1 1 d . . . . .
H8 H 0.5058 0.2415 0.1732 0.041 Uiso 1 1 calc R U . . .
C9 C 0.4451(3) 0.3339(3) 0.2872(6) 0.0287(13) Uani 1 1 d . . . . .
H9 H 0.4867 0.3640 0.3403 0.034 Uiso 1 1 calc R U . . .
C10 C 0.4206(4) 0.3028(4) 0.0437(7) 0.0447(17) Uani 1 1 d . . . . .
H10A H 0.3728 0.2704 0.0641 0.054 Uiso 1 1 calc R U . . .
H10B H 0.4412 0.2906 -0.0514 0.054 Uiso 1 1 calc R U . . .
C11 C 0.5022(5) 0.5005(4) 0.1263(7) 0.0311(13) Uani 1 1 d . . . . .
C12 C 0.4585(5) 0.6318(4) 0.1391(7) 0.0466(19) Uani 1 1 d . . . . .
H12A H 0.4317 0.6251 0.2300 0.070 Uiso 1 1 calc R U . . .
H12B H 0.4294 0.6707 0.0825 0.070 Uiso 1 1 calc R U . . .
H12C H 0.5132 0.6502 0.1546 0.070 Uiso 1 1 calc R U . . .
C13 C 0.6188(4) 0.3723(3) 0.1837(7) 0.0355(14) Uani 1 1 d . . . . .
C14 C 0.7387(5) 0.4446(5) 0.1854(10) 0.074(3) Uani 1 1 d . . . . .
H14A H 0.7232 0.4752 0.2684 0.111 Uiso 1 1 calc R U . . .
H14B H 0.7717 0.4773 0.1234 0.111 Uiso 1 1 calc R U . . .
H14C H 0.7692 0.3981 0.2150 0.111 Uiso 1 1 calc R U . . .
C15 C 0.5594(4) 0.1688(3) 0.4320(9) 0.0460(17) Uani 1 1 d . U . . .
H15A H 0.5638 0.1747 0.5353 0.055 Uiso 1 1 calc R U . . .
H15B H 0.5884 0.2128 0.3863 0.055 Uiso 1 1 calc R U . . .
C16 C 0.5922(4) 0.0912(4) 0.3858(12) 0.072(3) Uani 1 1 d D U . . .
H16A H 0.6139 0.0945 0.2891 0.087 Uiso 1 1 calc R U . A 1
H16B H 0.6348 0.0729 0.4502 0.087 Uiso 1 1 calc R U . A 1
C17 C 0.5238(6) 0.0394(6) 0.391(2) 0.062(4) Uani 0.65(2) 1 d D U P B 1
H17A H 0.5132 0.0218 0.4888 0.074 Uiso 0.65(2) 1 calc R U P B 1
H17B H 0.5318 -0.0075 0.3307 0.074 Uiso 0.65(2) 1 calc R U P B 1
C17' C 0.5319(9) 0.0496(14) 0.298(3) 0.062(4) Uani 0.35(2) 1 d D U P B 2
H17C H 0.5293 -0.0072 0.3219 0.074 Uiso 0.35(2) 1 calc R U P B 2
H17D H 0.5441 0.0553 0.1964 0.074 Uiso 0.35(2) 1 calc R U P B 2
C18 C 0.4553(4) 0.0913(4) 0.3357(10) 0.061(2) Uani 1 1 d D U . . .
H18A H 0.4533 0.0909 0.2316 0.073 Uiso 1 1 calc R U . B 1
H18B H 0.4031 0.0737 0.3732 0.073 Uiso 1 1 calc R U . B 1
C19 C 0.3831(6) 0.1634(7) 0.7076(10) 0.091(4) Uani 1 1 d . U . . .
H19A H 0.4064 0.2138 0.7405 0.109 Uiso 1 1 calc R U . . .
H19B H 0.4269 0.1252 0.6924 0.109 Uiso 1 1 calc R U . . .
C20 C 0.3262(5) 0.1326(5) 0.8132(9) 0.074(2) Uani 1 1 d . U . . .
H20A H 0.3513 0.0909 0.8713 0.088 Uiso 1 1 calc R U . . .
H20B H 0.3071 0.1753 0.8757 0.088 Uiso 1 1 calc R U . . .
C21 C 0.2609(6) 0.1005(6) 0.7296(10) 0.079(3) Uani 1 1 d . U . . .
H21A H 0.2098 0.1043 0.7812 0.095 Uiso 1 1 calc R U . . .
H21B H 0.2710 0.0445 0.7055 0.095 Uiso 1 1 calc R U . . .
C22 C 0.2594(5) 0.1508(5) 0.5995(9) 0.069(2) Uani 1 1 d . U . . .
H22A H 0.2406 0.1200 0.5175 0.082 Uiso 1 1 calc R U . . .
H22B H 0.2239 0.1969 0.6126 0.082 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
Pd C9 2.016(6) . ?
Pd O5 2.103(3) . ?
Pd C2 2.141(5) . ?
Pd C1 2.153(6) . ?
Pd O6 2.236(5) . ?
Sb F5 1.821(5) . ?
Sb F6 1.843(5) . ?
Sb F1 1.851(4) . ?
Sb F3 1.858(5) . ?
Sb F2 1.858(4) . ?
Sb F4 1.872(4) . ?
O1 C11 1.215(8) . ?
O2 C11 1.327(8) . ?
O2 C12 1.435(7) . ?
O3 C13 1.197(8) . ?
O4 C13 1.350(8) . ?
O4 C14 1.430(9) . ?
O5 C18 1.435(7) . ?
O5 C15 1.452(7) . ?
O6 C19 1.424(10) . ?
O6 C22 1.427(8) . ?
C1 C2 1.373(11) . ?
C1 H1A 0.9500 . ?
C1 H1B 0.9500 . ?
C2 C3 1.498(11) . ?
C2 H2 1.0000 . ?
C3 C4 1.536(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.530(9) . ?
C4 C9 1.559(8) . ?
C4 H4 1.0000 . ?
C5 C10 1.532(8) . ?
C5 C6 1.554(9) . ?
C5 H5 1.0000 . ?
C6 C11 1.503(9) . ?
C6 C7 1.560(8) . ?
C6 H6 1.0000 . ?
C7 C13 1.516(9) . ?
C7 C8 1.539(8) . ?
C7 H7 1.0000 . ?
C8 C10 1.531(9) . ?
C8 C9 1.537(8) . ?
C8 H8 1.0000 . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.491(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.444(11) . ?
C16 C17' 1.488(18) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.540(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17' C18 1.509(17) . ?
C17' H17C 0.9900 . ?
C17' H17D 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.479(12) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.458(12) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.502(11) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?

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
C9 Pd O5 94.3(2) . . ?
C9 Pd C2 84.2(3) . . ?
O5 Pd C2 161.1(3) . . ?
C9 Pd C1 87.4(3) . . ?
O5 Pd C1 161.6(3) . . ?
C2 Pd C1 37.3(3) . . ?
C9 Pd O6 175.7(2) . . ?
O5 Pd O6 84.68(18) . . ?
C2 Pd O6 98.1(2) . . ?
C1 Pd O6 92.2(2) . . ?
F5 Sb F6 92.8(3) . . ?
F5 Sb F1 90.0(3) . . ?
F6 Sb F1 177.2(3) . . ?
F5 Sb F3 178.6(3) . . ?
F6 Sb F3 87.2(3) . . ?
F1 Sb F3 90.0(3) . . ?
F5 Sb F2 91.9(3) . . ?
F6 Sb F2 90.8(2) . . ?
F1 Sb F2 89.5(2) . . ?
F3 Sb F2 89.5(2) . . ?
F5 Sb F4 89.3(3) . . ?
F6 Sb F4 89.4(2) . . ?
F1 Sb F4 90.2(2) . . ?
F3 Sb F4 89.4(2) . . ?
F2 Sb F4 178.8(2) . . ?
C11 O2 C12 116.2(5) . . ?
C13 O4 C14 115.6(6) . . ?
C18 O5 C15 110.3(4) . . ?
C18 O5 Pd 122.7(3) . . ?
C15 O5 Pd 126.5(3) . . ?
C19 O6 C22 109.1(6) . . ?
C19 O6 Pd 118.0(4) . . ?
C22 O6 Pd 129.7(5) . . ?
C2 C1 Pd 70.9(4) . . ?
C2 C1 H1A 120.0 . . ?
Pd C1 H1A 105.6 . . ?
C2 C1 H1B 120.0 . . ?
Pd C1 H1B 93.4 . . ?
H1A C1 H1B 120.0 . . ?
C1 C2 C3 124.2(6) . . ?
C1 C2 Pd 71.8(4) . . ?
C3 C2 Pd 106.0(5) . . ?
C1 C2 H2 115.2 . . ?
C3 C2 H2 115.2 . . ?
Pd C2 H2 115.2 . . ?
C2 C3 C4 110.7(6) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
C5 C4 C3 111.8(5) . . ?
C5 C4 C9 102.3(5) . . ?
C3 C4 C9 111.2(5) . . ?
C5 C4 H4 110.5 . . ?
C3 C4 H4 110.5 . . ?
C9 C4 H4 110.5 . . ?
C4 C5 C10 101.6(5) . . ?
C4 C5 C6 108.9(5) . . ?
C10 C5 C6 101.2(5) . . ?
C4 C5 H5 114.5 . . ?
C10 C5 H5 114.5 . . ?
C6 C5 H5 114.5 . . ?
C11 C6 C5 111.1(5) . . ?
C11 C6 C7 115.2(6) . . ?
C5 C6 C7 102.4(5) . . ?
C11 C6 H6 109.3 . . ?
C5 C6 H6 109.3 . . ?
C7 C6 H6 109.3 . . ?
C13 C7 C8 117.0(5) . . ?
C13 C7 C6 119.1(5) . . ?
C8 C7 C6 103.2(5) . . ?
C13 C7 H7 105.4 . . ?
C8 C7 H7 105.4 . . ?
C6 C7 H7 105.4 . . ?
C10 C8 C9 103.5(5) . . ?
C10 C8 C7 98.3(5) . . ?
C9 C8 C7 108.6(5) . . ?
C10 C8 H8 114.9 . . ?
C9 C8 H8 114.9 . . ?
C7 C8 H8 114.9 . . ?
C8 C9 C4 103.6(5) . . ?
C8 C9 Pd 115.3(4) . . ?
C4 C9 Pd 112.2(4) . . ?
C8 C9 H9 108.5 . . ?
C4 C9 H9 108.5 . . ?
Pd C9 H9 108.5 . . ?
C8 C10 C5 94.9(5) . . ?
C8 C10 H10A 112.8 . . ?
C5 C10 H10A 112.8 . . ?
C8 C10 H10B 112.8 . . ?
C5 C10 H10B 112.8 . . ?
H10A C10 H10B 110.2 . . ?
O1 C11 O2 123.6(6) . . ?
O1 C11 C6 126.3(6) . . ?
O2 C11 C6 110.1(6) . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C13 O4 123.5(6) . . ?
O3 C13 C7 126.4(6) . . ?
O4 C13 C7 110.0(6) . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O5 C15 C16 105.0(5) . . ?
O5 C15 H15A 110.8 . . ?
C16 C15 H15A 110.8 . . ?
O5 C15 H15B 110.8 . . ?
C16 C15 H15B 110.8 . . ?
H15A C15 H15B 108.8 . . ?
C17 C16 C15 103.5(7) . . ?
C17' C16 C15 109.5(8) . . ?
C17 C16 H16A 111.1 . . ?
C15 C16 H16A 111.1 . . ?
C17 C16 H16B 111.1 . . ?
C15 C16 H16B 111.1 . . ?
H16A C16 H16B 109.0 . . ?
C16 C17 C18 103.4(8) . . ?
C16 C17 H17A 111.1 . . ?
C18 C17 H17A 111.1 . . ?
C16 C17 H17B 111.1 . . ?
C18 C17 H17B 111.1 . . ?
H17A C17 H17B 109.0 . . ?
C16 C17' C18 102.9(12) . . ?
C16 C17' H17C 111.2 . . ?
C18 C17' H17C 111.2 . . ?
C16 C17' H17D 111.2 . . ?
C18 C17' H17D 111.2 . . ?
H17C C17' H17D 109.1 . . ?
O5 C18 C17' 107.2(8) . . ?
O5 C18 C17 102.2(7) . . ?
O5 C18 H18A 111.3 . . ?
C17 C18 H18A 111.3 . . ?
O5 C18 H18B 111.3 . . ?
C17 C18 H18B 111.3 . . ?
H18A C18 H18B 109.2 . . ?
O6 C19 C20 107.6(7) . . ?
O6 C19 H19A 110.2 . . ?
C20 C19 H19A 110.2 . . ?
O6 C19 H19B 110.2 . . ?
C20 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
C21 C20 C19 104.2(8) . . ?
C21 C20 H20A 110.9 . . ?
C19 C20 H20A 110.9 . . ?
C21 C20 H20B 110.9 . . ?
C19 C20 H20B 110.9 . . ?
H20A C20 H20B 108.9 . . ?
C20 C21 C22 104.5(7) . . ?
C20 C21 H21A 110.9 . . ?
C22 C21 H21A 110.9 . . ?
C20 C21 H21B 110.9 . . ?
C22 C21 H21B 110.9 . . ?
H21A C21 H21B 108.9 . . ?
O6 C22 C21 104.8(7) . . ?
O6 C22 H22A 110.8 . . ?
C21 C22 H22A 110.8 . . ?
O6 C22 H22B 110.8 . . ?
C21 C22 H22B 110.8 . . ?
H22A C22 H22B 108.9 . . ?

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
Pd C1 C2 C3 -97.4(6) . . . . ?
C1 C2 C3 C4 36.1(9) . . . . ?
Pd C2 C3 C4 -42.5(6) . . . . ?
C2 C3 C4 C5 151.5(5) . . . . ?
C2 C3 C4 C9 38.0(8) . . . . ?
C3 C4 C5 C10 -78.4(6) . . . . ?
C9 C4 C5 C10 40.6(6) . . . . ?
C3 C4 C5 C6 175.3(5) . . . . ?
C9 C4 C5 C6 -65.7(6) . . . . ?
C4 C5 C6 C11 -46.7(6) . . . . ?
C10 C5 C6 C11 -153.2(5) . . . . ?
C4 C5 C6 C7 76.9(6) . . . . ?
C10 C5 C6 C7 -29.6(6) . . . . ?
C11 C6 C7 C13 -18.8(8) . . . . ?
C5 C6 C7 C13 -139.6(6) . . . . ?
C11 C6 C7 C8 112.8(6) . . . . ?
C5 C6 C7 C8 -8.0(6) . . . . ?
C13 C7 C8 C10 175.5(5) . . . . ?
C6 C7 C8 C10 42.6(6) . . . . ?
C13 C7 C8 C9 68.1(6) . . . . ?
C6 C7 C8 C9 -64.8(6) . . . . ?
C10 C8 C9 C4 -27.5(6) . . . . ?
C7 C8 C9 C4 76.2(6) . . . . ?
C10 C8 C9 Pd 95.5(5) . . . . ?
C7 C8 C9 Pd -160.8(4) . . . . ?
C5 C4 C9 C8 -7.9(6) . . . . ?
C3 C4 C9 C8 111.5(6) . . . . ?
C5 C4 C9 Pd -132.9(4) . . . . ?
C3 C4 C9 Pd -13.5(7) . . . . ?
C9 C8 C10 C5 51.2(6) . . . . ?
C7 C8 C10 C5 -60.3(5) . . . . ?
C4 C5 C10 C8 -56.4(6) . . . . ?
C6 C5 C10 C8 55.8(6) . . . . ?
C12 O2 C11 O1 -4.0(10) . . . . ?
C12 O2 C11 C6 174.3(5) . . . . ?
C5 C6 C11 O1 107.8(8) . . . . ?
C7 C6 C11 O1 -8.1(10) . . . . ?
C5 C6 C11 O2 -70.4(7) . . . . ?
C7 C6 C11 O2 173.7(5) . . . . ?
C14 O4 C13 O3 -7.2(9) . . . . ?
C14 O4 C13 C7 176.6(6) . . . . ?
C8 C7 C13 O3 -0.8(9) . . . . ?
C6 C7 C13 O3 124.5(7) . . . . ?
C8 C7 C13 O4 175.3(5) . . . . ?
C6 C7 C13 O4 -59.4(7) . . . . ?
C18 O5 C15 C16 7.1(9) . . . . ?
Pd O5 C15 C16 179.4(5) . . . . ?
O5 C15 C16 C17 -29.4(12) . . . . ?
O5 C15 C16 C17' 8.0(17) . . . . ?
C17' C16 C17 C18 -65.2(14) . . . . ?
C15 C16 C17 C18 39.4(14) . . . . ?
C17 C16 C17' C18 67.6(15) . . . . ?
C15 C16 C17' C18 -19(2) . . . . ?
C15 O5 C18 C17' -19.3(16) . . . . ?
Pd O5 C18 C17' 168.1(14) . . . . ?
C15 O5 C18 C17 16.4(11) . . . . ?
Pd O5 C18 C17 -156.1(8) . . . . ?
C16 C17' C18 O5 23(2) . . . . ?
C16 C17' C18 C17 -63.8(15) . . . . ?
C16 C17 C18 O5 -34.7(14) . . . . ?
C16 C17 C18 C17' 68.0(14) . . . . ?
C22 O6 C19 C20 -2.1(11) . . . . ?
Pd O6 C19 C20 159.6(6) . . . . ?
O6 C19 C20 C21 20.7(11) . . . . ?
C19 C20 C21 C22 -30.4(11) . . . . ?
C19 O6 C22 C21 -16.8(10) . . . . ?
Pd O6 C22 C21 -175.8(5) . . . . ?
C20 C21 C22 O6 29.5(10) . . . . ?

_refine_diff_density_max         0.375
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.079

_shelxl_version_number           2013-3



####################################################################### 
# 
# 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_clav014
_database_code_depnum_ccdc_archive 'CCDC 1034348'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-12-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H28 F6 N3 O10 Pd Sb'
_chemical_formula_weight         776.57

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   10.0271(7)
_cell_length_b                   19.0026(14)
_cell_length_c                   14.5138(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.7470(10)
_cell_angle_gamma                90
_cell_volume                     2762.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.60

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_F_000             1528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.571
_exptl_crystal_size_mid          0.322
_exptl_crystal_size_min          0.268
_exptl_absorpt_coefficient_mu    1.721
_shelx_estimated_absorpt_T_min   0.440
_shelx_estimated_absorpt_T_max   0.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6202
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'

_exptl_special_details           
; 
Data collection is performed with four batch runs at 
φ = 0.00 ° (600 frames), at φ = 90.00 ° 
(600 frames), at φ = 180 ° (600 frames) and 
at φ = 270 ° (600 frames). 
Frame width = 0.30 \& in ω. 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            35550
_diffrn_reflns_av_unetI/netI     0.0152
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.033
_diffrn_reflns_theta_max         27.726
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6464
_reflns_number_gt                5909
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0337P)²+3.7485P] 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         6464
_refine_ls_number_parameters     348
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_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
Pd Pd 1.00156(2) 0.18998(2) 1.01573(2) 0.02137(6) Uani 1 1 d . . . . .
O1 O 0.85655(19) 0.22845(10) 0.53063(12) 0.0307(4) Uani 1 1 d . . . . .
O2 O 0.77993(19) 0.12833(10) 0.58586(12) 0.0322(4) Uani 1 1 d . . . . .
O3 O 1.0157(2) 0.33913(10) 0.66607(11) 0.0310(4) Uani 1 1 d . . . . .
O4 O 0.9472(2) 0.36144(10) 0.80695(12) 0.0361(4) Uani 1 1 d . . . . .
C1 C 1.1969(3) 0.14845(16) 1.00226(18) 0.0340(6) Uani 1 1 d . . . . .
H1A H 1.2463 0.1659 0.9494 0.041 Uiso 1 1 calc R U . . .
H1B H 1.2531 0.1439 1.0599 0.041 Uiso 1 1 calc R U . . .
C2 C 1.1062(3) 0.09522(14) 0.98375(17) 0.0317(6) Uani 1 1 d . . . . .
H2 H 1.1041 0.0570 1.0310 0.038 Uiso 1 1 calc R U . . .
C3 C 1.0580(3) 0.07490(14) 0.88720(17) 0.0324(6) Uani 1 1 d . . . . .
H3A H 0.9709 0.0506 0.8895 0.039 Uiso 1 1 calc R U . . .
H3B H 1.1225 0.0417 0.8612 0.039 Uiso 1 1 calc R U . . .
C4 C 1.0428(2) 0.13951(13) 0.82417(15) 0.0238(5) Uani 1 1 d . . . . .
H4 H 1.1281 0.1488 0.7933 0.029 Uiso 1 1 calc R U . . .
C5 C 0.9270(2) 0.13011(12) 0.75134(15) 0.0229(5) Uani 1 1 d . . . . .
H5 H 0.9221 0.0826 0.7217 0.028 Uiso 1 1 calc R U . . .
C6 C 0.9332(2) 0.19235(12) 0.68324(15) 0.0215(4) Uani 1 1 d . . . . .
H6 H 1.0286 0.2025 0.6711 0.026 Uiso 1 1 calc R U . . .
C7 C 0.8750(2) 0.25486(12) 0.73910(15) 0.0211(4) Uani 1 1 d . . . . .
H7 H 0.7834 0.2648 0.7119 0.025 Uiso 1 1 calc R U . . .
C8 C 0.8582(2) 0.22232(12) 0.83592(14) 0.0210(4) Uani 1 1 d . . . . .
H8 H 0.7994 0.2496 0.8767 0.025 Uiso 1 1 calc R U . . .
C9 C 0.9990(2) 0.20644(12) 0.87802(15) 0.0212(4) Uani 1 1 d . . . . .
H9 H 1.0600 0.2464 0.8646 0.025 Uiso 1 1 calc R U . . .
C10 C 0.8054(2) 0.14960(13) 0.80714(16) 0.0254(5) Uani 1 1 d . . . . .
H10A H 0.7214 0.1520 0.7685 0.031 Uiso 1 1 calc R U . . .
H10B H 0.7941 0.1179 0.8604 0.031 Uiso 1 1 calc R U . . .
C11 C 0.8549(2) 0.18451(13) 0.59274(16) 0.0231(5) Uani 1 1 d . . . . .
C12 C 0.7030(4) 0.11876(18) 0.4988(2) 0.0483(8) Uani 1 1 d . . . . .
H12A H 0.6412 0.1583 0.4891 0.072 Uiso 1 1 calc R U . . .
H12B H 0.6524 0.0747 0.5008 0.072 Uiso 1 1 calc R U . . .
H12C H 0.7639 0.1169 0.4480 0.072 Uiso 1 1 calc R U . . .
C13 C 0.9541(3) 0.32151(13) 0.73285(16) 0.0253(5) Uani 1 1 d . . . . .
C14 C 1.0180(5) 0.42832(16) 0.8045(2) 0.0557(10) Uani 1 1 d . . . . .
H14A H 1.1137 0.4195 0.7998 0.083 Uiso 1 1 calc R U . . .
H14B H 1.0031 0.4548 0.8610 0.083 Uiso 1 1 calc R U . . .
H14C H 0.9847 0.4556 0.7509 0.083 Uiso 1 1 calc R U . . .
C15 C 0.3119(6) 0.3855(3) 0.0172(4) 0.0902(16) Uani 1 1 d . . . . .
H15A H 0.3552 0.4278 -0.0058 0.135 Uiso 1 1 calc R U . . .
H15B H 0.2923 0.3530 -0.0341 0.135 Uiso 1 1 calc R U . . .
H15C H 0.3715 0.3626 0.0635 0.135 Uiso 1 1 calc R U . . .
N1 N 0.1897(4) 0.4049(3) 0.0584(3) 0.0795(12) Uani 1 1 d . . . . .
O5 O 0.0889(5) 0.3828(4) 0.0250(4) 0.190(4) Uani 1 1 d . . . . .
O6 O 0.1954(5) 0.4372(2) 0.1286(4) 0.1306(18) Uani 1 1 d . . . . .
C16 C 0.5743(5) 0.1393(3) 0.0009(3) 0.0795(14) Uani 1 1 d . . . . .
H16A H 0.5073 0.1480 0.0466 0.119 Uiso 1 1 calc R U . . .
H16B H 0.5304 0.1206 -0.0557 0.119 Uiso 1 1 calc R U . . .
H16C H 0.6194 0.1836 -0.0130 0.119 Uiso 1 1 calc R U . . .
N2 N 0.6704(4) 0.0894(2) 0.0372(3) 0.0687(9) Uani 1 1 d . . . . .
O7 O 0.6702(8) 0.0335(3) 0.0050(4) 0.181(3) Uani 1 1 d . . . . .
O8 O 0.7467(5) 0.1043(3) 0.0954(4) 0.161(3) Uani 1 1 d . . . . .
C17 C 0.5303(8) 0.4985(3) 0.7297(5) 0.119(3) Uani 1 1 d . . . . .
H17A H 0.4876 0.4937 0.6679 0.178 Uiso 1 1 calc R U . . .
H17B H 0.5965 0.4610 0.7399 0.178 Uiso 1 1 calc R U . . .
H17C H 0.5747 0.5443 0.7352 0.178 Uiso 1 1 calc R U . . .
N3 N 0.4326(7) 0.4934(2) 0.7964(5) 0.1087(18) Uani 1 1 d . . . . .
O9 O 0.3221(6) 0.4974(3) 0.7731(8) 0.215(4) Uani 1 1 d . . . . .
O10 O 0.4794(8) 0.4821(3) 0.8766(4) 0.170(3) Uani 1 1 d . . . . .
Sb Sb 0.41405(2) 0.25751(2) 0.75034(2) 0.03384(6) Uani 1 1 d . . . . .
F1 F 0.2736(2) 0.22993(11) 0.66892(15) 0.0555(5) Uani 1 1 d . . . . .
F2 F 0.4151(3) 0.16779(14) 0.80253(19) 0.0833(8) Uani 1 1 d . . . . .
F3 F 0.5366(2) 0.22740(14) 0.66614(16) 0.0672(6) Uani 1 1 d . . . . .
F4 F 0.5542(2) 0.28412(16) 0.83115(17) 0.0764(7) Uani 1 1 d . . . . .
F5 F 0.4121(2) 0.34650(11) 0.69651(17) 0.0661(6) Uani 1 1 d . . . . .
F6 F 0.2900(2) 0.28682(16) 0.83370(18) 0.0784(7) Uani 1 1 d . . . . .


_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
Pd C9 2.022(2) . ?
Pd C1 2.129(3) . ?
Pd O1 2.1434(18) 4_566 ?
Pd C2 2.146(2) . ?
Pd O3 2.2488(17) 4_566 ?
O1 C11 1.229(3) . ?
O1 Pd 2.1433(18) 4_565 ?
O2 C11 1.307(3) . ?
O2 C12 1.460(3) . ?
O3 C13 1.221(3) . ?
O3 Pd 2.2489(17) 4_565 ?
O4 C13 1.321(3) . ?
O4 C14 1.457(4) . ?
C1 C2 1.378(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.510(3) . ?
C2 H2 1.0000 . ?
C3 C4 1.534(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.542(3) . ?
C4 C9 1.567(3) . ?
C4 H4 1.0000 . ?
C5 C10 1.541(3) . ?
C5 C6 1.545(3) . ?
C5 H5 1.0000 . ?
C6 C11 1.505(3) . ?
C6 C7 1.567(3) . ?
C6 H6 1.0000 . ?
C7 C13 1.500(3) . ?
C7 C8 1.552(3) . ?
C7 H7 1.0000 . ?
C8 C10 1.531(3) . ?
C8 C9 1.541(3) . ?
C8 H8 1.0000 . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 N1 1.436(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N1 O5 1.177(6) . ?
N1 O6 1.189(6) . ?
C16 N2 1.435(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N2 O8 1.148(6) . ?
N2 O7 1.161(6) . ?
C17 N3 1.413(8) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N3 O9 1.145(8) . ?
N3 O10 1.252(8) . ?
Sb F4 1.857(2) . ?
Sb F6 1.861(2) . ?
Sb F5 1.863(2) . ?
Sb F3 1.864(2) . ?
Sb F2 1.865(2) . ?
Sb F1 1.8696(19) . ?

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
C9 Pd C1 86.26(10) . . ?
C9 Pd O1 90.64(8) . 4_566 ?
C1 Pd O1 155.34(10) . 4_566 ?
C9 Pd C2 84.21(9) . . ?
C1 Pd C2 37.61(11) . . ?
O1 Pd C2 165.86(9) 4_566 . ?
C9 Pd O3 173.91(8) . 4_566 ?
C1 Pd O3 88.99(9) . 4_566 ?
O1 Pd O3 95.26(7) 4_566 4_566 ?
C2 Pd O3 89.69(8) . 4_566 ?
C11 O1 Pd 126.72(16) . 4_565 ?
C11 O2 C12 116.5(2) . . ?
C13 O3 Pd 133.79(17) . 4_565 ?
C13 O4 C14 115.8(2) . . ?
C2 C1 Pd 71.87(15) . . ?
C2 C1 H1A 116.4 . . ?
Pd C1 H1A 116.4 . . ?
C2 C1 H1B 116.4 . . ?
Pd C1 H1B 116.4 . . ?
H1A C1 H1B 113.4 . . ?
C1 C2 C3 123.2(3) . . ?
C1 C2 Pd 70.53(15) . . ?
C3 C2 Pd 106.11(16) . . ?
C1 C2 H2 115.8 . . ?
C3 C2 H2 115.8 . . ?
Pd C2 H2 115.8 . . ?
C2 C3 C4 111.5(2) . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 C5 111.5(2) . . ?
C3 C4 C9 112.00(19) . . ?
C5 C4 C9 102.49(18) . . ?
C3 C4 H4 110.2 . . ?
C5 C4 H4 110.2 . . ?
C9 C4 H4 110.2 . . ?
C10 C5 C4 101.57(18) . . ?
C10 C5 C6 102.08(19) . . ?
C4 C5 C6 107.33(19) . . ?
C10 C5 H5 114.8 . . ?
C4 C5 H5 114.8 . . ?
C6 C5 H5 114.8 . . ?
C11 C6 C5 116.58(19) . . ?
C11 C6 C7 109.59(19) . . ?
C5 C6 C7 102.83(17) . . ?
C11 C6 H6 109.2 . . ?
C5 C6 H6 109.2 . . ?
C7 C6 H6 109.2 . . ?
C13 C7 C8 118.16(19) . . ?
C13 C7 C6 113.4(2) . . ?
C8 C7 C6 103.04(18) . . ?
C13 C7 H7 107.2 . . ?
C8 C7 H7 107.2 . . ?
C6 C7 H7 107.2 . . ?
C10 C8 C9 103.30(19) . . ?
C10 C8 C7 99.43(17) . . ?
C9 C8 C7 107.48(18) . . ?
C10 C8 H8 115.0 . . ?
C9 C8 H8 115.0 . . ?
C7 C8 H8 115.0 . . ?
C8 C9 C4 103.55(18) . . ?
C8 C9 Pd 112.99(15) . . ?
C4 C9 Pd 112.15(15) . . ?
C8 C9 H9 109.3 . . ?
C4 C9 H9 109.3 . . ?
Pd C9 H9 109.3 . . ?
C8 C10 C5 95.03(18) . . ?
C8 C10 H10A 112.7 . . ?
C5 C10 H10A 112.7 . . ?
C8 C10 H10B 112.7 . . ?
C5 C10 H10B 112.7 . . ?
H10A C10 H10B 110.2 . . ?
O1 C11 O2 121.8(2) . . ?
O1 C11 C6 123.2(2) . . ?
O2 C11 C6 114.9(2) . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C13 O4 122.5(2) . . ?
O3 C13 C7 124.7(2) . . ?
O4 C13 C7 112.8(2) . . ?
O4 C14 H14A 109.5 . . ?
O4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O5 N1 O6 122.8(6) . . ?
O5 N1 C15 118.1(6) . . ?
O6 N1 C15 118.8(5) . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O8 N2 O7 120.8(6) . . ?
O8 N2 C16 121.3(5) . . ?
O7 N2 C16 118.0(5) . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O9 N3 O10 126.8(9) . . ?
O9 N3 C17 119.1(9) . . ?
O10 N3 C17 114.0(7) . . ?
F4 Sb F6 90.97(12) . . ?
F4 Sb F5 90.57(12) . . ?
F6 Sb F5 90.40(13) . . ?
F4 Sb F3 89.69(11) . . ?
F6 Sb F3 179.28(12) . . ?
F5 Sb F3 89.87(12) . . ?
F4 Sb F2 90.17(13) . . ?
F6 Sb F2 90.03(14) . . ?
F5 Sb F2 179.13(12) . . ?
F3 Sb F2 89.70(13) . . ?
F4 Sb F1 179.50(11) . . ?
F6 Sb F1 89.32(11) . . ?
F5 Sb F1 89.82(10) . . ?
F3 Sb F1 90.01(10) . . ?
F2 Sb F1 89.42(11) . . ?

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
Pd C1 C2 C3 96.9(2) . . . . ?
C1 C2 C3 C4 -36.5(4) . . . . ?
Pd C2 C3 C4 40.4(3) . . . . ?
C2 C3 C4 C5 -147.2(2) . . . . ?
C2 C3 C4 C9 -33.0(3) . . . . ?
C3 C4 C5 C10 81.5(2) . . . . ?
C9 C4 C5 C10 -38.5(2) . . . . ?
C3 C4 C5 C6 -171.83(19) . . . . ?
C9 C4 C5 C6 68.2(2) . . . . ?
C10 C5 C6 C11 -89.7(2) . . . . ?
C4 C5 C6 C11 163.9(2) . . . . ?
C10 C5 C6 C7 30.2(2) . . . . ?
C4 C5 C6 C7 -76.2(2) . . . . ?
C11 C6 C7 C13 -100.2(2) . . . . ?
C5 C6 C7 C13 135.19(19) . . . . ?
C11 C6 C7 C8 130.88(19) . . . . ?
C5 C6 C7 C8 6.3(2) . . . . ?
C13 C7 C8 C10 -166.5(2) . . . . ?
C6 C7 C8 C10 -40.6(2) . . . . ?
C13 C7 C8 C9 -59.3(3) . . . . ?
C6 C7 C8 C9 66.7(2) . . . . ?
C10 C8 C9 C4 29.8(2) . . . . ?
C7 C8 C9 C4 -74.8(2) . . . . ?
C10 C8 C9 Pd -91.79(18) . . . . ?
C7 C8 C9 Pd 163.68(15) . . . . ?
C3 C4 C9 C8 -114.2(2) . . . . ?
C5 C4 C9 C8 5.5(2) . . . . ?
C3 C4 C9 Pd 8.0(3) . . . . ?
C5 C4 C9 Pd 127.58(16) . . . . ?
C9 C8 C10 C5 -52.38(19) . . . . ?
C7 C8 C10 C5 58.24(19) . . . . ?
C4 C5 C10 C8 55.8(2) . . . . ?
C6 C5 C10 C8 -54.98(19) . . . . ?
Pd O1 C11 O2 -165.22(18) 4_565 . . . ?
Pd O1 C11 C6 17.5(4) 4_565 . . . ?
C12 O2 C11 O1 2.8(4) . . . . ?
C12 O2 C11 C6 -179.7(2) . . . . ?
C5 C6 C11 O1 -176.2(2) . . . . ?
C7 C6 C11 O1 67.5(3) . . . . ?
C5 C6 C11 O2 6.3(3) . . . . ?
C7 C6 C11 O2 -109.9(2) . . . . ?
Pd O3 C13 O4 -155.98(19) 4_565 . . . ?
Pd O3 C13 C7 21.6(4) 4_565 . . . ?
C14 O4 C13 O3 -0.1(4) . . . . ?
C14 O4 C13 C7 -177.9(3) . . . . ?
C8 C7 C13 O3 152.1(2) . . . . ?
C6 C7 C13 O3 31.3(3) . . . . ?
C8 C7 C13 O4 -30.1(3) . . . . ?
C6 C7 C13 O4 -150.8(2) . . . . ?

_refine_diff_density_max         0.813
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.082

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_clav008s-sr
_database_code_depnum_ccdc_archive 'CCDC 1034422'
_audit_update_record             
;
2014-11-17 deposited with the CCDC.
2014-12-24 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.006 0.000 0.500 1256 395 tetrachloroethylene
_platon_squeeze_details          
;
PLATON Reference : 
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
Spek, A.L. (2009). Acta Cryst. D65, 148-155.

Void space analysis consistent with
a fifth, severely disordered C2CH2Cl4 molecule
of solvation.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C56 H76 O16 Pd4, 4(F6 Sb), 5(C2 H2 Cl4)'
_chemical_formula_sum            'C66 H86 Cl20 F24 O16 Pd4 Sb4'
_chemical_formula_weight         3212.94

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'
O O 0.0106 0.0060 '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'
Sb Sb -0.5866 1.5461 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   16.4284(14)
_cell_length_b                   19.3745(17)
_cell_length_c                   21.4447(19)
_cell_angle_alpha                66.181(2)
_cell_angle_beta                 88.434(2)
_cell_angle_gamma                72.775(2)
_cell_volume                     5930.9(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    8466
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      22.27

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_F_000             3108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.088
_exptl_absorpt_coefficient_mu    2.025
_shelx_estimated_absorpt_T_min   0.709
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6811
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'APEX2 (Bruker, 2007)'

_exptl_special_details           
; 
Data collection is performed with four batch runs at 
φ = 0.00 ° (600 frames), at φ = 90.00 ° 
(600 frames), at φ = 180 ° (600 frames) and 
at φ = 270 ° (600 frames). 
Frame width = 0.30 \& in ω. 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            79047
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.585
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             27085
_reflns_number_gt                15699
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0629P)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         27085
_refine_ls_number_parameters     985
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1494
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.054
_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 0.39995(3) 0.84126(3) 0.30190(3) 0.03620(13) Uani 1 1 d . . . . .
Pd2 Pd 0.82835(3) 0.56285(3) 0.41878(2) 0.03374(12) Uani 1 1 d . . . . .
Pd3 Pd 0.82980(3) 0.50335(3) 0.10066(2) 0.02951(11) Uani 1 1 d . . . . .
Pd4 Pd 0.39634(3) 0.79813(3) -0.02618(2) 0.03199(12) Uani 1 1 d . . . . .
Sb1 Sb 0.11888(2) 0.58529(2) 0.14818(2) 0.03912(12) Uani 1 1 d G . . . .
F1 F 0.09734(2) 0.60693(2) 0.05663(2) 0.0687(13) Uani 1 1 d G . . . .
F2 F 0.13592(2) 0.56589(2) 0.23940(2) 0.0761(14) Uani 1 1 d G . . . .
F3 F 0.14213(2) 0.68163(2) 0.11991(2) 0.0741(14) Uani 1 1 d G . . . .
F4 F 0.09219(2) 0.49063(2) 0.17313(2) 0.0663(13) Uani 1 1 d G . . . .
F5 F 0.00305(2) 0.63685(2) 0.14716(2) 0.0664(13) Uani 1 1 d G . . . .
F6 F 0.23310(2) 0.52953(2) 0.14997(2) 0.0722(14) Uani 1 1 d G . . . .
Sb2 Sb 0.53846(2) 0.50822(2) 0.29574(2) 0.04523(13) Uani 1 1 d G . . . .
F7 F 0.47623(2) 0.45373(2) 0.27395(2) 0.214(6) Uani 1 1 d G . . . .
F8 F 0.59753(2) 0.56300(2) 0.31993(2) 0.158(4) Uani 1 1 d G . . . .
F9 F 0.46457(2) 0.60275(2) 0.23045(2) 0.0884(17) Uani 1 1 d G . . . .
F10 F 0.60860(2) 0.41156(2) 0.36190(2) 0.113(2) Uani 1 1 d G . . . .
F11 F 0.46514(2) 0.51504(2) 0.36244(2) 0.132(3) Uani 1 1 d G . . . .
F12 F 0.61459(2) 0.49668(2) 0.23219(2) 0.189(5) Uani 1 1 d G . . . .
Sb3 Sb 0.31162(2) 0.13621(2) 0.07394(2) 0.05068(14) Uani 1 1 d G . . . .
F13 F 0.24349(3) 0.07965(2) 0.12848(2) 0.0837(16) Uani 1 1 d G . . . .
F14 F 0.37584(2) 0.19614(2) 0.01839(2) 0.0644(13) Uani 1 1 d G . . . .
F15 F 0.27811(3) 0.11549(2) 0.00240(2) 0.0751(14) Uani 1 1 d G . . . .
F16 F 0.34059(2) 0.15695(2) 0.14711(2) 0.114(2) Uani 1 1 d G . . . .
F17 F 0.21714(2) 0.22769(2) 0.04732(2) 0.0943(19) Uani 1 1 d G . . . .
F18 F 0.40692(3) 0.04568(2) 0.10415(2) 0.0755(15) Uani 1 1 d G . . . .
Sb4 Sb 0.17995(2) 0.20626(2) 0.48050(2) 0.07013(19) Uani 0.664(3) 1 d G U P A 1
F19 F 0.25218(2) 0.10249(2) 0.51194(2) 0.202(4) Uani 0.664(3) 1 d G U P A 1
F20 F 0.10429(2) 0.30820(2) 0.44980(2) 0.180(4) Uani 0.664(3) 1 d G U P A 1
F21 F 0.17280(2) 0.20747(2) 0.39321(2) 0.146(3) Uani 0.664(3) 1 d G U P A 1
F22 F 0.18772(2) 0.20032(2) 0.56967(2) 0.125(3) Uani 0.664(3) 1 d G U P A 1
F23 F 0.08767(2) 0.16629(2) 0.50191(2) 0.196(4) Uani 0.664(3) 1 d G U P A 1
F24 F 0.27267(2) 0.24541(2) 0.46343(2) 0.152(3) Uani 0.664(3) 1 d G U P A 1
Sb4' Sb 0.17642(2) 0.21020(2) 0.47088(2) 0.07013(19) Uani 0.336(3) 1 d G U P A
2
F19' F 0.24951(2) 0.14239(2) 0.43784(2) 0.202(4) Uani 0.336(3) 1 d G U P A 2
F20' F 0.10221(2) 0.27450(2) 0.50611(2) 0.180(4) Uani 0.336(3) 1 d G U P A 2
F21' F 0.08969(2) 0.22938(2) 0.40579(2) 0.146(3) Uani 0.336(3) 1 d G U P A 2
F22' F 0.26543(2) 0.18653(2) 0.53631(2) 0.125(3) Uani 0.336(3) 1 d G U P A 2
F23' F 0.14675(3) 0.12340(2) 0.53294(2) 0.196(4) Uani 0.336(3) 1 d G U P A 2
F24' F 0.21048(2) 0.29538(2) 0.41188(2) 0.152(3) Uani 0.336(3) 1 d G U P A 2
O1 O 0.79254(3) 0.57779(3) 0.51588(2) 0.0451(12) Uani 1 1 d G . . . .
O2 O 0.72475(2) 0.51498(3) 0.43929(2) 0.0362(10) Uani 1 1 d G . . . .
O3 O 0.68444(3) 0.61054(3) 0.57446(2) 0.0445(12) Uani 1 1 d G . . . .
O4 O 0.59413(2) 0.52584(2) 0.47272(2) 0.0353(10) Uani 1 1 d G . . . .
O5 O 0.95056(2) 0.41122(3) 0.16183(2) 0.0386(11) Uani 1 1 d G . . . .
O6 O 0.77417(2) 0.43651(3) 0.18577(2) 0.0346(10) Uani 1 1 d G . . . .
O7 O 1.03644(2) 0.34721(3) 0.25770(3) 0.0405(11) Uani 1 1 d G . . . .
O8 O 0.79203(2) 0.36452(2) 0.29985(2) 0.0372(10) Uani 1 1 d G . . . .
O9 O 0.41882(3) 0.74014(2) -0.09908(2) 0.0428(11) Uani 1 1 d G . . . .
O10 O 0.41180(2) 0.67900(2) 0.04453(2) 0.0334(10) Uani 1 1 d G . . . .
O11 O 0.48355(3) 0.62813(2) -0.11166(2) 0.0426(11) Uani 1 1 d G . . . .
O12 O 0.48067(2) 0.54985(2) 0.09397(2) 0.0316(10) Uani 1 1 d G . . . .
O13 O 0.26847(3) 0.90861(2) 0.25188(2) 0.0411(11) Uani 1 1 d G . . . .
O14 O 0.36856(3) 0.74586(2) 0.29258(2) 0.0359(10) Uani 1 1 d G . . . .
O15 O 0.16122(3) 0.94943(2) 0.17194(2) 0.0434(11) Uani 1 1 d G . . . .
O16 O 0.29325(2) 0.71185(2) 0.23209(2) 0.0343(10) Uani 1 1 d G . . . .
Cl1 Cl 0.98542(2) 0.18902(3) 0.62909(2) 0.1135(11) Uani 1 1 d G . . . .
Cl2 Cl 0.87600(2) 0.35210(3) 0.55392(2) 0.0748(6) Uani 1 1 d G . . . .
Cl3 Cl 0.77895(2) 0.21589(3) 0.60684(2) 0.0946(9) Uani 1 1 d G . . . .
Cl4 Cl 0.79397(2) 0.28414(2) 0.46169(2) 0.0818(7) Uani 1 1 d G . . . .
Cl5 Cl 0.38480(3) 0.29715(3) 0.81547(2) 0.1029(10) Uani 1 1 d G . . . .
Cl6 Cl 0.20381(4) 0.29551(3) 0.84841(2) 0.0712(6) Uani 1 1 d G . . . .
Cl7 Cl 0.43634(4) 0.10886(3) 0.87197(2) 0.0889(8) Uani 1 1 d G . . . .
Cl8 Cl 0.29107(3) 0.20941(3) 0.75373(2) 0.0799(7) Uani 1 1 d G . . . .
Cl9 Cl 0.09730(4) 0.13993(4) 0.95609(2) 0.0782(7) Uani 1 1 d G . . . .
Cl10 Cl -0.00365(4) 0.06337(4) 0.91509(2) 0.1016(9) Uani 1 1 d G . . . .
Cl11 Cl -0.07183(3) 0.22500(4) 0.77592(2) 0.1011(10) Uani 1 1 d G . . . .
Cl12 Cl 0.11011(4) 0.14551(3) 0.80163(2) 0.1053(10) Uani 1 1 d G . . . .
Cl13 Cl 0.91052(2) 0.20837(3) 0.18780(2) 0.1492(16) Uani 1 1 d G . . . .
Cl14 Cl 1.03757(2) 0.22843(4) 0.09203(3) 0.1127(11) Uani 1 1 d G . . . .
Cl15 Cl 0.76903(2) 0.27189(3) 0.05255(2) 0.1312(13) Uani 1 1 d G . . . .
Cl16 Cl 0.91095(2) 0.13068(3) 0.07610(3) 0.0908(8) Uani 1 1 d G . . . .
C1 C 0.44884(3) 0.93888(2) 0.27323(3) 0.070(3) Uani 1 1 d G . . . .
H1A H 0.5117 0.9266 0.2724 0.084 Uiso 1 1 calc R U . . .
H1B H 0.4159 0.9885 0.2344 0.084 Uiso 1 1 calc R U . . .
C2 C 0.4185(6) 0.9250(4) 0.3369(4) 0.065(2) Uani 1 1 d . . . . .
H2 H 0.3656 0.9661 0.3383 0.077 Uiso 1 1 calc R U . . .
C3 C 0.4778(5) 0.8785(4) 0.4013(4) 0.057(2) Uani 1 1 d . . . . .
H3A H 0.4455 0.8556 0.4399 0.069 Uiso 1 1 calc R U . . .
H3B H 0.5024 0.9142 0.4115 0.069 Uiso 1 1 calc R U . . .
C4 C 0.5509(5) 0.8110(4) 0.3946(3) 0.0448(17) Uani 1 1 d . . . . .
H4 H 0.6003 0.8301 0.3755 0.054 Uiso 1 1 calc R U . . .
C5 C 0.5805(4) 0.7379(4) 0.4636(3) 0.0418(16) Uani 1 1 d . . . . .
H5 H 0.5861 0.7507 0.5037 0.050 Uiso 1 1 calc R U . . .
C6 C 0.6634(4) 0.6816(4) 0.4530(3) 0.0371(15) Uani 1 1 d . . . . .
H6 H 0.6982 0.7145 0.4239 0.044 Uiso 1 1 calc R U . . .
C7 C 0.6264(4) 0.6453(4) 0.4085(3) 0.0288(13) Uani 1 1 d . . . . .
H7 H 0.6489 0.6622 0.3627 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5292(4) 0.6904(3) 0.3984(3) 0.0299(13) Uani 1 1 d . . . . .
H8 H 0.4918 0.6657 0.3842 0.036 Uiso 1 1 calc R U . . .
C9 C 0.5193(4) 0.7760(4) 0.3497(3) 0.0321(14) Uani 1 1 d . . . . .
H9 H 0.5593 0.7754 0.3138 0.039 Uiso 1 1 calc R U . . .
C10 C 0.5139(4) 0.6952(4) 0.4678(3) 0.0380(15) Uani 1 1 d . . . . .
H10A H 0.4549 0.7276 0.4686 0.046 Uiso 1 1 calc R U . . .
H10B H 0.5286 0.6423 0.5069 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7195(4) 0.6188(4) 0.5176(3) 0.0352(15) Uani 1 1 d . . . . .
C12 C 0.6527(4) 0.5564(4) 0.4412(3) 0.0327(14) Uani 1 1 d . . . . .
C13 C 0.7372(5) 0.5534(4) 0.6374(3) 0.0499(19) Uani 1 1 d . . . . .
H13A H 0.7652 0.5036 0.6330 0.075 Uiso 1 1 calc R U . . .
H13B H 0.7013 0.5437 0.6753 0.075 Uiso 1 1 calc R U . . .
H13C H 0.7808 0.5743 0.6466 0.075 Uiso 1 1 calc R U . . .
C14 C 0.6196(4) 0.4387(4) 0.5080(4) 0.0439(17) Uani 1 1 d . . . . .
H14A H 0.6738 0.4189 0.5368 0.066 Uiso 1 1 calc R U . . .
H14B H 0.6267 0.4162 0.4739 0.066 Uiso 1 1 calc R U . . .
H14C H 0.5751 0.4230 0.5366 0.066 Uiso 1 1 calc R U . . .
C15 C 0.8868(4) 0.6544(4) 0.3773(4) 0.0458(18) Uani 1 1 d . . . . .
H15A H 0.8850 0.6794 0.3267 0.055 Uiso 1 1 calc R U . . .
H15B H 0.8761 0.6928 0.3984 0.055 Uiso 1 1 calc R U . . .
C16 C 0.9508(4) 0.5827(4) 0.4111(3) 0.0419(17) Uani 1 1 d . . . . .
H16 H 0.9794 0.5760 0.4547 0.050 Uiso 1 1 calc R U . . .
C17 C 1.0024(4) 0.5331(4) 0.3770(4) 0.0420(17) Uani 1 1 d . . . . .
H17A H 1.0247 0.4772 0.4109 0.050 Uiso 1 1 calc R U . . .
H17B H 1.0519 0.5516 0.3595 0.050 Uiso 1 1 calc R U . . .
C18 C 0.9492(4) 0.5375(4) 0.3181(3) 0.0308(14) Uani 1 1 d . . . . .
H18 H 0.9526 0.5820 0.2743 0.037 Uiso 1 1 calc R U . . .
C19 C 0.9773(4) 0.4588(4) 0.3109(3) 0.0378(16) Uani 1 1 d . . . . .
H19 H 1.0409 0.4337 0.3169 0.045 Uiso 1 1 calc R U . . .
C20 C 0.9330(4) 0.4702(4) 0.2426(3) 0.0314(14) Uani 1 1 d . . . . .
H20 H 0.9348 0.5222 0.2065 0.038 Uiso 1 1 calc R U . . .
C21 C 0.8359(3) 0.4803(4) 0.2589(3) 0.0294(13) Uani 1 1 d . . . . .
H21 H 0.8005 0.5362 0.2297 0.035 Uiso 1 1 calc R U . . .
C22 C 0.8406(4) 0.4696(4) 0.3355(3) 0.0309(14) Uani 1 1 d . . . . .
H22 H 0.7921 0.4549 0.3610 0.037 Uiso 1 1 calc R U . . .
C23 C 0.8539(4) 0.5459(4) 0.3329(3) 0.0331(14) Uani 1 1 d . . . . .
H23 H 0.8158 0.5923 0.2933 0.040 Uiso 1 1 calc R U . . .
C24 C 0.9300(4) 0.4076(4) 0.3645(3) 0.0374(15) Uani 1 1 d . . . . .
H24A H 0.9356 0.3569 0.3613 0.045 Uiso 1 1 calc R U . . .
H24B H 0.9470 0.3978 0.4121 0.045 Uiso 1 1 calc R U . . .
C25 C 0.9732(4) 0.4075(4) 0.2170(3) 0.0359(15) Uani 1 1 d . . . . .
C26 C 0.7980(4) 0.4245(4) 0.2448(3) 0.0303(14) Uani 1 1 d . . . . .
C27 C 1.0845(5) 0.2899(4) 0.2331(4) 0.058(2) Uani 1 1 d . . . . .
H27A H 1.1078 0.3168 0.1907 0.088 Uiso 1 1 calc R U . . .
H27B H 1.0469 0.2634 0.2240 0.088 Uiso 1 1 calc R U . . .
H27C H 1.1317 0.2504 0.2678 0.088 Uiso 1 1 calc R U . . .
C28 C 0.7530(5) 0.3087(4) 0.2890(4) 0.0516(19) Uani 1 1 d . . . . .
H28A H 0.6926 0.3365 0.2710 0.077 Uiso 1 1 calc R U . . .
H28B H 0.7572 0.2633 0.3327 0.077 Uiso 1 1 calc R U . . .
H28C H 0.7837 0.2900 0.2562 0.077 Uiso 1 1 calc R U . . .
C29 C 0.8944(4) 0.5828(4) 0.0353(3) 0.0408(16) Uani 1 1 d . . . . .
H29A H 0.8610 0.6399 0.0144 0.049 Uiso 1 1 calc R U . . .
H29B H 0.9547 0.5723 0.0510 0.049 Uiso 1 1 calc R U . . .
C30 C 0.8800(4) 0.5367(4) 0.0034(3) 0.0360(15) Uani 1 1 d . . . . .
H30 H 0.9324 0.4963 0.0001 0.043 Uiso 1 1 calc R U . . .
C31 C 0.8053(4) 0.5636(4) -0.0495(3) 0.0354(15) Uani 1 1 d . . . . .
H31A H 0.7944 0.5166 -0.0509 0.042 Uiso 1 1 calc R U . . .
H31B H 0.8194 0.5951 -0.0953 0.042 Uiso 1 1 calc R U . . .
C32 C 0.7236(4) 0.6146(4) -0.0320(3) 0.0320(14) Uani 1 1 d . . . . .
H32 H 0.7187 0.6723 -0.0548 0.038 Uiso 1 1 calc R U . . .
C33 C 0.6432(4) 0.6001(4) -0.0526(3) 0.0292(13) Uani 1 1 d . . . . .
H33 H 0.6436 0.5967 -0.0979 0.035 Uiso 1 1 calc R U . . .
C34 C 0.5645(4) 0.6667(4) -0.0483(3) 0.0296(13) Uani 1 1 d . . . . .
H34 H 0.5796 0.7172 -0.0654 0.035 Uiso 1 1 calc R U . . .
C35 C 0.5620(3) 0.6362(3) 0.0328(3) 0.0248(12) Uani 1 1 d . . . . .
H35 H 0.5729 0.6762 0.0470 0.030 Uiso 1 1 calc R U . . .
C36 C 0.6415(3) 0.5595(4) 0.0610(3) 0.0279(13) Uani 1 1 d . . . . .
H36 H 0.6412 0.5221 0.1094 0.033 Uiso 1 1 calc R U . . .
C37 C 0.7207(3) 0.5872(3) 0.0468(3) 0.0265(13) Uani 1 1 d . . . . .
H37 H 0.7113 0.6342 0.0580 0.032 Uiso 1 1 calc R U . . .
C38 C 0.6386(4) 0.5254(4) 0.0069(3) 0.0308(14) Uani 1 1 d . . . . .
H38A H 0.6887 0.4784 0.0138 0.037 Uiso 1 1 calc R U . . .
H38B H 0.5846 0.5136 0.0037 0.037 Uiso 1 1 calc R U . . .
C39 C 0.4824(4) 0.6822(4) -0.0889(3) 0.0318(14) Uani 1 1 d . . . . .
C40 C 0.4782(4) 0.6239(4) 0.0572(3) 0.0284(13) Uani 1 1 d . . . . .
C41 C 0.4097(5) 0.6426(5) -0.1561(4) 0.057(2) Uani 1 1 d . . . . .
H41A H 0.3576 0.6527 -0.1334 0.085 Uiso 1 1 calc R U . . .
H41B H 0.4162 0.5960 -0.1656 0.085 Uiso 1 1 calc R U . . .
H41C H 0.4053 0.6889 -0.1992 0.085 Uiso 1 1 calc R U . . .
C42 C 0.3979(4) 0.5399(4) 0.1206(3) 0.0401(16) Uani 1 1 d . . . . .
H42A H 0.3734 0.5781 0.1405 0.060 Uiso 1 1 calc R U . . .
H42B H 0.4083 0.4858 0.1559 0.060 Uiso 1 1 calc R U . . .
H42C H 0.3578 0.5492 0.0830 0.060 Uiso 1 1 calc R U . . .
C43 C 0.4246(5) 0.9047(4) -0.0901(4) 0.0479(18) Uani 1 1 d . . . . .
H43A H 0.4496 0.9293 -0.0663 0.058 Uiso 1 1 calc R U . . .
H43B H 0.4515 0.9051 -0.1321 0.058 Uiso 1 1 calc R U . . .
C44 C 0.3363(4) 0.9224(4) -0.0942(3) 0.0419(16) Uani 1 1 d . . . . .
H44 H 0.3076 0.9327 -0.1390 0.050 Uiso 1 1 calc R U . . .
C45 C 0.2818(4) 0.9579(4) -0.0517(3) 0.0402(16) Uani 1 1 d . . . . .
H45A H 0.2268 0.9464 -0.0498 0.048 Uiso 1 1 calc R U . . .
H45B H 0.2691 1.0163 -0.0741 0.048 Uiso 1 1 calc R U . . .
C46 C 0.3231(4) 0.9272(4) 0.0215(3) 0.0342(14) Uani 1 1 d . . . . .
H46 H 0.3567 0.9614 0.0244 0.041 Uiso 1 1 calc R U . . .
C47 C 0.2562(4) 0.9205(4) 0.0737(3) 0.0347(15) Uani 1 1 d . . . . .
H47 H 0.2029 0.9673 0.0584 0.042 Uiso 1 1 calc R U . . .
C48 C 0.3013(4) 0.9007(4) 0.1439(3) 0.0345(14) Uani 1 1 d . . . . .
H48 H 0.3422 0.9321 0.1355 0.041 Uiso 1 1 calc R U . . .
C49 C 0.3558(4) 0.8105(3) 0.1686(3) 0.0294(13) Uani 1 1 d . . . . .
H49 H 0.4179 0.8064 0.1716 0.035 Uiso 1 1 calc R U . . .
C50 C 0.3362(4) 0.7926(4) 0.1072(3) 0.0298(13) Uani 1 1 d . . . . .
H50 H 0.3493 0.7351 0.1175 0.036 Uiso 1 1 calc R U . . .
C51 C 0.3805(4) 0.8393(4) 0.0473(3) 0.0325(14) Uani 1 1 d . . . . .
H51 H 0.4381 0.8346 0.0658 0.039 Uiso 1 1 calc R U . . .
C52 C 0.2410(4) 0.8429(4) 0.0854(3) 0.0332(14) Uani 1 1 d . . . . .
H52A H 0.2182 0.8431 0.0431 0.040 Uiso 1 1 calc R U . . .
H52B H 0.2040 0.8271 0.1224 0.040 Uiso 1 1 calc R U . . .
C53 C 0.2426(4) 0.9194(4) 0.1948(3) 0.0362(15) Uani 1 1 d . . . . .
C54 C 0.3384(4) 0.7546(3) 0.2365(3) 0.0299(13) Uani 1 1 d . . . . .
C55 C 0.1006(5) 0.9730(5) 0.2166(4) 0.065(2) Uani 1 1 d . . . . .
H55A H 0.1174 0.9330 0.2640 0.097 Uiso 1 1 calc R U . . .
H55B H 0.0429 0.9771 0.2017 0.097 Uiso 1 1 calc R U . . .
H55C H 0.1011 1.0245 0.2140 0.097 Uiso 1 1 calc R U . . .
C56 C 0.2753(5) 0.6535(4) 0.2950(4) 0.0475(18) Uani 1 1 d . . . . .
H56A H 0.3293 0.6165 0.3224 0.071 Uiso 1 1 calc R U . . .
H56B H 0.2432 0.6241 0.2835 0.071 Uiso 1 1 calc R U . . .
H56C H 0.2412 0.6808 0.3213 0.071 Uiso 1 1 calc R U . . .
C59 C 0.8496(6) 0.2245(5) 0.5438(4) 0.065(2) Uani 1 1 d . . . . .
H59 H 0.8780 0.1702 0.5459 0.079 Uiso 1 1 calc R U . . .
C60 C 0.9176(6) 0.2561(5) 0.5526(4) 0.066(2) Uani 1 1 d . . . . .
H60 H 0.9528 0.2611 0.5131 0.079 Uiso 1 1 calc R U . . .
C61 C 0.3113(8) 0.1844(7) 0.8419(5) 0.110(4) Uani 1 1 d . . . . .
H61 H 0.2692 0.1601 0.8697 0.132 Uiso 1 1 calc R U . . .
C62 C 0.3301(11) 0.2318(9) 0.8621(6) 0.159(7) Uani 1 1 d . . . . .
H62 H 0.3525 0.2048 0.9118 0.191 Uiso 1 1 calc R U . . .
C63 C 0.0232(5) 0.1998(5) 0.8302(5) 0.067(2) Uani 1 1 d . . . . .
H63 H 0.0334 0.2496 0.8266 0.080 Uiso 1 1 calc R U . . .
C64 C 0.0106(5) 0.1530(5) 0.9024(4) 0.062(2) Uani 1 1 d . . . . .
H64 H -0.0423 0.1853 0.9140 0.074 Uiso 1 1 calc R U . . .
C65 C 0.8809(6) 0.2347(6) 0.0568(5) 0.084(3) Uani 1 1 d . . . . .
H65 H 0.8963 0.2612 0.0095 0.101 Uiso 1 1 calc R U . . .
C66 C 0.9248(6) 0.2571(7) 0.1011(5) 0.090(3) Uani 1 1 d . . . . .
H66 H 0.9024 0.3159 0.0865 0.108 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
Pd1 C9 2.021(6) . ?
Pd1 C1 2.1292 . ?
Pd1 C2 2.139(7) . ?
Pd1 O14 2.1425 . ?
Pd1 O13 2.2013 . ?
Pd2 C23 2.011(6) . ?
Pd2 O2 2.1246 . ?
Pd2 C15 2.132(6) . ?
Pd2 C16 2.148(6) . ?
Pd2 O1 2.2550 . ?
Pd3 C37 2.014(5) . ?
Pd3 O6 2.1316 . ?
Pd3 C30 2.140(6) . ?
Pd3 C29 2.146(6) . ?
Pd3 O5 2.2353 . ?
Pd4 C51 2.014(6) . ?
Pd4 O10 2.1303 . ?
Pd4 C43 2.146(6) . ?
Pd4 C44 2.175(6) . ?
Pd4 O9 2.2325 . ?
Sb1 F2 1.8493 . ?
Sb1 F1 1.8549 . ?
Sb1 F6 1.8600 . ?
Sb1 F5 1.8650 . ?
Sb1 F3 1.8690 . ?
Sb1 F4 1.8743 . ?
Sb2 F8 1.8492 . ?
Sb2 F7 1.8552 . ?
Sb2 F12 1.8598 . ?
Sb2 F11 1.8651 . ?
Sb2 F9 1.8690 . ?
Sb2 F10 1.8744 . ?
Sb3 F14 1.8493 . ?
Sb3 F13 1.8549 . ?
Sb3 F18 1.8598 . ?
Sb3 F17 1.8650 . ?
Sb3 F15 1.8687 . ?
Sb3 F16 1.8744 . ?
Sb4 F20 1.8493 . ?
Sb4 F19 1.8550 . ?
Sb4 F24 1.8599 . ?
Sb4 F23 1.8650 . ?
Sb4 F21 1.8690 . ?
Sb4 F22 1.8743 . ?
Sb4' F20' 1.8491 . ?
Sb4' F19' 1.8550 . ?
Sb4' F24' 1.8599 . ?
Sb4' F23' 1.8652 . ?
Sb4' F21' 1.8690 . ?
Sb4' F22' 1.8742 . ?
O1 C11 1.236(7) . ?
O2 C12 1.228(6) . ?
O3 C11 1.306(6) . ?
O3 C13 1.444(6) . ?
O4 C12 1.308(6) . ?
O4 C14 1.471(6) . ?
O5 C25 1.218(7) . ?
O6 C26 1.243(6) . ?
O7 C25 1.308(7) . ?
O7 C27 1.438(7) . ?
O8 C26 1.307(6) . ?
O8 C28 1.502(6) . ?
O9 C39 1.232(6) . ?
O10 C40 1.224(6) . ?
O11 C39 1.318(6) . ?
O11 C41 1.451(6) . ?
O12 C40 1.317(6) . ?
O12 C42 1.496(6) . ?
O13 C53 1.222(7) . ?
O14 C54 1.239(6) . ?
O15 C53 1.309(7) . ?
O15 C55 1.466(7) . ?
O16 C54 1.296(6) . ?
O16 C56 1.459(7) . ?
Cl1 C60 1.773(8) . ?
Cl2 C60 1.794(9) . ?
Cl3 C59 1.747(8) . ?
Cl4 C59 1.758(8) . ?
Cl5 C62 1.735(10) . ?
Cl6 C62 2.035(19) . ?
Cl7 C61 2.075(14) . ?
Cl8 C61 1.766(10) . ?
Cl9 C64 1.749(8) . ?
Cl10 C64 1.732(9) . ?
Cl11 C63 1.794(9) . ?
Cl12 C63 1.762(9) . ?
Cl13 C66 1.758(10) . ?
Cl14 C66 1.799(10) . ?
Cl15 C65 1.754(9) . ?
Cl16 C65 1.796(10) . ?
C1 C2 1.388(10) . ?
C2 C3 1.489(10) . ?
C3 C4 1.545(10) . ?
C4 C5 1.539(9) . ?
C4 C9 1.555(8) . ?
C5 C10 1.536(9) . ?
C5 C6 1.549(9) . ?
C6 C11 1.514(9) . ?
C6 C7 1.614(8) . ?
C7 C12 1.498(8) . ?
C7 C8 1.548(8) . ?
C8 C9 1.523(8) . ?
C8 C10 1.539(8) . ?
C15 C16 1.386(10) . ?
C16 C17 1.494(9) . ?
C17 C18 1.515(8) . ?
C18 C19 1.527(9) . ?
C18 C23 1.562(8) . ?
C19 C24 1.548(8) . ?
C19 C20 1.557(8) . ?
C20 C25 1.502(9) . ?
C20 C21 1.596(8) . ?
C21 C26 1.522(8) . ?
C21 C22 1.571(8) . ?
C22 C23 1.538(8) . ?
C22 C24 1.545(8) . ?
C29 C30 1.395(9) . ?
C30 C31 1.513(8) . ?
C31 C32 1.551(8) . ?
C32 C33 1.540(8) . ?
C32 C37 1.559(8) . ?
C33 C38 1.515(8) . ?
C33 C34 1.564(8) . ?
C34 C39 1.511(8) . ?
C34 C35 1.598(8) . ?
C35 C40 1.510(8) . ?
C35 C36 1.564(8) . ?
C36 C37 1.528(7) . ?
C36 C38 1.557(8) . ?
C43 C44 1.385(9) . ?
C44 C45 1.484(9) . ?
C45 C46 1.531(8) . ?
C46 C47 1.542(8) . ?
C46 C51 1.552(8) . ?
C47 C52 1.518(8) . ?
C47 C48 1.547(8) . ?
C48 C53 1.517(9) . ?
C48 C49 1.578(8) . ?
C49 C54 1.504(8) . ?
C49 C50 1.554(8) . ?
C50 C52 1.544(8) . ?
C50 C51 1.549(8) . ?
C59 C60 1.472(12) . ?
C61 C62 1.275(14) . ?
C63 C64 1.491(11) . ?
C65 C66 1.472(13) . ?

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
C9 Pd1 C1 84.16(17) . . ?
C9 Pd1 C2 83.6(3) . . ?
C1 Pd1 C2 38.0(3) . . ?
C9 Pd1 O14 95.93(17) . . ?
C1 Pd1 O14 157.2 . . ?
C2 Pd1 O14 164.8(3) . . ?
C9 Pd1 O13 177.97(17) . . ?
C1 Pd1 O13 97.8 . . ?
C2 Pd1 O13 97.7(2) . . ?
O14 Pd1 O13 82.4 . . ?
C23 Pd2 O2 96.04(17) . . ?
C23 Pd2 C15 85.6(3) . . ?
O2 Pd2 C15 155.6(2) . . ?
C23 Pd2 C16 83.3(2) . . ?
O2 Pd2 C16 166.6(2) . . ?
C15 Pd2 C16 37.8(3) . . ?
C23 Pd2 O1 176.03(17) . . ?
O2 Pd2 O1 80.0 . . ?
C15 Pd2 O1 98.1(2) . . ?
C16 Pd2 O1 100.54(18) . . ?
C37 Pd3 O6 97.84(16) . . ?
C37 Pd3 C30 84.1(2) . . ?
O6 Pd3 C30 157.95(18) . . ?
C37 Pd3 C29 85.9(2) . . ?
O6 Pd3 C29 163.68(19) . . ?
C30 Pd3 C29 38.0(2) . . ?
C37 Pd3 O5 178.94(17) . . ?
O6 Pd3 O5 81.8 . . ?
C30 Pd3 O5 96.56(17) . . ?
C29 Pd3 O5 94.17(18) . . ?
C51 Pd4 O10 93.49(17) . . ?
C51 Pd4 C43 87.1(3) . . ?
O10 Pd4 C43 161.6(2) . . ?
C51 Pd4 C44 83.6(2) . . ?
O10 Pd4 C44 160.97(19) . . ?
C43 Pd4 C44 37.4(2) . . ?
C51 Pd4 O9 174.20(17) . . ?
O10 Pd4 O9 80.9 . . ?
C43 Pd4 O9 97.8(2) . . ?
C44 Pd4 O9 102.20(18) . . ?
F2 Sb1 F1 177.8 . . ?
F2 Sb1 F6 90.8 . . ?
F1 Sb1 F6 91.4 . . ?
F2 Sb1 F5 89.4 . . ?
F1 Sb1 F5 88.3 . . ?
F6 Sb1 F5 177.3 . . ?
F2 Sb1 F3 91.4 . . ?
F1 Sb1 F3 88.5 . . ?
F6 Sb1 F3 92.4 . . ?
F5 Sb1 F3 90.3 . . ?
F2 Sb1 F4 90.7 . . ?
F1 Sb1 F4 89.4 . . ?
F6 Sb1 F4 88.9 . . ?
F5 Sb1 F4 88.4 . . ?
F3 Sb1 F4 177.5 . . ?
F8 Sb2 F7 177.8 . . ?
F8 Sb2 F12 90.9 . . ?
F7 Sb2 F12 91.4 . . ?
F8 Sb2 F11 89.4 . . ?
F7 Sb2 F11 88.3 . . ?
F12 Sb2 F11 177.3 . . ?
F8 Sb2 F9 91.4 . . ?
F7 Sb2 F9 88.5 . . ?
F12 Sb2 F9 92.4 . . ?
F11 Sb2 F9 90.3 . . ?
F8 Sb2 F10 90.7 . . ?
F7 Sb2 F10 89.4 . . ?
F12 Sb2 F10 88.9 . . ?
F11 Sb2 F10 88.4 . . ?
F9 Sb2 F10 177.5 . . ?
F14 Sb3 F13 177.8 . . ?
F14 Sb3 F18 90.8 . . ?
F13 Sb3 F18 91.4 . . ?
F14 Sb3 F17 89.4 . . ?
F13 Sb3 F17 88.3 . . ?
F18 Sb3 F17 177.3 . . ?
F14 Sb3 F15 91.4 . . ?
F13 Sb3 F15 88.5 . . ?
F18 Sb3 F15 92.4 . . ?
F17 Sb3 F15 90.3 . . ?
F14 Sb3 F16 90.6 . . ?
F13 Sb3 F16 89.4 . . ?
F18 Sb3 F16 88.9 . . ?
F17 Sb3 F16 88.4 . . ?
F15 Sb3 F16 177.5 . . ?
F20 Sb4 F19 177.7 . . ?
F20 Sb4 F24 90.9 . . ?
F19 Sb4 F24 91.4 . . ?
F20 Sb4 F23 89.4 . . ?
F19 Sb4 F23 88.3 . . ?
F24 Sb4 F23 177.3 . . ?
F20 Sb4 F21 91.4 . . ?
F19 Sb4 F21 88.5 . . ?
F24 Sb4 F21 92.4 . . ?
F23 Sb4 F21 90.3 . . ?
F20 Sb4 F22 90.7 . . ?
F19 Sb4 F22 89.4 . . ?
F24 Sb4 F22 88.9 . . ?
F23 Sb4 F22 88.4 . . ?
F21 Sb4 F22 177.5 . . ?
F20' Sb4' F19' 177.8 . . ?
F20' Sb4' F24' 90.8 . . ?
F19' Sb4' F24' 91.4 . . ?
F20' Sb4' F23' 89.4 . . ?
F19' Sb4' F23' 88.3 . . ?
F24' Sb4' F23' 177.3 . . ?
F20' Sb4' F21' 91.4 . . ?
F19' Sb4' F21' 88.5 . . ?
F24' Sb4' F21' 92.4 . . ?
F23' Sb4' F21' 90.3 . . ?
F20' Sb4' F22' 90.7 . . ?
F19' Sb4' F22' 89.4 . . ?
F24' Sb4' F22' 88.9 . . ?
F23' Sb4' F22' 88.4 . . ?
F21' Sb4' F22' 177.5 . . ?
C11 O1 Pd2 119.5(3) . . ?
C12 O2 Pd2 120.4(3) . . ?
C11 O3 C13 116.7(4) . . ?
C12 O4 C14 116.6(4) . . ?
C25 O5 Pd3 120.1(3) . . ?
C26 O6 Pd3 119.9(3) . . ?
C25 O7 C27 118.7(4) . . ?
C26 O8 C28 116.3(4) . . ?
C39 O9 Pd4 120.7(3) . . ?
C40 O10 Pd4 124.3(3) . . ?
C39 O11 C41 117.7(4) . . ?
C40 O12 C42 114.8(4) . . ?
C53 O13 Pd1 125.3(3) . . ?
C54 O14 Pd1 120.0(3) . . ?
C53 O15 C55 117.6(4) . . ?
C54 O16 C56 118.9(4) . . ?
C2 C1 Pd1 71.4(3) . . ?
C1 C2 C3 121.2(7) . . ?
C1 C2 Pd1 70.6(3) . . ?
C3 C2 Pd1 106.9(5) . . ?
C2 C3 C4 110.7(6) . . ?
C5 C4 C3 111.7(6) . . ?
C5 C4 C9 101.7(5) . . ?
C3 C4 C9 111.5(6) . . ?
C10 C5 C4 102.9(5) . . ?
C10 C5 C6 103.2(5) . . ?
C4 C5 C6 106.4(6) . . ?
C11 C6 C5 116.0(5) . . ?
C11 C6 C7 113.5(5) . . ?
C5 C6 C7 102.1(5) . . ?
C12 C7 C8 117.1(5) . . ?
C12 C7 C6 112.9(5) . . ?
C8 C7 C6 101.7(5) . . ?
C9 C8 C10 103.0(5) . . ?
C9 C8 C7 105.8(5) . . ?
C10 C8 C7 102.3(5) . . ?
C8 C9 C4 104.6(5) . . ?
C8 C9 Pd1 115.1(4) . . ?
C4 C9 Pd1 112.5(4) . . ?
C5 C10 C8 94.2(5) . . ?
O1 C11 O3 122.9(5) . . ?
O1 C11 C6 122.0(5) . . ?
O3 C11 C6 115.0(5) . . ?
O2 C12 O4 122.3(5) . . ?
O2 C12 C7 122.2(5) . . ?
O4 C12 C7 115.5(5) . . ?
C16 C15 Pd2 71.7(4) . . ?
C15 C16 C17 124.4(6) . . ?
C15 C16 Pd2 70.5(4) . . ?
C17 C16 Pd2 105.9(4) . . ?
C16 C17 C18 111.4(5) . . ?
C17 C18 C19 111.0(5) . . ?
C17 C18 C23 111.7(5) . . ?
C19 C18 C23 101.8(5) . . ?
C18 C19 C24 103.7(5) . . ?
C18 C19 C20 109.2(5) . . ?
C24 C19 C20 101.5(5) . . ?
C25 C20 C19 115.6(5) . . ?
C25 C20 C21 116.1(5) . . ?
C19 C20 C21 102.1(5) . . ?
C26 C21 C22 115.4(5) . . ?
C26 C21 C20 113.8(5) . . ?
C22 C21 C20 102.4(4) . . ?
C23 C22 C24 102.7(5) . . ?
C23 C22 C21 105.2(5) . . ?
C24 C22 C21 101.6(5) . . ?
C22 C23 C18 104.5(5) . . ?
C22 C23 Pd2 113.5(4) . . ?
C18 C23 Pd2 112.5(4) . . ?
C22 C24 C19 93.9(5) . . ?
O5 C25 O7 120.6(5) . . ?
O5 C25 C20 123.6(5) . . ?
O7 C25 C20 115.8(5) . . ?
O6 C26 O8 123.7(5) . . ?
O6 C26 C21 122.2(5) . . ?
O8 C26 C21 114.1(5) . . ?
C30 C29 Pd3 70.8(4) . . ?
C29 C30 C31 124.2(6) . . ?
C29 C30 Pd3 71.3(3) . . ?
C31 C30 Pd3 106.0(4) . . ?
C30 C31 C32 110.6(5) . . ?
C33 C32 C31 110.5(5) . . ?
C33 C32 C37 101.5(4) . . ?
C31 C32 C37 111.9(5) . . ?
C38 C33 C32 104.5(5) . . ?
C38 C33 C34 103.7(5) . . ?
C32 C33 C34 106.4(5) . . ?
C39 C34 C33 115.2(5) . . ?
C39 C34 C35 115.7(5) . . ?
C33 C34 C35 101.1(4) . . ?
C40 C35 C36 114.8(5) . . ?
C40 C35 C34 114.3(4) . . ?
C36 C35 C34 102.5(4) . . ?
C37 C36 C38 103.1(5) . . ?
C37 C36 C35 106.5(5) . . ?
C38 C36 C35 101.3(4) . . ?
C36 C37 C32 104.1(4) . . ?
C36 C37 Pd3 113.8(4) . . ?
C32 C37 Pd3 112.4(4) . . ?
C33 C38 C36 93.5(4) . . ?
O9 C39 O11 122.6(5) . . ?
O9 C39 C34 122.7(5) . . ?
O11 C39 C34 114.7(5) . . ?
O10 C40 O12 121.4(5) . . ?
O10 C40 C35 122.6(5) . . ?
O12 C40 C35 116.1(5) . . ?
C44 C43 Pd4 72.5(4) . . ?
C43 C44 C45 123.5(7) . . ?
C43 C44 Pd4 70.2(4) . . ?
C45 C44 Pd4 105.5(4) . . ?
C44 C45 C46 113.5(5) . . ?
C45 C46 C47 111.8(5) . . ?
C45 C46 C51 111.0(5) . . ?
C47 C46 C51 101.2(5) . . ?
C52 C47 C46 103.4(5) . . ?
C52 C47 C48 102.0(5) . . ?
C46 C47 C48 108.1(5) . . ?
C53 C48 C47 115.5(5) . . ?
C53 C48 C49 114.8(5) . . ?
C47 C48 C49 103.0(5) . . ?
C54 C49 C50 113.9(5) . . ?
C54 C49 C48 116.0(5) . . ?
C50 C49 C48 102.1(5) . . ?
C52 C50 C51 101.9(5) . . ?
C52 C50 C49 101.0(5) . . ?
C51 C50 C49 106.1(5) . . ?
C50 C51 C46 104.8(5) . . ?
C50 C51 Pd4 112.4(4) . . ?
C46 C51 Pd4 113.5(4) . . ?
C47 C52 C50 94.7(5) . . ?
O13 C53 O15 122.3(5) . . ?
O13 C53 C48 123.5(5) . . ?
O15 C53 C48 114.2(5) . . ?
O14 C54 O16 121.8(5) . . ?
O14 C54 C49 123.7(5) . . ?
O16 C54 C49 114.4(5) . . ?
C60 C59 Cl3 114.2(6) . . ?
C60 C59 Cl4 108.8(6) . . ?
Cl3 C59 Cl4 110.8(5) . . ?
C59 C60 Cl1 110.0(6) . . ?
C59 C60 Cl2 112.7(6) . . ?
Cl1 C60 Cl2 109.6(5) . . ?
C62 C61 Cl8 121.0(9) . . ?
C62 C61 Cl7 89.8(11) . . ?
Cl8 C61 Cl7 106.5(6) . . ?
C61 C62 Cl5 123.4(9) . . ?
C61 C62 Cl6 89.8(11) . . ?
Cl5 C62 Cl6 107.4(8) . . ?
C64 C63 Cl12 111.9(6) . . ?
C64 C63 Cl11 108.8(6) . . ?
Cl12 C63 Cl11 108.1(5) . . ?
C63 C64 Cl10 113.1(6) . . ?
C63 C64 Cl9 108.4(6) . . ?
Cl10 C64 Cl9 111.9(4) . . ?
C66 C65 Cl15 112.1(8) . . ?
C66 C65 Cl16 116.3(7) . . ?
Cl15 C65 Cl16 108.9(5) . . ?
C65 C66 Cl13 111.5(7) . . ?
C65 C66 Cl14 108.2(8) . . ?
Cl13 C66 Cl14 108.4(6) . . ?

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
Pd1 C1 C2 C3 98.5(6) . . . . ?
C1 C2 C3 C4 -35.6(9) . . . . ?
Pd1 C2 C3 C4 41.6(8) . . . . ?
C2 C3 C4 C5 -147.7(6) . . . . ?
C2 C3 C4 C9 -34.7(9) . . . . ?
C3 C4 C5 C10 81.9(6) . . . . ?
C9 C4 C5 C10 -37.1(7) . . . . ?
C3 C4 C5 C6 -170.0(5) . . . . ?
C9 C4 C5 C6 71.0(6) . . . . ?
C10 C5 C6 C11 -90.6(6) . . . . ?
C4 C5 C6 C11 161.5(5) . . . . ?
C10 C5 C6 C7 33.2(6) . . . . ?
C4 C5 C6 C7 -74.7(6) . . . . ?
C11 C6 C7 C12 1.9(7) . . . . ?
C5 C6 C7 C12 -123.6(5) . . . . ?
C11 C6 C7 C8 128.2(5) . . . . ?
C5 C6 C7 C8 2.7(6) . . . . ?
C12 C7 C8 C9 -166.5(5) . . . . ?
C6 C7 C8 C9 70.0(5) . . . . ?
C12 C7 C8 C10 85.9(6) . . . . ?
C6 C7 C8 C10 -37.6(5) . . . . ?
C10 C8 C9 C4 31.5(6) . . . . ?
C7 C8 C9 C4 -75.5(6) . . . . ?
C10 C8 C9 Pd1 -92.4(5) . . . . ?
C7 C8 C9 Pd1 160.6(4) . . . . ?
C5 C4 C9 C8 3.2(7) . . . . ?
C3 C4 C9 C8 -115.9(6) . . . . ?
C5 C4 C9 Pd1 128.8(5) . . . . ?
C3 C4 C9 Pd1 9.7(7) . . . . ?
C4 C5 C10 C8 55.0(6) . . . . ?
C6 C5 C10 C8 -55.5(5) . . . . ?
C9 C8 C10 C5 -52.5(5) . . . . ?
C7 C8 C10 C5 57.2(5) . . . . ?
Pd2 O1 C11 O3 156.9(4) . . . . ?
Pd2 O1 C11 C6 -21.7(7) . . . . ?
C13 O3 C11 O1 3.6(7) . . . . ?
C13 O3 C11 C6 -177.6(5) . . . . ?
C5 C6 C11 O1 -169.7(5) . . . . ?
C7 C6 C11 O1 72.6(7) . . . . ?
C5 C6 C11 O3 11.5(8) . . . . ?
C7 C6 C11 O3 -106.2(6) . . . . ?
Pd2 O2 C12 O4 -159.1(3) . . . . ?
Pd2 O2 C12 C7 19.9(7) . . . . ?
C14 O4 C12 O2 1.8(7) . . . . ?
C14 O4 C12 C7 -177.3(5) . . . . ?
C8 C7 C12 O2 165.1(5) . . . . ?
C6 C7 C12 O2 -77.3(7) . . . . ?
C8 C7 C12 O4 -15.8(7) . . . . ?
C6 C7 C12 O4 101.8(6) . . . . ?
Pd2 C15 C16 C17 96.4(6) . . . . ?
C15 C16 C17 C18 -34.9(9) . . . . ?
Pd2 C16 C17 C18 42.1(7) . . . . ?
C16 C17 C18 C19 -146.7(6) . . . . ?
C16 C17 C18 C23 -33.9(8) . . . . ?
C17 C18 C19 C24 82.5(6) . . . . ?
C23 C18 C19 C24 -36.4(6) . . . . ?
C17 C18 C19 C20 -169.9(5) . . . . ?
C23 C18 C19 C20 71.2(6) . . . . ?
C18 C19 C20 C25 161.9(5) . . . . ?
C24 C19 C20 C25 -89.0(6) . . . . ?
C18 C19 C20 C21 -71.2(6) . . . . ?
C24 C19 C20 C21 37.9(6) . . . . ?
C25 C20 C21 C26 -0.8(7) . . . . ?
C19 C20 C21 C26 -127.5(5) . . . . ?
C25 C20 C21 C22 124.5(5) . . . . ?
C19 C20 C21 C22 -2.2(6) . . . . ?
C26 C21 C22 C23 -163.3(5) . . . . ?
C20 C21 C22 C23 72.5(5) . . . . ?
C26 C21 C22 C24 90.0(6) . . . . ?
C20 C21 C22 C24 -34.3(6) . . . . ?
C24 C22 C23 C18 32.1(6) . . . . ?
C21 C22 C23 C18 -73.8(5) . . . . ?
C24 C22 C23 Pd2 -90.9(5) . . . . ?
C21 C22 C23 Pd2 163.2(4) . . . . ?
C17 C18 C23 C22 -116.0(6) . . . . ?
C19 C18 C23 C22 2.4(6) . . . . ?
C17 C18 C23 Pd2 7.6(7) . . . . ?
C19 C18 C23 Pd2 126.1(4) . . . . ?
C23 C22 C24 C19 -52.1(5) . . . . ?
C21 C22 C24 C19 56.6(5) . . . . ?
C18 C19 C24 C22 54.9(5) . . . . ?
C20 C19 C24 C22 -58.4(5) . . . . ?
Pd3 O5 C25 O7 170.0(3) . . . . ?
Pd3 O5 C25 C20 -11.0(7) . . . . ?
C27 O7 C25 O5 6.5(7) . . . . ?
C27 O7 C25 C20 -172.6(5) . . . . ?
C19 C20 C25 O5 -173.8(5) . . . . ?
C21 C20 C25 O5 66.7(7) . . . . ?
C19 C20 C25 O7 5.2(7) . . . . ?
C21 C20 C25 O7 -114.3(5) . . . . ?
Pd3 O6 C26 O8 -155.2(3) . . . . ?
Pd3 O6 C26 C21 25.9(6) . . . . ?
C28 O8 C26 O6 -0.5(7) . . . . ?
C28 O8 C26 C21 178.5(5) . . . . ?
C22 C21 C26 O6 164.9(5) . . . . ?
C20 C21 C26 O6 -77.0(7) . . . . ?
C22 C21 C26 O8 -14.2(7) . . . . ?
C20 C21 C26 O8 103.9(5) . . . . ?
Pd3 C29 C30 C31 97.0(6) . . . . ?
C29 C30 C31 C32 -36.4(8) . . . . ?
Pd3 C30 C31 C32 41.5(6) . . . . ?
C30 C31 C32 C33 -145.4(5) . . . . ?
C30 C31 C32 C37 -33.0(7) . . . . ?
C31 C32 C33 C38 82.9(6) . . . . ?
C37 C32 C33 C38 -36.0(6) . . . . ?
C31 C32 C33 C34 -167.8(5) . . . . ?
C37 C32 C33 C34 73.4(5) . . . . ?
C38 C33 C34 C39 -90.7(6) . . . . ?
C32 C33 C34 C39 159.4(5) . . . . ?
C38 C33 C34 C35 34.9(5) . . . . ?
C32 C33 C34 C35 -75.0(5) . . . . ?
C39 C34 C35 C40 2.5(7) . . . . ?
C33 C34 C35 C40 -122.7(5) . . . . ?
C39 C34 C35 C36 127.4(5) . . . . ?
C33 C34 C35 C36 2.2(5) . . . . ?
C40 C35 C36 C37 -165.2(5) . . . . ?
C34 C35 C36 C37 70.3(5) . . . . ?
C40 C35 C36 C38 87.4(5) . . . . ?
C34 C35 C36 C38 -37.2(5) . . . . ?
C38 C36 C37 C32 32.8(6) . . . . ?
C35 C36 C37 C32 -73.4(5) . . . . ?
C38 C36 C37 Pd3 -89.9(5) . . . . ?
C35 C36 C37 Pd3 164.0(4) . . . . ?
C33 C32 C37 C36 1.1(6) . . . . ?
C31 C32 C37 C36 -116.8(5) . . . . ?
C33 C32 C37 Pd3 124.7(4) . . . . ?
C31 C32 C37 Pd3 6.8(6) . . . . ?
C32 C33 C38 C36 54.3(5) . . . . ?
C34 C33 C38 C36 -57.0(5) . . . . ?
C37 C36 C38 C33 -52.7(5) . . . . ?
C35 C36 C38 C33 57.4(5) . . . . ?
Pd4 O9 C39 O11 152.7(3) . . . . ?
Pd4 O9 C39 C34 -26.1(7) . . . . ?
C41 O11 C39 O9 6.3(7) . . . . ?
C41 O11 C39 C34 -174.8(5) . . . . ?
C33 C34 C39 O9 -168.8(5) . . . . ?
C35 C34 C39 O9 73.6(7) . . . . ?
C33 C34 C39 O11 12.3(7) . . . . ?
C35 C34 C39 O11 -105.3(5) . . . . ?
Pd4 O10 C40 O12 -170.4(3) . . . . ?
Pd4 O10 C40 C35 10.3(6) . . . . ?
C42 O12 C40 O10 -2.5(6) . . . . ?
C42 O12 C40 C35 176.8(4) . . . . ?
C36 C35 C40 O10 173.5(5) . . . . ?
C34 C35 C40 O10 -68.4(7) . . . . ?
C36 C35 C40 O12 -5.8(7) . . . . ?
C34 C35 C40 O12 112.3(5) . . . . ?
Pd4 C43 C44 C45 95.9(6) . . . . ?
C43 C44 C45 C46 -37.1(9) . . . . ?
Pd4 C44 C45 C46 39.1(7) . . . . ?
C44 C45 C46 C47 -144.9(6) . . . . ?
C44 C45 C46 C51 -32.7(8) . . . . ?
C45 C46 C47 C52 80.2(6) . . . . ?
C51 C46 C47 C52 -38.0(6) . . . . ?
C45 C46 C47 C48 -172.1(5) . . . . ?
C51 C46 C47 C48 69.7(6) . . . . ?
C52 C47 C48 C53 -91.7(6) . . . . ?
C46 C47 C48 C53 159.8(5) . . . . ?
C52 C47 C48 C49 34.3(6) . . . . ?
C46 C47 C48 C49 -74.3(6) . . . . ?
C53 C48 C49 C54 3.9(7) . . . . ?
C47 C48 C49 C54 -122.6(5) . . . . ?
C53 C48 C49 C50 128.3(5) . . . . ?
C47 C48 C49 C50 1.9(6) . . . . ?
C54 C49 C50 C52 89.2(6) . . . . ?
C48 C49 C50 C52 -36.6(5) . . . . ?
C54 C49 C50 C51 -164.8(5) . . . . ?
C48 C49 C50 C51 69.4(5) . . . . ?
C52 C50 C51 C46 30.5(6) . . . . ?
C49 C50 C51 C46 -74.9(5) . . . . ?
C52 C50 C51 Pd4 -93.3(5) . . . . ?
C49 C50 C51 Pd4 161.4(4) . . . . ?
C45 C46 C51 C50 -115.0(6) . . . . ?
C47 C46 C51 C50 3.9(6) . . . . ?
C45 C46 C51 Pd4 8.1(6) . . . . ?
C47 C46 C51 Pd4 126.9(4) . . . . ?
C46 C47 C52 C50 56.0(5) . . . . ?
C48 C47 C52 C50 -56.1(5) . . . . ?
C51 C50 C52 C47 -52.0(5) . . . . ?
C49 C50 C52 C47 57.3(5) . . . . ?
Pd1 O13 C53 O15 169.4(3) . . . . ?
Pd1 O13 C53 C48 -11.6(7) . . . . ?
C55 O15 C53 O13 2.1(8) . . . . ?
C55 O15 C53 C48 -176.9(5) . . . . ?
C47 C48 C53 O13 -178.6(5) . . . . ?
C49 C48 C53 O13 61.7(8) . . . . ?
C47 C48 C53 O15 0.5(7) . . . . ?
C49 C48 C53 O15 -119.2(5) . . . . ?
Pd1 O14 C54 O16 -156.8(3) . . . . ?
Pd1 O14 C54 C49 27.7(6) . . . . ?
C56 O16 C54 O14 1.9(7) . . . . ?
C56 O16 C54 C49 177.8(5) . . . . ?
C50 C49 C54 O14 161.6(5) . . . . ?
C48 C49 C54 O14 -80.2(7) . . . . ?
C50 C49 C54 O16 -14.1(7) . . . . ?
C48 C49 C54 O16 104.0(6) . . . . ?
Cl3 C59 C60 Cl1 64.7(7) . . . . ?
Cl4 C59 C60 Cl1 -170.9(4) . . . . ?
Cl3 C59 C60 Cl2 -58.0(7) . . . . ?
Cl4 C59 C60 Cl2 66.4(7) . . . . ?
Cl8 C61 C62 Cl5 -31(2) . . . . ?
Cl7 C61 C62 Cl5 78.4(14) . . . . ?
Cl8 C61 C62 Cl6 80.1(11) . . . . ?
Cl7 C61 C62 Cl6 -170.7(4) . . . . ?
Cl12 C63 C64 Cl10 -56.4(7) . . . . ?
Cl11 C63 C64 Cl10 63.0(7) . . . . ?
Cl12 C63 C64 Cl9 68.3(7) . . . . ?
Cl11 C63 C64 Cl9 -172.3(4) . . . . ?
Cl15 C65 C66 Cl13 69.0(9) . . . . ?
Cl16 C65 C66 Cl13 -57.3(10) . . . . ?
Cl15 C65 C66 Cl14 -171.9(5) . . . . ?
Cl16 C65 C66 Cl14 61.8(8) . . . . ?

_refine_diff_density_max         1.980
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.141

_shelxl_version_number           2013-2



