# Electronic Supplementary Material (ESI) for Green Chemistry.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_3-A
_database_code_depnum_ccdc_archive 'CCDC 1565396'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H68 N2 P4 Pd2 S4, 2(F6 P), C4 H10 O'
_chemical_formula_sum            'C82 H78 F12 N2 O P6 Pd2 S4'
_chemical_formula_weight         1862.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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                   9.3104(5)
_cell_length_b                   10.7032(4)
_cell_length_c                   21.2565(12)
_cell_angle_alpha                86.197(4)
_cell_angle_beta                 78.500(4)
_cell_angle_gamma                88.333(3)
_cell_volume                     2070.87(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4866
_cell_measurement_theta_min      4.1120
_cell_measurement_theta_max      73.4130

_exptl_crystal_description       'platy needles'
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_F_000             946
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    6.162
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            11827
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.140
_diffrn_reflns_theta_max         73.672
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             7903
_reflns_number_gt                6434
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0518P)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         7903
_refine_ls_number_parameters     591
_refine_ls_number_restraints     1099
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1041
_refine_ls_wR_factor_gt          0.0964
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.071
_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 0.83076(3) 0.40577(2) 0.28154(2) 0.03381(8) Uani 1 1 d . . . . .
P1 P 0.77212(10) 0.54792(8) 0.20329(4) 0.03598(19) Uani 1 1 d D . . . .
P2 P 0.74711(9) 0.23089(8) 0.24486(4) 0.03462(18) Uani 1 1 d . . . . .
S1 S 0.89084(10) 0.30246(8) 0.37350(4) 0.03936(19) Uani 1 1 d . . . . .
C2 C 0.9614(4) 0.4436(4) 0.38671(16) 0.0383(7) Uani 1 1 d . . . . .
S3 S 0.95040(10) 0.55668(9) 0.32679(4) 0.0412(2) Uani 1 1 d . . . . .
N4 N 1.0204(4) 0.4626(3) 0.43703(15) 0.0449(7) Uani 1 1 d . . . . .
C5 C 1.0234(5) 0.3683(4) 0.48983(19) 0.0498(10) Uani 1 1 d . . . . .
H5A H 1.1252 0.3544 0.4962 0.060 Uiso 1 1 calc R U . . .
H5B H 0.9865 0.2879 0.4794 0.060 Uiso 1 1 calc R U . . .
C6 C 1.0723(5) 0.5864(4) 0.44918(19) 0.0486(9) Uani 1 1 d . . . . .
H6A H 1.0664 0.6468 0.4124 0.058 Uiso 1 1 calc R U . . .
H6B H 1.1757 0.5796 0.4542 0.058 Uiso 1 1 calc R U . . .
C7 C 0.6219(4) 0.6505(3) 0.23741(18) 0.0421(8) Uani 1 1 d . . . . .
C8 C 0.5770(4) 0.6534(4) 0.3041(2) 0.0471(9) Uani 1 1 d . . . . .
H8A H 0.6253 0.6016 0.3317 0.057 Uiso 1 1 calc R U . . .
C9 C 0.4628(5) 0.7311(5) 0.3299(2) 0.0613(11) Uani 1 1 d . . . . .
H9A H 0.4319 0.7319 0.3753 0.074 Uiso 1 1 calc R U . . .
C10 C 0.3932(6) 0.8078(5) 0.2901(3) 0.0690(14) Uani 1 1 d . . . . .
H10A H 0.3140 0.8608 0.3081 0.083 Uiso 1 1 calc R U . . .
C11 C 0.4391(6) 0.8075(4) 0.2238(3) 0.0659(13) Uani 1 1 d . . . . .
H11A H 0.3930 0.8621 0.1965 0.079 Uiso 1 1 calc R U . . .
C12 C 0.5503(5) 0.7288(4) 0.1977(2) 0.0538(10) Uani 1 1 d . . . . .
H12A H 0.5791 0.7273 0.1523 0.065 Uiso 1 1 calc R U . . .
C13 C 0.7164(4) 0.4969(3) 0.13201(17) 0.0390(7) Uani 1 1 d . . . . .
C14 C 0.8141(5) 0.4936(5) 0.07363(19) 0.0524(10) Uani 1 1 d . . . . .
H14A H 0.9113 0.5222 0.0699 0.063 Uiso 1 1 calc R U . . .
C15 C 0.7707(5) 0.4488(5) 0.0206(2) 0.0605(12) Uani 1 1 d . . . . .
H15A H 0.8376 0.4486 -0.0195 0.073 Uiso 1 1 calc R U . . .
C16 C 0.6310(5) 0.4044(4) 0.0258(2) 0.0536(10) Uani 1 1 d . . . . .
H16A H 0.6027 0.3719 -0.0103 0.064 Uiso 1 1 calc R U . . .
C17 C 0.5320(5) 0.4071(4) 0.0836(2) 0.0484(9) Uani 1 1 d . . . . .
H17A H 0.4355 0.3770 0.0872 0.058 Uiso 1 1 calc R U . . .
C18 C 0.5746(4) 0.4543(3) 0.13669(18) 0.0411(8) Uani 1 1 d . . . . .
H18A H 0.5063 0.4573 0.1763 0.049 Uiso 1 1 calc R U . . .
C19 C 0.9360(7) 0.6411(7) 0.1708(3) 0.0369(15) Uani 0.74(3) 1 d DG U P A 1
C20 C 1.0730(7) 0.5838(10) 0.1672(3) 0.0447(14) Uani 0.74(3) 1 d G U P A 1
H20A H 1.0805 0.4985 0.1819 0.054 Uiso 0.74(3) 1 calc R U P A 1
C21 C 1.1991(8) 0.6511(13) 0.1420(2) 0.0489(18) Uani 0.74(3) 1 d G U P A 1
H21A H 1.2928 0.6119 0.1395 0.059 Uiso 0.74(3) 1 calc R U P A 1
C22 C 1.1882(12) 0.7759(12) 0.1205(2) 0.050(2) Uani 0.74(3) 1 d G U P A 1
H22A H 1.2743 0.8219 0.1033 0.060 Uiso 0.74(3) 1 calc R U P A 1
C23 C 1.0511(14) 0.8333(9) 0.1241(2) 0.052(2) Uani 0.74(3) 1 d G U P A 1
H23A H 1.0437 0.9185 0.1094 0.063 Uiso 0.74(3) 1 calc R U P A 1
C24 C 0.9250(11) 0.7659(7) 0.1493(3) 0.0473(15) Uani 0.74(3) 1 d G U P A 1
H24A H 0.8314 0.8051 0.1518 0.057 Uiso 0.74(3) 1 calc R U P A 1
C19' C 0.9149(18) 0.6614(17) 0.1756(11) 0.038(5) Uiso 0.26(3) 1 d DG U P A 2
C20' C 1.0577(19) 0.6147(18) 0.1681(9) 0.035(4) Uiso 0.26(3) 1 d G U P A 2
H20B H 1.0756 0.5303 0.1817 0.042 Uiso 0.26(3) 1 calc R U P A 2
C21' C 1.1745(19) 0.691(2) 0.1406(8) 0.043(4) Uiso 0.26(3) 1 d G U P A 2
H21B H 1.2721 0.6595 0.1354 0.051 Uiso 0.26(3) 1 calc R U P A 2
C22' C 1.148(3) 0.815(2) 0.1206(7) 0.044(4) Uiso 0.26(3) 1 d G U P A 2
H22B H 1.2282 0.8672 0.1018 0.053 Uiso 0.26(3) 1 calc R U P A 2
C23' C 1.006(3) 0.8615(18) 0.1281(9) 0.061(6) Uiso 0.26(3) 1 d G U P A 2
H23B H 0.9877 0.9458 0.1144 0.073 Uiso 0.26(3) 1 calc R U P A 2
C24' C 0.889(2) 0.7848(18) 0.1556(11) 0.043(4) Uiso 0.26(3) 1 d G U P A 2
H24B H 0.7911 0.8167 0.1607 0.052 Uiso 0.26(3) 1 calc R U P A 2
C25 C 0.5504(4) 0.2309(4) 0.25116(17) 0.0406(8) Uani 1 1 d . . . . .
C26 C 0.4672(5) 0.3190(4) 0.2890(2) 0.0511(9) Uani 1 1 d . . . . .
H26A H 0.5150 0.3793 0.3081 0.061 Uiso 1 1 calc R U . . .
C27 C 0.3163(5) 0.3193(6) 0.2990(2) 0.0682(13) Uani 1 1 d . . . . .
H27A H 0.2603 0.3799 0.3246 0.082 Uiso 1 1 calc R U . . .
C28 C 0.2466(5) 0.2310(6) 0.2714(2) 0.0735(16) Uani 1 1 d . . . . .
H28A H 0.1426 0.2312 0.2783 0.088 Uiso 1 1 calc R U . . .
C29 C 0.3261(5) 0.1436(6) 0.2346(3) 0.0680(13) Uani 1 1 d . . . . .
H29A H 0.2772 0.0845 0.2153 0.082 Uiso 1 1 calc R U . . .
C30 C 0.4788(4) 0.1404(4) 0.2251(2) 0.0510(9) Uani 1 1 d . . . . .
H30A H 0.5336 0.0771 0.2011 0.061 Uiso 1 1 calc R U . . .
C31 C 0.8489(4) 0.2073(3) 0.16387(17) 0.0384(7) Uani 1 1 d . . . . .
C32 C 0.7910(5) 0.1657(4) 0.11378(19) 0.0490(9) Uani 1 1 d . . . . .
H32A H 0.6894 0.1483 0.1201 0.059 Uiso 1 1 calc R U . . .
C33 C 0.8819(5) 0.1497(5) 0.0543(2) 0.0577(11) Uani 1 1 d . . . . .
H33A H 0.8419 0.1213 0.0202 0.069 Uiso 1 1 calc R U . . .
C34 C 1.0293(5) 0.1745(5) 0.0445(2) 0.0576(11) Uani 1 1 d . . . . .
H34A H 1.0906 0.1631 0.0038 0.069 Uiso 1 1 calc R U . . .
C35 C 1.0875(5) 0.2157(4) 0.0940(2) 0.0547(10) Uani 1 1 d . . . . .
H35A H 1.1895 0.2314 0.0877 0.066 Uiso 1 1 calc R U . . .
C36 C 0.9973(4) 0.2344(4) 0.15303(19) 0.0471(9) Uani 1 1 d . . . . .
H36A H 1.0374 0.2661 0.1864 0.057 Uiso 1 1 calc R U . . .
C37 C 0.7770(4) 0.0879(3) 0.29224(18) 0.0411(8) Uani 1 1 d . . . . .
C38 C 0.8895(5) 0.0017(4) 0.2715(2) 0.0539(10) Uani 1 1 d . . . . .
H38A H 0.9546 0.0168 0.2314 0.065 Uiso 1 1 calc R U . . .
C39 C 0.9058(6) -0.1061(5) 0.3099(3) 0.0695(14) Uani 1 1 d . . . . .
H39A H 0.9827 -0.1643 0.2960 0.083 Uiso 1 1 calc R U . . .
C40 C 0.8124(7) -0.1288(5) 0.3673(3) 0.0686(13) Uani 1 1 d . . . . .
H40A H 0.8232 -0.2039 0.3924 0.082 Uiso 1 1 calc R U . . .
C41 C 0.7038(6) -0.0452(5) 0.3890(2) 0.0682(13) Uani 1 1 d . . . . .
H41A H 0.6398 -0.0615 0.4293 0.082 Uiso 1 1 calc R U . . .
C42 C 0.6869(5) 0.0644(4) 0.3518(2) 0.0575(11) Uani 1 1 d . . . . .
H42A H 0.6126 0.1237 0.3675 0.069 Uiso 1 1 calc R U . . .
P10 P 0.5031(16) 0.5195(8) 0.4994(7) 0.0585(18) Uani 0.457(2) 1 d D U P B -1
F11 F 0.4195(17) 0.6521(10) 0.4915(8) 0.090(3) Uani 0.457(2) 1 d D U P B -1
F12 F 0.6490(16) 0.5820(11) 0.4583(7) 0.083(3) Uani 0.457(2) 1 d D U P B -1
F13 F 0.4598(16) 0.4796(10) 0.4356(7) 0.080(3) Uani 0.457(2) 1 d D U P B -1
F14 F 0.3578(15) 0.4623(10) 0.5411(7) 0.080(3) Uani 0.457(2) 1 d D U P B -1
F15 F 0.5482(18) 0.5641(11) 0.5630(7) 0.089(3) Uani 0.457(2) 1 d D U P B -1
F16 F 0.5898(15) 0.3901(10) 0.5068(7) 0.082(3) Uani 0.457(2) 1 d D U P B -1
P10' P 0.548(3) 0.614(3) 0.5097(15) 0.087(5) Uiso 0.043(2) 1 d D U P B -2
F11' F 0.489(6) 0.754(3) 0.519(3) 0.100(10) Uiso 0.043(2) 1 d D U P B -2
F12' F 0.653(6) 0.658(5) 0.444(2) 0.091(10) Uiso 0.043(2) 1 d D U P B -2
F13' F 0.421(5) 0.588(6) 0.472(3) 0.080(6) Uiso 0.043(2) 1 d D U P B -2
F14' F 0.443(6) 0.570(5) 0.5758(19) 0.082(6) Uiso 0.043(2) 1 d D U P B -2
F15' F 0.675(5) 0.639(6) 0.548(3) 0.103(10) Uiso 0.043(2) 1 d D U P B -2
F16' F 0.607(6) 0.474(4) 0.501(3) 0.082(6) Uiso 0.043(2) 1 d D U P B -2
P20 P 0.5050(14) 0.0007(13) 0.0102(5) 0.064(3) Uani 0.261(4) 1 d D U P C -1
F21 F 0.3421(15) 0.0258(15) 0.0454(7) 0.098(5) Uani 0.261(4) 1 d D U P C -1
F22 F 0.5393(19) -0.0435(17) 0.0775(6) 0.102(4) Uani 0.261(4) 1 d D U P C -1
F23 F 0.5434(17) 0.1383(13) 0.0240(7) 0.078(4) Uani 0.261(4) 1 d D U P C -1
F24 F 0.4672(17) 0.0521(17) -0.0549(6) 0.109(4) Uani 0.261(4) 1 d D U P C -1
F25 F 0.4640(16) -0.1339(12) -0.0018(7) 0.069(3) Uani 0.261(4) 1 d D U P C -1
F26 F 0.6689(12) -0.0200(13) -0.0226(6) 0.060(3) Uani 0.261(4) 1 d D U P C -1
P20' P 0.5021(12) -0.0106(9) 0.0067(4) 0.041(2) Uiso 0.239(4) 1 d D U P C -2
F21' F 0.3348(13) -0.0192(15) 0.0110(8) 0.084(4) Uiso 0.239(4) 1 d D U P C -2
F22' F 0.4708(17) 0.0159(15) 0.0807(6) 0.090(4) Uiso 0.239(4) 1 d D U P C -2
F23' F 0.507(2) 0.1280(12) -0.0147(9) 0.102(5) Uiso 0.239(4) 1 d D U P C -2
F24' F 0.5316(18) -0.0541(16) -0.0635(6) 0.109(4) Uiso 0.239(4) 1 d D U P C -2
F25' F 0.5010(15) -0.1575(11) 0.0322(7) 0.088(4) Uiso 0.239(4) 1 d D U P C -2
F26' F 0.6689(14) -0.0187(15) 0.0079(8) 0.100(5) Uiso 0.239(4) 1 d D U P C -2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 P2 2.2888(9) . ?
Pd1 P1 2.3146(9) . ?
Pd1 S1 2.3388(8) . ?
Pd1 S3 2.3479(9) . ?
P1 C19' 1.810(10) . ?
P1 C7 1.816(4) . ?
P1 C13 1.817(3) . ?
P1 C19 1.838(4) . ?
P2 C25 1.810(4) . ?
P2 C37 1.821(4) . ?
P2 C31 1.822(4) . ?
S1 C2 1.727(4) . ?
C2 N4 1.325(4) . ?
C2 S3 1.714(4) . ?
N4 C5 1.463(5) . ?
N4 C6 1.479(5) . ?
C5 C6 1.519(6) 2_766 ?
C6 C5 1.519(6) 2_766 ?
C7 C8 1.398(6) . ?
C7 C12 1.399(5) . ?
C8 C9 1.378(6) . ?
C9 C10 1.380(7) . ?
C10 C11 1.390(8) . ?
C11 C12 1.368(7) . ?
C13 C14 1.387(6) . ?
C13 C18 1.392(5) . ?
C14 C15 1.390(5) . ?
C15 C16 1.379(6) . ?
C16 C17 1.381(6) . ?
C17 C18 1.397(5) . ?
C19 C20 1.3900 . ?
C19 C24 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C19' C20' 1.3900 . ?
C19' C24' 1.3900 . ?
C20' C21' 1.3900 . ?
C21' C22' 1.3900 . ?
C22' C23' 1.3900 . ?
C23' C24' 1.3900 . ?
C25 C30 1.395(6) . ?
C25 C26 1.395(6) . ?
C26 C27 1.378(6) . ?
C27 C28 1.385(8) . ?
C28 C29 1.365(8) . ?
C29 C30 1.395(6) . ?
C31 C32 1.389(5) . ?
C31 C36 1.391(5) . ?
C32 C33 1.392(6) . ?
C33 C34 1.377(7) . ?
C34 C35 1.377(6) . ?
C35 C36 1.387(6) . ?
C37 C42 1.385(6) . ?
C37 C38 1.399(6) . ?
C38 C39 1.391(6) . ?
C39 C40 1.360(8) . ?
C40 C41 1.361(8) . ?
C41 C42 1.394(6) . ?
P10 F14 1.578(10) . ?
P10 F13 1.578(10) . ?
P10 F16 1.597(10) . ?
P10 F12 1.599(10) . ?
P10 F15 1.599(10) . ?
P10 F11 1.614(10) . ?
P10' F11' 1.588(13) . ?
P10' F13' 1.592(13) . ?
P10' F14' 1.592(13) . ?
P10' F12' 1.593(13) . ?
P10' F16' 1.595(13) . ?
P10' F15' 1.599(13) . ?
P20 F25 1.551(11) . ?
P20 F24 1.557(12) . ?
P20 F26 1.562(11) . ?
P20 F22 1.567(11) . ?
P20 F21 1.575(11) . ?
P20 F23 1.586(11) . ?
P20' F23' 1.521(11) . ?
P20' F21' 1.547(11) . ?
P20' F26' 1.558(11) . ?
P20' F24' 1.560(11) . ?
P20' F22' 1.585(11) . ?
P20' F25' 1.629(11) . ?

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
P2 Pd1 P1 97.15(3) . . ?
P2 Pd1 S1 95.05(3) . . ?
P1 Pd1 S1 167.05(3) . . ?
P2 Pd1 S3 168.36(3) . . ?
P1 Pd1 S3 92.97(3) . . ?
S1 Pd1 S3 75.36(3) . . ?
C19' P1 C7 100.3(7) . . ?
C19' P1 C13 106.6(8) . . ?
C7 P1 C13 103.25(17) . . ?
C7 P1 C19 109.6(3) . . ?
C13 P1 C19 103.7(2) . . ?
C19' P1 Pd1 112.0(7) . . ?
C7 P1 Pd1 110.69(13) . . ?
C13 P1 Pd1 121.58(12) . . ?
C19 P1 Pd1 107.4(2) . . ?
C25 P2 C37 101.70(18) . . ?
C25 P2 C31 113.26(16) . . ?
C37 P2 C31 105.29(17) . . ?
C25 P2 Pd1 113.75(13) . . ?
C37 P2 Pd1 113.11(12) . . ?
C31 P2 Pd1 109.29(12) . . ?
C2 S1 Pd1 85.90(12) . . ?
N4 C2 S3 123.3(3) . . ?
N4 C2 S1 123.9(3) . . ?
S3 C2 S1 112.75(19) . . ?
C2 S3 Pd1 85.90(12) . . ?
C2 N4 C5 123.4(3) . . ?
C2 N4 C6 122.8(3) . . ?
C5 N4 C6 113.3(3) . . ?
N4 C5 C6 109.0(3) . 2_766 ?
N4 C6 C5 108.7(3) . 2_766 ?
C8 C7 C12 118.8(4) . . ?
C8 C7 P1 120.3(3) . . ?
C12 C7 P1 120.9(3) . . ?
C9 C8 C7 120.3(4) . . ?
C8 C9 C10 120.2(5) . . ?
C9 C10 C11 119.9(5) . . ?
C12 C11 C10 120.2(4) . . ?
C11 C12 C7 120.6(4) . . ?
C14 C13 C18 119.0(3) . . ?
C14 C13 P1 121.5(3) . . ?
C18 C13 P1 119.4(3) . . ?
C13 C14 C15 120.4(4) . . ?
C16 C15 C14 120.3(4) . . ?
C15 C16 C17 120.1(4) . . ?
C16 C17 C18 119.7(4) . . ?
C13 C18 C17 120.5(4) . . ?
C20 C19 C24 120.0 . . ?
C20 C19 P1 118.6(3) . . ?
C24 C19 P1 121.4(3) . . ?
C21 C20 C19 120.0 . . ?
C20 C21 C22 120.0 . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C24 120.0 . . ?
C23 C24 C19 120.0 . . ?
C20' C19' C24' 120.0 . . ?
C20' C19' P1 115.7(9) . . ?
C24' C19' P1 123.9(9) . . ?
C19' C20' C21' 120.0 . . ?
C22' C21' C20' 120.0 . . ?
C21' C22' C23' 120.0 . . ?
C24' C23' C22' 120.0 . . ?
C23' C24' C19' 120.0 . . ?
C30 C25 C26 119.1(4) . . ?
C30 C25 P2 123.0(3) . . ?
C26 C25 P2 117.6(3) . . ?
C27 C26 C25 120.6(4) . . ?
C26 C27 C28 119.7(5) . . ?
C29 C28 C27 120.6(4) . . ?
C28 C29 C30 120.4(5) . . ?
C25 C30 C29 119.5(4) . . ?
C32 C31 C36 118.9(4) . . ?
C32 C31 P2 125.7(3) . . ?
C36 C31 P2 115.3(3) . . ?
C31 C32 C33 119.8(4) . . ?
C34 C33 C32 120.7(4) . . ?
C35 C34 C33 119.7(4) . . ?
C34 C35 C36 120.0(4) . . ?
C35 C36 C31 120.7(4) . . ?
C42 C37 C38 118.4(4) . . ?
C42 C37 P2 118.9(3) . . ?
C38 C37 P2 122.7(3) . . ?
C39 C38 C37 119.8(5) . . ?
C40 C39 C38 120.5(5) . . ?
C39 C40 C41 120.8(5) . . ?
C40 C41 C42 119.7(5) . . ?
C37 C42 C41 120.8(4) . . ?
F14 P10 F13 91.0(7) . . ?
F14 P10 F16 91.2(6) . . ?
F13 P10 F16 91.2(6) . . ?
F14 P10 F12 178.0(8) . . ?
F13 P10 F12 90.1(7) . . ?
F16 P10 F12 90.4(7) . . ?
F14 P10 F15 90.2(7) . . ?
F13 P10 F15 178.2(8) . . ?
F16 P10 F15 90.1(7) . . ?
F12 P10 F15 88.6(7) . . ?
F14 P10 F11 90.2(7) . . ?
F13 P10 F11 89.4(7) . . ?
F16 P10 F11 178.5(9) . . ?
F12 P10 F11 88.3(6) . . ?
F15 P10 F11 89.3(6) . . ?
F11' P10' F13' 90.4(8) . . ?
F11' P10' F14' 90.2(8) . . ?
F13' P10' F14' 90.3(8) . . ?
F11' P10' F12' 90.2(8) . . ?
F13' P10' F12' 90.1(8) . . ?
F14' P10' F12' 179.5(11) . . ?
F11' P10' F16' 179.5(11) . . ?
F13' P10' F16' 90.2(8) . . ?
F14' P10' F16' 89.9(8) . . ?
F12' P10' F16' 89.8(8) . . ?
F11' P10' F15' 89.8(8) . . ?
F13' P10' F15' 179.8(12) . . ?
F14' P10' F15' 89.9(8) . . ?
F12' P10' F15' 89.8(8) . . ?
F16' P10' F15' 89.7(8) . . ?
F25 P20 F24 91.2(7) . . ?
F25 P20 F26 92.4(7) . . ?
F24 P20 F26 91.1(7) . . ?
F25 P20 F22 91.6(7) . . ?
F24 P20 F22 176.5(10) . . ?
F26 P20 F22 90.8(7) . . ?
F25 P20 F21 89.8(7) . . ?
F24 P20 F21 90.3(8) . . ?
F26 P20 F21 177.3(9) . . ?
F22 P20 F21 87.7(7) . . ?
F25 P20 F23 178.5(10) . . ?
F24 P20 F23 89.4(7) . . ?
F26 P20 F23 88.9(7) . . ?
F22 P20 F23 87.8(7) . . ?
F21 P20 F23 88.8(7) . . ?
F23' P20' F21' 94.0(7) . . ?
F23' P20' F26' 93.3(7) . . ?
F21' P20' F26' 172.3(8) . . ?
F23' P20' F24' 93.9(7) . . ?
F21' P20' F24' 90.7(7) . . ?
F26' P20' F24' 91.1(7) . . ?
F23' P20' F22' 93.1(7) . . ?
F21' P20' F22' 88.6(7) . . ?
F26' P20' F22' 88.7(7) . . ?
F24' P20' F22' 173.0(8) . . ?
F23' P20' F25' 177.2(9) . . ?
F21' P20' F25' 87.7(7) . . ?
F26' P20' F25' 84.9(7) . . ?
F24' P20' F25' 88.3(7) . . ?
F22' P20' F25' 84.7(6) . . ?

_refine_diff_density_max         0.578
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.074


####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1565399'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H48 N6 Pd S4 2+, 2(I3 1-), 2(C2 H3 N)'
_chemical_formula_sum            'C32 H54 I10 N6 Pd S4'
_chemical_formula_weight         2026.45

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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                   8.062(2)
_cell_length_b                   11.316(2)
_cell_length_c                   16.619(2)
_cell_angle_alpha                71.723(2)
_cell_angle_beta                 87.627(3)
_cell_angle_gamma                82.627(2)
_cell_volume                     1427.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7191
_cell_measurement_theta_min      1.909
_cell_measurement_theta_max      27.242

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.357
_exptl_crystal_F_000             928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    5.905
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2286
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS-2007/4 (Bruker)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker Smart APEXII CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18207
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.909
_diffrn_reflns_theta_max         27.242
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6393
_reflns_number_gt                5054
_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       Smart
_computing_cell_refinement       'Saint V7.51A'
_computing_data_reduction        'Saint V7.51A'
_computing_structure_solution    'Sir2004 Burla et al., 2007)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0425P)²+3.1844P] 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         6393
_refine_ls_number_parameters     250
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1126
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.5000 0.5000 0.03184(13) Uani 1 2 d S . P . .
I2 I -0.18984(5) 0.41178(4) 0.26806(3) 0.05940(13) Uani 1 1 d . . . . .
I3 I -0.08082(5) 0.46484(5) 0.41346(3) 0.06687(14) Uani 1 1 d . . . . .
I4 I -0.15786(7) 0.78610(6) 0.31431(4) 0.08112(17) Uani 1 1 d . . . . .
I5 I -0.21082(7) 1.03953(6) 0.22763(4) 0.08813(18) Uani 1 1 d . . . . .
I1 I -0.30376(8) 0.35567(7) 0.11622(4) 0.0946(2) Uani 1 1 d . . . . .
S11 S 0.45895(17) 0.32660(10) 0.46392(8) 0.0405(3) Uani 1 1 d . . . . .
S21 S 0.39786(18) 0.62006(10) 0.36989(8) 0.0421(3) Uani 1 1 d . . . . .
C21 C 0.3501(6) 0.5197(4) 0.3206(3) 0.0310(9) Uani 1 1 d . . . . .
N21 N 0.2981(5) 0.5606(4) 0.2418(2) 0.0381(9) Uani 1 1 d D . . . .
N11 N 0.3164(5) 0.3047(3) 0.3315(2) 0.0338(8) Uani 1 1 d D . . . .
C91 C 0.2768(7) 0.6937(4) 0.1909(3) 0.0407(11) Uani 1 1 d . . . . .
H91 H 0.2357 0.7429 0.2284 0.049 Uiso 1 1 calc R U . . .
C81 C 0.3015(9) 0.1090(5) 0.3011(4) 0.0541(14) Uani 1 1 d . . . . .
H81A H 0.3835 0.1327 0.2563 0.065 Uiso 1 1 calc R U . . .
H81B H 0.1910 0.1397 0.2768 0.065 Uiso 1 1 calc R U . . .
C31 C 0.3287(6) 0.1666(4) 0.3702(3) 0.0356(10) Uani 1 1 d . . . . .
H31 H 0.4419 0.1359 0.3929 0.043 Uiso 1 1 calc R U . . .
C61 C 0.2043(8) -0.0776(5) 0.4134(4) 0.0597(16) Uani 1 1 d . . . . .
H61A H 0.2265 -0.1679 0.4382 0.072 Uiso 1 1 calc R U . . .
H61B H 0.0891 -0.0572 0.3941 0.072 Uiso 1 1 calc R U . . .
C41 C 0.2042(7) 0.1277(4) 0.4419(3) 0.0434(11) Uani 1 1 d . . . . .
H41A H 0.0910 0.1555 0.4206 0.052 Uiso 1 1 calc R U . . .
H41B H 0.2214 0.1659 0.4851 0.052 Uiso 1 1 calc R U . . .
C51 C 0.2295(7) -0.0151(5) 0.4797(4) 0.0505(13) Uani 1 1 d . . . . .
H51A H 0.3416 -0.0419 0.5027 0.061 Uiso 1 1 calc R U . . .
H51B H 0.1507 -0.0410 0.5257 0.061 Uiso 1 1 calc R U . . .
C101 C 0.1462(9) 0.7155(6) 0.1233(4) 0.0605(16) Uani 1 1 d . . . . .
H10A H 0.0408 0.6914 0.1496 0.073 Uiso 1 1 calc R U . . .
H10B H 0.1812 0.6646 0.0869 0.073 Uiso 1 1 calc R U . . .
C114 C 0.4414(8) 0.7352(6) 0.1542(4) 0.0645(17) Uani 1 1 d . . . . .
H11A H 0.4865 0.6861 0.1181 0.077 Uiso 1 1 calc R U . . .
H11B H 0.5206 0.7214 0.1996 0.077 Uiso 1 1 calc R U . . .
C112 C 0.2849(11) 0.8998(7) 0.0344(4) 0.083(2) Uani 1 1 d . . . . .
H11C H 0.2660 0.9892 0.0050 0.099 Uiso 1 1 calc R U . . .
H11D H 0.3258 0.8581 -0.0067 0.099 Uiso 1 1 calc R U . . .
C71 C 0.3189(10) -0.0345(5) 0.3394(5) 0.0698(19) Uani 1 1 d . . . . .
H71A H 0.2946 -0.0707 0.2961 0.084 Uiso 1 1 calc R U . . .
H71B H 0.4335 -0.0651 0.3576 0.084 Uiso 1 1 calc R U . . .
C111 C 0.1235(10) 0.8549(6) 0.0706(5) 0.074(2) Uani 1 1 d . . . . .
H11E H 0.0458 0.8676 0.0248 0.089 Uiso 1 1 calc R U . . .
H11F H 0.0757 0.9042 0.1061 0.089 Uiso 1 1 calc R U . . .
C113 C 0.4167(10) 0.8746(7) 0.1025(5) 0.080(2) Uani 1 1 d . . . . .
H11G H 0.3822 0.9241 0.1399 0.096 Uiso 1 1 calc R U . . .
H11H H 0.5218 0.8996 0.0763 0.096 Uiso 1 1 calc R U . . .
C11 C 0.3682(6) 0.3807(4) 0.3672(3) 0.0301(9) Uani 1 1 d . . . . .
N1S N 0.2118(8) 0.3969(5) 0.1445(3) 0.0658(14) Uani 1 1 d . . . . .
C2S C 0.1993(9) 0.3575(6) 0.0926(4) 0.0641(16) Uani 1 1 d . . . . .
C1S C 0.1875(17) 0.2981(14) 0.0273(8) 0.152(5) Uani 1 1 d . . . . .
H1SA H 0.1106 0.2367 0.0452 0.228 Uiso 1 1 calc R U . . .
H1SB H 0.2957 0.2581 0.0181 0.228 Uiso 1 1 calc R U . . .
H1SC H 0.1483 0.3605 -0.0244 0.228 Uiso 1 1 calc R U . . .
H21 H 0.276(8) 0.505(5) 0.211(4) 0.068(19) Uiso 1 1 d D . . . .
H11 H 0.252(6) 0.336(5) 0.281(2) 0.048(15) Uiso 1 1 d 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 S21 2.2841(12) 2_666 ?
Pd S21 2.2841(12) . ?
Pd S11 2.2892(11) . ?
Pd S11 2.2892(11) 2_666 ?
I2 I3 2.8625(7) . ?
I2 I1 2.9933(7) . ?
I4 I5 2.7617(10) . ?
S11 C11 1.690(4) . ?
S21 C21 1.682(4) . ?
C21 N21 1.312(6) . ?
C21 C11 1.511(6) . ?
N21 C91 1.470(6) . ?
N21 H21 0.96(2) . ?
N11 C11 1.303(5) . ?
N11 C31 1.483(5) . ?
N11 H11 0.956(19) . ?
C91 C114 1.506(8) . ?
C91 C101 1.513(7) . ?
C91 H91 0.9800 . ?
C81 C31 1.523(7) . ?
C81 C71 1.537(8) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C31 C41 1.520(7) . ?
C31 H31 0.9800 . ?
C61 C71 1.499(10) . ?
C61 C51 1.517(8) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C41 C51 1.528(7) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C101 C111 1.537(8) . ?
C101 H10A 0.9700 . ?
C101 H10B 0.9700 . ?
C114 C113 1.533(9) . ?
C114 H11A 0.9700 . ?
C114 H11B 0.9700 . ?
C112 C111 1.492(11) . ?
C112 C113 1.521(10) . ?
C112 H11C 0.9700 . ?
C112 H11D 0.9700 . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C111 H11E 0.9700 . ?
C111 H11F 0.9700 . ?
C113 H11G 0.9700 . ?
C113 H11H 0.9700 . ?
N1S C2S 1.100(8) . ?
C2S C1S 1.456(11) . ?
C1S H1SA 0.9600 . ?
C1S H1SB 0.9600 . ?
C1S H1SC 0.9600 . ?

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
S21 Pd S21 180.0 2_666 . ?
S21 Pd S11 91.95(4) 2_666 . ?
S21 Pd S11 88.05(4) . . ?
S21 Pd S11 88.05(4) 2_666 2_666 ?
S21 Pd S11 91.95(4) . 2_666 ?
S11 Pd S11 180.0 . 2_666 ?
I3 I2 I1 179.87(2) . . ?
C11 S11 Pd 106.16(15) . . ?
C21 S21 Pd 106.35(15) . . ?
N21 C21 C11 119.4(4) . . ?
N21 C21 S21 120.8(3) . . ?
C11 C21 S21 119.8(3) . . ?
C21 N21 C91 123.6(4) . . ?
C21 N21 H21 122(4) . . ?
C91 N21 H21 114(4) . . ?
C11 N11 C31 124.6(4) . . ?
C11 N11 H11 121(3) . . ?
C31 N11 H11 114(3) . . ?
N21 C91 C114 110.8(5) . . ?
N21 C91 C101 109.5(4) . . ?
C114 C91 C101 112.3(5) . . ?
N21 C91 H91 108.0 . . ?
C114 C91 H91 108.0 . . ?
C101 C91 H91 108.0 . . ?
C31 C81 C71 109.3(5) . . ?
C31 C81 H81A 109.8 . . ?
C71 C81 H81A 109.8 . . ?
C31 C81 H81B 109.8 . . ?
C71 C81 H81B 109.8 . . ?
H81A C81 H81B 108.3 . . ?
N11 C31 C41 112.3(4) . . ?
N11 C31 C81 108.5(4) . . ?
C41 C31 C81 110.6(4) . . ?
N11 C31 H31 108.5 . . ?
C41 C31 H31 108.5 . . ?
C81 C31 H31 108.5 . . ?
C71 C61 C51 110.6(5) . . ?
C71 C61 H61A 109.5 . . ?
C51 C61 H61A 109.5 . . ?
C71 C61 H61B 109.5 . . ?
C51 C61 H61B 109.5 . . ?
H61A C61 H61B 108.1 . . ?
C31 C41 C51 108.8(4) . . ?
C31 C41 H41A 109.9 . . ?
C51 C41 H41A 109.9 . . ?
C31 C41 H41B 109.9 . . ?
C51 C41 H41B 109.9 . . ?
H41A C41 H41B 108.3 . . ?
C61 C51 C41 111.2(5) . . ?
C61 C51 H51A 109.4 . . ?
C41 C51 H51A 109.4 . . ?
C61 C51 H51B 109.4 . . ?
C41 C51 H51B 109.4 . . ?
H51A C51 H51B 108.0 . . ?
C91 C101 C111 109.3(5) . . ?
C91 C101 H10A 109.8 . . ?
C111 C101 H10A 109.8 . . ?
C91 C101 H10B 109.8 . . ?
C111 C101 H10B 109.8 . . ?
H10A C101 H10B 108.3 . . ?
C91 C114 C113 109.9(6) . . ?
C91 C114 H11A 109.7 . . ?
C113 C114 H11A 109.7 . . ?
C91 C114 H11B 109.7 . . ?
C113 C114 H11B 109.7 . . ?
H11A C114 H11B 108.2 . . ?
C111 C112 C113 111.9(6) . . ?
C111 C112 H11C 109.2 . . ?
C113 C112 H11C 109.2 . . ?
C111 C112 H11D 109.2 . . ?
C113 C112 H11D 109.2 . . ?
H11C C112 H11D 107.9 . . ?
C61 C71 C81 112.7(5) . . ?
C61 C71 H71A 109.1 . . ?
C81 C71 H71A 109.1 . . ?
C61 C71 H71B 109.1 . . ?
C81 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C112 C111 C101 112.1(6) . . ?
C112 C111 H11E 109.2 . . ?
C101 C111 H11E 109.2 . . ?
C112 C111 H11F 109.2 . . ?
C101 C111 H11F 109.2 . . ?
H11E C111 H11F 107.9 . . ?
C112 C113 C114 110.6(6) . . ?
C112 C113 H11G 109.5 . . ?
C114 C113 H11G 109.5 . . ?
C112 C113 H11H 109.5 . . ?
C114 C113 H11H 109.5 . . ?
H11G C113 H11H 108.1 . . ?
N11 C11 C21 119.4(4) . . ?
N11 C11 S11 121.3(3) . . ?
C21 C11 S11 119.2(3) . . ?
N1S C2S C1S 176.5(10) . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?

_refine_diff_density_max         1.124
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_3-B
_database_code_depnum_ccdc_archive 'CCDC 1565397'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H68 N2 P4 Pd2 S4, 2(F6 P), C4 H10 O'
_chemical_formula_sum            'C82 H78 F12 N2 O P6 Pd2 S4'
_chemical_formula_weight         1862.32

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 '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'
S S 0.1246 0.1234 '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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   20.6104(5)
_cell_length_b                   15.5218(4)
_cell_length_c                   26.8129(9)
_cell_angle_alpha                90
_cell_angle_beta                 107.289(3)
_cell_angle_gamma                90
_cell_volume                     8190.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7561
_cell_measurement_theta_min      2.5880
_cell_measurement_theta_max      28.1780

_exptl_crystal_description       blocks
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             3784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.732
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            28414
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.451
_diffrn_reflns_theta_max         28.330
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             16222
_reflns_number_gt                12432
_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       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_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)+(0.0364P)²+15.2565P] 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         16222
_refine_ls_number_parameters     1003
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.0969
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.042
_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
Pd1 Pd 0.28900(2) 0.75475(2) 0.62577(2) 0.02266(8) Uani 1 1 d . . . . .
Pd2 Pd 0.68471(2) 0.33404(2) 0.84710(2) 0.02096(7) Uani 1 1 d . . . . .
P1 P 0.17638(5) 0.74099(6) 0.62478(4) 0.0245(2) Uani 1 1 d . . . . .
P2 P 0.29207(5) 0.89709(6) 0.60343(4) 0.0229(2) Uani 1 1 d . . . . .
P3 P 0.80000(5) 0.35302(7) 0.85713(4) 0.0237(2) Uani 1 1 d . . . . .
P4 P 0.68569(5) 0.19467(6) 0.87627(4) 0.0236(2) Uani 1 1 d . . . . .
S1 S 0.40729(5) 0.73425(7) 0.64767(4) 0.0314(2) Uani 1 1 d . . . . .
C2 C 0.39263(19) 0.6346(3) 0.67162(16) 0.0301(9) Uani 1 1 d . . . . .
S3 S 0.30690(5) 0.61392(7) 0.65695(5) 0.0360(3) Uani 1 1 d . . . . .
N4 N 0.43924(16) 0.5803(2) 0.69639(14) 0.0336(8) Uani 1 1 d . . . . .
C5 C 0.51167(19) 0.5971(3) 0.70690(17) 0.0359(10) Uani 1 1 d . . . . .
H5A H 0.5186 0.6545 0.6933 0.043 Uiso 1 1 calc R U . . .
H5B H 0.5320 0.5533 0.6892 0.043 Uiso 1 1 calc R U . . .
C6 C 0.5458(2) 0.5937(2) 0.76568(17) 0.0327(9) Uani 1 1 d . . . . .
H6A H 0.5955 0.6011 0.7732 0.039 Uiso 1 1 calc R U . . .
H6B H 0.5285 0.6410 0.7830 0.039 Uiso 1 1 calc R U . . .
N7 N 0.53137(15) 0.5101(2) 0.78620(13) 0.0296(8) Uani 1 1 d . . . . .
C8 C 0.45867(19) 0.4931(3) 0.77557(17) 0.0346(10) Uani 1 1 d . . . . .
H8A H 0.4387 0.5360 0.7940 0.042 Uiso 1 1 calc R U . . .
H8B H 0.4521 0.4352 0.7887 0.042 Uiso 1 1 calc R U . . .
C9 C 0.4231(2) 0.4978(3) 0.71756(18) 0.0362(10) Uani 1 1 d . . . . .
H9A H 0.4380 0.4492 0.6997 0.043 Uiso 1 1 calc R U . . .
H9B H 0.3734 0.4931 0.7111 0.043 Uiso 1 1 calc R U . . .
S10 S 0.56730(5) 0.35459(6) 0.83134(4) 0.0279(2) Uani 1 1 d . . . . .
C11 C 0.57943(18) 0.4546(2) 0.80729(15) 0.0255(8) Uani 1 1 d . . . . .
S12 S 0.66414(5) 0.47445(6) 0.81637(4) 0.0282(2) Uani 1 1 d . . . . .
C13 C 0.1481(2) 0.6344(3) 0.59980(16) 0.0325(9) Uani 1 1 d . . . . .
C14 C 0.1711(3) 0.6016(3) 0.5602(2) 0.0525(13) Uani 1 1 d . . . . .
H14A H 0.2032 0.6334 0.5486 0.063 Uiso 1 1 calc R U . . .
C15 C 0.1482(3) 0.5229(4) 0.5373(3) 0.0784(19) Uani 1 1 d . . . . .
H15A H 0.1646 0.5010 0.5102 0.094 Uiso 1 1 calc R U . . .
C16 C 0.1018(3) 0.4770(4) 0.5540(3) 0.086(2) Uani 1 1 d . . . . .
H16A H 0.0835 0.4248 0.5372 0.104 Uiso 1 1 calc R U . . .
C17 C 0.0823(3) 0.5066(3) 0.5944(3) 0.0709(18) Uani 1 1 d . . . . .
H17A H 0.0522 0.4727 0.6071 0.085 Uiso 1 1 calc R U . . .
C18 C 0.1046(2) 0.5847(3) 0.6181(2) 0.0472(12) Uani 1 1 d . . . . .
H18A H 0.0900 0.6039 0.6467 0.057 Uiso 1 1 calc R U . . .
C19 C 0.10714(19) 0.8105(3) 0.58900(16) 0.0329(10) Uani 1 1 d . . . . .
C20 C 0.0623(2) 0.7840(4) 0.54165(19) 0.0482(13) Uani 1 1 d . . . . .
H20A H 0.0679 0.7293 0.5275 0.058 Uiso 1 1 calc R U . . .
C21 C 0.0100(2) 0.8370(5) 0.5154(2) 0.0668(18) Uani 1 1 d . . . . .
H21A H -0.0197 0.8194 0.4826 0.080 Uiso 1 1 calc R U . . .
C22 C 0.0005(3) 0.9134(5) 0.5356(3) 0.0686(19) Uani 1 1 d . . . . .
H22A H -0.0373 0.9479 0.5178 0.082 Uiso 1 1 calc R U . . .
C23 C 0.0452(3) 0.9429(4) 0.5822(3) 0.0660(17) Uani 1 1 d . . . . .
H23A H 0.0392 0.9981 0.5955 0.079 Uiso 1 1 calc R U . . .
C24 C 0.0991(2) 0.8896(3) 0.6091(2) 0.0444(12) Uani 1 1 d . . . . .
H24A H 0.1301 0.9083 0.6411 0.053 Uiso 1 1 calc R U . . .
C25 C 0.17193(19) 0.7515(2) 0.69112(15) 0.0266(8) Uani 1 1 d . . . . .
C26 C 0.1090(2) 0.7509(3) 0.70142(17) 0.0337(9) Uani 1 1 d . . . . .
H26A H 0.0684 0.7418 0.6737 0.040 Uiso 1 1 calc R U . . .
C27 C 0.1055(2) 0.7635(3) 0.75141(18) 0.0407(11) Uani 1 1 d . . . . .
H27A H 0.0627 0.7620 0.7581 0.049 Uiso 1 1 calc R U . . .
C28 C 0.1641(2) 0.7782(3) 0.79176(18) 0.0476(12) Uani 1 1 d . . . . .
H28A H 0.1616 0.7873 0.8262 0.057 Uiso 1 1 calc R U . . .
C29 C 0.2260(2) 0.7799(3) 0.78216(18) 0.0482(12) Uani 1 1 d . . . . .
H29A H 0.2661 0.7911 0.8100 0.058 Uiso 1 1 calc R U . . .
C30 C 0.2303(2) 0.7655(3) 0.73249(16) 0.0354(10) Uani 1 1 d . . . . .
H30A H 0.2735 0.7650 0.7265 0.042 Uiso 1 1 calc R U . . .
C31 C 0.23222(18) 0.9340(3) 0.54322(15) 0.0301(9) Uani 1 1 d . . . . .
C32 C 0.19122(19) 0.8742(3) 0.50972(15) 0.0364(10) Uani 1 1 d . . . . .
H32A H 0.1939 0.8150 0.5192 0.044 Uiso 1 1 calc R U . . .
C33 C 0.1464(2) 0.9004(4) 0.46253(18) 0.0565(15) Uani 1 1 d . . . . .
H33A H 0.1181 0.8595 0.4399 0.068 Uiso 1 1 calc R U . . .
C34 C 0.1433(3) 0.9863(5) 0.4488(2) 0.0665(19) Uani 1 1 d . . . . .
H34A H 0.1126 1.0045 0.4165 0.080 Uiso 1 1 calc R U . . .
C35 C 0.1840(3) 1.0453(4) 0.4812(2) 0.0612(17) Uani 1 1 d . . . . .
H35A H 0.1810 1.1043 0.4714 0.073 Uiso 1 1 calc R U . . .
C36 C 0.2296(2) 1.0201(3) 0.5281(2) 0.0464(12) Uani 1 1 d . . . . .
H36A H 0.2589 1.0612 0.5498 0.056 Uiso 1 1 calc R U . . .
C37 C 0.37273(18) 0.9328(3) 0.59552(15) 0.0281(9) Uani 1 1 d . . . . .
C38 C 0.3984(2) 0.8882(3) 0.56068(17) 0.0367(10) Uani 1 1 d . . . . .
H38A H 0.3760 0.8379 0.5439 0.044 Uiso 1 1 calc R U . . .
C39 C 0.4565(2) 0.9171(3) 0.55036(19) 0.0464(12) Uani 1 1 d . . . . .
H39A H 0.4738 0.8867 0.5263 0.056 Uiso 1 1 calc R U . . .
C40 C 0.4894(2) 0.9891(4) 0.5746(2) 0.0497(13) Uani 1 1 d . . . . .
H40A H 0.5291 1.0088 0.5672 0.060 Uiso 1 1 calc R U . . .
C41 C 0.4652(2) 1.0325(4) 0.6093(2) 0.0548(14) Uani 1 1 d . . . . .
H41A H 0.4886 1.0820 0.6265 0.066 Uiso 1 1 calc R U . . .
C42 C 0.4067(2) 1.0050(3) 0.61987(19) 0.0431(11) Uani 1 1 d . . . . .
H42A H 0.3899 1.0361 0.6440 0.052 Uiso 1 1 calc R U . . .
C43 C 0.2824(2) 0.9598(2) 0.65772(17) 0.0311(9) Uani 1 1 d . . . . .
C44 C 0.2339(2) 1.0230(3) 0.6534(2) 0.0491(13) Uani 1 1 d . . . . .
H44A H 0.2043 1.0385 0.6201 0.059 Uiso 1 1 calc R U . . .
C45 C 0.2289(3) 1.0637(4) 0.6984(3) 0.0675(18) Uani 1 1 d . . . . .
H45A H 0.1958 1.1075 0.6959 0.081 Uiso 1 1 calc R U . . .
C46 C 0.2716(3) 1.0408(4) 0.7464(3) 0.0681(17) Uani 1 1 d . . . . .
H46A H 0.2676 1.0686 0.7769 0.082 Uiso 1 1 calc R U . . .
C47 C 0.3199(3) 0.9786(4) 0.7511(2) 0.0615(15) Uani 1 1 d . . . . .
H47A H 0.3496 0.9639 0.7845 0.074 Uiso 1 1 calc R U . . .
C48 C 0.3253(2) 0.9368(3) 0.70664(18) 0.0444(11) Uani 1 1 d . . . . .
H48A H 0.3582 0.8927 0.7096 0.053 Uiso 1 1 calc R U . . .
C49 C 0.82414(18) 0.3309(2) 0.79896(15) 0.0250(8) Uani 1 1 d . . . . .
C50 C 0.7742(2) 0.3227(3) 0.75129(15) 0.0313(9) Uani 1 1 d . . . . .
H50A H 0.7276 0.3255 0.7496 0.038 Uiso 1 1 calc R U . . .
C51 C 0.7928(2) 0.3105(3) 0.70578(17) 0.0414(11) Uani 1 1 d . . . . .
H51A H 0.7587 0.3046 0.6731 0.050 Uiso 1 1 calc R U . . .
C52 C 0.8596(2) 0.3069(3) 0.70809(18) 0.0467(12) Uani 1 1 d . . . . .
H52A H 0.8717 0.2978 0.6770 0.056 Uiso 1 1 calc R U . . .
C53 C 0.9100(2) 0.3164(3) 0.75516(18) 0.0401(11) Uani 1 1 d . . . . .
H53A H 0.9565 0.3148 0.7562 0.048 Uiso 1 1 calc R U . . .
C54 C 0.8926(2) 0.3280(3) 0.80030(16) 0.0322(9) Uani 1 1 d . . . . .
H54A H 0.9272 0.3340 0.8327 0.039 Uiso 1 1 calc R U . . .
C55 C 0.81856(17) 0.4673(2) 0.86885(15) 0.0252(8) Uani 1 1 d . . . . .
C56 C 0.84358(18) 0.5171(3) 0.83555(16) 0.0301(9) Uani 1 1 d . . . . .
H56A H 0.8540 0.4910 0.8068 0.036 Uiso 1 1 calc R U . . .
C57 C 0.8532(2) 0.6047(3) 0.84429(18) 0.0395(10) Uani 1 1 d . . . . .
H57A H 0.8701 0.6385 0.8213 0.047 Uiso 1 1 calc R U . . .
C58 C 0.8387(2) 0.6435(3) 0.8858(2) 0.0442(12) Uani 1 1 d . . . . .
H58A H 0.8470 0.7032 0.8922 0.053 Uiso 1 1 calc R U . . .
C59 C 0.8120(2) 0.5953(3) 0.91804(18) 0.0402(11) Uani 1 1 d . . . . .
H59A H 0.8008 0.6221 0.9462 0.048 Uiso 1 1 calc R U . . .
C60 C 0.80158(19) 0.5082(3) 0.90952(16) 0.0327(9) Uani 1 1 d . . . . .
H60A H 0.7825 0.4756 0.9317 0.039 Uiso 1 1 calc R U . . .
C61 C 0.86316(19) 0.2976(3) 0.90951(15) 0.0305(9) Uani 1 1 d . . . . .
C62 C 0.8829(2) 0.3301(3) 0.96028(16) 0.0384(10) Uani 1 1 d . . . . .
H62A H 0.8653 0.3836 0.9676 0.046 Uiso 1 1 calc R U . . .
C63 C 0.9283(2) 0.2842(3) 1.00004(18) 0.0498(13) Uani 1 1 d . . . . .
H63A H 0.9410 0.3062 1.0347 0.060 Uiso 1 1 calc R U . . .
C64 C 0.9551(2) 0.2071(3) 0.98989(19) 0.0520(13) Uani 1 1 d . . . . .
H64A H 0.9865 0.1764 1.0173 0.062 Uiso 1 1 calc R U . . .
C65 C 0.9360(2) 0.1751(3) 0.93991(19) 0.0492(13) Uani 1 1 d . . . . .
H65A H 0.9544 0.1220 0.9328 0.059 Uiso 1 1 calc R U . . .
C66 C 0.8902(2) 0.2194(3) 0.89982(17) 0.0362(10) Uani 1 1 d . . . . .
H66A H 0.8772 0.1963 0.8655 0.043 Uiso 1 1 calc R U . . .
C67 C 0.7006(2) 0.1966(3) 0.94669(15) 0.0305(9) Uani 1 1 d . . . . .
C68 C 0.7657(2) 0.1933(3) 0.98120(17) 0.0421(11) Uani 1 1 d . . . . .
H68A H 0.8034 0.1828 0.9686 0.051 Uiso 1 1 calc R U . . .
C69 C 0.7757(3) 0.2055(4) 1.03387(19) 0.0616(15) Uani 1 1 d . . . . .
H69A H 0.8204 0.2025 1.0574 0.074 Uiso 1 1 calc R U . . .
C70 C 0.7224(3) 0.2218(4) 1.0527(2) 0.0664(16) Uani 1 1 d . . . . .
H70A H 0.7298 0.2309 1.0890 0.080 Uiso 1 1 calc R U . . .
C71 C 0.6577(3) 0.2248(4) 1.0187(2) 0.0608(15) Uani 1 1 d . . . . .
H71A H 0.6203 0.2353 1.0318 0.073 Uiso 1 1 calc R U . . .
C72 C 0.6463(3) 0.2129(3) 0.96589(19) 0.0454(12) Uani 1 1 d . . . . .
H72A H 0.6014 0.2159 0.9427 0.055 Uiso 1 1 calc R U . . .
C73 C 0.60918(19) 0.1302(3) 0.84922(18) 0.0330(10) Uani 1 1 d . . . . .
C74 C 0.6006(2) 0.0552(3) 0.8749(2) 0.0458(12) Uani 1 1 d . . . . .
H74A H 0.6277 0.0456 0.9099 0.055 Uiso 1 1 calc R U . . .
C75 C 0.5533(3) -0.0051(3) 0.8502(3) 0.0622(16) Uani 1 1 d . . . . .
H75A H 0.5484 -0.0568 0.8677 0.075 Uiso 1 1 calc R U . . .
C76 C 0.5131(3) 0.0097(3) 0.8002(3) 0.0654(17) Uani 1 1 d . . . . .
H76A H 0.4800 -0.0317 0.7833 0.079 Uiso 1 1 calc R U . . .
C77 C 0.5201(2) 0.0838(3) 0.7741(2) 0.0575(15) Uani 1 1 d . . . . .
H77A H 0.4920 0.0934 0.7394 0.069 Uiso 1 1 calc R U . . .
C78 C 0.5693(2) 0.1454(3) 0.79912(19) 0.0394(11) Uani 1 1 d . . . . .
H78A H 0.5747 0.1967 0.7815 0.047 Uiso 1 1 calc R U . . .
C79 C 0.74542(19) 0.1227(2) 0.85926(15) 0.0271(8) Uani 1 1 d . . . . .
C80 C 0.7795(2) 0.0551(3) 0.89053(17) 0.0342(10) Uani 1 1 d . . . . .
H80A H 0.7757 0.0472 0.9247 0.041 Uiso 1 1 calc R U . . .
C81 C 0.8185(2) 0.0001(3) 0.8713(2) 0.0436(11) Uani 1 1 d . . . . .
H81A H 0.8424 -0.0455 0.8925 0.052 Uiso 1 1 calc R U . . .
C82 C 0.8232(2) 0.0106(3) 0.82110(19) 0.0408(11) Uani 1 1 d . . . . .
H82A H 0.8507 -0.0272 0.8083 0.049 Uiso 1 1 calc R U . . .
C83 C 0.7878(2) 0.0758(3) 0.78996(17) 0.0370(10) Uani 1 1 d . . . . .
H83A H 0.7901 0.0823 0.7553 0.044 Uiso 1 1 calc R U . . .
C84 C 0.74929(19) 0.1315(3) 0.80886(16) 0.0299(9) Uani 1 1 d . . . . .
H84A H 0.7250 0.1765 0.7872 0.036 Uiso 1 1 calc R U . . .
P10 P 0.44873(6) 0.74455(8) 0.85272(5) 0.0417(3) Uani 1 1 d . . . . .
F11 F 0.48648(18) 0.7923(2) 0.90548(14) 0.0864(11) Uani 1 1 d . . . . .
F12 F 0.4024(2) 0.8252(3) 0.8338(2) 0.1344(19) Uani 1 1 d . . . . .
F13 F 0.5005(2) 0.7797(3) 0.82606(18) 0.1119(15) Uani 1 1 d . . . . .
F14 F 0.4921(2) 0.6616(2) 0.87064(14) 0.0943(13) Uani 1 1 d . . . . .
F15 F 0.3945(2) 0.7100(3) 0.87777(16) 0.1221(18) Uani 1 1 d . . . . .
F16 F 0.40989(14) 0.69688(19) 0.79966(11) 0.0590(8) Uani 1 1 d . . . . .
P20 P 0.53244(5) 0.31735(7) 0.65256(4) 0.0348(3) Uani 1 1 d . . . . .
F21 F 0.53782(18) 0.3832(3) 0.69781(14) 0.0998(14) Uani 1 1 d . . . . .
F22 F 0.45223(14) 0.3260(2) 0.63394(15) 0.0798(11) Uani 1 1 d . . . . .
F23 F 0.53679(18) 0.3932(2) 0.61571(16) 0.0983(13) Uani 1 1 d . . . . .
F24 F 0.61249(13) 0.30827(19) 0.67251(13) 0.0656(9) Uani 1 1 d . . . . .
F25 F 0.52733(19) 0.2394(2) 0.68968(15) 0.0914(12) Uani 1 1 d . . . . .
F26 F 0.52846(15) 0.2485(2) 0.60873(12) 0.0738(10) Uani 1 1 d . . . . .
O90 O 0.2985(2) 0.5906(3) 0.49147(16) 0.0703(16) Uani 0.898(7) 1 d D U P A 1
C91 C 0.2828(3) 0.6693(4) 0.4686(3) 0.0518(16) Uani 0.898(7) 1 d D U P A 1
H91A H 0.3144 0.6832 0.4483 0.062 Uiso 0.898(7) 1 calc R U P A 1
H91B H 0.2878 0.7139 0.4959 0.062 Uiso 0.898(7) 1 calc R U P A 1
C92 C 0.2119(4) 0.6691(6) 0.4336(3) 0.089(3) Uani 0.898(7) 1 d D U P A 1
H92A H 0.2010 0.7259 0.4174 0.134 Uiso 0.898(7) 1 calc R U P A 1
H92B H 0.2072 0.6254 0.4064 0.134 Uiso 0.898(7) 1 calc R U P A 1
H92C H 0.1807 0.6559 0.4540 0.134 Uiso 0.898(7) 1 calc R U P A 1
C93 C 0.3659(4) 0.5857(6) 0.5231(3) 0.101(3) Uani 0.898(7) 1 d D U P A 1
H93A H 0.3963 0.6011 0.5020 0.121 Uiso 0.898(7) 1 calc R U P A 1
H93B H 0.3729 0.6287 0.5515 0.121 Uiso 0.898(7) 1 calc R U P A 1
C94 C 0.3842(4) 0.5047(5) 0.5452(4) 0.133(5) Uani 0.898(7) 1 d D . P A 1
H94A H 0.4318 0.5057 0.5668 0.200 Uiso 0.898(7) 1 calc R U P A 1
H94B H 0.3552 0.4894 0.5669 0.200 Uiso 0.898(7) 1 calc R U P A 1
H94C H 0.3786 0.4619 0.5173 0.200 Uiso 0.898(7) 1 calc R U P A 1
O90' O 0.3072(16) 0.673(2) 0.4836(15) 0.040(8) Uiso 0.102(7) 1 d D U P A 2
C91' C 0.2528(18) 0.625(3) 0.460(3) 0.080(7) Uiso 0.102(7) 1 d D U P A 2
H91C H 0.2490 0.5785 0.4841 0.096 Uiso 0.102(7) 1 calc R U P A 2
H91D H 0.2608 0.5974 0.4289 0.096 Uiso 0.102(7) 1 calc R U P A 2
C92' C 0.1884(19) 0.670(5) 0.443(3) 0.102(11) Uiso 0.102(7) 1 d D U P A 2
H92D H 0.1520 0.6299 0.4264 0.153 Uiso 0.102(7) 1 calc R U P A 2
H92E H 0.1790 0.6967 0.4735 0.153 Uiso 0.102(7) 1 calc R U P A 2
H92F H 0.1907 0.7156 0.4182 0.153 Uiso 0.102(7) 1 calc R U P A 2
C93' C 0.3697(17) 0.642(3) 0.488(3) 0.09(2) Uiso 0.102(7) 1 d D . P A 2
H93C H 0.4033 0.6852 0.5076 0.114 Uiso 0.102(7) 1 calc R U P A 2
H93D H 0.3748 0.6373 0.4528 0.114 Uiso 0.102(7) 1 calc R U P A 2
C94' C 0.387(4) 0.560(4) 0.514(3) 0.087(11) Uiso 0.102(7) 1 d D U P A 2
H94D H 0.4332 0.5438 0.5153 0.130 Uiso 0.102(7) 1 calc R U P A 2
H94E H 0.3836 0.5638 0.5498 0.130 Uiso 0.102(7) 1 calc R U P A 2
H94F H 0.3550 0.5158 0.4948 0.130 Uiso 0.102(7) 1 calc R U P A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 P2 2.2948(10) . ?
Pd1 P1 2.3232(10) . ?
Pd1 S3 2.3304(10) . ?
Pd1 S1 2.3536(10) . ?
Pd2 P4 2.2985(10) . ?
Pd2 S12 2.3240(10) . ?
Pd2 P3 2.3292(10) . ?
Pd2 S10 2.3512(10) . ?
P1 C13 1.814(4) . ?
P1 C25 1.815(4) . ?
P1 C19 1.818(4) . ?
P2 C31 1.809(4) . ?
P2 C43 1.810(4) . ?
P2 C37 1.823(4) . ?
P3 C49 1.805(4) . ?
P3 C61 1.822(4) . ?
P3 C55 1.822(4) . ?
P4 C79 1.818(4) . ?
P4 C67 1.821(4) . ?
P4 C73 1.826(4) . ?
S1 C2 1.735(4) . ?
C2 N4 1.302(5) . ?
C2 S3 1.722(4) . ?
N4 C5 1.458(5) . ?
N4 C9 1.478(5) . ?
C5 C6 1.524(6) . ?
C6 N7 1.473(5) . ?
N7 C11 1.308(5) . ?
N7 C8 1.464(5) . ?
C8 C9 1.511(6) . ?
S10 C11 1.728(4) . ?
C11 S12 1.717(4) . ?
C13 C18 1.380(6) . ?
C13 C14 1.383(6) . ?
C14 C15 1.384(7) . ?
C15 C16 1.371(8) . ?
C16 C17 1.341(8) . ?
C17 C18 1.383(7) . ?
C19 C24 1.371(6) . ?
C19 C20 1.392(6) . ?
C20 C21 1.372(7) . ?
C21 C22 1.342(9) . ?
C22 C23 1.390(9) . ?
C23 C24 1.402(7) . ?
C25 C30 1.390(5) . ?
C25 C26 1.405(5) . ?
C26 C27 1.377(6) . ?
C27 C28 1.380(6) . ?
C28 C29 1.375(6) . ?
C29 C30 1.380(6) . ?
C31 C32 1.390(6) . ?
C31 C36 1.392(6) . ?
C32 C33 1.387(6) . ?
C33 C34 1.380(8) . ?
C34 C35 1.365(8) . ?
C35 C36 1.384(7) . ?
C37 C42 1.379(6) . ?
C37 C38 1.388(6) . ?
C38 C39 1.382(6) . ?
C39 C40 1.367(7) . ?
C40 C41 1.356(7) . ?
C41 C42 1.386(6) . ?
C43 C44 1.381(6) . ?
C43 C48 1.393(6) . ?
C44 C45 1.394(7) . ?
C45 C46 1.373(8) . ?
C46 C47 1.365(8) . ?
C47 C48 1.390(6) . ?
C49 C50 1.388(5) . ?
C49 C54 1.402(5) . ?
C50 C51 1.396(6) . ?
C51 C52 1.360(6) . ?
C52 C53 1.384(6) . ?
C53 C54 1.372(6) . ?
C55 C56 1.390(5) . ?
C55 C60 1.393(5) . ?
C56 C57 1.385(6) . ?
C57 C58 1.374(6) . ?
C58 C59 1.375(6) . ?
C59 C60 1.377(6) . ?
C61 C66 1.393(6) . ?
C61 C62 1.394(6) . ?
C62 C63 1.388(6) . ?
C63 C64 1.379(7) . ?
C64 C65 1.373(7) . ?
C65 C66 1.384(6) . ?
C67 C72 1.387(6) . ?
C67 C68 1.387(6) . ?
C68 C69 1.378(6) . ?
C69 C70 1.362(7) . ?
C70 C71 1.375(8) . ?
C71 C72 1.376(7) . ?
C73 C78 1.371(6) . ?
C73 C74 1.392(6) . ?
C74 C75 1.371(7) . ?
C75 C76 1.369(8) . ?
C76 C77 1.376(8) . ?
C77 C78 1.410(6) . ?
C79 C84 1.384(5) . ?
C79 C80 1.394(5) . ?
C80 C81 1.374(6) . ?
C81 C82 1.387(6) . ?
C82 C83 1.375(6) . ?
C83 C84 1.368(5) . ?
P10 F13 1.549(4) . ?
P10 F15 1.560(4) . ?
P10 F14 1.560(3) . ?
P10 F12 1.564(4) . ?
P10 F11 1.582(3) . ?
P10 F16 1.592(3) . ?
P20 F23 1.557(3) . ?
P20 F21 1.565(3) . ?
P20 F26 1.573(3) . ?
P20 F24 1.582(3) . ?
P20 F22 1.584(3) . ?
P20 F25 1.589(3) . ?
O90 C91 1.361(6) . ?
O90 C93 1.397(7) . ?
C91 C92 1.483(8) . ?
C93 C94 1.393(8) . ?
O90' C91' 1.341(10) . ?
O90' C93' 1.345(10) . ?
C91' C92' 1.452(10) . ?
C93' C94' 1.451(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P2 Pd1 P1 100.98(4) . . ?
P2 Pd1 S3 169.43(4) . . ?
P1 Pd1 S3 88.22(4) . . ?
P2 Pd1 S1 95.07(4) . . ?
P1 Pd1 S1 161.40(4) . . ?
S3 Pd1 S1 75.04(4) . . ?
P4 Pd2 S12 170.25(4) . . ?
P4 Pd2 P3 100.04(4) . . ?
S12 Pd2 P3 89.70(3) . . ?
P4 Pd2 S10 95.35(3) . . ?
S12 Pd2 S10 74.90(3) . . ?
P3 Pd2 S10 164.52(4) . . ?
C13 P1 C25 109.83(18) . . ?
C13 P1 C19 103.3(2) . . ?
C25 P1 C19 101.75(19) . . ?
C13 P1 Pd1 107.36(14) . . ?
C25 P1 Pd1 108.78(12) . . ?
C19 P1 Pd1 125.19(13) . . ?
C31 P2 C43 109.80(19) . . ?
C31 P2 C37 101.73(17) . . ?
C43 P2 C37 104.61(19) . . ?
C31 P2 Pd1 118.26(15) . . ?
C43 P2 Pd1 106.82(14) . . ?
C37 P2 Pd1 114.81(13) . . ?
C49 P3 C61 105.00(18) . . ?
C49 P3 C55 103.70(18) . . ?
C61 P3 C55 105.15(18) . . ?
C49 P3 Pd2 114.19(12) . . ?
C61 P3 Pd2 119.99(13) . . ?
C55 P3 Pd2 107.32(12) . . ?
C79 P4 C67 110.63(18) . . ?
C79 P4 C73 97.63(18) . . ?
C67 P4 C73 106.3(2) . . ?
C79 P4 Pd2 115.55(13) . . ?
C67 P4 Pd2 108.62(13) . . ?
C73 P4 Pd2 117.46(14) . . ?
C2 S1 Pd1 86.07(13) . . ?
N4 C2 S3 123.2(3) . . ?
N4 C2 S1 125.6(3) . . ?
S3 C2 S1 111.2(2) . . ?
C2 S3 Pd1 87.09(14) . . ?
C2 N4 C5 122.8(3) . . ?
C2 N4 C9 122.7(3) . . ?
C5 N4 C9 114.5(3) . . ?
N4 C5 C6 109.0(3) . . ?
N7 C6 C5 109.5(3) . . ?
C11 N7 C8 124.4(3) . . ?
C11 N7 C6 122.0(3) . . ?
C8 N7 C6 113.3(3) . . ?
N7 C8 C9 110.3(3) . . ?
N4 C9 C8 110.0(3) . . ?
C11 S10 Pd2 86.19(13) . . ?
N7 C11 S12 123.4(3) . . ?
N7 C11 S10 125.3(3) . . ?
S12 C11 S10 111.2(2) . . ?
C11 S12 Pd2 87.29(13) . . ?
C18 C13 C14 118.3(4) . . ?
C18 C13 P1 123.4(3) . . ?
C14 C13 P1 118.3(3) . . ?
C13 C14 C15 121.1(5) . . ?
C16 C15 C14 119.5(5) . . ?
C17 C16 C15 119.4(5) . . ?
C16 C17 C18 122.3(5) . . ?
C13 C18 C17 119.2(5) . . ?
C24 C19 C20 119.9(4) . . ?
C24 C19 P1 119.4(3) . . ?
C20 C19 P1 120.7(4) . . ?
C21 C20 C19 119.9(5) . . ?
C22 C21 C20 120.6(6) . . ?
C21 C22 C23 121.1(5) . . ?
C22 C23 C24 118.7(6) . . ?
C19 C24 C23 119.8(5) . . ?
C30 C25 C26 118.4(4) . . ?
C30 C25 P1 120.8(3) . . ?
C26 C25 P1 120.7(3) . . ?
C27 C26 C25 120.6(4) . . ?
C26 C27 C28 120.0(4) . . ?
C29 C28 C27 120.1(4) . . ?
C28 C29 C30 120.5(4) . . ?
C29 C30 C25 120.4(4) . . ?
C32 C31 C36 119.3(4) . . ?
C32 C31 P2 119.2(3) . . ?
C36 C31 P2 121.4(4) . . ?
C33 C32 C31 120.4(5) . . ?
C34 C33 C32 119.5(5) . . ?
C35 C34 C33 120.5(5) . . ?
C34 C35 C36 120.7(5) . . ?
C35 C36 C31 119.6(5) . . ?
C42 C37 C38 118.8(4) . . ?
C42 C37 P2 123.0(3) . . ?
C38 C37 P2 118.0(3) . . ?
C39 C38 C37 120.0(4) . . ?
C40 C39 C38 120.4(5) . . ?
C41 C40 C39 120.1(4) . . ?
C40 C41 C42 120.4(5) . . ?
C37 C42 C41 120.3(4) . . ?
C44 C43 C48 120.2(4) . . ?
C44 C43 P2 124.3(4) . . ?
C48 C43 P2 115.4(3) . . ?
C43 C44 C45 119.2(5) . . ?
C46 C45 C44 120.1(5) . . ?
C47 C46 C45 121.1(5) . . ?
C46 C47 C48 119.6(5) . . ?
C47 C48 C43 119.8(5) . . ?
C50 C49 C54 119.1(4) . . ?
C50 C49 P3 119.6(3) . . ?
C54 C49 P3 121.2(3) . . ?
C49 C50 C51 119.7(4) . . ?
C52 C51 C50 120.2(4) . . ?
C51 C52 C53 120.9(4) . . ?
C54 C53 C52 119.7(4) . . ?
C53 C54 C49 120.4(4) . . ?
C56 C55 C60 118.5(4) . . ?
C56 C55 P3 121.9(3) . . ?
C60 C55 P3 119.3(3) . . ?
C57 C56 C55 120.0(4) . . ?
C58 C57 C56 120.8(4) . . ?
C57 C58 C59 119.7(4) . . ?
C58 C59 C60 120.1(4) . . ?
C59 C60 C55 120.9(4) . . ?
C66 C61 C62 118.7(4) . . ?
C66 C61 P3 120.1(3) . . ?
C62 C61 P3 121.1(3) . . ?
C63 C62 C61 119.9(4) . . ?
C64 C63 C62 120.8(5) . . ?
C65 C64 C63 119.4(4) . . ?
C64 C65 C66 120.7(5) . . ?
C65 C66 C61 120.4(4) . . ?
C72 C67 C68 119.1(4) . . ?
C72 C67 P4 118.8(3) . . ?
C68 C67 P4 121.5(3) . . ?
C69 C68 C67 119.9(5) . . ?
C70 C69 C68 120.9(5) . . ?
C69 C70 C71 119.4(5) . . ?
C70 C71 C72 120.9(5) . . ?
C71 C72 C67 119.7(5) . . ?
C78 C73 C74 120.1(4) . . ?
C78 C73 P4 119.4(3) . . ?
C74 C73 P4 118.9(3) . . ?
C75 C74 C73 120.5(5) . . ?
C76 C75 C74 119.7(5) . . ?
C75 C76 C77 120.9(5) . . ?
C76 C77 C78 119.6(5) . . ?
C73 C78 C77 119.1(5) . . ?
C84 C79 C80 119.8(4) . . ?
C84 C79 P4 115.1(3) . . ?
C80 C79 P4 124.6(3) . . ?
C81 C80 C79 119.2(4) . . ?
C80 C81 C82 120.6(4) . . ?
C83 C82 C81 119.9(4) . . ?
C84 C83 C82 120.1(4) . . ?
C83 C84 C79 120.5(4) . . ?
F13 P10 F15 177.9(3) . . ?
F13 P10 F14 91.3(3) . . ?
F15 P10 F14 90.2(3) . . ?
F13 P10 F12 90.3(3) . . ?
F15 P10 F12 88.2(3) . . ?
F14 P10 F12 177.5(3) . . ?
F13 P10 F11 91.4(2) . . ?
F15 P10 F11 90.1(2) . . ?
F14 P10 F11 91.5(2) . . ?
F12 P10 F11 90.3(2) . . ?
F13 P10 F16 89.1(2) . . ?
F15 P10 F16 89.48(19) . . ?
F14 P10 F16 88.96(18) . . ?
F12 P10 F16 89.2(2) . . ?
F11 P10 F16 179.3(2) . . ?
F23 P20 F21 89.6(2) . . ?
F23 P20 F26 92.3(2) . . ?
F21 P20 F26 177.8(2) . . ?
F23 P20 F24 91.77(19) . . ?
F21 P20 F24 88.26(17) . . ?
F26 P20 F24 90.56(16) . . ?
F23 P20 F22 89.3(2) . . ?
F21 P20 F22 90.91(19) . . ?
F26 P20 F22 90.24(18) . . ?
F24 P20 F22 178.7(2) . . ?
F23 P20 F25 179.4(2) . . ?
F21 P20 F25 90.8(2) . . ?
F26 P20 F25 87.3(2) . . ?
F24 P20 F25 88.68(19) . . ?
F22 P20 F25 90.3(2) . . ?
C91 O90 C93 112.5(6) . . ?
O90 C91 C92 110.0(6) . . ?
C94 C93 O90 113.7(7) . . ?
C91' O90' C93' 119(2) . . ?
O90' C91' C92' 115.7(17) . . ?
O90' C93' C94' 116.7(17) . . ?

_refine_diff_density_max         0.927
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.098

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1565398'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C90 H78 N2 P4 Pd2 S4, 2(F6 P), C4 H10 O'
_chemical_formula_sum            'C94 H88 F12 N2 O P6 Pd2 S4'
_chemical_formula_weight         2016.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'I a'
_space_group_name_Hall           'I -2ya'

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

_cell_length_a                   33.0045(5)
_cell_length_b                   10.85381(18)
_cell_length_c                   26.7343(4)
_cell_angle_alpha                90
_cell_angle_beta                 106.5109(16)
_cell_angle_gamma                90
_cell_volume                     9182.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7869
_cell_measurement_theta_min      4.2650
_cell_measurement_theta_max      73.2840

_exptl_crystal_description       tablets
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_F_000             4112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    5.606
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_reflns_number            14026
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.449
_diffrn_reflns_theta_max         73.744
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             9980
_reflns_number_gt                9490
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.942
_reflns_Friedel_fraction_full    0.982

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0626P)²+5.7330P] 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 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.455(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9980
_refine_ls_number_parameters     1046
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0986
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.57392(2) 0.47739(4) 0.87952(2) 0.02785(10) Uani 1 1 d . . . . .
Pd2 Pd 0.73512(2) 0.75800(4) 0.62349(2) 0.03132(10) Uani 1 1 d . . . . .
P1 P 0.52699(5) 0.61066(14) 0.90281(5) 0.0291(3) Uani 1 1 d . . . . .
P2 P 0.54996(5) 0.29762(14) 0.90501(5) 0.0287(3) Uani 1 1 d . . . . .
P3 P 0.78255(5) 0.89195(17) 0.60159(6) 0.0385(4) Uani 1 1 d . . . . .
P4 P 0.76067(5) 0.57748(15) 0.59989(5) 0.0316(3) Uani 1 1 d . . . . .
S1 S 0.61774(5) 0.36923(14) 0.84099(6) 0.0339(3) Uani 1 1 d . . . . .
C2 C 0.63040(18) 0.5101(6) 0.8206(2) 0.0324(12) Uani 1 1 d . . . . .
S3 S 0.61237(5) 0.63148(15) 0.84956(6) 0.0356(3) Uani 1 1 d . . . . .
N4 N 0.65041(16) 0.5226(5) 0.78444(19) 0.0336(11) Uani 1 1 d . . . . .
C5 C 0.66236(19) 0.6446(6) 0.7694(2) 0.0336(12) Uani 1 1 d . . . . .
H5A H 0.6898 0.6388 0.7613 0.040 Uiso 1 1 calc R U . . .
H5B H 0.6657 0.7028 0.7988 0.040 Uiso 1 1 calc R U . . .
C6 C 0.62878(19) 0.6926(6) 0.7220(2) 0.0348(12) Uani 1 1 d . . . . .
H6A H 0.6218 0.6288 0.6944 0.042 Uiso 1 1 calc R U . . .
H6B H 0.6027 0.7129 0.7317 0.042 Uiso 1 1 calc R U . . .
N7 N 0.64537(17) 0.8047(5) 0.7026(2) 0.0371(11) Uani 1 1 d . . . . .
C8 C 0.67172(19) 0.7926(6) 0.6741(2) 0.0353(13) Uani 1 1 d . . . . .
S9 S 0.68591(5) 0.65240(14) 0.65405(6) 0.0330(3) Uani 1 1 d . . . . .
S10 S 0.69739(5) 0.91338(15) 0.65394(7) 0.0409(4) Uani 1 1 d . . . . .
C11 C 0.6574(2) 0.4154(6) 0.7540(2) 0.0356(12) Uani 1 1 d . . . . .
H11A H 0.6629 0.4458 0.7216 0.043 Uiso 1 1 calc R U . . .
H11B H 0.6311 0.3663 0.7436 0.043 Uiso 1 1 calc R U . . .
C12 C 0.6930(2) 0.3320(6) 0.7815(2) 0.0364(13) Uani 1 1 d . . . . .
C13 C 0.7321(3) 0.3773(8) 0.8083(4) 0.066(2) Uani 1 1 d . . . . .
H13A H 0.7362 0.4637 0.8124 0.079 Uiso 1 1 calc R U . . .
C14 C 0.7655(3) 0.2980(10) 0.8294(5) 0.078(3) Uani 1 1 d . . . . .
H14A H 0.7924 0.3303 0.8474 0.093 Uiso 1 1 calc R U . . .
C15 C 0.7596(3) 0.1710(8) 0.8243(4) 0.062(2) Uani 1 1 d . . . . .
H15A H 0.7823 0.1160 0.8389 0.074 Uiso 1 1 calc R U . . .
C16 C 0.7207(3) 0.1275(8) 0.7981(4) 0.071(3) Uani 1 1 d . . . . .
H16A H 0.7163 0.0411 0.7943 0.085 Uiso 1 1 calc R U . . .
C17 C 0.6875(3) 0.2062(7) 0.7770(3) 0.058(2) Uani 1 1 d . . . . .
H17A H 0.6605 0.1735 0.7593 0.070 Uiso 1 1 calc R U . . .
C18 C 0.6317(2) 0.9246(6) 0.7168(3) 0.0443(15) Uani 1 1 d . . . . .
H18A H 0.6483 0.9902 0.7061 0.053 Uiso 1 1 calc R U . . .
H18B H 0.6375 0.9288 0.7552 0.053 Uiso 1 1 calc R U . . .
C19 C 0.5852(3) 0.9481(6) 0.6918(3) 0.0473(16) Uani 1 1 d . . . . .
C20 C 0.5654(3) 1.0427(7) 0.7121(4) 0.057(2) Uani 1 1 d . . . . .
H20A H 0.5808 1.0888 0.7416 0.069 Uiso 1 1 calc R U . . .
C21 C 0.5230(4) 1.0677(10) 0.6882(5) 0.080(3) Uani 1 1 d . . . . .
H21A H 0.5097 1.1312 0.7023 0.096 Uiso 1 1 calc R U . . .
C22 C 0.4999(4) 1.0056(12) 0.6459(5) 0.082(3) Uani 1 1 d . . . . .
H22A H 0.4709 1.0252 0.6305 0.099 Uiso 1 1 calc R U . . .
C23 C 0.5193(3) 0.9121(10) 0.6253(4) 0.071(2) Uani 1 1 d . . . . .
H23A H 0.5037 0.8666 0.5957 0.085 Uiso 1 1 calc R U . . .
C24 C 0.5617(3) 0.8863(8) 0.6484(3) 0.0537(18) Uani 1 1 d . . . . .
H24A H 0.5749 0.8238 0.6337 0.064 Uiso 1 1 calc R U . . .
C25 C 0.5052(2) 0.7176(6) 0.8492(2) 0.0328(12) Uani 1 1 d . . . . .
C26 C 0.5047(2) 0.6845(7) 0.7986(2) 0.0427(15) Uani 1 1 d . . . . .
H26A H 0.5172 0.6093 0.7924 0.051 Uiso 1 1 calc R U . . .
C27 C 0.4857(3) 0.7625(8) 0.7572(3) 0.0535(19) Uani 1 1 d . . . . .
H27A H 0.4856 0.7406 0.7228 0.064 Uiso 1 1 calc R U . . .
C28 C 0.4672(3) 0.8706(8) 0.7658(3) 0.0523(18) Uani 1 1 d . . . . .
H28A H 0.4542 0.9229 0.7372 0.063 Uiso 1 1 calc R U . . .
C29 C 0.4674(3) 0.9033(7) 0.8154(3) 0.0499(17) Uani 1 1 d . . . . .
H29A H 0.4539 0.9771 0.8211 0.060 Uiso 1 1 calc R U . . .
C30 C 0.4873(2) 0.8284(7) 0.8575(3) 0.0457(16) Uani 1 1 d . . . . .
H30A H 0.4885 0.8533 0.8920 0.055 Uiso 1 1 calc R U . . .
C31 C 0.4788(2) 0.5514(6) 0.9152(2) 0.0355(13) Uani 1 1 d . . . . .
C32 C 0.4414(2) 0.5441(7) 0.8747(3) 0.0387(14) Uani 1 1 d . . . . .
H32A H 0.4411 0.5693 0.8406 0.046 Uiso 1 1 calc R U . . .
C33 C 0.4045(2) 0.5003(8) 0.8837(3) 0.0491(17) Uani 1 1 d . . . . .
H33A H 0.3791 0.4971 0.8558 0.059 Uiso 1 1 calc R U . . .
C34 C 0.4045(3) 0.4612(8) 0.9332(4) 0.057(2) Uani 1 1 d . . . . .
H34A H 0.3793 0.4320 0.9396 0.069 Uiso 1 1 calc R U . . .
C35 C 0.4415(3) 0.4655(7) 0.9725(3) 0.0492(17) Uani 1 1 d . . . . .
H35A H 0.4416 0.4380 1.0063 0.059 Uiso 1 1 calc R U . . .
C36 C 0.4791(2) 0.5088(7) 0.9649(3) 0.0416(14) Uani 1 1 d . . . . .
H36A H 0.5045 0.5094 0.9928 0.050 Uiso 1 1 calc R U . . .
C37 C 0.5510(2) 0.7054(6) 0.9597(2) 0.0355(13) Uani 1 1 d . . . . .
C38 C 0.5271(2) 0.7678(6) 0.9870(3) 0.0391(15) Uani 1 1 d . . . . .
H38A H 0.4973 0.7583 0.9769 0.047 Uiso 1 1 calc R U . . .
C39 C 0.5463(3) 0.8437(8) 1.0288(3) 0.0512(18) Uani 1 1 d . . . . .
H39A H 0.5296 0.8858 1.0469 0.061 Uiso 1 1 calc R U . . .
C40 C 0.5891(3) 0.8582(8) 1.0438(3) 0.0529(19) Uani 1 1 d . . . . .
H40A H 0.6020 0.9111 1.0721 0.064 Uiso 1 1 calc R U . . .
C41 C 0.6136(2) 0.7958(8) 1.0178(3) 0.0529(19) Uani 1 1 d . . . . .
H41A H 0.6435 0.8040 1.0289 0.063 Uiso 1 1 calc R U . . .
C42 C 0.5945(2) 0.7210(7) 0.9755(3) 0.0420(15) Uani 1 1 d . . . . .
H42A H 0.6114 0.6802 0.9571 0.050 Uiso 1 1 calc R U . . .
C43 C 0.4963(2) 0.2657(6) 0.8663(3) 0.0343(13) Uani 1 1 d . . . . .
C44 C 0.4887(2) 0.2810(7) 0.8124(3) 0.0425(15) Uani 1 1 d . . . . .
H44A H 0.5106 0.3099 0.7988 0.051 Uiso 1 1 calc R U . . .
C45 C 0.4498(2) 0.2543(7) 0.7792(3) 0.0437(16) Uani 1 1 d . . . . .
H45A H 0.4452 0.2613 0.7426 0.052 Uiso 1 1 calc R U . . .
C46 C 0.4171(2) 0.2174(7) 0.7984(4) 0.0506(19) Uani 1 1 d . . . . .
H46A H 0.3901 0.2008 0.7751 0.061 Uiso 1 1 calc R U . . .
C47 C 0.4237(2) 0.2046(8) 0.8516(3) 0.0510(17) Uani 1 1 d . . . . .
H47A H 0.4010 0.1804 0.8647 0.061 Uiso 1 1 calc R U . . .
C48 C 0.4636(2) 0.2272(7) 0.8862(3) 0.0422(16) Uani 1 1 d . . . . .
H48A H 0.4684 0.2165 0.9227 0.051 Uiso 1 1 calc R U . . .
C49 C 0.5549(2) 0.2924(7) 0.9746(2) 0.0355(13) Uani 1 1 d . . . . .
C50 C 0.5757(2) 0.3895(7) 1.0060(2) 0.0395(14) Uani 1 1 d . . . . .
H50A H 0.5868 0.4562 0.9911 0.047 Uiso 1 1 calc R U . . .
C51 C 0.5800(3) 0.3876(8) 1.0589(3) 0.0509(19) Uani 1 1 d . . . . .
H51A H 0.5942 0.4529 1.0805 0.061 Uiso 1 1 calc R U . . .
C52 C 0.5637(3) 0.2908(10) 1.0803(3) 0.061(2) Uani 1 1 d . . . . .
H52A H 0.5655 0.2914 1.1164 0.073 Uiso 1 1 calc R U . . .
C53 C 0.5449(3) 0.1941(10) 1.0500(3) 0.063(2) Uani 1 1 d . . . . .
H53A H 0.5345 0.1271 1.0655 0.075 Uiso 1 1 calc R U . . .
C54 C 0.5407(3) 0.1917(8) 0.9964(3) 0.0494(17) Uani 1 1 d . . . . .
H54A H 0.5283 0.1229 0.9757 0.059 Uiso 1 1 calc R U . . .
C55 C 0.58010(19) 0.1620(6) 0.8965(2) 0.0325(12) Uani 1 1 d . . . . .
C56 C 0.6219(2) 0.1514(6) 0.9286(3) 0.0396(14) Uani 1 1 d . . . . .
H56A H 0.6334 0.2126 0.9541 0.048 Uiso 1 1 calc R U . . .
C57 C 0.6461(2) 0.0527(7) 0.9229(3) 0.0476(16) Uani 1 1 d . . . . .
H57A H 0.6743 0.0462 0.9445 0.057 Uiso 1 1 calc R U . . .
C58 C 0.6301(3) -0.0377(7) 0.8862(3) 0.0476(17) Uani 1 1 d . . . . .
H58A H 0.6472 -0.1057 0.8826 0.057 Uiso 1 1 calc R U . . .
C59 C 0.5884(3) -0.0277(7) 0.8544(4) 0.0537(19) Uani 1 1 d . . . . .
H59A H 0.5769 -0.0892 0.8291 0.064 Uiso 1 1 calc R U . . .
C60 C 0.5642(2) 0.0714(7) 0.8600(3) 0.0414(14) Uani 1 1 d . . . . .
H60A H 0.5360 0.0777 0.8384 0.050 Uiso 1 1 calc R U . . .
C61 C 0.8033(2) 0.9984(7) 0.6560(3) 0.0445(17) Uani 1 1 d . . . . .
C62 C 0.8076(2) 0.9589(7) 0.7062(3) 0.0467(16) Uani 1 1 d . . . . .
H62A H 0.7969 0.8801 0.7115 0.056 Uiso 1 1 calc R U . . .
C63 C 0.8271(3) 1.0312(8) 0.7494(4) 0.058(2) Uani 1 1 d . . . . .
H63A H 0.8293 1.0039 0.7839 0.070 Uiso 1 1 calc R U . . .
C64 C 0.8433(3) 1.1458(9) 0.7402(4) 0.068(2) Uani 1 1 d . . . . .
H64A H 0.8579 1.1958 0.7688 0.082 Uiso 1 1 calc R U . . .
C65 C 0.8381(3) 1.1856(9) 0.6907(5) 0.072(3) Uani 1 1 d . . . . .
H65A H 0.8479 1.2656 0.6854 0.087 Uiso 1 1 calc R U . . .
C66 C 0.8192(3) 1.1143(9) 0.6478(4) 0.065(2) Uani 1 1 d . . . . .
H66A H 0.8170 1.1427 0.6135 0.078 Uiso 1 1 calc R U . . .
C67 C 0.7572(3) 0.9866(8) 0.5445(3) 0.0464(18) Uani 1 1 d . . . . .
C68 C 0.7137(2) 0.9898(7) 0.5259(3) 0.0485(17) Uani 1 1 d . . . . .
H68A H 0.6972 0.9459 0.5438 0.058 Uiso 1 1 calc R U . . .
C69 C 0.6938(3) 1.0560(9) 0.4814(4) 0.063(2) Uani 1 1 d . . . . .
H69A H 0.6638 1.0596 0.4694 0.075 Uiso 1 1 calc R U . . .
C70 C 0.7182(3) 1.1173(9) 0.4544(4) 0.066(2) Uani 1 1 d . . . . .
H70A H 0.7049 1.1607 0.4233 0.079 Uiso 1 1 calc R U . . .
C71 C 0.7617(3) 1.1153(10) 0.4727(4) 0.074(3) Uani 1 1 d . . . . .
H71A H 0.7781 1.1601 0.4549 0.089 Uiso 1 1 calc R U . . .
C72 C 0.7816(3) 1.0481(9) 0.5172(4) 0.064(3) Uani 1 1 d . . . . .
H72A H 0.8115 1.0438 0.5289 0.077 Uiso 1 1 calc R U . . .
C73 C 0.8307(2) 0.8330(7) 0.5885(3) 0.0416(15) Uani 1 1 d . . . . .
C74 C 0.8682(2) 0.8221(7) 0.6292(3) 0.0483(17) Uani 1 1 d . . . . .
H74A H 0.8688 0.8461 0.6636 0.058 Uiso 1 1 calc R U . . .
C75 C 0.9046(2) 0.7761(8) 0.6194(4) 0.058(2) Uani 1 1 d . . . . .
H75A H 0.9300 0.7690 0.6470 0.069 Uiso 1 1 calc R U . . .
C76 C 0.9037(3) 0.7406(9) 0.5691(4) 0.058(2) Uani 1 1 d . . . . .
H76A H 0.9284 0.7079 0.5627 0.070 Uiso 1 1 calc R U . . .
C77 C 0.8668(3) 0.7524(9) 0.5281(4) 0.061(2) Uani 1 1 d . . . . .
H77A H 0.8664 0.7304 0.4935 0.073 Uiso 1 1 calc R U . . .
C78 C 0.8308(2) 0.7968(8) 0.5387(3) 0.0505(18) Uani 1 1 d . . . . .
H78A H 0.8054 0.8028 0.5110 0.061 Uiso 1 1 calc R U . . .
C79 C 0.8150(2) 0.5485(7) 0.6390(3) 0.0359(13) Uani 1 1 d . . . . .
C80 C 0.8224(2) 0.5683(7) 0.6927(3) 0.0423(15) Uani 1 1 d . . . . .
H80A H 0.8007 0.5986 0.7063 0.051 Uiso 1 1 calc R U . . .
C81 C 0.8627(2) 0.5421(7) 0.7256(3) 0.0478(18) Uani 1 1 d . . . . .
H81A H 0.8682 0.5537 0.7622 0.057 Uiso 1 1 calc R U . . .
C82 C 0.8943(2) 0.5000(7) 0.7061(3) 0.0491(18) Uani 1 1 d . . . . .
H82A H 0.9213 0.4811 0.7290 0.059 Uiso 1 1 calc R U . . .
C83 C 0.8866(2) 0.4850(7) 0.6528(3) 0.0473(16) Uani 1 1 d . . . . .
H83A H 0.9088 0.4585 0.6391 0.057 Uiso 1 1 calc R U . . .
C84 C 0.8471(2) 0.5085(7) 0.6195(3) 0.0398(15) Uani 1 1 d . . . . .
H84A H 0.8419 0.4969 0.5830 0.048 Uiso 1 1 calc R U . . .
C85 C 0.7562(2) 0.5667(7) 0.5308(2) 0.0391(14) Uani 1 1 d . . . . .
C86 C 0.7377(2) 0.6643(7) 0.4986(3) 0.0448(16) Uani 1 1 d . . . . .
H86A H 0.7271 0.7333 0.5129 0.054 Uiso 1 1 calc R U . . .
C87 C 0.7346(3) 0.6611(9) 0.4457(3) 0.057(2) Uani 1 1 d . . . . .
H87A H 0.7222 0.7280 0.4238 0.068 Uiso 1 1 calc R U . . .
C88 C 0.7498(3) 0.5599(9) 0.4249(3) 0.063(2) Uani 1 1 d . . . . .
H88A H 0.7484 0.5579 0.3889 0.075 Uiso 1 1 calc R U . . .
C89 C 0.7669(3) 0.4627(9) 0.4567(3) 0.061(2) Uani 1 1 d . . . . .
H89A H 0.7769 0.3931 0.4423 0.073 Uiso 1 1 calc R U . . .
C90 C 0.7697(3) 0.4643(8) 0.5095(3) 0.0490(18) Uani 1 1 d . . . . .
H90A H 0.7809 0.3953 0.5309 0.059 Uiso 1 1 calc R U . . .
C91 C 0.7306(2) 0.4429(6) 0.6104(2) 0.0336(12) Uani 1 1 d . . . . .
C92 C 0.7447(2) 0.3659(7) 0.6528(3) 0.0485(17) Uani 1 1 d . . . . .
H92A H 0.7712 0.3807 0.6777 0.058 Uiso 1 1 calc R U . . .
C93 C 0.7199(3) 0.2665(8) 0.6592(4) 0.056(2) Uani 1 1 d . . . . .
H93A H 0.7301 0.2124 0.6880 0.067 Uiso 1 1 calc R U . . .
C94 C 0.6812(3) 0.2455(8) 0.6245(4) 0.055(2) Uani 1 1 d . . . . .
H94A H 0.6644 0.1779 0.6292 0.066 Uiso 1 1 calc R U . . .
C95 C 0.6668(2) 0.3254(7) 0.5823(3) 0.0504(17) Uani 1 1 d . . . . .
H95A H 0.6398 0.3126 0.5582 0.060 Uiso 1 1 calc R U . . .
C96 C 0.6913(2) 0.4225(7) 0.5751(3) 0.0419(15) Uani 1 1 d . . . . .
H96A H 0.6814 0.4757 0.5460 0.050 Uiso 1 1 calc R U . . .
P10 P 0.78969(6) 0.7225(2) 0.82752(8) 0.0448(4) Uani 1 1 d . . . . .
F11 F 0.7720(3) 0.8551(6) 0.8165(3) 0.096(2) Uani 1 1 d . . . . .
F12 F 0.75190(15) 0.6873(5) 0.85134(19) 0.0628(12) Uani 1 1 d . . . . .
F13 F 0.8173(2) 0.7615(7) 0.8840(2) 0.089(2) Uani 1 1 d . . . . .
F14 F 0.82692(17) 0.7539(6) 0.8027(3) 0.0752(16) Uani 1 1 d . . . . .
F15 F 0.76244(15) 0.6762(7) 0.77235(19) 0.0801(19) Uani 1 1 d . . . . .
F16 F 0.80780(19) 0.5856(6) 0.8397(3) 0.094(2) Uani 1 1 d . . . . .
P20 P 0.52247(6) 0.47146(18) 0.67529(7) 0.0418(4) Uani 1 1 d . . . . .
F21 F 0.4932(3) 0.5866(8) 0.6584(4) 0.142(4) Uani 1 1 d . . . . .
F22 F 0.4918(2) 0.4313(10) 0.7076(3) 0.115(3) Uani 1 1 d . . . . .
F23 F 0.55118(16) 0.5406(6) 0.72481(19) 0.0728(16) Uani 1 1 d . . . . .
F24 F 0.5529(3) 0.5131(9) 0.6428(3) 0.124(4) Uani 1 1 d . . . . .
F25 F 0.49452(19) 0.3987(8) 0.6272(3) 0.104(3) Uani 1 1 d . . . . .
F26 F 0.5507(3) 0.3565(8) 0.6913(5) 0.144(4) 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
Pd1 P2 2.2811(15) . ?
Pd1 S1 2.3190(15) . ?
Pd1 P1 2.3297(15) . ?
Pd1 S3 2.3720(16) . ?
Pd2 P4 2.2915(17) . ?
Pd2 S9 2.3180(15) . ?
Pd2 P3 2.3298(16) . ?
Pd2 S10 2.3735(17) . ?
P1 C37 1.820(7) . ?
P1 C25 1.826(7) . ?
P1 C31 1.832(7) . ?
P2 C43 1.814(6) . ?
P2 C49 1.820(6) . ?
P2 C55 1.826(7) . ?
P3 C61 1.832(9) . ?
P3 C67 1.832(7) . ?
P3 C73 1.837(7) . ?
P4 C85 1.815(7) . ?
P4 C79 1.829(7) . ?
P4 C91 1.833(6) . ?
S1 C2 1.715(7) . ?
C2 N4 1.323(8) . ?
C2 S3 1.718(6) . ?
N4 C5 1.470(8) . ?
N4 C11 1.475(8) . ?
C5 C6 1.518(8) . ?
C6 N7 1.487(8) . ?
N7 C8 1.316(9) . ?
N7 C18 1.463(9) . ?
C8 S9 1.722(7) . ?
C8 S10 1.727(7) . ?
C11 C12 1.500(9) . ?
C12 C13 1.376(11) . ?
C12 C17 1.378(10) . ?
C13 C14 1.385(12) . ?
C14 C15 1.393(14) . ?
C15 C16 1.363(14) . ?
C16 C17 1.377(13) . ?
C18 C19 1.510(11) . ?
C19 C24 1.374(12) . ?
C19 C20 1.406(11) . ?
C20 C21 1.390(15) . ?
C21 C22 1.352(18) . ?
C22 C23 1.395(16) . ?
C23 C24 1.389(12) . ?
C25 C30 1.387(10) . ?
C25 C26 1.396(9) . ?
C26 C27 1.392(10) . ?
C27 C28 1.372(12) . ?
C28 C29 1.373(12) . ?
C29 C30 1.391(10) . ?
C31 C32 1.392(9) . ?
C31 C36 1.404(9) . ?
C32 C33 1.390(10) . ?
C33 C34 1.390(13) . ?
C34 C35 1.368(13) . ?
C35 C36 1.396(11) . ?
C37 C42 1.387(10) . ?
C37 C38 1.393(10) . ?
C38 C39 1.387(10) . ?
C39 C40 1.361(12) . ?
C40 C41 1.385(12) . ?
C41 C42 1.390(10) . ?
C43 C48 1.396(10) . ?
C43 C44 1.400(10) . ?
C44 C45 1.370(10) . ?
C45 C46 1.379(12) . ?
C46 C47 1.382(13) . ?
C47 C48 1.400(11) . ?
C49 C54 1.384(11) . ?
C49 C50 1.400(10) . ?
C50 C51 1.380(9) . ?
C51 C52 1.377(14) . ?
C52 C53 1.362(15) . ?
C53 C54 1.399(11) . ?
C55 C60 1.380(9) . ?
C55 C56 1.407(9) . ?
C56 C57 1.370(10) . ?
C57 C58 1.381(11) . ?
C58 C59 1.402(12) . ?
C59 C60 1.373(11) . ?
C61 C62 1.375(11) . ?
C61 C66 1.404(11) . ?
C62 C63 1.395(11) . ?
C63 C64 1.402(14) . ?
C64 C65 1.358(16) . ?
C65 C66 1.377(14) . ?
C67 C68 1.379(11) . ?
C67 C72 1.401(11) . ?
C68 C69 1.386(11) . ?
C69 C70 1.394(14) . ?
C70 C71 1.376(15) . ?
C71 C72 1.391(12) . ?
C73 C78 1.391(11) . ?
C73 C74 1.400(9) . ?
C74 C75 1.393(13) . ?
C75 C76 1.391(14) . ?
C76 C77 1.394(12) . ?
C77 C78 1.384(13) . ?
C79 C84 1.376(11) . ?
C79 C80 1.402(10) . ?
C80 C81 1.399(10) . ?
C81 C82 1.371(13) . ?
C82 C83 1.384(12) . ?
C83 C84 1.379(10) . ?
C85 C90 1.379(11) . ?
C85 C86 1.391(10) . ?
C86 C87 1.391(10) . ?
C87 C88 1.387(15) . ?
C88 C89 1.371(14) . ?
C89 C90 1.390(11) . ?
C91 C92 1.379(9) . ?
C91 C96 1.387(9) . ?
C92 C93 1.393(11) . ?
C93 C94 1.368(12) . ?
C94 C95 1.397(11) . ?
C95 C96 1.375(10) . ?
P10 F11 1.550(6) . ?
P10 F15 1.576(5) . ?
P10 F13 1.584(6) . ?
P10 F14 1.590(6) . ?
P10 F12 1.600(5) . ?
P10 F16 1.600(7) . ?
P20 F26 1.543(8) . ?
P20 F21 1.565(8) . ?
P20 F25 1.565(5) . ?
P20 F22 1.568(6) . ?
P20 F24 1.571(6) . ?
P20 F23 1.581(5) . ?

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
P2 Pd1 S1 90.72(5) . . ?
P2 Pd1 P1 97.93(6) . . ?
S1 Pd1 P1 168.24(5) . . ?
P2 Pd1 S3 165.50(6) . . ?
S1 Pd1 S3 75.28(5) . . ?
P1 Pd1 S3 96.47(5) . . ?
P4 Pd2 S9 91.36(5) . . ?
P4 Pd2 P3 97.95(6) . . ?
S9 Pd2 P3 170.15(6) . . ?
P4 Pd2 S10 166.41(6) . . ?
S9 Pd2 S10 75.05(5) . . ?
P3 Pd2 S10 95.64(6) . . ?
C37 P1 C25 106.1(3) . . ?
C37 P1 C31 104.0(3) . . ?
C25 P1 C31 101.3(3) . . ?
C37 P1 Pd1 114.2(2) . . ?
C25 P1 Pd1 109.1(2) . . ?
C31 P1 Pd1 120.5(2) . . ?
C43 P2 C49 111.5(3) . . ?
C43 P2 C55 104.7(3) . . ?
C49 P2 C55 102.0(3) . . ?
C43 P2 Pd1 111.0(2) . . ?
C49 P2 Pd1 113.2(2) . . ?
C55 P2 Pd1 113.9(2) . . ?
C61 P3 C67 106.7(4) . . ?
C61 P3 C73 102.8(4) . . ?
C67 P3 C73 104.7(4) . . ?
C61 P3 Pd2 108.7(3) . . ?
C67 P3 Pd2 112.2(3) . . ?
C73 P3 Pd2 120.7(2) . . ?
C85 P4 C79 110.7(3) . . ?
C85 P4 C91 102.3(3) . . ?
C79 P4 C91 105.2(3) . . ?
C85 P4 Pd2 113.9(3) . . ?
C79 P4 Pd2 111.6(2) . . ?
C91 P4 Pd2 112.4(2) . . ?
C2 S1 Pd1 85.9(2) . . ?
N4 C2 S1 122.7(5) . . ?
N4 C2 S3 124.0(5) . . ?
S1 C2 S3 113.2(4) . . ?
C2 S3 Pd1 84.2(2) . . ?
C2 N4 C5 121.4(5) . . ?
C2 N4 C11 120.7(5) . . ?
C5 N4 C11 117.6(5) . . ?
N4 C5 C6 110.4(5) . . ?
N7 C6 C5 108.5(5) . . ?
C8 N7 C18 122.9(6) . . ?
C8 N7 C6 119.4(6) . . ?
C18 N7 C6 117.7(5) . . ?
N7 C8 S9 123.4(5) . . ?
N7 C8 S10 124.7(5) . . ?
S9 C8 S10 111.9(4) . . ?
C8 S9 Pd2 87.3(2) . . ?
C8 S10 Pd2 85.4(2) . . ?
N4 C11 C12 115.4(5) . . ?
C13 C12 C17 118.7(7) . . ?
C13 C12 C11 121.8(6) . . ?
C17 C12 C11 119.3(6) . . ?
C12 C13 C14 120.6(8) . . ?
C13 C14 C15 120.3(9) . . ?
C16 C15 C14 118.5(8) . . ?
C15 C16 C17 121.4(8) . . ?
C16 C17 C12 120.6(8) . . ?
N7 C18 C19 112.7(6) . . ?
C24 C19 C20 118.0(8) . . ?
C24 C19 C18 123.4(7) . . ?
C20 C19 C18 118.5(8) . . ?
C21 C20 C19 118.9(10) . . ?
C22 C21 C20 122.9(9) . . ?
C21 C22 C23 118.7(10) . . ?
C24 C23 C22 119.3(10) . . ?
C19 C24 C23 122.2(8) . . ?
C30 C25 C26 119.4(6) . . ?
C30 C25 P1 121.1(5) . . ?
C26 C25 P1 119.4(5) . . ?
C27 C26 C25 119.5(7) . . ?
C28 C27 C26 120.6(7) . . ?
C27 C28 C29 120.2(7) . . ?
C28 C29 C30 120.2(7) . . ?
C25 C30 C29 120.1(7) . . ?
C32 C31 C36 118.9(6) . . ?
C32 C31 P1 120.3(5) . . ?
C36 C31 P1 120.8(5) . . ?
C33 C32 C31 120.8(7) . . ?
C32 C33 C34 120.4(7) . . ?
C35 C34 C33 118.7(7) . . ?
C34 C35 C36 122.4(7) . . ?
C35 C36 C31 118.8(7) . . ?
C42 C37 C38 118.1(6) . . ?
C42 C37 P1 119.4(5) . . ?
C38 C37 P1 122.4(5) . . ?
C39 C38 C37 121.0(7) . . ?
C40 C39 C38 120.2(7) . . ?
C39 C40 C41 120.0(7) . . ?
C40 C41 C42 120.0(7) . . ?
C37 C42 C41 120.6(7) . . ?
C48 C43 C44 119.9(6) . . ?
C48 C43 P2 125.0(6) . . ?
C44 C43 P2 115.1(5) . . ?
C45 C44 C43 120.1(7) . . ?
C44 C45 C46 120.5(7) . . ?
C45 C46 C47 120.2(7) . . ?
C46 C47 C48 120.4(7) . . ?
C43 C48 C47 118.9(8) . . ?
C54 C49 C50 120.5(6) . . ?
C54 C49 P2 120.9(6) . . ?
C50 C49 P2 118.5(5) . . ?
C51 C50 C49 119.7(7) . . ?
C52 C51 C50 119.8(8) . . ?
C53 C52 C51 120.5(7) . . ?
C52 C53 C54 121.3(8) . . ?
C49 C54 C53 118.1(8) . . ?
C60 C55 C56 118.8(6) . . ?
C60 C55 P2 123.5(5) . . ?
C56 C55 P2 117.7(5) . . ?
C57 C56 C55 119.8(6) . . ?
C56 C57 C58 121.3(7) . . ?
C57 C58 C59 119.0(7) . . ?
C60 C59 C58 119.7(7) . . ?
C59 C60 C55 121.3(7) . . ?
C62 C61 C66 119.6(8) . . ?
C62 C61 P3 119.3(6) . . ?
C66 C61 P3 120.8(7) . . ?
C61 C62 C63 121.8(8) . . ?
C62 C63 C64 117.6(9) . . ?
C65 C64 C63 120.3(8) . . ?
C64 C65 C66 122.4(9) . . ?
C65 C66 C61 118.3(9) . . ?
C68 C67 C72 119.5(7) . . ?
C68 C67 P3 119.8(6) . . ?
C72 C67 P3 120.4(6) . . ?
C67 C68 C69 121.0(8) . . ?
C68 C69 C70 119.2(8) . . ?
C71 C70 C69 120.5(8) . . ?
C70 C71 C72 120.2(9) . . ?
C71 C72 C67 119.6(9) . . ?
C78 C73 C74 118.6(7) . . ?
C78 C73 P3 121.2(5) . . ?
C74 C73 P3 120.2(6) . . ?
C75 C74 C73 120.2(8) . . ?
C76 C75 C74 119.9(7) . . ?
C75 C76 C77 120.7(8) . . ?
C78 C77 C76 118.6(9) . . ?
C77 C78 C73 122.0(7) . . ?
C84 C79 C80 120.5(6) . . ?
C84 C79 P4 124.9(5) . . ?
C80 C79 P4 114.6(5) . . ?
C81 C80 C79 118.1(7) . . ?
C82 C81 C80 121.1(7) . . ?
C81 C82 C83 119.7(7) . . ?
C84 C83 C82 120.3(7) . . ?
C79 C84 C83 120.1(7) . . ?
C90 C85 C86 119.8(7) . . ?
C90 C85 P4 121.9(6) . . ?
C86 C85 P4 118.3(6) . . ?
C87 C86 C85 120.1(8) . . ?
C88 C87 C86 119.8(8) . . ?
C89 C88 C87 119.5(7) . . ?
C88 C89 C90 121.2(9) . . ?
C85 C90 C89 119.5(8) . . ?
C92 C91 C96 119.7(6) . . ?
C92 C91 P4 122.5(5) . . ?
C96 C91 P4 117.7(5) . . ?
C91 C92 C93 119.8(7) . . ?
C94 C93 C92 120.9(7) . . ?
C93 C94 C95 118.9(7) . . ?
C96 C95 C94 120.7(7) . . ?
C95 C96 C91 120.1(6) . . ?
F11 P10 F15 92.0(4) . . ?
F11 P10 F13 90.9(4) . . ?
F15 P10 F13 176.9(4) . . ?
F11 P10 F14 90.9(4) . . ?
F15 P10 F14 88.9(3) . . ?
F13 P10 F14 92.1(4) . . ?
F11 P10 F12 90.2(4) . . ?
F15 P10 F12 89.7(3) . . ?
F13 P10 F12 89.2(3) . . ?
F14 P10 F12 178.3(3) . . ?
F11 P10 F16 179.2(4) . . ?
F15 P10 F16 88.5(4) . . ?
F13 P10 F16 88.5(4) . . ?
F14 P10 F16 89.7(4) . . ?
F12 P10 F16 89.2(3) . . ?
F26 P20 F21 179.0(6) . . ?
F26 P20 F25 89.3(5) . . ?
F21 P20 F25 89.7(5) . . ?
F26 P20 F22 93.2(6) . . ?
F21 P20 F22 86.5(6) . . ?
F25 P20 F22 89.4(4) . . ?
F26 P20 F24 87.5(6) . . ?
F21 P20 F24 92.8(6) . . ?
F25 P20 F24 90.7(3) . . ?
F22 P20 F24 179.4(6) . . ?
F26 P20 F23 88.9(4) . . ?
F21 P20 F23 92.1(4) . . ?
F25 P20 F23 178.0(5) . . ?
F22 P20 F23 89.9(3) . . ?
F24 P20 F23 90.1(3) . . ?

_refine_diff_density_max         1.293
_refine_diff_density_min         -1.033
_refine_diff_density_rms         0.075


