# Electronic Supplementary Material (ESI) for ChemComm.
# 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_HexAz
_database_code_depnum_ccdc_archive 'CCDC 1577493'
_audit_update_record             
;
2017-10-01 deposited with the CCDC.
2017-12-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H46 N4 S2'
_chemical_formula_sum            'C68 H46 N4 S2'
_chemical_formula_weight         983.21

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'

_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                   13.296(3)
_cell_length_b                   13.957(3)
_cell_length_c                   17.986(4)
_cell_angle_alpha                87.92(5)
_cell_angle_beta                 79.12(4)
_cell_angle_gamma                75.01(3)
_cell_volume                     3165.9(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    168(120)
_cell_measurement_reflns_used    3888
_cell_measurement_theta_min      2.8584
_cell_measurement_theta_max      28.1034

_exptl_crystal_description       parallelepipped
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_F_000             1028
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.123
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      168(120)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19968
_diffrn_reflns_av_unetI/netI     0.1598
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.865
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             10727
_reflns_number_gt                5865
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0658P)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         10727
_refine_ls_number_parameters     671
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0722
_refine_ls_wR_factor_ref         0.1902
_refine_ls_wR_factor_gt          0.1672
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.19025(8) -0.16722(7) 0.03448(5) 0.0239(3) Uani 1 1 d . . . . .
N1 N 0.3498(2) -0.2897(2) -0.07087(15) 0.0208(7) Uani 1 1 d . . . . .
C1 C 0.4374(3) -0.3112(3) -0.12391(18) 0.0232(9) Uani 1 1 d . . . . .
C3 C 0.4245(3) -0.4558(3) -0.06960(19) 0.0239(9) Uani 1 1 d . . . . .
H3 H 0.4363 -0.5221 -0.0559 0.029 Uiso 1 1 calc R U . . .
N3 N 0.3507(3) 0.1643(2) -0.19912(15) 0.0247(8) Uani 1 1 d . . . . .
S2 S 0.49169(8) 0.04596(6) -0.30963(5) 0.0228(3) Uani 1 1 d . . . . .
N2 N 0.1491(2) 0.0356(2) 0.00585(15) 0.0211(7) Uani 1 1 d . . . . .
C2 C 0.4860(3) -0.4171(3) -0.12594(19) 0.0261(9) Uani 1 1 d . . . . .
H2 H 0.5464 -0.4515 -0.1587 0.031 Uiso 1 1 calc R U . . .
N4 N 0.5487(2) -0.1520(2) -0.27283(15) 0.0242(8) Uani 1 1 d . . . . .
C4 C 0.3389(3) -0.3763(3) -0.03542(18) 0.0202(8) Uani 1 1 d . . . . .
C6 C 0.1797(3) -0.2874(3) 0.05570(18) 0.0229(9) Uani 1 1 d . . . . .
C5 C 0.2573(3) -0.3765(3) 0.02507(18) 0.0217(9) Uani 1 1 d . . . . .
C5C C 0.2546(3) -0.6452(3) 0.0591(2) 0.0265(9) Uani 1 1 d . . . . .
H5C H 0.2624 -0.7019 0.0307 0.032 Uiso 1 1 calc R U . . .
C15 C 0.2609(3) 0.1124(2) -0.08245(18) 0.0211(9) Uani 1 1 d . . . . .
C19 C 0.3404(3) 0.2479(2) -0.24164(19) 0.0241(9) Uani 1 1 d . . . . .
C10E C -0.2321(3) 0.1323(3) 0.22543(18) 0.0229(9) Uani 1 1 d . . . . .
H10E H -0.2913 0.1816 0.2179 0.027 Uiso 1 1 calc R U . . .
C24 C 0.5886(3) -0.0080(3) -0.38683(18) 0.0214(9) Uani 1 1 d . . . . .
C23 C 0.6162(3) 0.0676(3) -0.43580(19) 0.0254(9) Uani 1 1 d . . . . .
H23 H 0.6687 0.0544 -0.4790 0.030 Uiso 1 1 calc R U . . .
C22 C 0.5582(3) 0.1614(3) -0.41318(18) 0.0243(9) Uani 1 1 d . . . . .
H22 H 0.5673 0.2179 -0.4399 0.029 Uiso 1 1 calc R U . . .
C21 C 0.4828(3) 0.1648(3) -0.34513(19) 0.0260(9) Uani 1 1 d . . . . .
C10F C -0.1527(3) 0.0949(3) 0.16454(19) 0.0246(9) Uani 1 1 d . . . . .
H10F H -0.1599 0.1192 0.1165 0.030 Uiso 1 1 calc R U . . .
C32 C 0.4349(3) -0.1368(3) -0.12054(18) 0.0212(9) Uani 1 1 d . . . . .
C31 C 0.3862(3) -0.0451(3) -0.14574(19) 0.0223(9) Uani 1 1 d . . . . .
H31 H 0.3853 -0.0289 -0.1963 0.027 Uiso 1 1 calc R U . . .
C30 C 0.4718(3) -0.2303(3) -0.16298(18) 0.0206(8) Uani 1 1 d . . . . .
C29 C 0.5269(3) -0.2345(2) -0.23822(19) 0.0196(8) Uani 1 1 d . . . . .
C28 C 0.5677(3) -0.3189(3) -0.29099(19) 0.0250(9) Uani 1 1 d . . . . .
H28 H 0.5616 -0.3833 -0.2815 0.030 Uiso 1 1 calc R U . . .
C27 C 0.6151(3) -0.2861(3) -0.35538(19) 0.0272(9) Uani 1 1 d . . . . .
H27 H 0.6502 -0.3234 -0.3988 0.033 Uiso 1 1 calc R U . . .
C26 C 0.6007(3) -0.1798(3) -0.34377(18) 0.0211(9) Uani 1 1 d . . . . .
C25 C 0.6296(3) -0.1108(3) -0.39810(18) 0.0209(8) Uani 1 1 d . . . . .
C25C C 0.7544(3) -0.1549(3) -0.60603(19) 0.0254(9) Uani 1 1 d . . . . .
H25C H 0.7389 -0.1321 -0.6528 0.030 Uiso 1 1 calc R U . . .
C14 C 0.1691(3) 0.1205(3) -0.02251(19) 0.0208(8) Uani 1 1 d . . . . .
C10D C -0.2242(3) 0.0966(3) 0.29805(19) 0.0242(9) Uani 1 1 d . . . . .
C38 C 0.3547(3) 0.0143(3) 0.05360(19) 0.0269(9) Uani 1 1 d . . . . .
H38 H 0.3164 0.0804 0.0572 0.032 Uiso 1 1 calc R U . . .
C37 C 0.3857(3) -0.0256(3) 0.1195(2) 0.0303(10) Uani 1 1 d . . . . .
H37 H 0.3653 0.0170 0.1613 0.036 Uiso 1 1 calc R U . . .
C36 C 0.4437(3) -0.1214(3) 0.1314(2) 0.0327(10) Uani 1 1 d . . . . .
H36 H 0.4522 -0.1356 0.1811 0.039 Uiso 1 1 calc R U . . .
C35 C 0.4908(3) -0.1988(3) 0.0795(2) 0.0299(10) Uani 1 1 d . . . . .
H35 H 0.5308 -0.2561 0.0984 0.036 Uiso 1 1 calc R U . . .
C34 C 0.4858(3) -0.2020(3) 0.00276(19) 0.0240(9) Uani 1 1 d . . . . .
H34 H 0.5233 -0.2610 -0.0226 0.029 Uiso 1 1 calc R U . . .
C33 C 0.4329(3) -0.1294(3) -0.04077(18) 0.0211(9) Uani 1 1 d . . . . .
C13 C 0.0915(3) 0.2057(3) 0.01787(19) 0.0242(9) Uani 1 1 d . . . . .
H13 H 0.0858 0.2724 0.0073 0.029 Uiso 1 1 calc R U . . .
C39 C 0.3722(3) -0.0298(3) -0.01743(18) 0.0207(9) Uani 1 1 d . . . . .
C11 C 0.0639(3) 0.0624(3) 0.06466(18) 0.0201(8) Uani 1 1 d . . . . .
C16 C 0.2701(3) 0.1843(3) -0.13888(19) 0.0229(9) Uani 1 1 d . . . . .
C10G C -0.3139(3) 0.1337(3) 0.36325(19) 0.0291(10) Uani 1 1 d . . . . .
H10A H -0.2859 0.1461 0.4063 0.044 Uiso 1 1 calc R U . . .
H10B H -0.3531 0.0847 0.3757 0.044 Uiso 1 1 calc R U . . .
H10C H -0.3598 0.1940 0.3493 0.044 Uiso 1 1 calc R U . . .
C25F C 0.7998(3) -0.2183(3) -0.4666(2) 0.0318(10) Uani 1 1 d . . . . .
H25F H 0.8166 -0.2396 -0.4198 0.038 Uiso 1 1 calc R U . . .
C17 C 0.2046(3) 0.2853(3) -0.1427(2) 0.0267(9) Uani 1 1 d . . . . .
H17 H 0.1437 0.3158 -0.1086 0.032 Uiso 1 1 calc R U . . .
C20 C 0.4094(3) 0.2511(3) -0.31114(19) 0.0255(9) Uani 1 1 d . . . . .
C20C C 0.3991(4) 0.5197(3) -0.3553(2) 0.0346(11) Uani 1 1 d . . . . .
H20C H 0.4076 0.5742 -0.3312 0.042 Uiso 1 1 calc R U . . .
C10A C -0.0632(3) 0.0227(3) 0.17299(19) 0.0237(9) Uani 1 1 d . . . . .
C20B C 0.4107(3) 0.4300(3) -0.3185(2) 0.0284(10) Uani 1 1 d . . . . .
H20B H 0.4264 0.4257 -0.2700 0.034 Uiso 1 1 calc R U . . .
C10 C 0.0273(3) -0.0104(3) 0.10837(18) 0.0207(9) Uani 1 1 d . . . . .
C10C C -0.1351(3) 0.0242(3) 0.30698(19) 0.0261(10) Uani 1 1 d . . . . .
H10D H -0.1285 -0.0007 0.3550 0.031 Uiso 1 1 calc R U . . .
C7 C 0.0837(3) -0.2844(3) 0.10678(19) 0.0239(9) Uani 1 1 d . . . . .
H7 H 0.0622 -0.3409 0.1242 0.029 Uiso 1 1 calc R U . . .
C25A C 0.7050(3) -0.1503(3) -0.46921(19) 0.0246(9) Uani 1 1 d . . . . .
C25E C 0.8705(3) -0.2556(3) -0.5318(2) 0.0316(10) Uani 1 1 d . . . . .
H25E H 0.9337 -0.3021 -0.5284 0.038 Uiso 1 1 calc R U . . .
C10B C -0.0549(3) -0.0125(3) 0.24591(19) 0.0249(9) Uani 1 1 d . . . . .
H10G H 0.0049 -0.0611 0.2535 0.030 Uiso 1 1 calc R U . . .
C5F C 0.2333(3) -0.4777(3) 0.14172(19) 0.0264(9) Uani 1 1 d . . . . .
H5F H 0.2261 -0.4214 0.1704 0.032 Uiso 1 1 calc R U . . .
C25D C 0.8481(3) -0.2244(3) -0.6024(2) 0.0296(10) Uani 1 1 d . . . . .
C18 C 0.2502(3) 0.3259(3) -0.20585(19) 0.0263(9) Uani 1 1 d . . . . .
H18 H 0.2282 0.3904 -0.2227 0.032 Uiso 1 1 calc R U . . .
C25B C 0.6829(3) -0.1187(3) -0.54014(19) 0.0249(9) Uani 1 1 d . . . . .
H25B H 0.6194 -0.0727 -0.5434 0.030 Uiso 1 1 calc R U . . .
C20A C 0.3998(3) 0.3469(3) -0.35167(19) 0.0281(10) Uani 1 1 d . . . . .
C5E C 0.2290(3) -0.5651(3) 0.1779(2) 0.0263(9) Uani 1 1 d . . . . .
H5E H 0.2186 -0.5665 0.2305 0.032 Uiso 1 1 calc R U . . .
C8 C 0.0254(3) -0.1892(3) 0.12810(19) 0.0244(9) Uani 1 1 d . . . . .
H8 H -0.0393 -0.1757 0.1614 0.029 Uiso 1 1 calc R U . . .
C12 C 0.0312(3) 0.1688(3) 0.07228(19) 0.0237(9) Uani 1 1 d . . . . .
H12 H -0.0227 0.2051 0.1090 0.028 Uiso 1 1 calc R U . . .
C40 C 0.3385(3) 0.0200(3) -0.08452(18) 0.0218(9) Uani 1 1 d . . . . .
C5B C 0.2582(3) -0.5572(3) 0.0220(2) 0.0252(9) Uani 1 1 d . . . . .
H5B H 0.2672 -0.5555 -0.0306 0.030 Uiso 1 1 calc R U . . .
C9 C 0.0718(3) -0.1146(3) 0.09550(18) 0.0240(9) Uani 1 1 d . . . . .
C5A C 0.2484(3) -0.4709(3) 0.06262(19) 0.0215(8) Uani 1 1 d . . . . .
C20D C 0.3755(4) 0.5303(3) -0.4264(2) 0.0485(14) Uani 1 1 d . . . . .
C25G C 0.9267(3) -0.2665(3) -0.6743(2) 0.0392(11) Uani 1 1 d . . . . .
H25A H 0.9642 -0.3334 -0.6657 0.059 Uiso 1 1 calc R U . . .
H25D H 0.9763 -0.2266 -0.6874 0.059 Uiso 1 1 calc R U . . .
H25G H 0.8892 -0.2659 -0.7150 0.059 Uiso 1 1 calc R U . . .
C5D C 0.2397(3) -0.6517(3) 0.1378(2) 0.0282(9) Uani 1 1 d . . . . .
C5G C 0.2350(4) -0.7480(3) 0.1768(2) 0.0367(11) Uani 1 1 d . . . . .
H5GA H 0.2137 -0.7364 0.2304 0.055 Uiso 1 1 calc R U . . .
H5GB H 0.3038 -0.7939 0.1663 0.055 Uiso 1 1 calc R U . . .
H5GC H 0.1848 -0.7752 0.1586 0.055 Uiso 1 1 calc R U . . .
C20G C 0.3656(5) 0.6278(3) -0.4673(3) 0.076(2) Uani 1 1 d . . . . .
H20A H 0.3948 0.6155 -0.5201 0.114 Uiso 1 1 calc R U . . .
H20D H 0.4036 0.6669 -0.4464 0.114 Uiso 1 1 calc R U . . .
H20E H 0.2922 0.6631 -0.4613 0.114 Uiso 1 1 calc R U . . .
C20F C 0.3734(4) 0.3570(3) -0.4236(2) 0.0391(12) Uani 1 1 d . . . . .
H20F H 0.3630 0.3030 -0.4471 0.047 Uiso 1 1 calc R U . . .
C20E C 0.3625(4) 0.4472(3) -0.4601(2) 0.0538(15) Uani 1 1 d . . . . .
H20G H 0.3462 0.4523 -0.5084 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C9 1.741(4) . ?
S1 C6 1.742(4) . ?
N1 C1 1.333(5) . ?
N1 C4 1.374(4) . ?
C1 C30 1.437(5) . ?
C1 C2 1.451(5) . ?
C3 C2 1.365(5) . ?
C3 C4 1.427(5) . ?
C3 H3 0.9300 . ?
N3 C16 1.353(4) . ?
N3 C19 1.363(4) . ?
S2 C21 1.739(4) . ?
S2 C24 1.747(4) . ?
N2 C14 1.343(4) . ?
N2 C11 1.378(4) . ?
C2 H2 0.9300 . ?
N4 C26 1.349(4) . ?
N4 C29 1.359(4) . ?
C4 C5 1.384(5) . ?
C6 C7 1.417(5) . ?
C6 C5 1.444(5) . ?
C5 C5A 1.480(5) . ?
C5C C5B 1.385(5) . ?
C5C C5D 1.395(5) . ?
C5C H5C 0.9300 . ?
C15 C16 1.413(5) . ?
C15 C40 1.424(5) . ?
C15 C14 1.451(5) . ?
C19 C20 1.411(5) . ?
C19 C18 1.457(5) . ?
C10E C10F 1.381(5) . ?
C10E C10D 1.394(5) . ?
C10E H10E 0.9300 . ?
C24 C25 1.405(5) . ?
C24 C23 1.426(5) . ?
C23 C22 1.368(5) . ?
C23 H23 0.9300 . ?
C22 C21 1.422(5) . ?
C22 H22 0.9300 . ?
C21 C20 1.413(5) . ?
C10F C10A 1.375(5) . ?
C10F H10F 0.9300 . ?
C32 C31 1.379(5) . ?
C32 C33 1.437(4) . ?
C32 C30 1.459(5) . ?
C31 C40 1.397(5) . ?
C31 H31 0.9300 . ?
C30 C29 1.408(5) . ?
C29 C28 1.463(5) . ?
C28 C27 1.335(4) . ?
C28 H28 0.9300 . ?
C27 C26 1.464(5) . ?
C27 H27 0.9300 . ?
C26 C25 1.418(5) . ?
C25 C25A 1.492(5) . ?
C25C C25D 1.377(5) . ?
C25C C25B 1.391(5) . ?
C25C H25C 0.9300 . ?
C14 C13 1.467(5) . ?
C10D C10C 1.375(5) . ?
C10D C10G 1.504(5) . ?
C38 C37 1.379(5) . ?
C38 C39 1.391(5) . ?
C38 H38 0.9300 . ?
C37 C36 1.391(5) . ?
C37 H37 0.9300 . ?
C36 C35 1.391(5) . ?
C36 H36 0.9300 . ?
C35 C34 1.397(5) . ?
C35 H35 0.9300 . ?
C34 C33 1.385(5) . ?
C34 H34 0.9300 . ?
C33 C39 1.447(5) . ?
C13 C12 1.322(5) . ?
C13 H13 0.9300 . ?
C39 C40 1.457(5) . ?
C11 C10 1.393(5) . ?
C11 C12 1.439(5) . ?
C16 C17 1.459(5) . ?
C10G H10A 0.9600 . ?
C10G H10B 0.9600 . ?
C10G H10C 0.9600 . ?
C25F C25A 1.375(5) . ?
C25F C25E 1.380(5) . ?
C25F H25F 0.9300 . ?
C17 C18 1.361(5) . ?
C17 H17 0.9300 . ?
C20 C20A 1.487(5) . ?
C20C C20D 1.367(5) . ?
C20C C20B 1.382(5) . ?
C20C H20C 0.9300 . ?
C10A C10B 1.398(5) . ?
C10A C10 1.495(5) . ?
C20B C20A 1.375(5) . ?
C20B H20B 0.9300 . ?
C10 C9 1.431(5) . ?
C10C C10B 1.386(5) . ?
C10C H10D 0.9300 . ?
C7 C8 1.381(5) . ?
C7 H7 0.9300 . ?
C25A C25B 1.394(5) . ?
C25E C25D 1.389(5) . ?
C25E H25E 0.9300 . ?
C10B H10G 0.9300 . ?
C5F C5E 1.370(5) . ?
C5F C5A 1.402(5) . ?
C5F H5F 0.9300 . ?
C25D C25G 1.529(5) . ?
C18 H18 0.9300 . ?
C25B H25B 0.9300 . ?
C20A C20F 1.397(5) . ?
C5E C5D 1.391(5) . ?
C5E H5E 0.9300 . ?
C8 C9 1.400(5) . ?
C8 H8 0.9300 . ?
C12 H12 0.9300 . ?
C5B C5A 1.396(5) . ?
C5B H5B 0.9300 . ?
C20D C20E 1.392(6) . ?
C20D C20G 1.510(5) . ?
C25G H25A 0.9600 . ?
C25G H25D 0.9600 . ?
C25G H25G 0.9600 . ?
C5D C5G 1.504(5) . ?
C5G H5GA 0.9600 . ?
C5G H5GB 0.9600 . ?
C5G H5GC 0.9600 . ?
C20G H20A 0.9600 . ?
C20G H20D 0.9600 . ?
C20G H20E 0.9600 . ?
C20F C20E 1.385(5) . ?
C20F H20F 0.9300 . ?
C20E H20G 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 S1 C6 92.56(17) . . ?
C1 N1 C4 108.0(3) . . ?
N1 C1 C30 118.1(3) . . ?
N1 C1 C2 110.0(3) . . ?
C30 C1 C2 131.7(3) . . ?
C2 C3 C4 107.8(3) . . ?
C2 C3 H3 126.1 . . ?
C4 C3 H3 126.1 . . ?
C16 N3 C19 106.5(3) . . ?
C21 S2 C24 92.43(17) . . ?
C14 N2 C11 106.3(3) . . ?
C3 C2 C1 105.5(3) . . ?
C3 C2 H2 127.2 . . ?
C1 C2 H2 127.2 . . ?
C26 N4 C29 106.8(3) . . ?
N1 C4 C5 121.2(3) . . ?
N1 C4 C3 108.6(3) . . ?
C5 C4 C3 130.2(3) . . ?
C7 C6 C5 125.3(3) . . ?
C7 C6 S1 109.9(3) . . ?
C5 C6 S1 124.8(3) . . ?
C4 C5 C6 123.1(3) . . ?
C4 C5 C5A 119.9(3) . . ?
C6 C5 C5A 117.0(3) . . ?
C5B C5C C5D 122.1(3) . . ?
C5B C5C H5C 118.9 . . ?
C5D C5C H5C 118.9 . . ?
C16 C15 C40 121.6(3) . . ?
C16 C15 C14 124.1(3) . . ?
C40 C15 C14 114.0(3) . . ?
N3 C19 C20 121.5(3) . . ?
N3 C19 C18 110.5(3) . . ?
C20 C19 C18 128.0(3) . . ?
C10F C10E C10D 120.5(4) . . ?
C10F C10E H10E 119.8 . . ?
C10D C10E H10E 119.8 . . ?
C25 C24 C23 126.4(3) . . ?
C25 C24 S2 123.8(3) . . ?
C23 C24 S2 109.8(3) . . ?
C22 C23 C24 113.7(3) . . ?
C22 C23 H23 123.2 . . ?
C24 C23 H23 123.2 . . ?
C23 C22 C21 113.9(3) . . ?
C23 C22 H22 123.1 . . ?
C21 C22 H22 123.1 . . ?
C20 C21 C22 125.7(3) . . ?
C20 C21 S2 124.2(3) . . ?
C22 C21 S2 110.1(3) . . ?
C10A C10F C10E 121.8(3) . . ?
C10A C10F H10F 119.1 . . ?
C10E C10F H10F 119.1 . . ?
C31 C32 C33 108.7(3) . . ?
C31 C32 C30 127.5(3) . . ?
C33 C32 C30 123.4(3) . . ?
C32 C31 C40 110.3(3) . . ?
C32 C31 H31 124.8 . . ?
C40 C31 H31 124.8 . . ?
C29 C30 C1 125.0(3) . . ?
C29 C30 C32 120.7(3) . . ?
C1 C30 C32 114.0(3) . . ?
N4 C29 C30 121.1(3) . . ?
N4 C29 C28 109.5(3) . . ?
C30 C29 C28 129.4(3) . . ?
C27 C28 C29 107.2(3) . . ?
C27 C28 H28 126.4 . . ?
C29 C28 H28 126.4 . . ?
C28 C27 C26 106.1(3) . . ?
C28 C27 H27 126.9 . . ?
C26 C27 H27 126.9 . . ?
N4 C26 C25 122.3(3) . . ?
N4 C26 C27 110.4(3) . . ?
C25 C26 C27 127.2(3) . . ?
C24 C25 C26 121.9(3) . . ?
C24 C25 C25A 120.0(3) . . ?
C26 C25 C25A 118.1(3) . . ?
C25D C25C C25B 120.4(3) . . ?
C25D C25C H25C 119.8 . . ?
C25B C25C H25C 119.8 . . ?
N2 C14 C15 117.2(3) . . ?
N2 C14 C13 110.1(3) . . ?
C15 C14 C13 132.7(3) . . ?
C10C C10D C10E 118.1(3) . . ?
C10C C10D C10G 121.8(3) . . ?
C10E C10D C10G 120.0(3) . . ?
C37 C38 C39 129.6(4) . . ?
C37 C38 H38 115.2 . . ?
C39 C38 H38 115.2 . . ?
C38 C37 C36 128.4(4) . . ?
C38 C37 H37 115.8 . . ?
C36 C37 H37 115.8 . . ?
C37 C36 C35 129.1(3) . . ?
C37 C36 H36 115.4 . . ?
C35 C36 H36 115.4 . . ?
C36 C35 C34 128.5(4) . . ?
C36 C35 H35 115.7 . . ?
C34 C35 H35 115.7 . . ?
C33 C34 C35 129.0(3) . . ?
C33 C34 H34 115.5 . . ?
C35 C34 H34 115.5 . . ?
C34 C33 C32 125.8(3) . . ?
C34 C33 C39 127.6(3) . . ?
C32 C33 C39 106.5(3) . . ?
C12 C13 C14 106.3(3) . . ?
C12 C13 H13 126.9 . . ?
C14 C13 H13 126.9 . . ?
C38 C39 C33 127.6(3) . . ?
C38 C39 C40 125.3(3) . . ?
C33 C39 C40 106.9(3) . . ?
N2 C11 C10 120.1(3) . . ?
N2 C11 C12 109.4(3) . . ?
C10 C11 C12 130.5(3) . . ?
N3 C16 C15 120.1(3) . . ?
N3 C16 C17 110.5(3) . . ?
C15 C16 C17 129.3(3) . . ?
C10D C10G H10A 109.5 . . ?
C10D C10G H10B 109.5 . . ?
H10A C10G H10B 109.5 . . ?
C10D C10G H10C 109.5 . . ?
H10A C10G H10C 109.5 . . ?
H10B C10G H10C 109.5 . . ?
C25A C25F C25E 121.5(4) . . ?
C25A C25F H25F 119.2 . . ?
C25E C25F H25F 119.2 . . ?
C18 C17 C16 106.4(3) . . ?
C18 C17 H17 126.8 . . ?
C16 C17 H17 126.8 . . ?
C19 C20 C21 121.7(3) . . ?
C19 C20 C20A 118.8(3) . . ?
C21 C20 C20A 119.4(3) . . ?
C20D C20C C20B 121.5(4) . . ?
C20D C20C H20C 119.2 . . ?
C20B C20C H20C 119.2 . . ?
C10F C10A C10B 117.7(3) . . ?
C10F C10A C10 121.6(3) . . ?
C10B C10A C10 120.4(3) . . ?
C20A C20B C20C 121.7(4) . . ?
C20A C20B H20B 119.1 . . ?
C20C C20B H20B 119.1 . . ?
C11 C10 C9 123.8(3) . . ?
C11 C10 C10A 117.9(3) . . ?
C9 C10 C10A 118.3(3) . . ?
C10D C10C C10B 121.4(3) . . ?
C10D C10C H10D 119.3 . . ?
C10B C10C H10D 119.3 . . ?
C8 C7 C6 113.1(3) . . ?
C8 C7 H7 123.4 . . ?
C6 C7 H7 123.4 . . ?
C25F C25A C25B 117.8(3) . . ?
C25F C25A C25 120.7(3) . . ?
C25B C25A C25 121.4(3) . . ?
C25F C25E C25D 120.6(4) . . ?
C25F C25E H25E 119.7 . . ?
C25D C25E H25E 119.7 . . ?
C10C C10B C10A 120.6(4) . . ?
C10C C10B H10G 119.7 . . ?
C10A C10B H10G 119.7 . . ?
C5E C5F C5A 121.8(3) . . ?
C5E C5F H5F 119.1 . . ?
C5A C5F H5F 119.1 . . ?
C25C C25D C25E 118.7(3) . . ?
C25C C25D C25G 121.2(3) . . ?
C25E C25D C25G 120.1(4) . . ?
C17 C18 C19 106.0(3) . . ?
C17 C18 H18 127.0 . . ?
C19 C18 H18 127.0 . . ?
C25C C25B C25A 121.0(4) . . ?
C25C C25B H25B 119.5 . . ?
C25A C25B H25B 119.5 . . ?
C20B C20A C20F 117.5(3) . . ?
C20B C20A C20 121.7(3) . . ?
C20F C20A C20 120.8(3) . . ?
C5F C5E C5D 121.6(3) . . ?
C5F C5E H5E 119.2 . . ?
C5D C5E H5E 119.2 . . ?
C7 C8 C9 114.5(3) . . ?
C7 C8 H8 122.8 . . ?
C9 C8 H8 122.8 . . ?
C13 C12 C11 107.9(3) . . ?
C13 C12 H12 126.1 . . ?
C11 C12 H12 126.1 . . ?
C31 C40 C15 128.8(3) . . ?
C31 C40 C39 106.9(3) . . ?
C15 C40 C39 123.8(3) . . ?
C5C C5B C5A 120.6(3) . . ?
C5C C5B H5B 119.7 . . ?
C5A C5B H5B 119.7 . . ?
C8 C9 C10 125.3(3) . . ?
C8 C9 S1 109.9(3) . . ?
C10 C9 S1 124.8(3) . . ?
C5B C5A C5F 117.0(3) . . ?
C5B C5A C5 122.4(3) . . ?
C5F C5A C5 120.5(3) . . ?
C20C C20D C20E 117.3(4) . . ?
C20C C20D C20G 121.4(4) . . ?
C20E C20D C20G 121.3(4) . . ?
C25D C25G H25A 109.5 . . ?
C25D C25G H25D 109.5 . . ?
H25A C25G H25D 109.5 . . ?
C25D C25G H25G 109.5 . . ?
H25A C25G H25G 109.5 . . ?
H25D C25G H25G 109.5 . . ?
C5E C5D C5C 116.8(3) . . ?
C5E C5D C5G 122.1(3) . . ?
C5C C5D C5G 121.1(3) . . ?
C5D C5G H5GA 109.5 . . ?
C5D C5G H5GB 109.5 . . ?
H5GA C5G H5GB 109.5 . . ?
C5D C5G H5GC 109.5 . . ?
H5GA C5G H5GC 109.5 . . ?
H5GB C5G H5GC 109.5 . . ?
C20D C20G H20A 109.5 . . ?
C20D C20G H20D 109.5 . . ?
H20A C20G H20D 109.5 . . ?
C20D C20G H20E 109.5 . . ?
H20A C20G H20E 109.5 . . ?
H20D C20G H20E 109.5 . . ?
C20E C20F C20A 120.3(4) . . ?
C20E C20F H20F 119.9 . . ?
C20A C20F H20F 119.9 . . ?
C20F C20E C20D 121.7(4) . . ?
C20F C20E H20G 119.2 . . ?
C20D C20E H20G 119.2 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.017 0.492 999 186 ' '
_platon_squeeze_details          
;
;


_refine_diff_density_max         0.498
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.070

_shelxl_version_number           2013-2


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: deuterated chloroform'
####################################################################### 
# 
# 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_PdSNaph
_database_code_depnum_ccdc_archive 'CCDC 1577494'
_audit_update_record             
;
2017-10-01 deposited with the CCDC.
2017-12-19 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         ?
_chemical_formula_sum            'C82 H44 D16 N4 O Pd S2'
_chemical_formula_weight         1303.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0.0000 0.0000 '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                   11.111(2)
_cell_length_b                   16.969(3)
_cell_length_c                   18.186(3)
_cell_angle_alpha                106.13(3)
_cell_angle_beta                 93.46(2)
_cell_angle_gamma                90.79(2)
_cell_volume                     3286.2(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    79.9(6)
_cell_measurement_reflns_used    1656
_cell_measurement_theta_min      3.0330
_cell_measurement_theta_max      23.0490

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.397
_shelx_estimated_absorpt_T_min   0.925
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      79.9(6)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_reflns_number            26208
_diffrn_reflns_av_unetI/netI     0.3716
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.748
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12892
_reflns_number_gt                5184
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0352P)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         12892
_refine_ls_number_parameters     817
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.2224
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.2101
_refine_ls_wR_factor_gt          0.1503
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_restrained_S_all      0.966
_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 0.41961(7) 0.82794(4) 0.38660(4) 0.0151(2) Uani 1 1 d . . . . .
S31 S 0.6143(2) 0.82634(13) 0.43105(12) 0.0155(6) Uani 1 1 d . . . . .
S34 S 0.0355(2) 0.68098(13) 0.12066(12) 0.0173(6) Uani 1 1 d . . . . .
O45 O 0.0565(6) 0.9779(4) 0.3040(3) 0.0244(17) Uani 1 1 d . . . . .
N32 N 0.3861(7) 0.7300(4) 0.4298(4) 0.0137(18) Uani 1 1 d . U . . .
N33 N 0.0184(7) 0.6238(4) 0.2671(4) 0.0161(19) Uani 1 1 d . . . . .
N35 N 0.1552(7) 0.8509(4) 0.1512(4) 0.0168(19) Uani 1 1 d . . . . .
H35 H 0.1250 0.8187 0.1748 0.020 Uiso 1 1 calc R U . . .
N36 N 0.4695(6) 0.9262(4) 0.3476(4) 0.0108(17) Uani 1 1 d . . . . .
C1 C 0.6779(9) 0.9258(5) 0.4653(5) 0.018(2) Uani 1 1 d . . . . .
C2 C 0.7274(8) 0.9339(5) 0.5418(5) 0.015(2) Uani 1 1 d . . . . .
H2 H 0.7767 0.9784 0.5691 0.018 Uiso 1 1 calc R U . . .
C3 C 0.6969(8) 0.8718(5) 0.5713(5) 0.017(2) Uani 1 1 d . U . . .
H3 H 0.7239 0.8702 0.6202 0.021 Uiso 1 1 calc R U . . .
C4 C 0.6200(8) 0.8092(5) 0.5211(5) 0.015(2) Uani 1 1 d . . . . .
C5 C 0.5518(8) 0.7461(5) 0.5335(5) 0.015(2) Uani 1 1 d . . . . .
C6 C 0.4504(8) 0.7036(5) 0.4856(4) 0.013(2) Uani 1 1 d . U . . .
C7 C 0.3983(8) 0.6296(5) 0.4917(5) 0.019(2) Uani 1 1 d . . . . .
H7 H 0.4257 0.5994 0.5246 0.023 Uiso 1 1 calc R U . . .
C8 C 0.2991(9) 0.6104(5) 0.4398(5) 0.017(2) Uani 1 1 d . . . . .
H8 H 0.2468 0.5651 0.4311 0.021 Uiso 1 1 calc R U . . .
C9 C 0.2926(8) 0.6729(5) 0.4027(5) 0.015(2) Uani 1 1 d . . . . .
C10 C 0.1931(9) 0.6839(5) 0.3525(5) 0.015(2) Uani 1 1 d . . . . .
C11 C 0.1225(8) 0.6123(5) 0.3088(5) 0.014(2) Uani 1 1 d . . . . .
C12 C 0.1463(9) 0.5307(5) 0.2834(5) 0.021(2) Uani 1 1 d . . . . .
H12 H 0.2094 0.5050 0.3026 0.025 Uiso 1 1 calc R U . . .
C13 C 0.0612(9) 0.4919(5) 0.2244(5) 0.022(3) Uani 1 1 d . . . . .
H13 H 0.0564 0.4362 0.1987 0.027 Uiso 1 1 calc R U . . .
C14 C -0.0143(9) 0.5509(5) 0.2109(5) 0.017(2) Uani 1 1 d . U . . .
C15 C -0.0928(8) 0.5459(5) 0.1409(5) 0.013(2) Uani 1 1 d . U . . .
C16 C -0.0781(8) 0.6017(5) 0.0994(5) 0.017(2) Uani 1 1 d . . . . .
C17 C -0.1438(9) 0.6064(5) 0.0298(5) 0.019(2) Uani 1 1 d . . . . .
H17 H -0.2084 0.5707 0.0075 0.023 Uiso 1 1 calc R U . . .
C18 C -0.1064(8) 0.6654(5) -0.0010(5) 0.016(2) Uani 1 1 d . . . . .
H18 H -0.1423 0.6720 -0.0464 0.019 Uiso 1 1 calc R U . . .
C19 C -0.0051(8) 0.7185(5) 0.0420(5) 0.014(2) Uani 1 1 d . U . . .
C20 C 0.0418(8) 0.7858(5) 0.0245(4) 0.013(2) Uani 1 1 d . . . . .
C21 C 0.1256(8) 0.8468(5) 0.0752(5) 0.014(2) Uani 1 1 d . U . . .
C22 C 0.1884(8) 0.9110(5) 0.0619(5) 0.015(2) Uani 1 1 d . . . . .
H22 H 0.1844 0.9253 0.0160 0.018 Uiso 1 1 calc R U . . .
C23 C 0.2590(9) 0.9515(5) 0.1275(5) 0.021(2) Uani 1 1 d . . . . .
H23 H 0.3106 0.9966 0.1325 0.025 Uiso 1 1 calc R U . . .
C24 C 0.2395(8) 0.9133(5) 0.1846(5) 0.013(2) Uani 1 1 d . . . . .
C25 C 0.2911(8) 0.9168(4) 0.2603(5) 0.011(2) Uani 1 1 d . . . . .
C26 C 0.4147(9) 0.9356(5) 0.2790(5) 0.012(2) Uani 1 1 d . U . . .
C27 C 0.4952(9) 0.9764(5) 0.2442(5) 0.023(3) Uani 1 1 d . . . . .
H27 H 0.4814 0.9876 0.1972 0.027 Uiso 1 1 calc R U . . .
C28 C 0.5967(9) 0.9963(5) 0.2914(5) 0.020(2) Uani 1 1 d . . . . .
H28 H 0.6638 1.0258 0.2840 0.023 Uiso 1 1 calc R U . . .
C29 C 0.5818(8) 0.9640(5) 0.3539(5) 0.012(2) Uani 1 1 d . . . . .
C30 C 0.6701(9) 0.9775(5) 0.4196(5) 0.016(2) Uani 1 1 d . . . . .
C37 C 0.2469(8) 0.8248(5) 0.3434(4) 0.012(2) Uani 1 1 d . U . . .
C38 C 0.1634(8) 0.7597(5) 0.3384(5) 0.012(2) Uani 1 1 d . . . . .
C39 C 0.0393(9) 0.7686(5) 0.3103(5) 0.017(2) Uani 1 1 d . . . . .
C40 C -0.0389(9) 0.6992(5) 0.2812(5) 0.016(2) Uani 1 1 d . . . . .
C41 C -0.1606(9) 0.7073(5) 0.2644(5) 0.018(2) Uani 1 1 d . . . . .
H41 H -0.2119 0.6611 0.2481 0.021 Uiso 1 1 calc R U . . .
C42 C -0.2057(9) 0.7860(5) 0.2723(4) 0.015(2) Uani 1 1 d . . . . .
H42 H -0.2881 0.7928 0.2653 0.018 Uiso 1 1 calc R U . . .
C43 C -0.1261(8) 0.8538(6) 0.2906(4) 0.019(2) Uani 1 1 d . . . . .
H43 H -0.1541 0.9054 0.2915 0.022 Uiso 1 1 calc R U . . .
C44 C -0.0054(9) 0.8440(5) 0.3076(5) 0.018(2) Uani 1 1 d . . . . .
C45 C 0.0862(9) 0.9085(5) 0.3071(5) 0.017(2) Uani 1 1 d . . . . .
C46 C 0.2121(8) 0.8846(5) 0.3061(5) 0.013(2) Uani 1 1 d . U . . .
C47 C 0.5824(9) 0.7244(5) 0.6066(5) 0.016(2) Uani 1 1 d . . . . .
C48 C 0.6849(9) 0.6821(5) 0.6158(5) 0.025(3) Uani 1 1 d . . . . .
H48 H 0.7308 0.6611 0.5741 0.030 Uiso 1 1 calc R U . . .
C49 C 0.7201(9) 0.6705(5) 0.6863(5) 0.024(3) Uani 1 1 d . . . . .
H49 H 0.7877 0.6398 0.6906 0.029 Uiso 1 1 calc R U . . .
C50 C 0.6578(9) 0.7030(5) 0.7501(5) 0.018(2) Uani 1 1 d . . . . .
C51 C 0.5546(10) 0.7435(6) 0.7406(5) 0.032(3) Uani 1 1 d . . . . .
H51 H 0.5087 0.7640 0.7825 0.039 Uiso 1 1 calc R U . . .
C52 C 0.5164(9) 0.7549(6) 0.6691(5) 0.029(3) Uani 1 1 d . . . . .
H52 H 0.4464 0.7831 0.6643 0.035 Uiso 1 1 calc R U . . .
C53 C 0.7019(9) 0.6955(6) 0.8288(5) 0.030(3) Uani 1 1 d . . . . .
H53A H 0.6338 0.6921 0.8580 0.044 Uiso 1 1 calc R U . . .
H53B H 0.7517 0.7428 0.8552 0.044 Uiso 1 1 calc R U . . .
H53C H 0.7479 0.6469 0.8228 0.044 Uiso 1 1 calc R U . . .
C54 C -0.1754(8) 0.4730(5) 0.1160(5) 0.014(2) Uani 1 1 d . U . . .
C55 C -0.2370(8) 0.4470(5) 0.1692(5) 0.013(2) Uani 1 1 d . . . . .
H55 H -0.2272 0.4757 0.2210 0.016 Uiso 1 1 calc R U . . .
C56 C -0.3125(8) 0.3790(5) 0.1458(5) 0.020(2) Uani 1 1 d . . . . .
H56 H -0.3536 0.3623 0.1822 0.024 Uiso 1 1 calc R U . . .
C57 C -0.3295(9) 0.3341(5) 0.0696(5) 0.016(2) Uani 1 1 d . . . . .
C58 C -0.2691(8) 0.3599(5) 0.0168(5) 0.015(2) Uani 1 1 d . . . . .
H58 H -0.2807 0.3313 -0.0348 0.018 Uiso 1 1 calc R U . . .
C59 C -0.1909(8) 0.4275(5) 0.0389(5) 0.015(2) Uani 1 1 d . . . . .
H59 H -0.1485 0.4430 0.0023 0.019 Uiso 1 1 calc R U . . .
C60 C -0.4107(9) 0.2591(5) 0.0431(5) 0.031(3) Uani 1 1 d . . . . .
H60A H -0.4860 0.2729 0.0218 0.046 Uiso 1 1 calc R U . . .
H60B H -0.4251 0.2382 0.0859 0.046 Uiso 1 1 calc R U . . .
H60C H -0.3730 0.2180 0.0047 0.046 Uiso 1 1 calc R U . . .
C61 C 0.0131(8) 0.7971(5) -0.0526(5) 0.013(2) Uani 1 1 d . . . . .
C62 C -0.0340(8) 0.8717(5) -0.0627(5) 0.019(2) Uani 1 1 d . . . . .
H62 H -0.0495 0.9149 -0.0204 0.023 Uiso 1 1 calc R U . . .
C63 C -0.0559(9) 0.8788(5) -0.1348(5) 0.021(2) Uani 1 1 d . . . . .
H63 H -0.0904 0.9265 -0.1407 0.025 Uiso 1 1 calc R U . . .
C64 C -0.0296(9) 0.8189(6) -0.1992(5) 0.026(3) Uani 1 1 d . . . . .
C65 C 0.0156(9) 0.7462(5) -0.1894(5) 0.022(2) Uani 1 1 d . . . . .
H65 H 0.0314 0.7039 -0.2324 0.026 Uiso 1 1 calc R U . . .
C66 C 0.0374(8) 0.7355(5) -0.1186(5) 0.015(2) Uani 1 1 d . . . . .
H66 H 0.0689 0.6865 -0.1139 0.019 Uiso 1 1 calc R U . . .
C67 C -0.0477(11) 0.8313(6) -0.2779(5) 0.045(3) Uani 1 1 d . . . . .
H67A H 0.0170 0.8070 -0.3083 0.067 Uiso 1 1 calc R U . . .
H67B H -0.0484 0.8890 -0.2735 0.067 Uiso 1 1 calc R U . . .
H67C H -0.1231 0.8058 -0.3020 0.067 Uiso 1 1 calc R U . . .
C68 C 0.7546(8) 1.0498(5) 0.4349(5) 0.012(2) Uani 1 1 d . U . . .
C69 C 0.8768(9) 1.0432(6) 0.4536(5) 0.023(2) Uani 1 1 d . . . . .
H69 H 0.9068 0.9924 0.4538 0.027 Uiso 1 1 calc R U . . .
C70 C 0.9543(9) 1.1117(5) 0.4719(5) 0.024(3) Uani 1 1 d . . . . .
H70 H 1.0347 1.1064 0.4868 0.029 Uiso 1 1 calc R U . . .
C71 C 0.9149(9) 1.1878(5) 0.4686(5) 0.018(2) Uani 1 1 d . . . . .
C72 C 0.7944(9) 1.1938(5) 0.4481(4) 0.016(2) Uani 1 1 d . . . . .
H72 H 0.7656 1.2442 0.4455 0.019 Uiso 1 1 calc R U . . .
C73 C 0.7156(8) 1.1265(5) 0.4314(4) 0.014(2) Uani 1 1 d . . . . .
H73 H 0.6350 1.1324 0.4175 0.017 Uiso 1 1 calc R U . . .
C74 C 1.0009(9) 1.2608(5) 0.4908(5) 0.028(3) Uani 1 1 d . . . . .
H74A H 1.0463 1.2619 0.4478 0.042 Uiso 1 1 calc R U . . .
H74B H 1.0551 1.2570 0.5328 0.042 Uiso 1 1 calc R U . . .
H74C H 0.9565 1.3102 0.5060 0.042 Uiso 1 1 calc R U . . .
C75 C 0.5117(10) 0.7344(6) 0.1529(5) 0.027(3) Uani 1 1 d . . . . .
D75 D 0.5344 0.7886 0.1576 0.033 Uiso 1 1 calc R U . . .
C76 C 0.5779(11) 0.6703(6) 0.1135(6) 0.039(3) Uani 1 1 d . . . . .
D76 D 0.6472 0.6822 0.0918 0.047 Uiso 1 1 calc R U . . .
C77 C 0.5463(9) 0.5891(6) 0.1047(5) 0.030(3) Uani 1 1 d . . . . .
D77 D 0.5929 0.5477 0.0766 0.036 Uiso 1 1 calc R U . . .
C78 C 0.4436(10) 0.5689(6) 0.1380(5) 0.027(3) Uani 1 1 d . . . . .
C79 C 0.3757(9) 0.6338(6) 0.1774(5) 0.029(3) Uani 1 1 d . . . . .
D79 D 0.3058 0.6233 0.1992 0.035 Uiso 1 1 calc R U . . .
C80 C 0.4129(10) 0.7153(6) 0.1841(5) 0.029(3) Uani 1 1 d . . . . .
D80 D 0.3671 0.7577 0.2114 0.034 Uiso 1 1 calc R U . . .
C81 C 0.4076(10) 0.4817(6) 0.1302(6) 0.047(3) Uani 1 1 d . . . . .
D81A D 0.3220 0.4773 0.1335 0.071 Uiso 1 1 calc R U . . .
D81B D 0.4483 0.4640 0.1706 0.071 Uiso 1 1 calc R U . . .
D81C D 0.4293 0.4477 0.0815 0.071 Uiso 1 1 calc R U . . .
C82 C 0.7178(10) -0.1421(6) 0.0512(6) 0.039(3) Uani 1 1 d . . . . .
D82 D 0.7133 -0.1982 0.0270 0.047 Uiso 1 1 calc R U . . .
C83 C 0.6418(10) -0.0905(6) 0.0246(6) 0.044(3) Uani 1 1 d . . . . .
D83 D 0.5888 -0.1117 -0.0181 0.053 Uiso 1 1 calc R U . . .
C84 C 0.6451(10) -0.0078(6) 0.0618(6) 0.039(3) Uani 1 1 d . . . . .
D84 D 0.5927 0.0265 0.0445 0.046 Uiso 1 1 calc R U . . .
C85 C 0.7255(10) 0.0251(6) 0.1246(5) 0.030(3) Uani 1 1 d . . . . .
C86 C 0.8035(10) -0.0283(6) 0.1484(5) 0.034(3) Uani 1 1 d . . . . .
D86 D 0.8597 -0.0074 0.1896 0.041 Uiso 1 1 calc R U . . .
C87 C 0.7988(10) -0.1121(6) 0.1120(5) 0.040(3) Uani 1 1 d . . . . .
D87 D 0.8504 -0.1470 0.1290 0.048 Uiso 1 1 calc R U . . .
C88 C 0.7263(10) 0.1166(6) 0.1657(6) 0.046(3) Uani 1 1 d . . . . .
D88A D 0.7680 0.1465 0.1367 0.069 Uiso 1 1 calc R U . . .
D88B D 0.7665 0.1265 0.2158 0.069 Uiso 1 1 calc R U . . .
D88C D 0.6448 0.1344 0.1706 0.069 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C37 2.023(9) . ?
Pd1 N32 2.065(7) . ?
Pd1 N36 2.065(7) . ?
Pd1 S31 2.266(3) . ?
S31 C4 1.739(9) . ?
S31 C1 1.751(8) . ?
S34 C19 1.759(8) . ?
S34 C16 1.777(9) . ?
O45 C45 1.243(9) . ?
N32 C9 1.380(10) . ?
N32 C6 1.385(9) . ?
N33 C11 1.391(10) . ?
N33 C14 1.395(9) . ?
N33 C40 1.403(10) . ?
N35 C24 1.383(10) . ?
N35 C21 1.383(9) . ?
N35 H35 0.8600 . ?
N36 C29 1.379(11) . ?
N36 C26 1.406(10) . ?
C1 C30 1.365(11) . ?
C1 C2 1.434(11) . ?
C2 C3 1.356(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.425(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(12) . ?
C5 C6 1.435(11) . ?
C5 C47 1.498(11) . ?
C6 C7 1.410(11) . ?
C7 C8 1.380(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.406(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.439(11) . ?
C10 C38 1.419(11) . ?
C10 C11 1.444(11) . ?
C11 C12 1.368(11) . ?
C12 C13 1.396(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.379(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.481(11) . ?
C15 C16 1.378(11) . ?
C15 C54 1.479(11) . ?
C16 C17 1.445(11) . ?
C17 C18 1.348(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.472(11) . ?
C18 H18 0.9300 . ?
C19 C20 1.371(11) . ?
C20 C21 1.459(11) . ?
C20 C61 1.485(11) . ?
C21 C22 1.371(11) . ?
C22 C23 1.388(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.394(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.444(11) . ?
C25 C26 1.405(12) . ?
C25 C46 1.447(12) . ?
C26 C27 1.405(12) . ?
C27 C28 1.354(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.409(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.464(11) . ?
C30 C68 1.487(12) . ?
C37 C38 1.413(11) . ?
C37 C46 1.415(11) . ?
C38 C39 1.466(12) . ?
C39 C44 1.392(11) . ?
C39 C40 1.412(12) . ?
C40 C41 1.385(12) . ?
C41 C42 1.407(11) . ?
C41 H41 0.9300 . ?
C42 C43 1.393(11) . ?
C42 H42 0.9300 . ?
C43 C44 1.380(12) . ?
C43 H43 0.9300 . ?
C44 C45 1.486(12) . ?
C45 C46 1.461(12) . ?
C47 C52 1.372(12) . ?
C47 C48 1.381(12) . ?
C48 C49 1.385(11) . ?
C48 H48 0.9300 . ?
C49 C50 1.371(12) . ?
C49 H49 0.9300 . ?
C50 C51 1.371(12) . ?
C50 C53 1.526(11) . ?
C51 C52 1.409(12) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 C55 1.380(11) . ?
C54 C59 1.400(10) . ?
C55 C56 1.370(11) . ?
C55 H55 0.9300 . ?
C56 C57 1.384(11) . ?
C56 H56 0.9300 . ?
C57 C58 1.365(12) . ?
C57 C60 1.498(11) . ?
C58 C59 1.381(11) . ?
C58 H58 0.9300 . ?
C59 H59 0.9300 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C61 C66 1.399(11) . ?
C61 C62 1.430(11) . ?
C62 C63 1.357(11) . ?
C62 H62 0.9300 . ?
C63 C64 1.371(12) . ?
C63 H63 0.9300 . ?
C64 C65 1.390(12) . ?
C64 C67 1.505(12) . ?
C65 C66 1.359(11) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 C69 1.394(12) . ?
C68 C73 1.394(11) . ?
C69 C70 1.388(12) . ?
C69 H69 0.9300 . ?
C70 C71 1.386(11) . ?
C70 H70 0.9300 . ?
C71 C72 1.380(12) . ?
C71 C74 1.501(11) . ?
C72 C73 1.383(11) . ?
C72 H72 0.9300 . ?
C73 H73 0.9300 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 C80 1.342(13) . ?
C75 C76 1.375(13) . ?
C75 D75 0.9300 . ?
C76 C77 1.379(13) . ?
C76 D76 0.9300 . ?
C77 C78 1.404(14) . ?
C77 D77 0.9300 . ?
C78 C79 1.395(12) . ?
C78 C81 1.495(13) . ?
C79 C80 1.407(13) . ?
C79 D79 0.9300 . ?
C80 D80 0.9300 . ?
C81 D81A 0.9600 . ?
C81 D81B 0.9600 . ?
C81 D81C 0.9600 . ?
C82 C87 1.359(13) . ?
C82 C83 1.385(13) . ?
C82 D82 0.9300 . ?
C83 C84 1.378(12) . ?
C83 D83 0.9300 . ?
C84 C85 1.387(12) . ?
C84 D84 0.9300 . ?
C85 C86 1.398(13) . ?
C85 C88 1.524(12) . ?
C86 C87 1.390(12) . ?
C86 D86 0.9300 . ?
C87 D87 0.9300 . ?
C88 D88A 0.9600 . ?
C88 D88B 0.9600 . ?
C88 D88C 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
C37 Pd1 N32 91.9(3) . . ?
C37 Pd1 N36 93.5(3) . . ?
N32 Pd1 N36 174.7(3) . . ?
C37 Pd1 S31 177.5(2) . . ?
N32 Pd1 S31 87.3(2) . . ?
N36 Pd1 S31 87.3(2) . . ?
C4 S31 C1 94.0(4) . . ?
C4 S31 Pd1 109.9(3) . . ?
C1 S31 Pd1 111.4(3) . . ?
C19 S34 C16 95.8(4) . . ?
C9 N32 C6 105.4(7) . . ?
C9 N32 Pd1 124.3(6) . . ?
C6 N32 Pd1 130.2(6) . . ?
C11 N33 C14 109.3(7) . . ?
C11 N33 C40 122.8(7) . . ?
C14 N33 C40 127.8(7) . . ?
C24 N35 C21 111.7(8) . . ?
C24 N35 H35 124.1 . . ?
C21 N35 H35 124.1 . . ?
C29 N36 C26 104.4(7) . . ?
C29 N36 Pd1 128.4(6) . . ?
C26 N36 Pd1 120.0(5) . . ?
C30 C1 C2 134.1(8) . . ?
C30 C1 S31 119.3(7) . . ?
C2 C1 S31 106.5(6) . . ?
C3 C2 C1 115.0(8) . . ?
C3 C2 H2 122.5 . . ?
C1 C2 H2 122.5 . . ?
C2 C3 C4 114.5(8) . . ?
C2 C3 H3 122.7 . . ?
C4 C3 H3 122.7 . . ?
C5 C4 C3 132.2(8) . . ?
C5 C4 S31 120.2(6) . . ?
C3 C4 S31 107.5(7) . . ?
C4 C5 C6 126.3(8) . . ?
C4 C5 C47 116.2(8) . . ?
C6 C5 C47 117.4(8) . . ?
N32 C6 C7 110.0(7) . . ?
N32 C6 C5 125.8(8) . . ?
C7 C6 C5 124.1(8) . . ?
C8 C7 C6 107.2(8) . . ?
C8 C7 H7 126.4 . . ?
C6 C7 H7 126.4 . . ?
C7 C8 C9 106.7(8) . . ?
C7 C8 H8 126.7 . . ?
C9 C8 H8 126.7 . . ?
N32 C9 C8 110.7(8) . . ?
N32 C9 C10 123.5(8) . . ?
C8 C9 C10 125.2(8) . . ?
C38 C10 C9 124.7(8) . . ?
C38 C10 C11 116.8(7) . . ?
C9 C10 C11 118.4(8) . . ?
C12 C11 N33 106.4(7) . . ?
C12 C11 C10 133.5(9) . . ?
N33 C11 C10 118.3(7) . . ?
C11 C12 C13 109.4(8) . . ?
C11 C12 H12 125.3 . . ?
C13 C12 H12 125.3 . . ?
C14 C13 C12 107.8(8) . . ?
C14 C13 H13 126.1 . . ?
C12 C13 H13 126.1 . . ?
C13 C14 N33 106.6(7) . . ?
C13 C14 C15 127.4(7) . . ?
N33 C14 C15 124.3(8) . . ?
C16 C15 C54 124.2(8) . . ?
C16 C15 C14 120.7(8) . . ?
C54 C15 C14 114.9(7) . . ?
C15 C16 C17 128.9(8) . . ?
C15 C16 S34 124.9(7) . . ?
C17 C16 S34 106.1(7) . . ?
C18 C17 C16 116.5(8) . . ?
C18 C17 H17 121.8 . . ?
C16 C17 H17 121.8 . . ?
C17 C18 C19 115.4(8) . . ?
C17 C18 H18 122.3 . . ?
C19 C18 H18 122.3 . . ?
C20 C19 C18 125.5(8) . . ?
C20 C19 S34 128.3(7) . . ?
C18 C19 S34 106.1(6) . . ?
C19 C20 C21 124.8(7) . . ?
C19 C20 C61 119.5(7) . . ?
C21 C20 C61 115.7(7) . . ?
C22 C21 N35 105.3(7) . . ?
C22 C21 C20 130.4(8) . . ?
N35 C21 C20 124.3(8) . . ?
C21 C22 C23 109.5(8) . . ?
C21 C22 H22 125.3 . . ?
C23 C22 H22 125.3 . . ?
C22 C23 C24 108.5(8) . . ?
C22 C23 H23 125.7 . . ?
C24 C23 H23 125.7 . . ?
N35 C24 C23 104.8(7) . . ?
N35 C24 C25 117.3(8) . . ?
C23 C24 C25 137.5(8) . . ?
C26 C25 C24 120.1(8) . . ?
C26 C25 C46 124.6(8) . . ?
C24 C25 C46 114.2(8) . . ?
C25 C26 C27 129.0(8) . . ?
C25 C26 N36 120.4(8) . . ?
C27 C26 N36 109.9(8) . . ?
C28 C27 C26 107.6(8) . . ?
C28 C27 H27 126.2 . . ?
C26 C27 H27 126.2 . . ?
C27 C28 C29 107.4(9) . . ?
C27 C28 H28 126.3 . . ?
C29 C28 H28 126.3 . . ?
N36 C29 C28 110.7(8) . . ?
N36 C29 C30 125.7(8) . . ?
C28 C29 C30 123.3(9) . . ?
C1 C30 C29 122.4(8) . . ?
C1 C30 C68 120.0(8) . . ?
C29 C30 C68 117.5(8) . . ?
C38 C37 C46 117.3(8) . . ?
C38 C37 Pd1 123.6(6) . . ?
C46 C37 Pd1 118.4(7) . . ?
C37 C38 C10 124.8(8) . . ?
C37 C38 C39 117.3(8) . . ?
C10 C38 C39 117.7(8) . . ?
C44 C39 C40 116.9(8) . . ?
C44 C39 C38 122.5(8) . . ?
C40 C39 C38 120.6(8) . . ?
C41 C40 N33 124.2(8) . . ?
C41 C40 C39 121.3(8) . . ?
N33 C40 C39 114.4(8) . . ?
C40 C41 C42 119.3(8) . . ?
C40 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
C43 C42 C41 119.6(9) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 119.7(9) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C39 122.0(9) . . ?
C43 C44 C45 120.8(9) . . ?
C39 C44 C45 115.9(9) . . ?
O45 C45 C46 121.9(9) . . ?
O45 C45 C44 121.5(9) . . ?
C46 C45 C44 116.6(8) . . ?
C37 C46 C25 123.3(9) . . ?
C37 C46 C45 118.2(9) . . ?
C25 C46 C45 118.1(8) . . ?
C52 C47 C48 118.4(9) . . ?
C52 C47 C5 120.0(8) . . ?
C48 C47 C5 121.2(9) . . ?
C47 C48 C49 120.9(9) . . ?
C47 C48 H48 119.5 . . ?
C49 C48 H48 119.5 . . ?
C50 C49 C48 121.5(9) . . ?
C50 C49 H49 119.2 . . ?
C48 C49 H49 119.2 . . ?
C49 C50 C51 117.5(9) . . ?
C49 C50 C53 121.5(9) . . ?
C51 C50 C53 121.0(9) . . ?
C50 C51 C52 121.6(9) . . ?
C50 C51 H51 119.2 . . ?
C52 C51 H51 119.2 . . ?
C47 C52 C51 119.9(9) . . ?
C47 C52 H52 120.1 . . ?
C51 C52 H52 120.1 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 C59 118.5(8) . . ?
C55 C54 C15 120.3(7) . . ?
C59 C54 C15 121.2(9) . . ?
C56 C55 C54 119.9(8) . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C55 C56 C57 122.1(9) . . ?
C55 C56 H56 119.0 . . ?
C57 C56 H56 119.0 . . ?
C58 C57 C56 118.1(8) . . ?
C58 C57 C60 119.2(8) . . ?
C56 C57 C60 122.7(9) . . ?
C57 C58 C59 121.2(8) . . ?
C57 C58 H58 119.4 . . ?
C59 C58 H58 119.4 . . ?
C58 C59 C54 120.2(9) . . ?
C58 C59 H59 119.9 . . ?
C54 C59 H59 119.9 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C66 C61 C62 117.4(8) . . ?
C66 C61 C20 120.3(8) . . ?
C62 C61 C20 122.2(7) . . ?
C63 C62 C61 119.3(8) . . ?
C63 C62 H62 120.4 . . ?
C61 C62 H62 120.4 . . ?
C62 C63 C64 123.0(9) . . ?
C62 C63 H63 118.5 . . ?
C64 C63 H63 118.5 . . ?
C63 C64 C65 117.7(9) . . ?
C63 C64 C67 121.4(9) . . ?
C65 C64 C67 120.9(8) . . ?
C66 C65 C64 121.6(8) . . ?
C66 C65 H65 119.2 . . ?
C64 C65 H65 119.2 . . ?
C65 C66 C61 120.9(8) . . ?
C65 C66 H66 119.5 . . ?
C61 C66 H66 119.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C69 C68 C73 117.3(8) . . ?
C69 C68 C30 120.8(8) . . ?
C73 C68 C30 121.9(8) . . ?
C70 C69 C68 120.7(9) . . ?
C70 C69 H69 119.6 . . ?
C68 C69 H69 119.6 . . ?
C71 C70 C69 121.6(9) . . ?
C71 C70 H70 119.2 . . ?
C69 C70 H70 119.2 . . ?
C72 C71 C70 117.6(8) . . ?
C72 C71 C74 122.5(8) . . ?
C70 C71 C74 119.9(8) . . ?
C71 C72 C73 121.4(9) . . ?
C71 C72 H72 119.3 . . ?
C73 C72 H72 119.3 . . ?
C72 C73 C68 121.3(8) . . ?
C72 C73 H73 119.4 . . ?
C68 C73 H73 119.4 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C80 C75 C76 117.1(10) . . ?
C80 C75 D75 121.4 . . ?
C76 C75 D75 121.4 . . ?
C75 C76 C77 123.0(12) . . ?
C75 C76 D76 118.5 . . ?
C77 C76 D76 118.5 . . ?
C76 C77 C78 120.1(10) . . ?
C76 C77 D77 120.0 . . ?
C78 C77 D77 120.0 . . ?
C79 C78 C77 117.1(10) . . ?
C79 C78 C81 121.5(11) . . ?
C77 C78 C81 121.4(10) . . ?
C78 C79 C80 120.0(11) . . ?
C78 C79 D79 120.0 . . ?
C80 C79 D79 120.0 . . ?
C75 C80 C79 122.8(10) . . ?
C75 C80 D80 118.6 . . ?
C79 C80 D80 118.6 . . ?
C78 C81 D81A 109.5 . . ?
C78 C81 D81B 109.5 . . ?
D81A C81 D81B 109.5 . . ?
C78 C81 D81C 109.5 . . ?
D81A C81 D81C 109.5 . . ?
D81B C81 D81C 109.5 . . ?
C87 C82 C83 121.1(10) . . ?
C87 C82 D82 119.5 . . ?
C83 C82 D82 119.5 . . ?
C84 C83 C82 119.7(10) . . ?
C84 C83 D83 120.1 . . ?
C82 C83 D83 120.1 . . ?
C83 C84 C85 120.9(10) . . ?
C83 C84 D84 119.5 . . ?
C85 C84 D84 119.5 . . ?
C84 C85 C86 117.8(9) . . ?
C84 C85 C88 120.1(9) . . ?
C86 C85 C88 122.1(9) . . ?
C87 C86 C85 121.4(10) . . ?
C87 C86 D86 119.3 . . ?
C85 C86 D86 119.3 . . ?
C82 C87 C86 119.0(10) . . ?
C82 C87 D87 120.5 . . ?
C86 C87 D87 120.5 . . ?
C85 C88 D88A 109.5 . . ?
C85 C88 D88B 109.5 . . ?
D88A C88 D88B 109.5 . . ?
C85 C88 D88C 109.5 . . ?
D88A C88 D88C 109.5 . . ?
D88B C88 D88C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 S31 C1 C30 -165.0(9) . . . . ?
Pd1 S31 C1 C30 -51.9(9) . . . . ?
C4 S31 C1 C2 13.7(7) . . . . ?
Pd1 S31 C1 C2 126.9(6) . . . . ?
C30 C1 C2 C3 168.4(11) . . . . ?
S31 C1 C2 C3 -10.0(10) . . . . ?
C1 C2 C3 C4 -0.4(12) . . . . ?
C2 C3 C4 C5 -165.8(9) . . . . ?
C2 C3 C4 S31 10.7(10) . . . . ?
C1 S31 C4 C5 163.0(8) . . . . ?
Pd1 S31 C4 C5 48.5(8) . . . . ?
C1 S31 C4 C3 -14.0(7) . . . . ?
Pd1 S31 C4 C3 -128.5(5) . . . . ?
C3 C4 C5 C6 158.8(9) . . . . ?
S31 C4 C5 C6 -17.3(13) . . . . ?
C3 C4 C5 C47 -16.8(14) . . . . ?
S31 C4 C5 C47 167.0(6) . . . . ?
C9 N32 C6 C7 1.3(10) . . . . ?
Pd1 N32 C6 C7 -175.2(6) . . . . ?
C9 N32 C6 C5 -175.9(8) . . . . ?
Pd1 N32 C6 C5 7.6(13) . . . . ?
C4 C5 C6 N32 -16.2(14) . . . . ?
C47 C5 C6 N32 159.5(8) . . . . ?
C4 C5 C6 C7 167.0(9) . . . . ?
C47 C5 C6 C7 -17.4(13) . . . . ?
N32 C6 C7 C8 -1.0(10) . . . . ?
C5 C6 C7 C8 176.3(8) . . . . ?
C6 C7 C8 C9 0.2(10) . . . . ?
C6 N32 C9 C8 -1.2(10) . . . . ?
Pd1 N32 C9 C8 175.6(6) . . . . ?
C6 N32 C9 C10 169.9(8) . . . . ?
Pd1 N32 C9 C10 -13.3(12) . . . . ?
C7 C8 C9 N32 0.6(10) . . . . ?
C7 C8 C9 C10 -170.3(8) . . . . ?
N32 C9 C10 C38 -14.9(14) . . . . ?
C8 C9 C10 C38 154.9(9) . . . . ?
N32 C9 C10 C11 160.5(8) . . . . ?
C8 C9 C10 C11 -29.7(13) . . . . ?
C14 N33 C11 C12 -5.9(10) . . . . ?
C40 N33 C11 C12 175.2(8) . . . . ?
C14 N33 C11 C10 160.8(8) . . . . ?
C40 N33 C11 C10 -18.0(13) . . . . ?
C38 C10 C11 C12 151.0(10) . . . . ?
C9 C10 C11 C12 -24.8(15) . . . . ?
C38 C10 C11 N33 -11.4(13) . . . . ?
C9 C10 C11 N33 172.8(8) . . . . ?
N33 C11 C12 C13 2.4(11) . . . . ?
C10 C11 C12 C13 -161.5(10) . . . . ?
C11 C12 C13 C14 2.1(11) . . . . ?
C12 C13 C14 N33 -5.6(11) . . . . ?
C12 C13 C14 C15 159.8(9) . . . . ?
C11 N33 C14 C13 7.2(10) . . . . ?
C40 N33 C14 C13 -174.0(9) . . . . ?
C11 N33 C14 C15 -158.8(9) . . . . ?
C40 N33 C14 C15 19.9(14) . . . . ?
C13 C14 C15 C16 -120.2(11) . . . . ?
N33 C14 C15 C16 42.8(13) . . . . ?
C13 C14 C15 C54 53.4(13) . . . . ?
N33 C14 C15 C54 -143.5(9) . . . . ?
C54 C15 C16 C17 6.1(15) . . . . ?
C14 C15 C16 C17 179.1(8) . . . . ?
C54 C15 C16 S34 -170.3(7) . . . . ?
C14 C15 C16 S34 2.7(13) . . . . ?
C19 S34 C16 C15 178.0(8) . . . . ?
C19 S34 C16 C17 0.9(7) . . . . ?
C15 C16 C17 C18 -176.7(9) . . . . ?
S34 C16 C17 C18 0.2(10) . . . . ?
C16 C17 C18 C19 -1.5(12) . . . . ?
C17 C18 C19 C20 -175.0(9) . . . . ?
C17 C18 C19 S34 2.1(10) . . . . ?
C16 S34 C19 C20 175.3(9) . . . . ?
C16 S34 C19 C18 -1.6(6) . . . . ?
C18 C19 C20 C21 167.5(8) . . . . ?
S34 C19 C20 C21 -8.9(14) . . . . ?
C18 C19 C20 C61 -16.3(14) . . . . ?
S34 C19 C20 C61 167.3(7) . . . . ?
C24 N35 C21 C22 -3.1(10) . . . . ?
C24 N35 C21 C20 178.2(8) . . . . ?
C19 C20 C21 C22 172.1(9) . . . . ?
C61 C20 C21 C22 -4.2(14) . . . . ?
C19 C20 C21 N35 -9.6(14) . . . . ?
C61 C20 C21 N35 174.1(8) . . . . ?
N35 C21 C22 C23 2.5(10) . . . . ?
C20 C21 C22 C23 -179.0(9) . . . . ?
C21 C22 C23 C24 -1.0(11) . . . . ?
C21 N35 C24 C23 2.5(10) . . . . ?
C21 N35 C24 C25 -171.3(7) . . . . ?
C22 C23 C24 N35 -0.9(10) . . . . ?
C22 C23 C24 C25 171.0(10) . . . . ?
N35 C24 C25 C26 139.5(8) . . . . ?
C23 C24 C25 C26 -31.7(15) . . . . ?
N35 C24 C25 C46 -29.2(11) . . . . ?
C23 C24 C25 C46 159.6(10) . . . . ?
C24 C25 C26 C27 21.5(13) . . . . ?
C46 C25 C26 C27 -171.1(8) . . . . ?
C24 C25 C26 N36 -169.6(7) . . . . ?
C46 C25 C26 N36 -2.2(12) . . . . ?
C29 N36 C26 C25 -169.0(7) . . . . ?
Pd1 N36 C26 C25 38.2(9) . . . . ?
C29 N36 C26 C27 1.8(9) . . . . ?
Pd1 N36 C26 C27 -151.0(6) . . . . ?
C25 C26 C27 C28 166.7(8) . . . . ?
N36 C26 C27 C28 -3.1(10) . . . . ?
C26 C27 C28 C29 3.1(10) . . . . ?
C26 N36 C29 C28 0.1(9) . . . . ?
Pd1 N36 C29 C28 149.7(6) . . . . ?
C26 N36 C29 C30 174.1(7) . . . . ?
Pd1 N36 C29 C30 -36.3(11) . . . . ?
C27 C28 C29 N36 -2.0(10) . . . . ?
C27 C28 C29 C30 -176.2(8) . . . . ?
C2 C1 C30 C29 -159.3(10) . . . . ?
S31 C1 C30 C29 19.1(13) . . . . ?
C2 C1 C30 C68 21.7(17) . . . . ?
S31 C1 C30 C68 -159.9(7) . . . . ?
N36 C29 C30 C1 29.9(13) . . . . ?
C28 C29 C30 C1 -156.9(9) . . . . ?
N36 C29 C30 C68 -151.1(8) . . . . ?
C28 C29 C30 C68 22.2(12) . . . . ?
C46 C37 C38 C10 161.4(8) . . . . ?
Pd1 C37 C38 C10 -9.3(12) . . . . ?
C46 C37 C38 C39 -13.2(12) . . . . ?
Pd1 C37 C38 C39 176.2(6) . . . . ?
C9 C10 C38 C37 27.6(14) . . . . ?
C11 C10 C38 C37 -147.9(9) . . . . ?
C9 C10 C38 C39 -157.9(8) . . . . ?
C11 C10 C38 C39 26.6(12) . . . . ?
C37 C38 C39 C44 -16.8(13) . . . . ?
C10 C38 C39 C44 168.2(8) . . . . ?
C37 C38 C39 C40 160.3(8) . . . . ?
C10 C38 C39 C40 -14.6(13) . . . . ?
C11 N33 C40 C41 -154.0(9) . . . . ?
C14 N33 C40 C41 27.4(14) . . . . ?
C11 N33 C40 C39 29.8(12) . . . . ?
C14 N33 C40 C39 -148.9(9) . . . . ?
C44 C39 C40 C41 -11.8(13) . . . . ?
C38 C39 C40 C41 170.9(8) . . . . ?
C44 C39 C40 N33 164.5(8) . . . . ?
C38 C39 C40 N33 -12.7(12) . . . . ?
N33 C40 C41 C42 -172.3(8) . . . . ?
C39 C40 C41 C42 3.7(13) . . . . ?
C40 C41 C42 C43 5.3(12) . . . . ?
C41 C42 C43 C44 -5.7(13) . . . . ?
C42 C43 C44 C39 -2.8(14) . . . . ?
C42 C43 C44 C45 163.7(8) . . . . ?
C40 C39 C44 C43 11.4(13) . . . . ?
C38 C39 C44 C43 -171.4(8) . . . . ?
C40 C39 C44 C45 -155.8(8) . . . . ?
C38 C39 C44 C45 21.5(12) . . . . ?
C43 C44 C45 O45 11.9(13) . . . . ?
C39 C44 C45 O45 179.3(8) . . . . ?
C43 C44 C45 C46 -164.8(8) . . . . ?
C39 C44 C45 C46 2.6(11) . . . . ?
C38 C37 C46 C25 -136.0(8) . . . . ?
Pd1 C37 C46 C25 35.2(10) . . . . ?
C38 C37 C46 C45 37.2(11) . . . . ?
Pd1 C37 C46 C45 -151.7(6) . . . . ?
C26 C25 C46 C37 -39.8(12) . . . . ?
C24 C25 C46 C37 128.2(8) . . . . ?
C26 C25 C46 C45 147.0(8) . . . . ?
C24 C25 C46 C45 -44.9(10) . . . . ?
O45 C45 C46 C37 151.5(8) . . . . ?
C44 C45 C46 C37 -31.8(11) . . . . ?
O45 C45 C46 C25 -35.0(12) . . . . ?
C44 C45 C46 C25 141.7(8) . . . . ?
C4 C5 C47 C52 97.9(11) . . . . ?
C6 C5 C47 C52 -78.2(11) . . . . ?
C4 C5 C47 C48 -74.3(11) . . . . ?
C6 C5 C47 C48 109.6(10) . . . . ?
C52 C47 C48 C49 0.1(14) . . . . ?
C5 C47 C48 C49 172.5(8) . . . . ?
C47 C48 C49 C50 -2.5(15) . . . . ?
C48 C49 C50 C51 3.8(14) . . . . ?
C48 C49 C50 C53 -175.5(9) . . . . ?
C49 C50 C51 C52 -2.9(15) . . . . ?
C53 C50 C51 C52 176.4(9) . . . . ?
C48 C47 C52 C51 0.8(14) . . . . ?
C5 C47 C52 C51 -171.7(9) . . . . ?
C50 C51 C52 C47 0.6(15) . . . . ?
C16 C15 C54 C55 -143.7(9) . . . . ?
C14 C15 C54 C55 42.9(12) . . . . ?
C16 C15 C54 C59 37.8(13) . . . . ?
C14 C15 C54 C59 -135.6(9) . . . . ?
C59 C54 C55 C56 -0.9(13) . . . . ?
C15 C54 C55 C56 -179.4(8) . . . . ?
C54 C55 C56 C57 0.3(14) . . . . ?
C55 C56 C57 C58 -0.5(14) . . . . ?
C55 C56 C57 C60 179.3(8) . . . . ?
C56 C57 C58 C59 1.5(13) . . . . ?
C60 C57 C58 C59 -178.4(8) . . . . ?
C57 C58 C59 C54 -2.2(13) . . . . ?
C55 C54 C59 C58 1.9(13) . . . . ?
C15 C54 C59 C58 -179.6(8) . . . . ?
C19 C20 C61 C66 -55.6(13) . . . . ?
C21 C20 C61 C66 120.9(9) . . . . ?
C19 C20 C61 C62 127.6(9) . . . . ?
C21 C20 C61 C62 -55.9(12) . . . . ?
C66 C61 C62 C63 1.7(13) . . . . ?
C20 C61 C62 C63 178.6(9) . . . . ?
C61 C62 C63 C64 -3.2(15) . . . . ?
C62 C63 C64 C65 3.5(16) . . . . ?
C62 C63 C64 C67 -175.9(10) . . . . ?
C63 C64 C65 C66 -2.3(15) . . . . ?
C67 C64 C65 C66 177.1(10) . . . . ?
C64 C65 C66 C61 1.1(15) . . . . ?
C62 C61 C66 C65 -0.7(14) . . . . ?
C20 C61 C66 C65 -177.6(9) . . . . ?
C1 C30 C68 C69 42.7(13) . . . . ?
C29 C30 C68 C69 -136.4(9) . . . . ?
C1 C30 C68 C73 -137.3(9) . . . . ?
C29 C30 C68 C73 43.6(12) . . . . ?
C73 C68 C69 C70 3.4(13) . . . . ?
C30 C68 C69 C70 -176.5(8) . . . . ?
C68 C69 C70 C71 -3.3(14) . . . . ?
C69 C70 C71 C72 1.5(14) . . . . ?
C69 C70 C71 C74 178.5(9) . . . . ?
C70 C71 C72 C73 0.0(13) . . . . ?
C74 C71 C72 C73 -176.9(8) . . . . ?
C71 C72 C73 C68 0.3(13) . . . . ?
C69 C68 C73 C72 -2.0(13) . . . . ?
C30 C68 C73 C72 178.0(8) . . . . ?
C80 C75 C76 C77 0.6(15) . . . . ?
C75 C76 C77 C78 -1.3(16) . . . . ?
C76 C77 C78 C79 1.8(14) . . . . ?
C76 C77 C78 C81 -179.4(9) . . . . ?
C77 C78 C79 C80 -1.7(13) . . . . ?
C81 C78 C79 C80 179.5(9) . . . . ?
C76 C75 C80 C79 -0.5(14) . . . . ?
C78 C79 C80 C75 1.1(14) . . . . ?
C87 C82 C83 C84 -2.2(18) . . . . ?
C82 C83 C84 C85 1.5(18) . . . . ?
C83 C84 C85 C86 0.5(17) . . . . ?
C83 C84 C85 C88 -179.0(10) . . . . ?
C84 C85 C86 C87 -1.8(16) . . . . ?
C88 C85 C86 C87 177.7(10) . . . . ?
C83 C82 C87 C86 1.0(17) . . . . ?
C85 C86 C87 C82 1.0(16) . . . . ?

_refine_diff_density_max         0.653
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.129



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: deuterated toluene'
