# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_PDA2
_database_code_depnum_ccdc_archive 'CCDC 1892199'
loop_
_audit_author_name
_audit_author_address
'Vincent M. Lynch'
;University of Texas 
United States of America
;
_audit_update_record             
;
2019-07-19 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4 C12 H9 N3 O2 S 2-, 4 Pd 2+, 6 C3 H7 N O'
_chemical_formula_sum            'C66 H78 N18 O14 Pd4 S4'
_chemical_formula_weight         1901.30

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

_cell_length_a                   13.984(2)
_cell_length_b                   13.984(2)
_cell_length_c                   37.261(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7287(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9415
_cell_measurement_theta_min      1.55
_cell_measurement_theta_max      25.0

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_F_000             3840
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.163
_shelx_estimated_absorpt_T_min   0.913
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed fine focus tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31890
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_av_R_equivalents  0.1194
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         25.341
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3327
_reflns_number_gt                2559
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'

_computing_structure_solution    
;

Sheldrick, G. M.  (2015). SHELXT.  Acta Cryst. A71, 3-8.
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'





_refine_special_details          
;
The Pd complex is a tetramer that sits around a four-fold rotoinversion 
symmetry element at 1/2, 1/4, 3/8.  A molecule of DMF is disordered 
around a crystallographic two-fold rotation axis.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0463P)²+79.4940P] 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         3327
_refine_ls_number_parameters     275
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.47756(3) 0.36233(3) 0.41847(2) 0.01474(17) Uani 1 1 d . . . . .
S1 S 0.36325(12) 0.35341(12) 0.37238(4) 0.0182(4) Uani 1 1 d . . . . .
O1 O 0.5861(3) 0.4120(3) 0.54181(12) 0.0245(11) Uani 1 1 d . . . . .
O2 O 0.4382(4) 0.3819(4) 0.55848(12) 0.0310(12) Uani 1 1 d . . . . .
N1 N 0.3626(4) 0.3404(4) 0.44958(13) 0.0170(12) Uani 1 1 d . . . . .
N2 N 0.2721(4) 0.3185(4) 0.43627(14) 0.0204(12) Uani 1 1 d . . . . .
N3 N 0.1860(5) 0.2892(5) 0.38511(18) 0.0276(14) Uani 1 1 d . . . . .
C1 C 0.5407(5) 0.3789(4) 0.46838(17) 0.0188(14) Uani 1 1 d . . . . .
C2 C 0.4725(5) 0.3699(4) 0.49500(16) 0.0198(14) Uani 1 1 d . . . . .
C3 C 0.4933(5) 0.3867(4) 0.53338(17) 0.0197(15) Uani 1 1 d . . . . .
C4 C 0.6565(5) 0.4189(5) 0.51586(18) 0.0235(16) Uani 1 1 d . . . . .
C5 C 0.7485(5) 0.4428(5) 0.5291(2) 0.0286(17) Uani 1 1 d . . . . .
H5 H 0.757982 0.455957 0.553837 0.034 Uiso 1 1 calc R U . . .
C6 C 0.8245(5) 0.4465(5) 0.5052(2) 0.0317(18) Uani 1 1 d . . . . .
H6 H 0.886874 0.461222 0.513695 0.038 Uiso 1 1 calc R U . . .
C7 C 0.8096(5) 0.4287(5) 0.46879(19) 0.0271(16) Uani 1 1 d . . . . .
H7 H 0.861739 0.430685 0.452469 0.033 Uiso 1 1 calc R U . . .
C8 C 0.7176(5) 0.4079(5) 0.45645(19) 0.0239(16) Uani 1 1 d . . . . .
H8 H 0.708478 0.397142 0.431513 0.029 Uiso 1 1 calc R U . . .
C9 C 0.6377(5) 0.4024(4) 0.47950(18) 0.0206(15) Uani 1 1 d . . . . .
C10 C 0.3750(5) 0.3433(4) 0.48443(17) 0.0189(14) Uani 1 1 d . . . . .
C11 C 0.2667(5) 0.3146(5) 0.40114(16) 0.0172(14) Uani 1 1 d . . . . .
C12 C 0.2949(5) 0.3207(5) 0.51017(18) 0.0253(16) Uani 1 1 d . . . . .
H12A H 0.243900 0.286798 0.497404 0.038 Uiso 1 1 calc R U . . .
H12B H 0.269572 0.380331 0.520198 0.038 Uiso 1 1 calc R U . . .
H12C H 0.319261 0.280358 0.529635 0.038 Uiso 1 1 calc R U . . .
O1B O 0.010(3) 0.241(3) 0.4248(2) 0.033(6) Uani 0.5 1 d . U P A -1
N1B N 0.003(5) 0.244(4) 0.4859(3) 0.034(4) Uani 0.5 1 d . U P A -1
C1B C -0.0295(11) 0.2136(11) 0.4550(4) 0.035(3) Uani 0.5 1 d . U P A -1
H1B H -0.082564 0.171194 0.454316 0.042 Uiso 0.5 1 calc R U P A -1
C2B C 0.0545(11) 0.3486(12) 0.4830(5) 0.040(4) Uani 0.5 1 d . U P A -1
H2B1 H 0.019244 0.388644 0.465917 0.060 Uiso 0.5 1 calc R U P A -1
H2B2 H 0.120437 0.340486 0.474611 0.060 Uiso 0.5 1 calc R U P A -1
H2B3 H 0.054697 0.379319 0.506603 0.060 Uiso 0.5 1 calc R U P A -1
C3B C -0.0265(13) 0.2175(12) 0.5221(4) 0.044(4) Uani 0.5 1 d . U P A -1
H3B1 H -0.061074 0.156585 0.521378 0.065 Uiso 0.5 1 calc R U P A -1
H3B2 H -0.068251 0.267330 0.531860 0.065 Uiso 0.5 1 calc R U P A -1
H3B3 H 0.030247 0.210918 0.537320 0.065 Uiso 0.5 1 calc R U P A -1
O1A O 0.9989(6) 0.4666(8) 0.5675(2) 0.102(3) Uani 1 1 d . . . . .
N1A N 0.9521(8) 0.4863(8) 0.6251(2) 0.089(3) Uani 1 1 d . . . . .
C3A C 0.8747(12) 0.4611(11) 0.6517(3) 0.120(6) Uani 1 1 d . . . . .
H3A1 H 0.829375 0.416688 0.640561 0.180 Uiso 1 1 calc R U . . .
H3A2 H 0.841038 0.519317 0.659051 0.180 Uiso 1 1 calc R U . . .
H3A3 H 0.903566 0.430785 0.672831 0.180 Uiso 1 1 calc R U . . .
C1A C 0.9506(9) 0.4504(12) 0.5933(3) 0.102(5) Uani 1 1 d . . . . .
H1A H 0.902957 0.402908 0.589739 0.122 Uiso 1 1 calc R U . . .
C2A C 1.0272(9) 0.5612(8) 0.6349(3) 0.082(4) Uani 1 1 d . . . . .
H2A1 H 1.076493 0.563102 0.616186 0.123 Uiso 1 1 calc R U . . .
H2A2 H 1.056549 0.544535 0.657900 0.123 Uiso 1 1 calc R U . . .
H2A3 H 0.996647 0.624096 0.636744 0.123 Uiso 1 1 calc R U . . .
H3NA H 0.136(5) 0.275(5) 0.3955(18) 0.014(19) Uiso 1 1 d . . . . .
H3NB H 0.175(6) 0.292(6) 0.363(2) 0.04(2) Uiso 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 N1 2.006(5) . ?
Pd1 C1 2.071(6) . ?
Pd1 S1 2.3495(16) . ?
Pd1 S1 2.3521(17) 10_666 ?
Pd1 Pd1 3.2038(11) 7_554 ?
S1 C11 1.807(7) . ?
O1 C3 1.381(8) . ?
O1 C4 1.383(8) . ?
O2 C3 1.214(8) . ?
N1 C10 1.311(8) . ?
N1 N2 1.393(7) . ?
N2 C11 1.312(8) . ?
N3 C11 1.326(9) . ?
N3 H3NA 0.82(7) . ?
N3 H3NB 0.84(9) . ?
C1 C2 1.381(9) . ?
C1 C9 1.456(9) . ?
C2 C10 1.468(9) . ?
C2 C3 1.478(8) . ?
C4 C9 1.399(9) . ?
C4 C5 1.419(10) . ?
C5 C6 1.386(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.396(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.396(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.412(10) . ?
C8 H8 0.9500 . ?
C10 C12 1.508(9) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O1B C1B 1.31(3) . ?
N1B C1B 1.31(4) . ?
N1B C3B 1.45(4) . ?
N1B C2B 1.64(7) . ?
C1B H1B 0.9500 . ?
C2B H2B1 0.9800 . ?
C2B H2B2 0.9800 . ?
C2B H2B3 0.9800 . ?
C3B H3B1 0.9800 . ?
C3B H3B2 0.9800 . ?
C3B H3B3 0.9800 . ?
O1A C1A 1.196(13) . ?
N1A C1A 1.286(14) . ?
N1A C3A 1.510(15) . ?
N1A C2A 1.527(14) . ?
C3A H3A1 0.9800 . ?
C3A H3A2 0.9800 . ?
C3A H3A3 0.9800 . ?
C1A H1A 0.9500 . ?
C2A H2A1 0.9800 . ?
C2A H2A2 0.9800 . ?
C2A H2A3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 C1 80.8(2) . . ?
N1 Pd1 S1 82.46(15) . . ?
C1 Pd1 S1 162.19(19) . . ?
N1 Pd1 S1 174.96(15) . 10_666 ?
C1 Pd1 S1 104.23(19) . 10_666 ?
S1 Pd1 S1 92.51(4) . 10_666 ?
N1 Pd1 Pd1 90.43(15) . 7_554 ?
C1 Pd1 Pd1 91.49(16) . 7_554 ?
S1 Pd1 Pd1 94.66(4) . 7_554 ?
S1 Pd1 Pd1 89.76(4) 10_666 7_554 ?
C11 S1 Pd1 95.2(2) . . ?
C11 S1 Pd1 105.5(2) . 16_656 ?
Pd1 S1 Pd1 114.46(7) . 16_656 ?
C3 O1 C4 121.8(5) . . ?
C10 N1 N2 118.7(5) . . ?
C10 N1 Pd1 117.5(4) . . ?
N2 N1 Pd1 123.8(4) . . ?
C11 N2 N1 114.6(5) . . ?
C11 N3 H3NA 125(5) . . ?
C11 N3 H3NB 126(6) . . ?
H3NA N3 H3NB 108(7) . . ?
C2 C1 C9 117.3(6) . . ?
C2 C1 Pd1 109.9(5) . . ?
C9 C1 Pd1 132.7(5) . . ?
C1 C2 C10 118.1(5) . . ?
C1 C2 C3 123.0(6) . . ?
C10 C2 C3 118.8(6) . . ?
O2 C3 O1 115.8(6) . . ?
O2 C3 C2 127.7(6) . . ?
O1 C3 C2 116.4(6) . . ?
O1 C4 C9 122.1(6) . . ?
O1 C4 C5 114.8(6) . . ?
C9 C4 C5 123.0(7) . . ?
C6 C5 C4 118.8(7) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C7 120.1(7) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 119.7(7) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 122.7(6) . . ?
C7 C8 H8 118.6 . . ?
C9 C8 H8 118.6 . . ?
C4 C9 C8 115.6(6) . . ?
C4 C9 C1 119.2(6) . . ?
C8 C9 C1 125.3(6) . . ?
N1 C10 C2 113.4(6) . . ?
N1 C10 C12 121.7(6) . . ?
C2 C10 C12 124.9(6) . . ?
N2 C11 N3 120.6(6) . . ?
N2 C11 S1 122.4(5) . . ?
N3 C11 S1 116.7(5) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C1B N1B C3B 130(6) . . ?
C1B N1B C2B 112(3) . . ?
C3B N1B C2B 114(3) . . ?
N1B C1B O1B 121(4) . . ?
N1B C1B H1B 119.5 . . ?
O1B C1B H1B 119.5 . . ?
N1B C2B H2B1 109.5 . . ?
N1B C2B H2B2 109.5 . . ?
H2B1 C2B H2B2 109.5 . . ?
N1B C2B H2B3 109.5 . . ?
H2B1 C2B H2B3 109.5 . . ?
H2B2 C2B H2B3 109.5 . . ?
N1B C3B H3B1 109.5 . . ?
N1B C3B H3B2 109.5 . . ?
H3B1 C3B H3B2 109.5 . . ?
N1B C3B H3B3 109.5 . . ?
H3B1 C3B H3B3 109.5 . . ?
H3B2 C3B H3B3 109.5 . . ?
C1A N1A C3A 120.1(12) . . ?
C1A N1A C2A 119.9(11) . . ?
C3A N1A C2A 119.8(9) . . ?
N1A C3A H3A1 109.5 . . ?
N1A C3A H3A2 109.5 . . ?
H3A1 C3A H3A2 109.5 . . ?
N1A C3A H3A3 109.5 . . ?
H3A1 C3A H3A3 109.5 . . ?
H3A2 C3A H3A3 109.5 . . ?
O1A C1A N1A 131.0(15) . . ?
O1A C1A H1A 114.5 . . ?
N1A C1A H1A 114.5 . . ?
N1A C2A H2A1 109.5 . . ?
N1A C2A H2A2 109.5 . . ?
H2A1 C2A H2A2 109.5 . . ?
N1A C2A H2A3 109.5 . . ?
H2A1 C2A H2A3 109.5 . . ?
H2A2 C2A H2A3 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
C10 N1 N2 C11 -178.2(6) . . . . ?
Pd1 N1 N2 C11 -1.1(7) . . . . ?
C9 C1 C2 C10 -178.1(5) . . . . ?
Pd1 C1 C2 C10 5.2(7) . . . . ?
C9 C1 C2 C3 2.4(9) . . . . ?
Pd1 C1 C2 C3 -174.3(5) . . . . ?
C4 O1 C3 O2 179.2(6) . . . . ?
C4 O1 C3 C2 -1.6(8) . . . . ?
C1 C2 C3 O2 178.9(6) . . . . ?
C10 C2 C3 O2 -0.6(10) . . . . ?
C1 C2 C3 O1 -0.2(9) . . . . ?
C10 C2 C3 O1 -179.8(5) . . . . ?
C3 O1 C4 C9 1.1(9) . . . . ?
C3 O1 C4 C5 -178.2(5) . . . . ?
O1 C4 C5 C6 176.8(6) . . . . ?
C9 C4 C5 C6 -2.5(10) . . . . ?
C4 C5 C6 C7 1.2(10) . . . . ?
C5 C6 C7 C8 0.6(10) . . . . ?
C6 C7 C8 C9 -1.1(10) . . . . ?
O1 C4 C9 C8 -177.3(6) . . . . ?
C5 C4 C9 C8 1.9(9) . . . . ?
O1 C4 C9 C1 1.2(9) . . . . ?
C5 C4 C9 C1 -179.6(6) . . . . ?
C7 C8 C9 C4 -0.1(10) . . . . ?
C7 C8 C9 C1 -178.5(6) . . . . ?
C2 C1 C9 C4 -2.9(9) . . . . ?
Pd1 C1 C9 C4 173.0(5) . . . . ?
C2 C1 C9 C8 175.5(6) . . . . ?
Pd1 C1 C9 C8 -8.7(10) . . . . ?
N2 N1 C10 C2 -178.3(5) . . . . ?
Pd1 N1 C10 C2 4.5(7) . . . . ?
N2 N1 C10 C12 1.8(9) . . . . ?
Pd1 N1 C10 C12 -175.5(4) . . . . ?
C1 C2 C10 N1 -6.5(8) . . . . ?
C3 C2 C10 N1 173.0(6) . . . . ?
C1 C2 C10 C12 173.4(6) . . . . ?
C3 C2 C10 C12 -7.1(9) . . . . ?
N1 N2 C11 N3 176.2(6) . . . . ?
N1 N2 C11 S1 -9.6(8) . . . . ?
Pd1 S1 C11 N2 13.0(6) . . . . ?
Pd1 S1 C11 N2 130.2(5) 16_656 . . . ?
Pd1 S1 C11 N3 -172.6(5) . . . . ?
Pd1 S1 C11 N3 -55.4(5) 16_656 . . . ?
C3B N1B C1B O1B -176(4) . . . . ?
C2B N1B C1B O1B 27(6) . . . . ?
C3A N1A C1A O1A 172.7(16) . . . . ?
C2A N1A C1A O1A -2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2B H2B1 O1A 0.98 2.39 3.28(2) 151.1 9_666
C2B H2B2 N2 0.98 2.58 3.531(17) 164.8 .
N3 H3NA O1B 0.82(7) 2.12(9) 2.94(5) 177(7) .
N3 H3NA O1B 0.82(7) 2.33(8) 3.15(4) 172(6) 7_454
N3 H3NB O2 0.84(9) 2.14(9) 2.971(8) 172(8) 4_454

_refine_diff_density_max         0.987
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.134

####################################################################### 
# 
# 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_PDA3
_database_code_depnum_ccdc_archive 'CCDC 1892200'
loop_
_audit_author_name
_audit_author_address
'Vincent M. Lynch'
;University of Texas 
United States of America
;
_audit_update_record             
;
2019-07-19 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H44 N12 O8 Pd4 S4'
_chemical_formula_weight         1518.83

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

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

_cell_length_a                   14.3910(17)
_cell_length_b                   14.3910(17)
_cell_length_c                   36.358(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7530(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4390
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.5

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_F_000             3008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.099
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
Abscor.  T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed fine focus tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with a Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29266
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         3.005
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4310
_reflns_number_gt                3416
_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.
;

# SQUEEZE RESULTS (Version = 300517)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.118 0.714 0.248 2883 991 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?




_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'

_computing_structure_solution    
;

SHELXT. G. M. Sheldrick (2015). Acta Cryst. A71, 3-8.
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 
  Two molecules of what appeared to be methanol and DMF were found to be 
badly disordered.  Attempts 
to model the disorder were unsatisfactory.  The contributions to the 
scattering factors due to these solvent molecules were removed by use of 
the utility SQUEEZE (Sluis and Spek, 1990) in PLATON (Spek, 2009).  
PLATON was used as incorporated in WinGX (Farrugia, 1999).

;





_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0210P)²+67.6145P] 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         4310
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.1120
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
C1 C 0.6283(3) 0.7856(4) 0.72086(12) 0.0307(11) Uani 1 1 d . . . . .
C2 C 0.6597(3) 0.8770(4) 0.73267(13) 0.0350(13) Uani 1 1 d . . . . .
C3 C 0.6732(4) 0.9538(4) 0.70958(15) 0.0407(13) Uani 1 1 d . . . . .
H3 H 0.663828 0.946856 0.683864 0.049 Uiso 1 1 calc R U . . .
C4 C 0.6999(4) 1.0393(4) 0.72327(16) 0.0459(15) Uani 1 1 d . . . . .
H4 H 0.707490 1.090619 0.707103 0.055 Uiso 1 1 calc R U . . .
C5 C 0.7155(4) 1.0502(5) 0.76083(17) 0.0493(16) Uani 1 1 d . . . . .
H5 H 0.734832 1.108681 0.770204 0.059 Uiso 1 1 calc R U . . .
C6 C 0.7033(4) 0.9770(5) 0.78419(16) 0.0489(16) Uani 1 1 d . . . . .
H6 H 0.714553 0.984045 0.809785 0.059 Uiso 1 1 calc R U . . .
C7 C 0.6743(4) 0.8930(4) 0.77022(14) 0.0387(13) Uani 1 1 d . . . . .
C8 C 0.6330(4) 0.7368(4) 0.78655(14) 0.0397(14) Uani 1 1 d . . . . .
C9 C 0.6146(3) 0.7184(4) 0.74766(12) 0.0326(12) Uani 1 1 d . . . . .
C10 C 0.5836(4) 0.6256(4) 0.73651(13) 0.0346(13) Uani 1 1 d . . . . .
C11 C 0.5561(4) 0.5261(4) 0.65076(13) 0.0334(12) Uani 1 1 d . . . . .
C12 C 0.5570(4) 0.5490(4) 0.76189(13) 0.0398(13) Uani 1 1 d . . . . .
H12A H 0.519396 0.503251 0.748570 0.060 Uiso 1 1 calc R U . . .
H12B H 0.520797 0.574356 0.782408 0.060 Uiso 1 1 calc R U . . .
H12C H 0.613139 0.518965 0.771417 0.060 Uiso 1 1 calc R U . . .
C13 C 0.4855(6) 0.3727(4) 0.65280(17) 0.0604(19) Uani 1 1 d . . . . .
H13A H 0.534442 0.339977 0.666324 0.091 Uiso 1 1 calc R U . . .
H13B H 0.456802 0.330275 0.635047 0.091 Uiso 1 1 calc R U . . .
H13C H 0.438200 0.394860 0.670114 0.091 Uiso 1 1 calc R U . . .
N1 N 0.5813(3) 0.6159(3) 0.70086(10) 0.0303(10) Uani 1 1 d . . . . .
N2 N 0.5554(3) 0.5298(3) 0.68667(11) 0.0363(11) Uani 1 1 d . . . . .
N3 N 0.5251(4) 0.4507(3) 0.63360(11) 0.0422(12) Uani 1 1 d . . . . .
H3N H 0.529009 0.448299 0.609468 0.051 Uiso 1 1 calc R U . . .
O1 O 0.6616(3) 0.8239(3) 0.79593(9) 0.0429(10) Uani 1 1 d . . . . .
O2 O 0.6265(3) 0.6812(3) 0.81177(10) 0.0507(11) Uani 1 1 d . . . . .
Pd1 Pd 0.60779(3) 0.72704(3) 0.66964(2) 0.02894(12) Uani 1 1 d . . . . .
S1 S 0.59943(10) 0.61793(10) 0.62180(3) 0.0336(3) 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
C1 C9 1.387(7) . ?
C1 C2 1.455(7) . ?
C1 Pd1 2.065(5) . ?
C2 C7 1.400(7) . ?
C2 C3 1.402(8) . ?
C3 C4 1.382(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.364(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(8) . ?
C6 H6 0.9500 . ?
C7 O1 1.377(7) . ?
C8 O2 1.220(7) . ?
C8 O1 1.362(7) . ?
C8 C9 1.463(7) . ?
C9 C10 1.465(8) . ?
C10 N1 1.304(6) . ?
C10 C12 1.488(7) . ?
C11 N2 1.306(6) . ?
C11 N3 1.329(7) . ?
C11 S1 1.801(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N3 1.439(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N1 N2 1.394(6) . ?
N1 Pd1 1.997(4) . ?
N3 H3N 0.8800 . ?
Pd1 S1 2.3439(14) 12_767 ?
Pd1 S1 2.3463(13) . ?
Pd1 Pd1 3.1719(9) 6_564 ?

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 C1 C2 117.8(4) . . ?
C9 C1 Pd1 109.2(4) . . ?
C2 C1 Pd1 132.8(4) . . ?
C7 C2 C3 115.7(5) . . ?
C7 C2 C1 118.9(5) . . ?
C3 C2 C1 125.4(5) . . ?
C4 C3 C2 121.7(5) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.8(6) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.2(6) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.2(5) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 O1 115.1(5) . . ?
C6 C7 C2 123.4(6) . . ?
O1 C7 C2 121.5(5) . . ?
O2 C8 O1 116.0(5) . . ?
O2 C8 C9 126.4(6) . . ?
O1 C8 C9 117.6(5) . . ?
C1 C9 C8 121.8(5) . . ?
C1 C9 C10 119.0(4) . . ?
C8 C9 C10 119.2(5) . . ?
N1 C10 C9 112.3(5) . . ?
N1 C10 C12 122.1(5) . . ?
C9 C10 C12 125.6(4) . . ?
N2 C11 N3 120.0(5) . . ?
N2 C11 S1 123.9(4) . . ?
N3 C11 S1 116.2(4) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 N1 N2 118.0(4) . . ?
C10 N1 Pd1 118.3(4) . . ?
N2 N1 Pd1 123.6(3) . . ?
C11 N2 N1 113.8(4) . . ?
C11 N3 C13 122.8(5) . . ?
C11 N3 H3N 118.6 . . ?
C13 N3 H3N 118.6 . . ?
C8 O1 C7 122.3(4) . . ?
N1 Pd1 C1 80.87(19) . . ?
N1 Pd1 S1 174.37(12) . 12_767 ?
C1 Pd1 S1 104.58(16) . 12_767 ?
N1 Pd1 S1 82.87(12) . . ?
C1 Pd1 S1 161.58(15) . . ?
S1 Pd1 S1 91.95(4) 12_767 . ?
N1 Pd1 Pd1 88.88(12) . 6_564 ?
C1 Pd1 Pd1 93.14(13) . 6_564 ?
S1 Pd1 Pd1 89.39(4) 12_767 6_564 ?
S1 Pd1 Pd1 95.12(4) . 6_564 ?
C11 S1 Pd1 102.99(18) . 15_566 ?
C11 S1 Pd1 94.31(17) . . ?
Pd1 S1 Pd1 114.53(6) 15_566 . ?

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
C9 C1 C2 C7 -0.2(7) . . . . ?
Pd1 C1 C2 C7 -174.4(4) . . . . ?
C9 C1 C2 C3 -177.2(5) . . . . ?
Pd1 C1 C2 C3 8.6(8) . . . . ?
C7 C2 C3 C4 0.4(8) . . . . ?
C1 C2 C3 C4 177.5(5) . . . . ?
C2 C3 C4 C5 1.2(9) . . . . ?
C3 C4 C5 C6 -1.0(9) . . . . ?
C4 C5 C6 C7 -0.7(9) . . . . ?
C5 C6 C7 O1 -178.4(5) . . . . ?
C5 C6 C7 C2 2.4(9) . . . . ?
C3 C2 C7 C6 -2.2(8) . . . . ?
C1 C2 C7 C6 -179.5(5) . . . . ?
C3 C2 C7 O1 178.7(5) . . . . ?
C1 C2 C7 O1 1.4(8) . . . . ?
C2 C1 C9 C8 -1.5(7) . . . . ?
Pd1 C1 C9 C8 174.0(4) . . . . ?
C2 C1 C9 C10 -179.6(4) . . . . ?
Pd1 C1 C9 C10 -4.1(6) . . . . ?
O2 C8 C9 C1 -177.0(5) . . . . ?
O1 C8 C9 C1 2.0(7) . . . . ?
O2 C8 C9 C10 1.1(8) . . . . ?
O1 C8 C9 C10 -179.9(4) . . . . ?
C1 C9 C10 N1 6.3(7) . . . . ?
C8 C9 C10 N1 -171.9(4) . . . . ?
C1 C9 C10 C12 -173.6(5) . . . . ?
C8 C9 C10 C12 8.2(8) . . . . ?
C9 C10 N1 N2 178.3(4) . . . . ?
C12 C10 N1 N2 -1.8(7) . . . . ?
C9 C10 N1 Pd1 -5.3(6) . . . . ?
C12 C10 N1 Pd1 174.6(4) . . . . ?
N3 C11 N2 N1 -174.2(4) . . . . ?
S1 C11 N2 N1 7.1(7) . . . . ?
C10 N1 N2 C11 -179.3(5) . . . . ?
Pd1 N1 N2 C11 4.5(6) . . . . ?
N2 C11 N3 C13 3.4(9) . . . . ?
S1 C11 N3 C13 -177.9(5) . . . . ?
O2 C8 O1 C7 178.3(5) . . . . ?
C9 C8 O1 C7 -0.8(7) . . . . ?
C6 C7 O1 C8 179.9(5) . . . . ?
C2 C7 O1 C8 -0.8(8) . . . . ?
N2 C11 S1 Pd1 -128.6(4) . . . 15_566 ?
N3 C11 S1 Pd1 52.6(4) . . . 15_566 ?
N2 C11 S1 Pd1 -12.2(5) . . . . ?
N3 C11 S1 Pd1 169.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N O2 0.88 2.10 2.891(6) 149.4 7_544

_refine_diff_density_max         0.901
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.106



####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1892201'
loop_
_audit_author_name
_audit_author_address
'Vincent M. Lynch'
;University of Texas 
United States of America
;
_audit_update_record             
;
2019-07-19 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_RINTA01_shelx               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The data crystals were very small and had considerable solvent 
voids in the unit cell.  Unfortunately, the crystals had dried out on 
transport.  The loss of solvent had a major impact on the crystal 
quality.  The data crystal used in this report was the best of several 
samples that were tried.
;
_vrf_PLAT020_shelx               
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.295 Report
RESPONSE: see above
;
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.930 Why?  
RESPONSE: Due to the poor scattering power of the data crystal and the 
limited instrument time available, it was decided to limit the 
resolution of the data set so that longer exposure times per frame 
could be used.
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on       Pd2       2.30 eA-3  
RESPONSE: The data crystal was of marginal quality.
;
_vrf_PLAT026_shelx               
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        36% Check 
RESPONSE: see above
;
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03146 Ang.  
RESPONSE: see above
;
_vrf_PLAT369_shelx               
;
PROBLEM: Long   C(sp2)-C(sp2) Bond  C44      - C45      .       1.57 Ang.  
RESPONSE: see above
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         18 Note  
RESPONSE: These reflections were probably blocked by the beamstop.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.595        798 Report
RESPONSE: These reflections were probably missed during data collection.
;
_vrf_PLAT919_shelx               
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check 
RESPONSE: This is the 020 reflection.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4 C14 H13 N3 O2 S 2-, 4 Pd 2+'
_chemical_formula_sum            'C56 H52 N12 O8 Pd4 S4'
_chemical_formula_weight         1574.93

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'

_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                   15.050(16)
_cell_length_b                   15.307(16)
_cell_length_c                   17.034(18)
_cell_angle_alpha                96.49(3)
_cell_angle_beta                 95.70(3)
_cell_angle_gamma                114.56(2)
_cell_volume                     3499(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1465
_cell_measurement_theta_min      3.50
_cell_measurement_theta_max      24.7

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.185
_shelx_estimated_absorpt_T_min   0.922
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with a Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35302
_diffrn_reflns_av_unetI/netI     0.3733
_diffrn_reflns_av_R_equivalents  0.2951
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.889
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.930
_reflns_number_total             11507
_reflns_number_gt                4169
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'

_computing_structure_solution    
;

Sir2004.  Burla M.C., Caliandro, R., Camalli M., Carrozzini, B., Cascarano G.L., 
De Caro, L., Giacovazzo C., Polidori G., Spagna R. 
;
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 
  A large region of the unit cell contained some highly disordered solvent. 
Attempts to model the disorder were unsatisfactory.  The contributions to the 
scattering factors due to these solvent molecules were removed by use of 
the utility SQUEEZE (Sluis and Spek, 1990) in PLATON (Spek, 2009).  
PLATON was used as incorporated in WinGX (Farrugia, 1999).

;










_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0753P)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         11507
_refine_ls_number_parameters     764
_refine_ls_number_restraints     1333
_refine_ls_R_factor_all          0.2560
_refine_ls_R_factor_gt           0.1236
_refine_ls_wR_factor_ref         0.3128
_refine_ls_wR_factor_gt          0.2552
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      0.973
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4679(14) 0.8489(14) 0.4578(11) 0.032(4) Uani 1 1 d . U . . .
C2 C 0.4114(14) 0.8732(13) 0.5094(11) 0.032(4) Uani 1 1 d . U . . .
C3 C 0.4580(15) 0.9276(14) 0.5952(12) 0.040(5) Uani 1 1 d . U . . .
C4 C 0.6128(14) 0.9298(14) 0.5694(11) 0.033(4) Uani 1 1 d . U . . .
C5 C 0.7167(14) 0.9654(14) 0.6054(12) 0.039(5) Uani 1 1 d . U . . .
H5 H 0.740752 1.002720 0.657826 0.047 Uiso 1 1 calc R U . . .
C6 C 0.7792(15) 0.9431(14) 0.5606(12) 0.040(5) Uani 1 1 d . U . . .
H6 H 0.846394 0.963085 0.583042 0.049 Uiso 1 1 calc R U . . .
C7 C 0.7408(14) 0.8879(14) 0.4775(11) 0.037(5) Uani 1 1 d . U . . .
H7 H 0.783898 0.874178 0.446379 0.044 Uiso 1 1 calc R U . . .
C8 C 0.6398(13) 0.8558(13) 0.4448(11) 0.029(4) Uani 1 1 d . U . . .
H8 H 0.615195 0.816923 0.393045 0.035 Uiso 1 1 calc R U . . .
C9 C 0.5733(15) 0.8805(16) 0.4879(12) 0.046(5) Uani 1 1 d . U . . .
C10 C 0.3023(15) 0.8417(15) 0.4852(12) 0.039(4) Uani 1 1 d . U . . .
C11 C 0.2320(15) 0.8629(16) 0.5353(12) 0.050(6) Uani 1 1 d . U . . .
H11A H 0.166963 0.840529 0.502237 0.075 Uiso 1 1 calc R U . . .
H11B H 0.258957 0.933208 0.554602 0.075 Uiso 1 1 calc R U . . .
H11C H 0.225055 0.828569 0.581181 0.075 Uiso 1 1 calc R U . . .
C12 C 0.1532(13) 0.7252(14) 0.2946(11) 0.030(4) Uani 1 1 d . U . . .
C13 C -0.0219(14) 0.6911(15) 0.2966(12) 0.050(5) Uani 1 1 d D U . . .
H13A H -0.078788 0.682822 0.256902 0.060 Uiso 1 1 calc R U . . .
H13B H 0.000781 0.754761 0.332057 0.060 Uiso 1 1 calc R U . . .
C14 C -0.0551(16) 0.6094(16) 0.3464(13) 0.065(6) Uani 1 1 d D U . . .
H14A H -0.057318 0.550033 0.315994 0.097 Uiso 1 1 calc R U . . .
H14B H -0.121096 0.596953 0.358733 0.097 Uiso 1 1 calc R U . . .
H14C H -0.008142 0.628915 0.396336 0.097 Uiso 1 1 calc R U . . .
C15 C 0.3394(15) 0.6264(14) 0.5274(11) 0.037(4) Uani 1 1 d . U . . .
C16 C 0.4353(14) 0.6615(15) 0.5746(11) 0.040(5) Uani 1 1 d . U . . .
C17 C 0.4549(15) 0.7096(15) 0.6592(12) 0.038(4) Uani 1 1 d . U . . .
C18 C 0.2835(16) 0.6762(15) 0.6498(12) 0.043(5) Uani 1 1 d . U . . .
C19 C 0.2109(16) 0.6888(16) 0.6918(13) 0.051(5) Uani 1 1 d . U . . .
H19 H 0.228139 0.719420 0.746365 0.062 Uiso 1 1 calc R U . . .
C20 C 0.1133(15) 0.6552(14) 0.6511(12) 0.042(5) Uani 1 1 d . U . . .
H20 H 0.063912 0.660238 0.679384 0.051 Uiso 1 1 calc R U . . .
C21 C 0.0886(15) 0.6153(14) 0.5713(12) 0.040(5) Uani 1 1 d . U . . .
H21 H 0.023563 0.596570 0.544047 0.049 Uiso 1 1 calc R U . . .
C22 C 0.1641(16) 0.6015(16) 0.5274(13) 0.052(5) Uani 1 1 d . U . . .
H22 H 0.145758 0.568808 0.473411 0.062 Uiso 1 1 calc R U . . .
C23 C 0.2623(15) 0.6370(15) 0.5661(12) 0.040(4) Uani 1 1 d . U . . .
C24 C 0.5149(14) 0.6474(14) 0.5370(12) 0.034(4) Uani 1 1 d . U . . .
C25 C 0.6178(13) 0.6706(13) 0.5813(11) 0.031(5) Uani 1 1 d . U . . .
H25A H 0.648188 0.636271 0.549675 0.047 Uiso 1 1 calc R U . . .
H25B H 0.611862 0.649510 0.633509 0.047 Uiso 1 1 calc R U . . .
H25C H 0.659329 0.741037 0.589073 0.047 Uiso 1 1 calc R U . . .
C26 C 0.5210(16) 0.5484(16) 0.3382(12) 0.047(5) Uani 1 1 d . U . . .
C27 C 0.6958(13) 0.5820(14) 0.3260(14) 0.063(6) Uani 1 1 d D U . . .
H27A H 0.728798 0.546555 0.298075 0.076 Uiso 1 1 calc R U . . .
H27B H 0.706386 0.579214 0.383745 0.076 Uiso 1 1 calc R U . . .
C28 C 0.7419(16) 0.6880(14) 0.3140(14) 0.067(7) Uani 1 1 d D U . . .
H28A H 0.734907 0.690746 0.256632 0.100 Uiso 1 1 calc R U . . .
H28B H 0.812248 0.718680 0.337292 0.100 Uiso 1 1 calc R U . . .
H28C H 0.708127 0.722827 0.340420 0.100 Uiso 1 1 calc R U . . .
C29 C 0.1511(14) 0.5221(15) 0.0674(12) 0.040(4) Uani 1 1 d . U . . .
C30 C 0.1256(15) 0.4211(16) 0.0364(13) 0.046(4) Uani 1 1 d . U . . .
C31 C 0.0990(15) 0.3866(17) -0.0533(13) 0.044(4) Uani 1 1 d . U . . .
C32 C 0.1081(14) 0.5480(15) -0.0744(12) 0.035(4) Uani 1 1 d . U . . .
C33 C 0.0946(14) 0.5998(15) -0.1338(12) 0.037(4) Uani 1 1 d . U . . .
H33 H 0.075378 0.570158 -0.188554 0.045 Uiso 1 1 calc R U . . .
C34 C 0.1104(14) 0.6984(15) -0.1097(12) 0.045(5) Uani 1 1 d . U . . .
H34 H 0.094750 0.732566 -0.147891 0.053 Uiso 1 1 calc R U . . .
C35 C 0.1505(16) 0.7468(17) -0.0268(13) 0.051(5) Uani 1 1 d . U . . .
H35 H 0.167795 0.814157 -0.011337 0.061 Uiso 1 1 calc R U . . .
C36 C 0.1632(15) 0.6884(15) 0.0317(13) 0.045(5) Uani 1 1 d . U . . .
H36 H 0.184520 0.717563 0.086527 0.054 Uiso 1 1 calc R U . . .
C37 C 0.1443(14) 0.5869(15) 0.0087(11) 0.037(4) Uani 1 1 d . U . . .
C38 C 0.1191(14) 0.3525(15) 0.0959(13) 0.042(4) Uani 1 1 d . U . . .
C39 C 0.0958(16) 0.2442(15) 0.0722(14) 0.059(6) Uani 1 1 d . U . . .
H39A H 0.133018 0.237019 0.029826 0.089 Uiso 1 1 calc R U . . .
H39B H 0.024729 0.206428 0.052731 0.089 Uiso 1 1 calc R U . . .
H39C H 0.114801 0.220169 0.118993 0.089 Uiso 1 1 calc R U . . .
C40 C 0.1497(16) 0.3926(18) 0.3085(15) 0.057(4) Uani 1 1 d . U . . .
C41 C 0.104(2) 0.2388(16) 0.3756(15) 0.092(7) Uani 1 1 d D U . . .
H41A H 0.157261 0.219508 0.366163 0.110 Uiso 1 1 calc R U . . .
H41B H 0.046391 0.202046 0.332168 0.110 Uiso 1 1 calc R U . . .
C42 C 0.073(2) 0.220(2) 0.4574(15) 0.095(9) Uani 1 1 d D U . . .
H42A H 0.124472 0.268665 0.499640 0.142 Uiso 1 1 calc R U . . .
H42B H 0.066372 0.154519 0.464900 0.142 Uiso 1 1 calc R U . . .
H42C H 0.010256 0.223025 0.460161 0.142 Uiso 1 1 calc R U . . .
C43 C 0.3812(13) 0.4914(15) 0.0761(12) 0.035(4) Uani 1 1 d . U . . .
C44 C 0.3826(15) 0.5361(16) 0.0055(13) 0.045(4) Uani 1 1 d . U . . .
C45 C 0.3647(16) 0.4699(18) -0.0776(14) 0.049(5) Uani 1 1 d . U . . .
C46 C 0.3528(17) 0.3324(18) -0.0110(14) 0.055(5) Uani 1 1 d . U . . .
C47 C 0.3388(18) 0.2378(18) -0.0247(16) 0.068(6) Uani 1 1 d . U . . .
H47 H 0.328125 0.204697 -0.077832 0.082 Uiso 1 1 calc R U . . .
C48 C 0.3403(18) 0.1894(19) 0.0411(16) 0.072(6) Uani 1 1 d . U . . .
H48 H 0.333430 0.124338 0.033228 0.086 Uiso 1 1 calc R U . . .
C49 C 0.3527(17) 0.2418(17) 0.1205(15) 0.062(5) Uani 1 1 d . U . . .
H49 H 0.350906 0.209989 0.165516 0.074 Uiso 1 1 calc R U . . .
C50 C 0.3666(15) 0.3342(16) 0.1309(14) 0.048(5) Uani 1 1 d . U . . .
H50 H 0.375807 0.366596 0.184075 0.057 Uiso 1 1 calc R U . . .
C51 C 0.3686(15) 0.3885(16) 0.0664(13) 0.044(4) Uani 1 1 d . U . . .
C52 C 0.3952(15) 0.6368(16) 0.0105(12) 0.044(4) Uani 1 1 d . U . . .
C53 C 0.3840(16) 0.6911(16) -0.0611(12) 0.054(6) Uani 1 1 d . U . . .
H53A H 0.402062 0.759571 -0.040087 0.081 Uiso 1 1 calc R U . . .
H53B H 0.315295 0.659891 -0.088625 0.081 Uiso 1 1 calc R U . . .
H53C H 0.427855 0.687325 -0.098899 0.081 Uiso 1 1 calc R U . . .
C54 C 0.4726(14) 0.8218(16) 0.1792(12) 0.042(4) Uani 1 1 d . U . . .
C55 C 0.467(2) 0.9788(19) 0.1424(16) 0.093(8) Uani 1 1 d D U . . .
H55A H 0.447686 1.025588 0.172659 0.111 Uiso 1 1 calc R U . . .
H55B H 0.410939 0.935563 0.099776 0.111 Uiso 1 1 calc R U . . .
C56 C 0.558(2) 1.032(3) 0.107(2) 0.170(14) Uani 1 1 d D U . . .
H56A H 0.545044 1.071612 0.070423 0.255 Uiso 1 1 calc R U . . .
H56B H 0.612676 1.073910 0.150028 0.255 Uiso 1 1 calc R U . . .
H56C H 0.576132 0.984380 0.077547 0.255 Uiso 1 1 calc R U . . .
N1 N 0.2759(11) 0.7983(11) 0.4076(9) 0.034(4) Uani 1 1 d . U . . .
N2 N 0.1732(12) 0.7637(12) 0.3702(10) 0.041(4) Uani 1 1 d . U . . .
N3 N 0.0591(10) 0.6908(11) 0.2544(9) 0.040(4) Uani 1 1 d D U . . .
H3 H 0.046506 0.668074 0.202720 0.048 Uiso 1 1 calc R U . . .
N4 N 0.4874(11) 0.6111(11) 0.4615(9) 0.035(4) Uani 1 1 d . U . . .
N5 N 0.5603(12) 0.5955(12) 0.4146(9) 0.042(4) Uani 1 1 d . U . . .
N6 N 0.5884(11) 0.5342(13) 0.2946(10) 0.056(5) Uani 1 1 d D U . . .
H6A H 0.566928 0.496074 0.247492 0.067 Uiso 1 1 calc R U . . .
N7 N 0.1376(12) 0.3959(12) 0.1725(10) 0.042(4) Uani 1 1 d . U . . .
N8 N 0.1275(12) 0.3375(13) 0.2357(11) 0.048(4) Uani 1 1 d . U . . .
N9 N 0.1377(15) 0.3444(15) 0.3791(14) 0.081(6) Uani 1 1 d D U . . .
H9 H 0.151818 0.380946 0.426497 0.097 Uiso 1 1 calc R U . . .
N10 N 0.4245(12) 0.6847(12) 0.0896(9) 0.042(4) Uani 1 1 d . U . . .
N11 N 0.4477(11) 0.7902(12) 0.0999(9) 0.040(4) Uani 1 1 d . U . . .
N12 N 0.4930(13) 0.9212(13) 0.1962(11) 0.060(5) Uani 1 1 d D U . . .
H12 H 0.524886 0.952402 0.244333 0.072 Uiso 1 1 calc R U . . .
O1 O 0.5570(10) 0.9558(9) 0.6210(7) 0.040(3) Uani 1 1 d . U . . .
O2 O 0.4155(10) 0.9515(11) 0.6490(8) 0.056(4) Uani 1 1 d . U . . .
O3 O 0.3779(10) 0.7127(11) 0.6927(8) 0.052(4) Uani 1 1 d . U . . .
O4 O 0.5404(10) 0.7578(11) 0.7007(8) 0.053(4) Uani 1 1 d . U . . .
O5 O 0.0900(10) 0.4468(10) -0.1018(8) 0.043(3) Uani 1 1 d . U . . .
O6 O 0.0851(14) 0.3028(12) -0.0858(10) 0.081(5) Uani 1 1 d . U . . .
O7 O 0.3503(11) 0.3783(12) -0.0810(9) 0.063(4) Uani 1 1 d . U . . .
O8 O 0.3641(12) 0.5065(11) -0.1411(9) 0.058(4) Uani 1 1 d . U . . .
Pd1 Pd 0.37825(12) 0.78026(12) 0.34637(9) 0.0368(5) Uani 1 1 d . U . . .
Pd2 Pd 0.34755(12) 0.57686(13) 0.40589(9) 0.0408(5) Uani 1 1 d . U . . .
Pd3 Pd 0.18350(12) 0.54626(12) 0.19500(9) 0.0379(5) Uani 1 1 d . U . . .
Pd4 Pd 0.41704(12) 0.60255(13) 0.17666(9) 0.0424(6) Uani 1 1 d . U . . .
S1 S 0.2468(4) 0.7210(4) 0.2343(3) 0.0362(14) Uani 1 1 d . U . . .
S2 S 0.3984(4) 0.5168(4) 0.2885(3) 0.0429(15) Uani 1 1 d . U . . .
S3 S 0.1833(4) 0.5212(5) 0.3324(3) 0.0480(15) Uani 1 1 d . U . . .
S4 S 0.4882(4) 0.7617(4) 0.2605(3) 0.0444(15) Uani 1 1 d . 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
C1 C2 1.40(3) . ?
C1 C9 1.47(3) . ?
C1 Pd1 2.095(17) . ?
C2 C10 1.50(3) . ?
C2 C3 1.54(2) . ?
C3 O2 1.27(2) . ?
C3 O1 1.38(2) . ?
C4 O1 1.41(2) . ?
C4 C9 1.44(3) . ?
C4 C5 1.46(2) . ?
C5 C6 1.39(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.49(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.42(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.44(3) . ?
C8 H8 0.9500 . ?
C10 N1 1.35(2) . ?
C10 C11 1.54(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.30(2) . ?
C12 N3 1.36(2) . ?
C12 S1 1.841(19) . ?
C13 N3 1.477(14) . ?
C13 C14 1.529(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.43(2) . ?
C15 C23 1.45(3) . ?
C15 Pd2 2.156(19) . ?
C16 C17 1.48(2) . ?
C16 C24 1.49(2) . ?
C17 O4 1.27(2) . ?
C17 O3 1.36(2) . ?
C18 O3 1.38(2) . ?
C18 C19 1.43(3) . ?
C18 C23 1.43(3) . ?
C19 C20 1.41(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.37(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.49(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.40(3) . ?
C22 H22 0.9500 . ?
C24 N4 1.29(2) . ?
C24 C25 1.53(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N5 1.36(2) . ?
C26 N6 1.39(2) . ?
C26 S2 1.79(2) . ?
C27 N6 1.480(14) . ?
C27 C28 1.524(10) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.45(3) . ?
C29 C37 1.51(3) . ?
C29 Pd3 2.13(2) . ?
C30 C31 1.51(3) . ?
C30 C38 1.52(3) . ?
C31 O6 1.26(2) . ?
C31 O5 1.34(3) . ?
C32 C33 1.40(3) . ?
C32 C37 1.43(2) . ?
C32 O5 1.47(2) . ?
C33 C34 1.43(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.46(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.46(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.46(3) . ?
C36 H36 0.9500 . ?
C38 N7 1.34(2) . ?
C38 C39 1.54(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 N8 1.34(2) . ?
C40 N9 1.47(3) . ?
C40 S3 1.80(2) . ?
C41 N9 1.470(15) . ?
C41 C42 1.531(10) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.45(3) . ?
C43 C51 1.49(3) . ?
C43 Pd4 2.124(17) . ?
C44 C52 1.47(3) . ?
C44 C45 1.57(3) . ?
C45 O8 1.27(3) . ?
C45 O7 1.32(3) . ?
C46 C47 1.36(3) . ?
C46 C51 1.43(3) . ?
C46 O7 1.46(3) . ?
C47 C48 1.41(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.45(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.33(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.45(3) . ?
C50 H50 0.9500 . ?
C52 N10 1.39(2) . ?
C52 C53 1.58(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 N11 1.34(2) . ?
C54 N12 1.41(3) . ?
C54 S4 1.79(2) . ?
C55 N12 1.472(15) . ?
C55 C56 1.502(10) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
N1 N2 1.46(2) . ?
N1 Pd1 2.035(16) . ?
N3 H3 0.8800 . ?
N4 N5 1.50(2) . ?
N4 Pd2 2.044(15) . ?
N6 H6A 0.8800 . ?
N7 N8 1.45(2) . ?
N7 Pd3 2.086(17) . ?
N9 H9 0.8800 . ?
N10 N11 1.49(2) . ?
N10 Pd4 2.033(19) . ?
N12 H12 0.8800 . ?
Pd1 S4 2.396(6) . ?
Pd1 S1 2.397(5) . ?
Pd1 Pd2 3.247(4) . ?
Pd2 S3 2.408(6) . ?
Pd2 S2 2.430(6) . ?
Pd3 S3 2.415(6) . ?
Pd3 S1 2.421(6) . ?
Pd4 S2 2.408(7) . ?
Pd4 S4 2.420(6) . ?

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
C2 C1 C9 117.6(16) . . ?
C2 C1 Pd1 108.5(13) . . ?
C9 C1 Pd1 133.7(14) . . ?
C1 C2 C10 121.8(16) . . ?
C1 C2 C3 120.8(17) . . ?
C10 C2 C3 117.3(17) . . ?
O2 C3 O1 112.7(16) . . ?
O2 C3 C2 127.6(18) . . ?
O1 C3 C2 119.7(17) . . ?
O1 C4 C9 123.2(17) . . ?
O1 C4 C5 112.7(15) . . ?
C9 C4 C5 123.9(18) . . ?
C6 C5 C4 118.0(17) . . ?
C6 C5 H5 121.0 . . ?
C4 C5 H5 121.0 . . ?
C5 C6 C7 120.0(18) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 119.9(18) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 121.9(16) . . ?
C7 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C4 C9 C8 115.7(17) . . ?
C4 C9 C1 119.3(18) . . ?
C8 C9 C1 124.6(17) . . ?
N1 C10 C2 108.6(17) . . ?
N1 C10 C11 123.9(17) . . ?
C2 C10 C11 127.3(16) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 N3 119.8(17) . . ?
N2 C12 S1 124.0(14) . . ?
N3 C12 S1 116.0(13) . . ?
N3 C13 C14 111.2(17) . . ?
N3 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
N3 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C23 117.4(16) . . ?
C16 C15 Pd2 108.6(13) . . ?
C23 C15 Pd2 133.7(14) . . ?
C15 C16 C17 120.8(17) . . ?
C15 C16 C24 118.4(16) . . ?
C17 C16 C24 120.8(17) . . ?
O4 C17 O3 116.4(16) . . ?
O4 C17 C16 124.7(19) . . ?
O3 C17 C16 118.5(17) . . ?
O3 C18 C19 115.9(17) . . ?
O3 C18 C23 121.7(18) . . ?
C19 C18 C23 122.1(19) . . ?
C20 C19 C18 119.0(19) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C21 C20 C19 121(2) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C20 C21 C22 119.9(19) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 119.8(18) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C18 117.7(19) . . ?
C22 C23 C15 122.9(18) . . ?
C18 C23 C15 119.1(18) . . ?
N4 C24 C16 112.6(16) . . ?
N4 C24 C25 122.4(17) . . ?
C16 C24 C25 125.0(16) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N5 C26 N6 114.1(17) . . ?
N5 C26 S2 126.3(15) . . ?
N6 C26 S2 119.2(14) . . ?
N6 C27 C28 111.2(17) . . ?
N6 C27 H27A 109.4 . . ?
C28 C27 H27A 109.4 . . ?
N6 C27 H27B 109.4 . . ?
C28 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C37 118.2(17) . . ?
C30 C29 Pd3 109.3(15) . . ?
C37 C29 Pd3 132.3(13) . . ?
C29 C30 C31 119(2) . . ?
C29 C30 C38 118.3(17) . . ?
C31 C30 C38 122.7(18) . . ?
O6 C31 O5 117.2(19) . . ?
O6 C31 C30 123(2) . . ?
O5 C31 C30 119.8(18) . . ?
C33 C32 C37 125.9(18) . . ?
C33 C32 O5 116.4(16) . . ?
C37 C32 O5 117.5(18) . . ?
C32 C33 C34 118.3(18) . . ?
C32 C33 H33 120.9 . . ?
C34 C33 H33 120.9 . . ?
C33 C34 C35 120(2) . . ?
C33 C34 H34 119.8 . . ?
C35 C34 H34 119.8 . . ?
C34 C35 C36 117.9(19) . . ?
C34 C35 H35 121.1 . . ?
C36 C35 H35 121.1 . . ?
C37 C36 C35 122.2(18) . . ?
C37 C36 H36 118.9 . . ?
C35 C36 H36 118.9 . . ?
C32 C37 C36 114.9(19) . . ?
C32 C37 C29 120.7(17) . . ?
C36 C37 C29 124.1(16) . . ?
N7 C38 C30 113.3(18) . . ?
N7 C38 C39 122(2) . . ?
C30 C38 C39 124.3(18) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N8 C40 N9 119(2) . . ?
N8 C40 S3 128(2) . . ?
N9 C40 S3 113.1(16) . . ?
N9 C41 C42 105(2) . . ?
N9 C41 H41A 110.8 . . ?
C42 C41 H41A 110.8 . . ?
N9 C41 H41B 110.8 . . ?
C42 C41 H41B 110.8 . . ?
H41A C41 H41B 108.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C51 118.7(17) . . ?
C44 C43 Pd4 106.9(14) . . ?
C51 C43 Pd4 133.9(16) . . ?
C43 C44 C52 121.7(18) . . ?
C43 C44 C45 117(2) . . ?
C52 C44 C45 121(2) . . ?
O8 C45 O7 121.0(19) . . ?
O8 C45 C44 119(2) . . ?
O7 C45 C44 120(2) . . ?
C47 C46 C51 125(3) . . ?
C47 C46 O7 117(2) . . ?
C51 C46 O7 118(2) . . ?
C46 C47 C48 119(2) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
C47 C48 C49 118(2) . . ?
C47 C48 H48 120.9 . . ?
C49 C48 H48 120.9 . . ?
C50 C49 C48 120(3) . . ?
C50 C49 H49 119.9 . . ?
C48 C49 H49 119.9 . . ?
C49 C50 C51 124(2) . . ?
C49 C50 H50 117.9 . . ?
C51 C50 H50 117.9 . . ?
C46 C51 C50 113(2) . . ?
C46 C51 C43 121(2) . . ?
C50 C51 C43 125.3(18) . . ?
N10 C52 C44 111(2) . . ?
N10 C52 C53 121.7(19) . . ?
C44 C52 C53 127.6(17) . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N11 C54 N12 110(2) . . ?
N11 C54 S4 131.4(17) . . ?
N12 C54 S4 118.7(14) . . ?
N12 C55 C56 106(3) . . ?
N12 C55 H55A 110.6 . . ?
C56 C55 H55A 110.6 . . ?
N12 C55 H55B 110.6 . . ?
C56 C55 H55B 110.6 . . ?
H55A C55 H55B 108.7 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C10 N1 N2 118.4(15) . . ?
C10 N1 Pd1 120.0(13) . . ?
N2 N1 Pd1 121.6(11) . . ?
C12 N2 N1 115.5(15) . . ?
C12 N3 C13 120.7(16) . . ?
C12 N3 H3 119.6 . . ?
C13 N3 H3 119.6 . . ?
C24 N4 N5 119.1(15) . . ?
C24 N4 Pd2 120.9(13) . . ?
N5 N4 Pd2 120.0(10) . . ?
C26 N5 N4 114.0(15) . . ?
C26 N6 C27 121.1(16) . . ?
C26 N6 H6A 119.4 . . ?
C27 N6 H6A 119.4 . . ?
C38 N7 N8 119.4(17) . . ?
C38 N7 Pd3 117.6(16) . . ?
N8 N7 Pd3 123.0(11) . . ?
C40 N8 N7 111.5(18) . . ?
C40 N9 C41 124(2) . . ?
C40 N9 H9 118.0 . . ?
C41 N9 H9 118.0 . . ?
C52 N10 N11 114.5(17) . . ?
C52 N10 Pd4 117.6(14) . . ?
N11 N10 Pd4 127.6(11) . . ?
C54 N11 N10 105.0(17) . . ?
C54 N12 C55 127.4(18) . . ?
C54 N12 H12 116.3 . . ?
C55 N12 H12 116.3 . . ?
C3 O1 C4 119.2(14) . . ?
C17 O3 C18 122.1(15) . . ?
C31 O5 C32 124.4(15) . . ?
C45 O7 C46 124.0(18) . . ?
N1 Pd1 C1 80.8(7) . . ?
N1 Pd1 S4 173.2(5) . . ?
C1 Pd1 S4 104.9(6) . . ?
N1 Pd1 S1 83.7(4) . . ?
C1 Pd1 S1 163.8(6) . . ?
S4 Pd1 S1 90.2(2) . . ?
N1 Pd1 Pd2 94.3(5) . . ?
C1 Pd1 Pd2 86.0(5) . . ?
S4 Pd1 Pd2 89.93(17) . . ?
S1 Pd1 Pd2 100.27(16) . . ?
N4 Pd2 C15 79.0(7) . . ?
N4 Pd2 S3 173.8(4) . . ?
C15 Pd2 S3 105.6(5) . . ?
N4 Pd2 S2 85.0(4) . . ?
C15 Pd2 S2 163.1(6) . . ?
S3 Pd2 S2 90.00(19) . . ?
N4 Pd2 Pd1 101.2(5) . . ?
C15 Pd2 Pd1 94.3(6) . . ?
S3 Pd2 Pd1 82.74(17) . . ?
S2 Pd2 Pd1 93.84(17) . . ?
N7 Pd3 C29 80.9(8) . . ?
N7 Pd3 S3 82.9(5) . . ?
C29 Pd3 S3 162.2(6) . . ?
N7 Pd3 S1 173.9(5) . . ?
C29 Pd3 S1 104.6(6) . . ?
S3 Pd3 S1 92.0(2) . . ?
N10 Pd4 C43 82.0(8) . . ?
N10 Pd4 S2 172.7(4) . . ?
C43 Pd4 S2 103.6(6) . . ?
N10 Pd4 S4 81.4(4) . . ?
C43 Pd4 S4 160.9(6) . . ?
S2 Pd4 S4 93.8(2) . . ?
C12 S1 Pd1 94.5(6) . . ?
C12 S1 Pd3 99.5(6) . . ?
Pd1 S1 Pd3 110.9(2) . . ?
C26 S2 Pd4 106.4(8) . . ?
C26 S2 Pd2 94.3(7) . . ?
Pd4 S2 Pd2 118.7(2) . . ?
C40 S3 Pd2 100.0(7) . . ?
C40 S3 Pd3 94.5(9) . . ?
Pd2 S3 Pd3 112.7(2) . . ?
C54 S4 Pd1 103.6(7) . . ?
C54 S4 Pd4 93.4(7) . . ?
Pd1 S4 Pd4 112.2(2) . . ?

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
C9 C1 C2 C10 -178.1(18) . . . . ?
Pd1 C1 C2 C10 6(2) . . . . ?
C9 C1 C2 C3 -2(3) . . . . ?
Pd1 C1 C2 C3 -178.0(14) . . . . ?
C1 C2 C3 O2 -178(2) . . . . ?
C10 C2 C3 O2 -1(3) . . . . ?
C1 C2 C3 O1 2(3) . . . . ?
C10 C2 C3 O1 178.3(18) . . . . ?
O1 C4 C5 C6 179.1(18) . . . . ?
C9 C4 C5 C6 -6(3) . . . . ?
C4 C5 C6 C7 2(3) . . . . ?
C5 C6 C7 C8 -2(3) . . . . ?
C6 C7 C8 C9 4(3) . . . . ?
O1 C4 C9 C8 -177.5(19) . . . . ?
C5 C4 C9 C8 8(3) . . . . ?
O1 C4 C9 C1 -5(3) . . . . ?
C5 C4 C9 C1 -179.3(19) . . . . ?
C7 C8 C9 C4 -7(3) . . . . ?
C7 C8 C9 C1 -179(2) . . . . ?
C2 C1 C9 C4 3(3) . . . . ?
Pd1 C1 C9 C4 177.8(15) . . . . ?
C2 C1 C9 C8 176(2) . . . . ?
Pd1 C1 C9 C8 -10(4) . . . . ?
C1 C2 C10 N1 -6(3) . . . . ?
C3 C2 C10 N1 178.0(17) . . . . ?
C1 C2 C10 C11 180(2) . . . . ?
C3 C2 C10 C11 4(3) . . . . ?
C23 C15 C16 C17 -2(3) . . . . ?
Pd2 C15 C16 C17 173.8(16) . . . . ?
C23 C15 C16 C24 177.3(19) . . . . ?
Pd2 C15 C16 C24 -7(2) . . . . ?
C15 C16 C17 O4 -167(2) . . . . ?
C24 C16 C17 O4 14(3) . . . . ?
C15 C16 C17 O3 5(3) . . . . ?
C24 C16 C17 O3 -174.0(19) . . . . ?
O3 C18 C19 C20 178.6(19) . . . . ?
C23 C18 C19 C20 5(3) . . . . ?
C18 C19 C20 C21 -3(3) . . . . ?
C19 C20 C21 C22 4(3) . . . . ?
C20 C21 C22 C23 -5(3) . . . . ?
C21 C22 C23 C18 7(3) . . . . ?
C21 C22 C23 C15 -180(2) . . . . ?
O3 C18 C23 C22 -180(2) . . . . ?
C19 C18 C23 C22 -6(3) . . . . ?
O3 C18 C23 C15 6(3) . . . . ?
C19 C18 C23 C15 180(2) . . . . ?
C16 C15 C23 C22 -177(2) . . . . ?
Pd2 C15 C23 C22 9(4) . . . . ?
C16 C15 C23 C18 -4(3) . . . . ?
Pd2 C15 C23 C18 -177.9(17) . . . . ?
C15 C16 C24 N4 6(3) . . . . ?
C17 C16 C24 N4 -175.2(19) . . . . ?
C15 C16 C24 C25 -173.1(19) . . . . ?
C17 C16 C24 C25 6(3) . . . . ?
C37 C29 C30 C31 3(3) . . . . ?
Pd3 C29 C30 C31 179.7(15) . . . . ?
C37 C29 C30 C38 -172.1(18) . . . . ?
Pd3 C29 C30 C38 4(2) . . . . ?
C29 C30 C31 O6 173(2) . . . . ?
C38 C30 C31 O6 -12(3) . . . . ?
C29 C30 C31 O5 -6(3) . . . . ?
C38 C30 C31 O5 168.7(19) . . . . ?
C37 C32 C33 C34 -5(3) . . . . ?
O5 C32 C33 C34 179.4(16) . . . . ?
C32 C33 C34 C35 7(3) . . . . ?
C33 C34 C35 C36 -7(3) . . . . ?
C34 C35 C36 C37 5(3) . . . . ?
C33 C32 C37 C36 3(3) . . . . ?
O5 C32 C37 C36 178.4(16) . . . . ?
C33 C32 C37 C29 177.2(19) . . . . ?
O5 C32 C37 C29 -8(3) . . . . ?
C35 C36 C37 C32 -3(3) . . . . ?
C35 C36 C37 C29 -177(2) . . . . ?
C30 C29 C37 C32 4(3) . . . . ?
Pd3 C29 C37 C32 -171.6(14) . . . . ?
C30 C29 C37 C36 177.1(18) . . . . ?
Pd3 C29 C37 C36 2(3) . . . . ?
C29 C30 C38 N7 1(3) . . . . ?
C31 C30 C38 N7 -174.6(18) . . . . ?
C29 C30 C38 C39 -178.2(18) . . . . ?
C31 C30 C38 C39 7(3) . . . . ?
C51 C43 C44 C52 -179.7(17) . . . . ?
Pd4 C43 C44 C52 -7(2) . . . . ?
C51 C43 C44 C45 3(3) . . . . ?
Pd4 C43 C44 C45 176.3(14) . . . . ?
C43 C44 C45 O8 179.1(19) . . . . ?
C52 C44 C45 O8 2(3) . . . . ?
C43 C44 C45 O7 -1(3) . . . . ?
C52 C44 C45 O7 -177.8(19) . . . . ?
C51 C46 C47 C48 0(4) . . . . ?
O7 C46 C47 C48 -180(2) . . . . ?
C46 C47 C48 C49 3(4) . . . . ?
C47 C48 C49 C50 -3(4) . . . . ?
C48 C49 C50 C51 1(4) . . . . ?
C47 C46 C51 C50 -1(3) . . . . ?
O7 C46 C51 C50 178.3(18) . . . . ?
C47 C46 C51 C43 -179(2) . . . . ?
O7 C46 C51 C43 1(3) . . . . ?
C49 C50 C51 C46 1(3) . . . . ?
C49 C50 C51 C43 178(2) . . . . ?
C44 C43 C51 C46 -3(3) . . . . ?
Pd4 C43 C51 C46 -174.1(16) . . . . ?
C44 C43 C51 C50 179.4(19) . . . . ?
Pd4 C43 C51 C50 9(3) . . . . ?
C43 C44 C52 N10 12(3) . . . . ?
C45 C44 C52 N10 -171.1(17) . . . . ?
C43 C44 C52 C53 -171.2(19) . . . . ?
C45 C44 C52 C53 6(3) . . . . ?
C2 C10 N1 N2 -178.5(15) . . . . ?
C11 C10 N1 N2 -4(3) . . . . ?
C2 C10 N1 Pd1 3(2) . . . . ?
C11 C10 N1 Pd1 177.0(16) . . . . ?
N3 C12 N2 N1 -180.0(16) . . . . ?
S1 C12 N2 N1 -4(3) . . . . ?
C10 N1 N2 C12 178.0(18) . . . . ?
Pd1 N1 N2 C12 -3(2) . . . . ?
N2 C12 N3 C13 -4(3) . . . . ?
S1 C12 N3 C13 -179.6(14) . . . . ?
C14 C13 N3 C12 -76(2) . . . . ?
C16 C24 N4 N5 178.1(16) . . . . ?
C25 C24 N4 N5 -3(3) . . . . ?
C16 C24 N4 Pd2 -1(2) . . . . ?
C25 C24 N4 Pd2 177.9(13) . . . . ?
N6 C26 N5 N4 179.8(18) . . . . ?
S2 C26 N5 N4 7(3) . . . . ?
C24 N4 N5 C26 173.9(19) . . . . ?
Pd2 N4 N5 C26 -7(2) . . . . ?
N5 C26 N6 C27 -10(3) . . . . ?
S2 C26 N6 C27 163.5(16) . . . . ?
C28 C27 N6 C26 -79(3) . . . . ?
C30 C38 N7 N8 175.9(16) . . . . ?
C39 C38 N7 N8 -5(3) . . . . ?
C30 C38 N7 Pd3 -6(2) . . . . ?
C39 C38 N7 Pd3 173.2(14) . . . . ?
N9 C40 N8 N7 176.4(17) . . . . ?
S3 C40 N8 N7 3(3) . . . . ?
C38 N7 N8 C40 179.4(17) . . . . ?
Pd3 N7 N8 C40 1(2) . . . . ?
N8 C40 N9 C41 1(3) . . . . ?
S3 C40 N9 C41 175.3(19) . . . . ?
C42 C41 N9 C40 -164(2) . . . . ?
C44 C52 N10 N11 174.9(15) . . . . ?
C53 C52 N10 N11 -2(3) . . . . ?
C44 C52 N10 Pd4 -11(2) . . . . ?
C53 C52 N10 Pd4 171.5(14) . . . . ?
N12 C54 N11 N10 -178.0(15) . . . . ?
S4 C54 N11 N10 5(2) . . . . ?
C52 N10 N11 C54 179.1(16) . . . . ?
Pd4 N10 N11 C54 6(2) . . . . ?
N11 C54 N12 C55 16(3) . . . . ?
S4 C54 N12 C55 -167(2) . . . . ?
C56 C55 N12 C54 -98(3) . . . . ?
O2 C3 O1 C4 176.6(17) . . . . ?
C2 C3 O1 C4 -3(3) . . . . ?
C9 C4 O1 C3 5(3) . . . . ?
C5 C4 O1 C3 179.8(17) . . . . ?
O4 C17 O3 C18 170.0(19) . . . . ?
C16 C17 O3 C18 -3(3) . . . . ?
C19 C18 O3 C17 -177.0(19) . . . . ?
C23 C18 O3 C17 -3(3) . . . . ?
O6 C31 O5 C32 -177.2(17) . . . . ?
C30 C31 O5 C32 2(3) . . . . ?
C33 C32 O5 C31 -179.7(19) . . . . ?
C37 C32 O5 C31 5(3) . . . . ?
O8 C45 O7 C46 178.2(19) . . . . ?
C44 C45 O7 C46 -2(3) . . . . ?
C47 C46 O7 C45 -179(2) . . . . ?
C51 C46 O7 C45 2(3) . . . . ?
N2 C12 S1 Pd1 7.9(18) . . . . ?
N3 C12 S1 Pd1 -176.4(14) . . . . ?
N2 C12 S1 Pd3 120.0(17) . . . . ?
N3 C12 S1 Pd3 -64.3(15) . . . . ?
N5 C26 S2 Pd4 118(2) . . . . ?
N6 C26 S2 Pd4 -55(2) . . . . ?
N5 C26 S2 Pd2 -4(2) . . . . ?
N6 C26 S2 Pd2 -176.1(18) . . . . ?
N8 C40 S3 Pd2 -118.1(19) . . . . ?
N9 C40 S3 Pd2 67.9(16) . . . . ?
N8 C40 S3 Pd3 -4(2) . . . . ?
N9 C40 S3 Pd3 -178.1(15) . . . . ?
N11 C54 S4 Pd1 -124.4(18) . . . . ?
N12 C54 S4 Pd1 59.0(16) . . . . ?
N11 C54 S4 Pd4 -11(2) . . . . ?
N12 C54 S4 Pd4 172.7(15) . . . . ?

_refine_diff_density_max         2.114
_refine_diff_density_min         -1.599
_refine_diff_density_rms         0.235



####################################################################### 
# 
# 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_PDA5
_database_code_depnum_ccdc_archive 'CCDC 1892202'
loop_
_audit_author_name
_audit_author_address
'Vincent M. Lynch'
;University of Texas 
United States of America
;
_audit_update_record             
;
2019-07-19 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H21 Cl N4 O3 Pd S'
_chemical_formula_weight         551.33

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'
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'
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'
Cl Cl 0.3639 0.7018 '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                   15.5188(2)
_cell_length_b                   8.30810(10)
_cell_length_c                   17.7320(3)
_cell_angle_alpha                90
_cell_angle_beta                 112.067(2)
_cell_angle_gamma                90
_cell_volume                     2118.74(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14311
_cell_measurement_theta_min      5.36
_cell_measurement_theta_max      74.1

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.038
_exptl_absorpt_coefficient_mu    9.424
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_correction_T_min  0.439
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed microfocus tube'
_diffrn_measurement_device_type  'Agilent SuperNova with an Atlas S2 CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19567
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.235
_diffrn_reflns_theta_max         74.122
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4257
_reflns_number_gt                4186
_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 V 1.171.38.43f, Rigaku Oxford Diffraction'
_computing_cell_refinement       
'CrysAlisPro V 1.171.38.43f, Rigaku Oxford Diffraction'
_computing_data_reduction        
'CrysAlisPro V 1.171.38.43f, Rigaku Oxford Diffraction'

_computing_structure_solution    
;

SHELXT. Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8. 
;
_computing_structure_refinement  'Shelxl-2016/6, Sheldrick, G. M.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'Shelxl-2016/6, Sheldrick, G. M.'





_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)+(0.0350P)²+1.6979P] 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         4257
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0571
_refine_ls_wR_factor_gt          0.0568
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.40794(2) 0.80694(2) 0.40885(2) 0.01160(6) Uani 1 1 d . . . . .
Cl1 Cl 0.27328(3) 0.93331(5) 0.32750(2) 0.01637(9) Uani 1 1 d . . . . .
S1 S 0.42350(3) 0.69701(5) 0.30115(3) 0.01490(10) Uani 1 1 d . . . . .
O1 O 0.41987(8) 0.96259(16) 0.63324(7) 0.0158(2) Uani 1 1 d . . . . .
O2 O 0.39427(9) 0.91080(16) 0.50834(7) 0.0173(3) Uani 1 1 d . . . . .
O3 O 0.48939(9) 0.56568(17) 0.13535(8) 0.0216(3) Uani 1 1 d . . . . .
N1 N 0.52796(10) 0.69875(17) 0.47522(9) 0.0130(3) Uani 1 1 d . . . . .
N2 N 0.57452(10) 0.61143(18) 0.43478(9) 0.0145(3) Uani 1 1 d . . . . .
N3 N 0.56845(11) 0.52702(19) 0.30808(9) 0.0162(3) Uani 1 1 d . . . . .
N4 N 0.37448(11) 0.6449(2) 0.01743(9) 0.0178(3) Uani 1 1 d . . . . .
C10 C 0.46827(12) 0.9548(2) 0.71592(10) 0.0144(3) Uani 1 1 d . . . . .
C2 C 0.57171(12) 0.7086(2) 0.55438(11) 0.0133(3) Uani 1 1 d . . . . .
C5 C 0.54926(13) 0.8656(2) 0.74677(11) 0.0159(3) Uani 1 1 d . . . . .
C19 C 0.40645(13) 0.5849(2) 0.09297(11) 0.0187(4) Uani 1 1 d . . . . .
H19 H 0.362115 0.554853 0.115541 0.022 Uiso 1 1 calc R U . . .
C11 C 0.44782(12) 0.8869(2) 0.57907(10) 0.0137(3) Uani 1 1 d . . . . .
C1 C 0.53107(12) 0.6068(2) 0.35592(11) 0.0140(3) Uani 1 1 d . . . . .
C9 C 0.43166(13) 1.0399(2) 0.76433(11) 0.0179(4) Uani 1 1 d . . . . .
H9 H 0.375408 1.098984 0.741212 0.021 Uiso 1 1 calc R U . . .
C4 C 0.57986(13) 0.7841(2) 0.69057(11) 0.0156(3) Uani 1 1 d . . . . .
H4 H 0.635271 0.722086 0.711236 0.019 Uiso 1 1 calc R U . . .
C3 C 0.53276(12) 0.7915(2) 0.60806(11) 0.0135(3) Uani 1 1 d . . . . .
C17 C 0.73709(13) 0.2490(2) 0.27930(12) 0.0204(4) Uani 1 1 d . . . . .
H17 H 0.749296 0.205185 0.234822 0.025 Uiso 1 1 calc R U . . .
C13 C 0.64517(12) 0.4226(2) 0.32992(11) 0.0152(3) Uani 1 1 d . . . . .
C18 C 0.66390(13) 0.3562(2) 0.26478(11) 0.0177(3) Uani 1 1 d . . . . .
H18 H 0.626271 0.384786 0.210464 0.021 Uiso 1 1 calc R U . . .
C6 C 0.59808(14) 0.8640(3) 0.83203(12) 0.0227(4) Uani 1 1 d . . . . .
H6 H 0.654371 0.805067 0.855257 0.027 Uiso 1 1 calc R U . . .
C12 C 0.66660(12) 0.6348(2) 0.59577(10) 0.0163(3) Uani 1 1 d . . . . .
H12A H 0.662374 0.543870 0.629392 0.024 Uiso 1 1 calc R U . . .
H12B H 0.709326 0.715714 0.630257 0.024 Uiso 1 1 calc R U . . .
H12C H 0.689824 0.596963 0.554567 0.024 Uiso 1 1 calc R U . . .
C8 C 0.48021(14) 1.0352(2) 0.84738(11) 0.0199(4) Uani 1 1 d . . . . .
H8 H 0.456766 1.091685 0.882195 0.024 Uiso 1 1 calc R U . . .
C14 C 0.70046(13) 0.3778(2) 0.40936(11) 0.0180(4) Uani 1 1 d . . . . .
H14 H 0.688670 0.421147 0.454134 0.022 Uiso 1 1 calc R U . . .
C15 C 0.77315(13) 0.2689(2) 0.42250(12) 0.0214(4) Uani 1 1 d . . . . .
H15 H 0.810129 0.237667 0.476570 0.026 Uiso 1 1 calc R U . . .
C16 C 0.79254(14) 0.2053(2) 0.35824(14) 0.0220(4) Uani 1 1 d . . . . .
H16 H 0.843009 0.132915 0.368137 0.026 Uiso 1 1 calc R U . . .
C20 C 0.43722(14) 0.6993(2) -0.02080(12) 0.0216(4) Uani 1 1 d . . . . .
H20A H 0.501560 0.690659 0.018093 0.032 Uiso 1 1 calc R U . . .
H20B H 0.423439 0.811691 -0.037838 0.032 Uiso 1 1 calc R U . . .
H20C H 0.429010 0.632226 -0.068477 0.032 Uiso 1 1 calc R U . . .
C21 C 0.27546(14) 0.6623(3) -0.02923(14) 0.0265(4) Uani 1 1 d . . . . .
H21A H 0.240480 0.620212 0.002402 0.040 Uiso 1 1 calc R U . . .
H21B H 0.258603 0.602107 -0.080280 0.040 Uiso 1 1 calc R U . . .
H21C H 0.260510 0.776408 -0.041267 0.040 Uiso 1 1 calc R U . . .
C7 C 0.56322(15) 0.9489(3) 0.88121(12) 0.0244(4) Uani 1 1 d . . . . .
H7 H 0.595916 0.948651 0.938515 0.029 Uiso 1 1 calc R U . . .
H3N H 0.5423(16) 0.536(3) 0.2586(16) 0.020(6) Uiso 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 N1 2.0038(15) . ?
Pd1 O2 2.0452(12) . ?
Pd1 S1 2.2104(4) . ?
Pd1 Cl1 2.2990(4) . ?
S1 C1 1.7533(18) . ?
O1 C11 1.349(2) . ?
O1 C10 1.375(2) . ?
O2 C11 1.233(2) . ?
O3 C19 1.233(2) . ?
N1 C2 1.312(2) . ?
N1 N2 1.397(2) . ?
N2 C1 1.305(2) . ?
N3 C1 1.365(2) . ?
N3 C13 1.405(2) . ?
N3 H3N 0.82(3) . ?
N4 C19 1.338(2) . ?
N4 C20 1.452(2) . ?
N4 C21 1.453(2) . ?
C10 C5 1.382(3) . ?
C10 C9 1.388(2) . ?
C2 C3 1.476(2) . ?
C2 C12 1.507(2) . ?
C5 C6 1.414(3) . ?
C5 C4 1.426(3) . ?
C19 H19 0.9500 . ?
C11 C3 1.456(2) . ?
C9 C8 1.380(3) . ?
C9 H9 0.9500 . ?
C4 C3 1.369(3) . ?
C4 H4 0.9500 . ?
C17 C16 1.388(3) . ?
C17 C18 1.389(3) . ?
C17 H17 0.9500 . ?
C13 C14 1.397(3) . ?
C13 C18 1.405(3) . ?
C18 H18 0.9500 . ?
C6 C7 1.380(3) . ?
C6 H6 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C8 C7 1.397(3) . ?
C8 H8 0.9500 . ?
C14 C15 1.396(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C7 H7 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 O2 93.29(6) . . ?
N1 Pd1 S1 86.73(4) . . ?
O2 Pd1 S1 179.39(4) . . ?
N1 Pd1 Cl1 177.02(4) . . ?
O2 Pd1 Cl1 89.09(4) . . ?
S1 Pd1 Cl1 90.874(15) . . ?
C1 S1 Pd1 95.08(6) . . ?
C11 O1 C10 122.97(14) . . ?
C11 O2 Pd1 124.10(11) . . ?
C2 N1 N2 114.96(15) . . ?
C2 N1 Pd1 126.40(12) . . ?
N2 N1 Pd1 118.51(11) . . ?
C1 N2 N1 114.00(14) . . ?
C1 N3 C13 129.96(15) . . ?
C1 N3 H3N 117.7(17) . . ?
C13 N3 H3N 112.2(17) . . ?
C19 N4 C20 121.47(16) . . ?
C19 N4 C21 121.48(17) . . ?
C20 N4 C21 117.04(16) . . ?
O1 C10 C5 119.90(16) . . ?
O1 C10 C9 116.67(16) . . ?
C5 C10 C9 123.43(17) . . ?
N1 C2 C3 123.13(16) . . ?
N1 C2 C12 120.91(16) . . ?
C3 C2 C12 115.96(15) . . ?
C10 C5 C6 118.05(17) . . ?
C10 C5 C4 118.03(16) . . ?
C6 C5 C4 123.89(17) . . ?
O3 C19 N4 124.61(17) . . ?
O3 C19 H19 117.7 . . ?
N4 C19 H19 117.7 . . ?
O2 C11 O1 112.02(15) . . ?
O2 C11 C3 128.44(16) . . ?
O1 C11 C3 119.54(15) . . ?
N2 C1 N3 120.73(16) . . ?
N2 C1 S1 125.58(14) . . ?
N3 C1 S1 113.69(13) . . ?
C8 C9 C10 117.36(17) . . ?
C8 C9 H9 121.3 . . ?
C10 C9 H9 121.3 . . ?
C3 C4 C5 122.78(17) . . ?
C3 C4 H4 118.6 . . ?
C5 C4 H4 118.6 . . ?
C4 C3 C11 116.78(16) . . ?
C4 C3 C2 119.00(16) . . ?
C11 C3 C2 124.19(16) . . ?
C16 C17 C18 120.57(18) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C14 C13 N3 125.33(16) . . ?
C14 C13 C18 119.08(17) . . ?
N3 C13 C18 115.56(16) . . ?
C17 C18 C13 120.43(18) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C7 C6 C5 119.42(18) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C2 C12 H12A 109.5 . . ?
C2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C8 C7 121.22(17) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C15 C14 C13 119.52(17) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C16 C15 C14 121.39(19) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.01(18) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C6 C7 C8 120.52(18) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?

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
C2 N1 N2 C1 -178.23(15) . . . . ?
Pd1 N1 N2 C1 -2.06(19) . . . . ?
C11 O1 C10 C5 -0.3(2) . . . . ?
C11 O1 C10 C9 179.49(16) . . . . ?
N2 N1 C2 C3 -178.14(15) . . . . ?
Pd1 N1 C2 C3 6.0(2) . . . . ?
N2 N1 C2 C12 2.2(2) . . . . ?
Pd1 N1 C2 C12 -173.63(12) . . . . ?
O1 C10 C5 C6 178.47(17) . . . . ?
C9 C10 C5 C6 -1.3(3) . . . . ?
O1 C10 C5 C4 0.1(3) . . . . ?
C9 C10 C5 C4 -179.72(17) . . . . ?
C20 N4 C19 O3 -2.2(3) . . . . ?
C21 N4 C19 O3 179.29(19) . . . . ?
Pd1 O2 C11 O1 -176.34(10) . . . . ?
Pd1 O2 C11 C3 3.8(3) . . . . ?
C10 O1 C11 O2 -179.73(15) . . . . ?
C10 O1 C11 C3 0.2(2) . . . . ?
N1 N2 C1 N3 179.42(15) . . . . ?
N1 N2 C1 S1 -0.6(2) . . . . ?
C13 N3 C1 N2 10.3(3) . . . . ?
C13 N3 C1 S1 -169.74(15) . . . . ?
Pd1 S1 C1 N2 2.37(16) . . . . ?
Pd1 S1 C1 N3 -177.61(12) . . . . ?
O1 C10 C9 C8 -179.04(16) . . . . ?
C5 C10 C9 C8 0.8(3) . . . . ?
C10 C5 C4 C3 0.3(3) . . . . ?
C6 C5 C4 C3 -177.98(18) . . . . ?
C5 C4 C3 C11 -0.5(3) . . . . ?
C5 C4 C3 C2 177.51(16) . . . . ?
O2 C11 C3 C4 -179.90(18) . . . . ?
O1 C11 C3 C4 0.2(2) . . . . ?
O2 C11 C3 C2 2.2(3) . . . . ?
O1 C11 C3 C2 -177.64(15) . . . . ?
N1 C2 C3 C4 174.58(17) . . . . ?
C12 C2 C3 C4 -5.7(2) . . . . ?
N1 C2 C3 C11 -7.6(3) . . . . ?
C12 C2 C3 C11 172.07(16) . . . . ?
C1 N3 C13 C14 0.3(3) . . . . ?
C1 N3 C13 C18 178.21(17) . . . . ?
C16 C17 C18 C13 0.3(3) . . . . ?
C14 C13 C18 C17 -0.8(3) . . . . ?
N3 C13 C18 C17 -178.80(16) . . . . ?
C10 C5 C6 C7 0.8(3) . . . . ?
C4 C5 C6 C7 179.06(19) . . . . ?
C10 C9 C8 C7 0.4(3) . . . . ?
N3 C13 C14 C15 178.06(17) . . . . ?
C18 C13 C14 C15 0.2(3) . . . . ?
C13 C14 C15 C16 0.8(3) . . . . ?
C14 C15 C16 C17 -1.3(3) . . . . ?
C18 C17 C16 C15 0.7(3) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C9 C8 C7 C6 -0.9(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N O3 0.82(3) 2.04(3) 2.858(2) 174(2) .

_refine_diff_density_max         0.415
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.073

