# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/cc1j3bvt
_database_code_depnum_ccdc_archive 'CCDC 1403396'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1515/ncrs-2014-9067 2014
_audit_update_record             
;
2015-05-27 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 O4 S2'
_chemical_formula_sum            'C12 H10 O4 S2'
_chemical_formula_weight         282.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   3.9254(12)
_cell_length_b                   6.0049(18)
_cell_length_c                   13.818(4)
_cell_angle_alpha                77.960(4)
_cell_angle_beta                 88.838(4)
_cell_angle_gamma                72.527(4)
_cell_volume                     303.54(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1441
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.56

_exptl_crystal_description       block
_exptl_crystal_colour            light-yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             146
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8610
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1679
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.04
_reflns_number_total             1053
_reflns_number_gt                976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       APEX2-2005
_computing_cell_refinement       APEX2-2005
_computing_data_reduction        'SAINT-2005 '
_computing_structure_solution    'SHELXTL-2008 [4]'
_computing_structure_refinement  'SHELXTL-2008 [4]'
_computing_molecular_graphics    'SHELXTL-2008 [4]'
_computing_publication_material  'SHELXTL-2008 [4]'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0890P)²+0.0880P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1053
_refine_ls_number_parameters     83
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1273
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 1.01296(14) 0.20551(9) 0.62438(4) 0.0381(3) Uani 1 1 d . . .
O1 O 0.5657(6) 0.2447(4) 0.87861(13) 0.0640(6) Uani 1 1 d . . .
O2 O 0.9132(5) -0.0599(3) 0.81742(13) 0.0493(5) Uani 1 1 d . . .
C1 C 0.9314(6) 0.4849(4) 0.54950(15) 0.0323(5) Uani 1 1 d . . .
C2 C 0.7319(6) 0.6573(4) 0.59635(17) 0.0415(6) Uani 1 1 d . . .
H2 H 0.6620 0.8197 0.5677 0.050 Uiso 1 1 calc R . .
C3 C 0.6437(7) 0.5636(4) 0.69223(17) 0.0435(6) Uani 1 1 d . . .
H3 H 0.5074 0.6571 0.7334 0.052 Uiso 1 1 calc R . .
C4 C 0.7786(6) 0.3223(4) 0.71824(16) 0.0365(5) Uani 1 1 d . . .
C5 C 0.7356(6) 0.1709(4) 0.81336(17) 0.0411(6) Uani 1 1 d . . .
C6 C 0.8879(8) -0.2257(5) 0.90785(19) 0.0573(7) Uani 1 1 d . . .
H6A H 0.9863 -0.1863 0.9627 0.086 Uiso 1 1 calc R . .
H6B H 1.0191 -0.3854 0.9024 0.086 Uiso 1 1 calc R . .
H6C H 0.6416 -0.2154 0.9183 0.086 Uiso 1 1 calc R . .


_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 C1 1.719(2) . ?
S1 C4 1.722(2) . ?
O1 C5 1.191(3) . ?
O2 C5 1.341(3) . ?
O2 C6 1.449(3) . ?
C1 C2 1.370(3) . ?
C1 C1 1.456(4) 2_766 ?
C2 C3 1.407(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.356(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.472(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 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
C1 S1 C4 91.71(10) . . ?
C5 O2 C6 116.2(2) . . ?
C2 C1 C1 128.3(3) . 2_766 ?
C2 C1 S1 110.88(16) . . ?
C1 C1 S1 120.8(2) 2_766 . ?
C1 C2 C3 113.1(2) . . ?
C1 C2 H2 123.5 . . ?
C3 C2 H2 123.5 . . ?
C4 C3 C2 112.8(2) . . ?
C4 C3 H3 123.6 . . ?
C2 C3 H3 123.6 . . ?
C3 C4 C5 126.1(2) . . ?
C3 C4 S1 111.56(17) . . ?
C5 C4 S1 122.33(18) . . ?
O1 C5 O2 124.4(2) . . ?
O1 C5 C4 124.1(2) . . ?
O2 C5 C4 111.5(2) . . ?
O2 C6 H6A 109.5 . . ?
O2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 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 S1 C1 C2 -0.05(18) . . . . ?
C4 S1 C1 C1 179.9(2) . . . 2_766 ?
C1 C1 C2 C3 179.7(3) 2_766 . . . ?
S1 C1 C2 C3 -0.3(3) . . . . ?
C1 C2 C3 C4 0.7(3) . . . . ?
C2 C3 C4 C5 179.7(2) . . . . ?
C2 C3 C4 S1 -0.7(3) . . . . ?
C1 S1 C4 C3 0.44(19) . . . . ?
C1 S1 C4 C5 -180.0(2) . . . . ?
C6 O2 C5 O1 0.6(4) . . . . ?
C6 O2 C5 C4 -179.7(2) . . . . ?
C3 C4 C5 O1 2.1(4) . . . . ?
S1 C4 C5 O1 -177.4(2) . . . . ?
C3 C4 C5 O2 -177.6(2) . . . . ?
S1 C4 C5 O2 2.9(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
C6 H6B O1 0.96 2.66 3.573(4) 159.6 1_645

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.102
####################################################################### 
# 
# 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_SM29
_database_code_depnum_ccdc_archive 'CCDC 1434719'
_audit_update_record             
;
2015-11-02 deposited with the CCDC.
2016-05-23 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            'C31 H26 Cl N2 O P Pd S'
_chemical_formula_weight         647.42

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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   9.4677(5)
_cell_length_b                   31.1867(15)
_cell_length_c                   10.2754(5)
_cell_angle_alpha                90
_cell_angle_beta                 107.706(2)
_cell_angle_gamma                90
_cell_volume                     2890.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4236
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      29.2

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.889
_shelx_estimated_absorpt_T_min   0.776
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_process_details   'SADABS (Bruker, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46957
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.227
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5652
_reflns_number_gt                5461
_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       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0169P)²+3.0204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5652
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.313
_refine_ls_restrained_S_all      1.313
_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
C1 C 0.0926(3) 0.17531(9) 0.1770(3) 0.0375(6) Uani 1 1 d . . . . .
C2 C 0.0062(4) 0.13923(12) 0.1329(4) 0.0566(8) Uani 1 1 d . . . . .
H2 H 0.0513 0.1129 0.1302 0.068 Uiso 1 1 calc R U . . .
C3 C -0.1469(4) 0.14202(15) 0.0930(5) 0.0762(12) Uani 1 1 d . . . . .
H3 H -0.2041 0.1176 0.0631 0.091 Uiso 1 1 calc R U . . .
C4 C -0.2143(4) 0.18065(16) 0.0974(4) 0.0732(12) Uani 1 1 d . . . . .
H4 H -0.3171 0.1824 0.0716 0.088 Uiso 1 1 calc R U . . .
C5 C -0.1300(4) 0.21665(14) 0.1399(4) 0.0670(10) Uani 1 1 d . . . . .
H5 H -0.1759 0.2429 0.1422 0.080 Uiso 1 1 calc R U . . .
C6 C 0.0231(4) 0.21420(11) 0.1795(3) 0.0506(8) Uani 1 1 d . . . . .
H6 H 0.0795 0.2388 0.2080 0.061 Uiso 1 1 calc R U . . .
C7 C 0.3561(3) 0.22361(10) 0.1907(3) 0.0419(6) Uani 1 1 d . . . . .
C8 C 0.3469(5) 0.23213(12) 0.0562(4) 0.0661(10) Uani 1 1 d . . . . .
H8 H 0.3155 0.2108 -0.0094 0.079 Uiso 1 1 calc R U . . .
C9 C 0.3840(6) 0.27210(15) 0.0187(5) 0.0892(15) Uani 1 1 d . . . . .
H9 H 0.3765 0.2776 -0.0721 0.107 Uiso 1 1 calc R U . . .
C10 C 0.4316(5) 0.30359(14) 0.1147(6) 0.0801(13) Uani 1 1 d . . . . .
H10 H 0.4570 0.3304 0.0893 0.096 Uiso 1 1 calc R U . . .
C11 C 0.4417(5) 0.29557(13) 0.2476(5) 0.0755(12) Uani 1 1 d . . . . .
H11 H 0.4743 0.3170 0.3128 0.091 Uiso 1 1 calc R U . . .
C12 C 0.4037(4) 0.25592(12) 0.2861(4) 0.0594(9) Uani 1 1 d . . . . .
H12 H 0.4103 0.2509 0.3770 0.071 Uiso 1 1 calc R U . . .
C13 C 0.3493(3) 0.16803(9) 0.4167(3) 0.0399(6) Uani 1 1 d . . . . .
C14 C 0.2479(4) 0.15733(12) 0.4839(3) 0.0538(8) Uani 1 1 d . . . . .
H14 H 0.1486 0.1534 0.4345 0.065 Uiso 1 1 calc R U . . .
C15 C 0.2939(5) 0.15245(15) 0.6243(4) 0.0687(11) Uani 1 1 d . . . . .
H15 H 0.2252 0.1449 0.6686 0.082 Uiso 1 1 calc R U . . .
C16 C 0.4392(5) 0.15851(13) 0.6991(3) 0.0620(10) Uani 1 1 d . . . . .
H16 H 0.4687 0.1556 0.7937 0.074 Uiso 1 1 calc R U . . .
C17 C 0.5414(4) 0.16893(12) 0.6329(3) 0.0557(8) Uani 1 1 d . . . . .
H17 H 0.6404 0.1729 0.6831 0.067 Uiso 1 1 calc R U . . .
C18 C 0.4975(4) 0.17356(11) 0.4926(3) 0.0500(8) Uani 1 1 d . . . . .
H18 H 0.5671 0.1804 0.4487 0.060 Uiso 1 1 calc R U . . .
C19 C 0.6597(3) 0.08264(10) 0.2961(3) 0.0427(7) Uani 1 1 d . . . . .
C20 C 0.7909(4) 0.07440(10) 0.4167(3) 0.0474(7) Uani 1 1 d . . . . .
C21 C 0.7823(4) 0.08218(13) 0.5464(3) 0.0625(9) Uani 1 1 d . . . . .
H21 H 0.6947 0.0923 0.5584 0.075 Uiso 1 1 calc R U . . .
C22 C 0.9070(5) 0.07461(14) 0.6601(4) 0.0761(13) Uani 1 1 d . . . . .
H22 H 0.9018 0.0795 0.7478 0.091 Uiso 1 1 calc R U . . .
C23 C 1.0352(5) 0.06013(14) 0.6422(4) 0.0792(13) Uani 1 1 d . . . . .
H23 H 1.1177 0.0553 0.7176 0.095 Uiso 1 1 calc R U . . .
C24 C 1.0432(5) 0.05262(17) 0.5143(5) 0.0876(15) Uani 1 1 d . . . . .
H24 H 1.1315 0.0427 0.5032 0.105 Uiso 1 1 calc R U . . .
C25 C 0.9222(4) 0.05946(14) 0.4003(4) 0.0682(11) Uani 1 1 d . . . . .
H25 H 0.9290 0.0541 0.3134 0.082 Uiso 1 1 calc R U . . .
C26 C 0.5132(3) 0.06017(9) -0.0423(3) 0.0355(6) Uani 1 1 d . . . . .
H26 H 0.4278 0.0684 -0.1105 0.043 Uiso 1 1 calc R U . . .
C27 C 0.6108(3) 0.03206(9) -0.0843(3) 0.0388(6) Uani 1 1 d . . . . .
C28 C 0.8035(4) -0.01698(12) -0.1073(4) 0.0619(10) Uani 1 1 d . . . . .
H28 H 0.8854 -0.0346 -0.0976 0.074 Uiso 1 1 calc R U . . .
C29 C 0.6973(4) -0.01109(12) -0.2263(4) 0.0586(9) Uani 1 1 d . . . . .
H29 H 0.6976 -0.0242 -0.3074 0.070 Uiso 1 1 calc R U . . .
C30 C 0.5847(3) 0.01716(10) -0.2157(3) 0.0456(7) Uani 1 1 d . . . . .
C31 C 0.4531(4) 0.02874(13) -0.3347(3) 0.0626(9) Uani 1 1 d . . . . .
H31A H 0.3640 0.0194 -0.3171 0.094 Uiso 1 1 calc R U . . .
H31B H 0.4612 0.0150 -0.4157 0.094 Uiso 1 1 calc R U . . .
H31C H 0.4500 0.0593 -0.3474 0.094 Uiso 1 1 calc R U . . .
N1 N 0.6545(3) 0.06361(8) 0.1818(2) 0.0413(5) Uani 1 1 d . . . . .
N2 N 0.5278(2) 0.07565(7) 0.0774(2) 0.0359(5) Uani 1 1 d . . . . .
O1 O 0.5599(2) 0.10847(7) 0.3153(2) 0.0497(5) Uani 1 1 d . . . . .
P1 P 0.29397(8) 0.17147(2) 0.23139(7) 0.03537(16) Uani 1 1 d . . . . .
S1 S 0.77393(8) 0.01090(3) 0.02442(9) 0.0509(2) Uani 1 1 d . . . . .
Cl1 Cl 0.22304(9) 0.12536(3) -0.06730(7) 0.0502(2) Uani 1 1 d . . . . .
Pd1 Pd 0.39800(2) 0.11900(2) 0.14002(2) 0.03512(9) 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 C2 1.384(4) . ?
C1 C6 1.384(4) . ?
C1 P1 1.821(3) . ?
C2 C3 1.384(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.370(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(5) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C12 1.382(5) . ?
C7 C8 1.384(5) . ?
C7 P1 1.820(3) . ?
C8 C9 1.381(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.367(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.363(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.383(4) . ?
C13 C18 1.393(4) . ?
C13 P1 1.818(3) . ?
C14 C15 1.383(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.370(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(4) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 O1 1.302(4) . ?
C19 N1 1.304(4) . ?
C19 C20 1.486(4) . ?
C20 C21 1.382(5) . ?
C20 C25 1.385(5) . ?
C21 C22 1.406(5) . ?
C21 H21 0.9300 . ?
C22 C23 1.359(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.359(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.383(5) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C26 N2 1.289(3) . ?
C26 C27 1.433(4) . ?
C26 H26 0.9300 . ?
C27 C30 1.377(4) . ?
C27 S1 1.738(3) . ?
C28 C29 1.339(5) . ?
C28 S1 1.702(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.412(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.500(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
N1 N2 1.396(3) . ?
N2 Pd1 2.057(2) . ?
O1 Pd1 2.005(2) . ?
P1 Pd1 2.2566(7) . ?
Cl1 Pd1 2.2748(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 118.8(3) . . ?
C2 C1 P1 120.5(2) . . ?
C6 C1 P1 120.8(2) . . ?
C3 C2 C1 120.5(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.0(4) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
C12 C7 C8 118.4(3) . . ?
C12 C7 P1 123.2(2) . . ?
C8 C7 P1 118.3(3) . . ?
C9 C8 C7 120.5(4) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C10 C9 C8 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.5(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.5(4) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
C14 C13 C18 119.0(3) . . ?
C14 C13 P1 120.9(2) . . ?
C18 C13 P1 120.0(2) . . ?
C15 C14 C13 120.0(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 119.4(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 120.4(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 120.2(3) . . ?
C17 C18 H18 119.9 . . ?
C13 C18 H18 119.9 . . ?
O1 C19 N1 126.0(3) . . ?
O1 C19 C20 116.2(3) . . ?
N1 C19 C20 117.7(3) . . ?
C21 C20 C25 119.7(3) . . ?
C21 C20 C19 119.6(3) . . ?
C25 C20 C19 120.7(3) . . ?
C20 C21 C22 119.4(4) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C23 C22 C21 120.2(4) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C22 C23 C24 120.2(4) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C25 121.1(4) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C24 C25 C20 119.5(4) . . ?
C24 C25 H25 120.3 . . ?
C20 C25 H25 120.3 . . ?
N2 C26 C27 128.7(3) . . ?
N2 C26 H26 115.7 . . ?
C27 C26 H26 115.7 . . ?
C30 C27 C26 124.2(3) . . ?
C30 C27 S1 111.2(2) . . ?
C26 C27 S1 124.6(2) . . ?
C29 C28 S1 113.4(3) . . ?
C29 C28 H28 123.3 . . ?
S1 C28 H28 123.3 . . ?
C28 C29 C30 113.0(3) . . ?
C28 C29 H29 123.5 . . ?
C30 C29 H29 123.5 . . ?
C27 C30 C29 111.8(3) . . ?
C27 C30 C31 125.1(3) . . ?
C29 C30 C31 123.1(3) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C19 N1 N2 111.0(2) . . ?
C26 N2 N1 116.7(2) . . ?
C26 N2 Pd1 130.05(19) . . ?
N1 N2 Pd1 113.10(16) . . ?
C19 O1 Pd1 110.91(17) . . ?
C13 P1 C7 106.42(14) . . ?
C13 P1 C1 105.49(13) . . ?
C7 P1 C1 104.60(13) . . ?
C13 P1 Pd1 111.70(10) . . ?
C7 P1 Pd1 109.88(10) . . ?
C1 P1 Pd1 117.95(10) . . ?
C28 S1 C27 90.66(16) . . ?
O1 Pd1 N2 78.89(9) . . ?
O1 Pd1 P1 93.21(6) . . ?
N2 Pd1 P1 169.89(7) . . ?
O1 Pd1 Cl1 174.43(7) . . ?
N2 Pd1 Cl1 95.66(6) . . ?
P1 Pd1 Cl1 92.33(3) . . ?

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
C6 C1 C2 C3 -0.4(5) . . . . ?
P1 C1 C2 C3 179.3(3) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C2 C3 C4 C5 0.8(7) . . . . ?
C3 C4 C5 C6 -0.5(6) . . . . ?
C4 C5 C6 C1 -0.2(6) . . . . ?
C2 C1 C6 C5 0.6(5) . . . . ?
P1 C1 C6 C5 -179.0(3) . . . . ?
C12 C7 C8 C9 -0.3(6) . . . . ?
P1 C7 C8 C9 176.0(4) . . . . ?
C7 C8 C9 C10 0.6(7) . . . . ?
C8 C9 C10 C11 -0.4(8) . . . . ?
C9 C10 C11 C12 -0.2(7) . . . . ?
C10 C11 C12 C7 0.5(6) . . . . ?
C8 C7 C12 C11 -0.2(6) . . . . ?
P1 C7 C12 C11 -176.4(3) . . . . ?
C18 C13 C14 C15 0.3(5) . . . . ?
P1 C13 C14 C15 176.2(3) . . . . ?
C13 C14 C15 C16 0.7(6) . . . . ?
C14 C15 C16 C17 -1.1(6) . . . . ?
C15 C16 C17 C18 0.5(6) . . . . ?
C16 C17 C18 C13 0.4(5) . . . . ?
C14 C13 C18 C17 -0.8(5) . . . . ?
P1 C13 C18 C17 -176.9(3) . . . . ?
O1 C19 C20 C21 20.1(4) . . . . ?
N1 C19 C20 C21 -159.8(3) . . . . ?
O1 C19 C20 C25 -159.2(3) . . . . ?
N1 C19 C20 C25 20.9(5) . . . . ?
C25 C20 C21 C22 -0.3(6) . . . . ?
C19 C20 C21 C22 -179.6(3) . . . . ?
C20 C21 C22 C23 0.6(6) . . . . ?
C21 C22 C23 C24 -0.4(7) . . . . ?
C22 C23 C24 C25 0.0(8) . . . . ?
C23 C24 C25 C20 0.3(7) . . . . ?
C21 C20 C25 C24 -0.2(6) . . . . ?
C19 C20 C25 C24 179.1(4) . . . . ?
N2 C26 C27 C30 179.8(3) . . . . ?
N2 C26 C27 S1 2.1(5) . . . . ?
S1 C28 C29 C30 0.3(4) . . . . ?
C26 C27 C30 C29 -178.1(3) . . . . ?
S1 C27 C30 C29 -0.1(4) . . . . ?
C26 C27 C30 C31 1.5(5) . . . . ?
S1 C27 C30 C31 179.5(3) . . . . ?
C28 C29 C30 C27 -0.1(5) . . . . ?
C28 C29 C30 C31 -179.7(4) . . . . ?
O1 C19 N1 N2 2.1(4) . . . . ?
C20 C19 N1 N2 -177.9(2) . . . . ?
C27 C26 N2 N1 -0.4(4) . . . . ?
C27 C26 N2 Pd1 175.6(2) . . . . ?
C19 N1 N2 C26 177.3(3) . . . . ?
C19 N1 N2 Pd1 0.7(3) . . . . ?
N1 C19 O1 Pd1 -3.8(4) . . . . ?
C20 C19 O1 Pd1 176.2(2) . . . . ?
C14 C13 P1 C7 128.0(3) . . . . ?
C18 C13 P1 C7 -56.1(3) . . . . ?
C14 C13 P1 C1 17.2(3) . . . . ?
C18 C13 P1 C1 -166.8(3) . . . . ?
C14 C13 P1 Pd1 -112.1(3) . . . . ?
C18 C13 P1 Pd1 63.9(3) . . . . ?
C12 C7 P1 C13 -13.0(3) . . . . ?
C8 C7 P1 C13 170.9(3) . . . . ?
C12 C7 P1 C1 98.4(3) . . . . ?
C8 C7 P1 C1 -77.8(3) . . . . ?
C12 C7 P1 Pd1 -134.1(3) . . . . ?
C8 C7 P1 Pd1 49.8(3) . . . . ?
C2 C1 P1 C13 -97.8(3) . . . . ?
C6 C1 P1 C13 81.9(3) . . . . ?
C2 C1 P1 C7 150.2(3) . . . . ?
C6 C1 P1 C7 -30.2(3) . . . . ?
C2 C1 P1 Pd1 27.8(3) . . . . ?
C6 C1 P1 Pd1 -152.6(2) . . . . ?
C29 C28 S1 C27 -0.3(3) . . . . ?
C30 C27 S1 C28 0.2(3) . . . . ?
C26 C27 S1 C28 178.2(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
C8 H8 Cl1 0.93 2.81 3.629(4) 147.4 .
C26 H26 Cl1 0.93 2.76 3.364(3) 123.1 .

_refine_diff_density_max         0.504
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.146

# start Validation Reply Form
_vrf_PLAT910_SM29                
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         11 Report
RESPONSE: These reflections were severely affected by primary extinction.
They were manually removed from the hkl data set.
;
_vrf_PLAT934_SM29                
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE: These also could be FO and FC mismatch due to
extinction, but as they are not serious, the reflections were
not omitted.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_sm30_0m
_database_code_depnum_ccdc_archive 'CCDC 1435108'
_audit_update_record             
;
2015-11-04 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 Cl N2 O2 P Pd S'
_chemical_formula_sum            'C32 H28 Cl N2 O2 P Pd S'
_chemical_formula_weight         677.44

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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.605(2)
_cell_length_b                   18.386(5)
_cell_length_c                   19.197(5)
_cell_angle_alpha                112.769(12)
_cell_angle_beta                 101.774(12)
_cell_angle_gamma                97.141(13)
_cell_volume                     2981.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4100
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      29

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_process_details   'SADABS;Sheldrick, 1996'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD Diffractometer'
_diffrn_measurement_method       'ω and φ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62787
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         30.11
_reflns_number_total             17579
_reflns_number_gt                11546
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SIR92 (Altornare et al., 1993)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-2008 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1135P)²+2.7079P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17147
_refine_ls_number_parameters     725
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1686
_refine_ls_wR_factor_gt          0.1168
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_restrained_S_all      0.846
_refine_ls_shift/su_max          0.004
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.05806(2) 0.060857(13) 0.241310(12) 0.03558(8) Uani 1 1 d . . .
Pd2 Pd 1.05313(2) 0.565020(15) 0.239802(13) 0.04146(8) Uani 1 1 d . . .
Cl2 Cl 1.28706(11) 0.55002(9) 0.25420(8) 0.0878(4) Uani 1 1 d . . .
P2 P 1.03472(8) 0.53091(5) 0.33978(5) 0.03919(17) Uani 1 1 d . . .
S1 S 1.00010(11) 0.14332(6) 0.00397(5) 0.0527(2) Uani 1 1 d . . .
S2 S 0.98889(11) 0.64289(6) -0.00078(5) 0.0540(2) Uani 1 1 d . . .
P1 P 1.04437(8) 0.03325(5) 0.34590(4) 0.03604(16) Uani 1 1 d . . .
Cl1 Cl 1.28062(10) 0.03057(7) 0.24738(6) 0.0605(2) Uani 1 1 d . . .
O1 O 0.8700(2) 0.09873(14) 0.23025(13) 0.0438(5) Uani 1 1 d . . .
O2 O 0.3867(3) 0.2829(2) 0.15962(18) 0.0715(8) Uani 1 1 d . . .
O3 O 0.8615(2) 0.59843(14) 0.22733(13) 0.0449(5) Uani 1 1 d . . .
O4 O 0.3702(3) 0.77827(19) 0.16248(18) 0.0703(8) Uani 1 1 d . . .
N1 N 0.9407(3) 0.12760(16) 0.13344(14) 0.0397(5) Uani 1 1 d . . .
N4 N 1.0494(3) 0.59747(16) 0.14880(14) 0.0384(5) Uani 1 1 d . . .
N3 N 0.9330(3) 0.63214(16) 0.13321(14) 0.0397(5) Uani 1 1 d . . .
C1 C 0.8551(3) 0.12868(18) 0.17849(16) 0.0375(6) Uani 1 1 d . . .
N2 N 1.0556(3) 0.09182(15) 0.14903(14) 0.0358(5) Uani 1 1 d . . .
C9 C 1.1388(3) 0.07897(18) 0.10309(17) 0.0393(6) Uani 1 1 d . . .
H9 H 1.2152 0.0554 0.1148 0.047 Uiso 1 1 calc R . .
C10 C 1.1283(3) 0.09650(18) 0.03605(18) 0.0400(6) Uani 1 1 d . . .
C13 C 1.2207(4) 0.0777(2) -0.0127(2) 0.0491(7) Uani 1 1 d . . .
C14 C 1.3424(4) 0.0379(3) -0.0021(3) 0.0661(10) Uani 1 1 d . . .
H14C H 1.4184 0.0742 0.0441 0.099 Uiso 1 1 calc R . .
H14A H 1.3798 0.0238 -0.0472 0.099 Uiso 1 1 calc R . .
H14B H 1.3081 -0.0102 0.0037 0.099 Uiso 1 1 calc R . .
C12 C 1.1831(5) 0.1019(2) -0.0747(2) 0.0637(10) Uani 1 1 d . . .
H12 H 1.2326 0.0936 -0.1130 0.076 Uiso 1 1 calc R . .
C11 C 1.0700(5) 0.1377(3) -0.0727(2) 0.0654(10) Uani 1 1 d . . .
H11 H 1.0334 0.1573 -0.1090 0.078 Uiso 1 1 calc R . .
C2 C 0.7304(3) 0.16736(19) 0.16993(17) 0.0404(6) Uani 1 1 d . . .
C3 C 0.6259(4) 0.1635(2) 0.2102(2) 0.0545(8) Uani 1 1 d . . .
H3 H 0.6333 0.1349 0.2410 0.065 Uiso 1 1 calc R . .
C4 C 0.5115(4) 0.2017(3) 0.2050(2) 0.0621(10) Uani 1 1 d . . .
H4 H 0.4424 0.1984 0.2319 0.075 Uiso 1 1 calc R . .
C5 C 0.5000(4) 0.2449(2) 0.1594(2) 0.0538(8) Uani 1 1 d . . .
C8 C 0.3604(6) 0.3209(3) 0.1085(3) 0.0885(16) Uani 1 1 d . . .
H8C H 0.4470 0.3597 0.1183 0.133 Uiso 1 1 calc R . .
H8B H 0.2821 0.3479 0.1173 0.133 Uiso 1 1 calc R . .
H8A H 0.3343 0.2809 0.0550 0.133 Uiso 1 1 calc R . .
C6 C 0.6007(4) 0.2473(2) 0.1168(2) 0.0566(9) Uani 1 1 d . . .
H6 H 0.5916 0.2746 0.0848 0.068 Uiso 1 1 calc R . .
C7 C 0.7145(4) 0.2085(2) 0.1227(2) 0.0509(8) Uani 1 1 d . . .
H7 H 0.7817 0.2101 0.0943 0.061 Uiso 1 1 calc R . .
C15 C 1.1317(4) 0.12173(18) 0.43850(18) 0.0428(6) Uani 1 1 d . . .
C20 C 1.2693(4) 0.1643(2) 0.4485(2) 0.0597(9) Uani 1 1 d . . .
H20 H 1.3133 0.1487 0.4077 0.072 Uiso 1 1 calc R . .
C19 C 1.3413(5) 0.2297(3) 0.5190(3) 0.0789(13) Uani 1 1 d . . .
H19 H 1.4340 0.2576 0.5252 0.095 Uiso 1 1 calc R . .
C18 C 1.2802(6) 0.2540(2) 0.5790(2) 0.0770(13) Uani 1 1 d . . .
H18 H 1.3305 0.2982 0.6261 0.092 Uiso 1 1 calc R . .
C17 C 1.1426(5) 0.2132(3) 0.5704(2) 0.0684(11) Uani 1 1 d . . .
H17 H 1.0994 0.2305 0.6114 0.082 Uiso 1 1 calc R . .
C16 C 1.0684(4) 0.1461(2) 0.50050(19) 0.0548(8) Uani 1 1 d . . .
H16 H 0.9769 0.1177 0.4953 0.066 Uiso 1 1 calc R . .
C21 C 0.8578(3) 0.00477(19) 0.34781(18) 0.0420(6) Uani 1 1 d . . .
C26 C 0.7672(3) 0.0586(2) 0.34787(19) 0.0480(7) Uani 1 1 d . . .
H26 H 0.8041 0.1085 0.3492 0.058 Uiso 1 1 calc R . .
C25 C 0.6237(4) 0.0378(2) 0.3459(2) 0.0550(8) Uani 1 1 d . . .
H25 H 0.5638 0.0739 0.3464 0.066 Uiso 1 1 calc R . .
C24 C 0.5675(4) -0.0366(3) 0.3434(2) 0.0628(9) Uani 1 1 d . . .
H24 H 0.4697 -0.0509 0.3409 0.075 Uiso 1 1 calc R . .
C23 C 0.6567(4) -0.0890(2) 0.3445(3) 0.0672(10) Uani 1 1 d . . .
H23 H 0.6195 -0.1385 0.3439 0.081 Uiso 1 1 calc R . .
C22 C 0.8016(4) -0.0690(2) 0.3465(2) 0.0551(8) Uani 1 1 d . . .
H22 H 0.8612 -0.1050 0.3469 0.066 Uiso 1 1 calc R . .
C27 C 1.1297(3) -0.04721(18) 0.35403(18) 0.0421(6) Uani 1 1 d . . .
C28 C 1.2198(4) -0.0387(2) 0.42411(19) 0.0503(7) Uani 1 1 d . . .
H28 H 1.2379 0.0091 0.4692 0.060 Uiso 1 1 calc R . .
C29 C 1.2833(4) -0.1018(2) 0.4271(2) 0.0647(10) Uani 1 1 d . . .
H29 H 1.3444 -0.0958 0.4743 0.078 Uiso 1 1 calc R . .
C30 C 1.2565(5) -0.1725(2) 0.3613(3) 0.0677(11) Uani 1 1 d . . .
H30 H 1.2999 -0.2142 0.3637 0.081 Uiso 1 1 calc R . .
C31 C 1.1656(5) -0.1822(2) 0.2914(3) 0.0682(11) Uani 1 1 d . . .
H31 H 1.1464 -0.2307 0.2468 0.082 Uiso 1 1 calc R . .
C32 C 1.1029(5) -0.1197(2) 0.2876(2) 0.0617(10) Uani 1 1 d . . .
H32 H 1.0422 -0.1262 0.2402 0.074 Uiso 1 1 calc R . .
C47 C 1.1674(3) 0.60244(19) 0.43075(19) 0.0438(7) Uani 1 1 d . . .
C48 C 1.2491(4) 0.5798(2) 0.4834(2) 0.0546(8) Uani 1 1 d . . .
H48 H 1.2393 0.5253 0.4726 0.065 Uiso 1 1 calc R . .
C49 C 1.3462(5) 0.6382(3) 0.5524(2) 0.0707(11) Uani 1 1 d . . .
H49 H 1.4012 0.6225 0.5878 0.085 Uiso 1 1 calc R . .
C50 C 1.3617(5) 0.7190(3) 0.5689(2) 0.0721(11) Uani 1 1 d . . .
H50 H 1.4278 0.7577 0.6151 0.086 Uiso 1 1 calc R . .
C51 C 1.2793(5) 0.7424(3) 0.5172(3) 0.0724(12) Uani 1 1 d . . .
H51 H 1.2879 0.7971 0.5288 0.087 Uiso 1 1 calc R . .
C52 C 1.1842(4) 0.6846(2) 0.4483(2) 0.0613(9) Uani 1 1 d . . .
H52 H 1.1303 0.7006 0.4128 0.074 Uiso 1 1 calc R . .
C53 C 0.8596(3) 0.5352(2) 0.36133(19) 0.0438(7) Uani 1 1 d . . .
C54 C 0.7336(4) 0.4912(3) 0.3010(2) 0.0636(10) Uani 1 1 d . . .
H54 H 0.7402 0.4624 0.2504 0.076 Uiso 1 1 calc R . .
C55 C 0.5991(4) 0.4898(3) 0.3153(3) 0.0717(11) Uani 1 1 d . . .
H55 H 0.5153 0.4600 0.2743 0.086 Uiso 1 1 calc R . .
C56 C 0.5879(4) 0.5318(3) 0.3887(3) 0.0665(10) Uani 1 1 d . . .
H56 H 0.4966 0.5306 0.3981 0.080 Uiso 1 1 calc R . .
C57 C 0.7104(4) 0.5756(2) 0.4489(2) 0.0604(9) Uani 1 1 d . . .
H57 H 0.7022 0.6040 0.4993 0.072 Uiso 1 1 calc R . .
C58 C 0.8465(4) 0.5780(2) 0.4356(2) 0.0507(7) Uani 1 1 d . . .
H58 H 0.9294 0.6087 0.4768 0.061 Uiso 1 1 calc R . .
C59 C 1.0566(3) 0.43067(19) 0.32973(18) 0.0439(7) Uani 1 1 d . . .
C60 C 1.1645(5) 0.3984(3) 0.2980(3) 0.0755(13) Uani 1 1 d . . .
H60 H 1.2205 0.4263 0.2781 0.091 Uiso 1 1 calc R . .
C61 C 1.1892(7) 0.3249(3) 0.2957(4) 0.0923(16) Uani 1 1 d . . .
H61 H 1.2624 0.3041 0.2748 0.111 Uiso 1 1 calc R . .
C62 C 1.1060(5) 0.2823(2) 0.3242(3) 0.0724(11) Uani 1 1 d . . .
H62 H 1.1240 0.2335 0.3234 0.087 Uiso 1 1 calc R . .
C63 C 0.9971(5) 0.3125(2) 0.3536(2) 0.0703(11) Uani 1 1 d . . .
H63 H 0.9391 0.2835 0.3718 0.084 Uiso 1 1 calc R . .
C64 C 0.9723(4) 0.3865(2) 0.3565(2) 0.0596(9) Uani 1 1 d . . .
H64 H 0.8979 0.4065 0.3767 0.071 Uiso 1 1 calc R . .
C41 C 1.1314(3) 0.58390(19) 0.10240(18) 0.0402(6) Uani 1 1 d . . .
H41 H 1.2089 0.5613 0.1149 0.048 Uiso 1 1 calc R . .
C42 C 1.1195(3) 0.59894(19) 0.03352(18) 0.0410(6) Uani 1 1 d . . .
C45 C 1.2127(4) 0.5799(2) -0.01448(19) 0.0479(7) Uani 1 1 d . . .
C46 C 1.3370(4) 0.5408(3) -0.0027(2) 0.0646(10) Uani 1 1 d . . .
H46C H 1.4151 0.5790 0.0414 0.097 Uiso 1 1 calc R . .
H46A H 1.3708 0.5233 -0.0490 0.097 Uiso 1 1 calc R . .
H46B H 1.3053 0.4949 0.0071 0.097 Uiso 1 1 calc R . .
C44 C 1.1742(5) 0.6021(3) -0.0777(2) 0.0653(11) Uani 1 1 d . . .
H44 H 1.2245 0.5936 -0.1157 0.078 Uiso 1 1 calc R . .
C43 C 1.0600(5) 0.6360(3) -0.0778(2) 0.0676(11) Uani 1 1 d . . .
H43 H 1.0226 0.6539 -0.1153 0.081 Uiso 1 1 calc R . .
C33 C 0.8462(3) 0.63032(18) 0.17699(17) 0.0381(6) Uani 1 1 d . . .
C34 C 0.7189(3) 0.66725(19) 0.16924(17) 0.0397(6) Uani 1 1 d . . .
C35 C 0.6122(4) 0.6574(2) 0.20629(18) 0.0445(7) Uani 1 1 d . . .
H35 H 0.6190 0.6255 0.2339 0.053 Uiso 1 1 calc R . .
C36 C 0.4966(4) 0.6947(2) 0.2023(2) 0.0522(8) Uani 1 1 d . . .
H36 H 0.4259 0.6879 0.2273 0.063 Uiso 1 1 calc R . .
C37 C 0.4854(4) 0.7424(2) 0.1610(2) 0.0519(8) Uani 1 1 d . . .
C40 C 0.3530(6) 0.8279(4) 0.1226(3) 0.0950(17) Uani 1 1 d . . .
H40C H 0.4424 0.8673 0.1388 0.142 Uiso 1 1 calc R . .
H40A H 0.2761 0.8550 0.1348 0.142 Uiso 1 1 calc R . .
H40B H 0.3288 0.7953 0.0670 0.142 Uiso 1 1 calc R . .
C38 C 0.5888(4) 0.7506(2) 0.1217(2) 0.0554(8) Uani 1 1 d . . .
H38 H 0.5805 0.7811 0.0927 0.066 Uiso 1 1 calc R . .
C39 C 0.7041(4) 0.7129(2) 0.1264(2) 0.0514(8) Uani 1 1 d . . .
H39 H 0.7733 0.7184 0.1001 0.062 Uiso 1 1 calc R . .


_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 O1 2.015(2) . ?
Pd1 N2 2.057(2) . ?
Pd1 Cl1 2.2667(10) . ?
Pd1 P1 2.2773(9) . ?
Pd2 O3 2.010(2) . ?
Pd2 N4 2.048(2) . ?
Pd2 P2 2.2694(9) . ?
Pd2 Cl2 2.2718(11) . ?
P2 C53 1.816(3) . ?
P2 C47 1.817(3) . ?
P2 C59 1.821(3) . ?
S1 C11 1.713(4) . ?
S1 C10 1.732(3) . ?
S2 C43 1.720(4) . ?
S2 C42 1.729(3) . ?
P1 C21 1.815(3) . ?
P1 C27 1.820(3) . ?
P1 C15 1.823(3) . ?
O1 C1 1.302(3) . ?
O2 C5 1.364(4) . ?
O2 C8 1.411(6) . ?
O3 C33 1.304(3) . ?
O4 C37 1.356(4) . ?
O4 C40 1.404(6) . ?
N1 C1 1.306(4) . ?
N1 N2 1.392(3) . ?
N4 C41 1.280(4) . ?
N4 N3 1.391(3) . ?
N3 C33 1.306(4) . ?
C1 C2 1.480(4) . ?
N2 C9 1.282(3) . ?
C9 C10 1.431(4) . ?
C9 H9 0.9300 . ?
C10 C13 1.396(4) . ?
C13 C12 1.421(5) . ?
C13 C14 1.473(5) . ?
C14 H14C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C12 C11 1.338(6) . ?
C12 H12 0.9300 . ?
C11 H11 0.9300 . ?
C2 C7 1.386(4) . ?
C2 C3 1.397(4) . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(5) . ?
C8 H8C 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8A 0.9600 . ?
C6 C7 1.386(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C15 C20 1.385(5) . ?
C15 C16 1.392(4) . ?
C20 C19 1.382(6) . ?
C20 H20 0.9300 . ?
C19 C18 1.347(7) . ?
C19 H19 0.9300 . ?
C18 C17 1.381(6) . ?
C18 H18 0.9300 . ?
C17 C16 1.393(5) . ?
C17 H17 0.9300 . ?
C16 H16 0.9300 . ?
C21 C22 1.384(4) . ?
C21 C26 1.397(4) . ?
C26 C25 1.373(4) . ?
C26 H26 0.9300 . ?
C25 C24 1.385(5) . ?
C25 H25 0.9300 . ?
C24 C23 1.369(5) . ?
C24 H24 0.9300 . ?
C23 C22 1.384(5) . ?
C23 H23 0.9300 . ?
C22 H22 0.9300 . ?
C27 C28 1.383(4) . ?
C27 C32 1.391(5) . ?
C28 C29 1.390(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.366(6) . ?
C29 H29 0.9300 . ?
C30 C31 1.376(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.381(5) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C47 C48 1.375(4) . ?
C47 C52 1.395(5) . ?
C48 C49 1.387(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.375(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.377(6) . ?
C50 H50 0.9300 . ?
C51 C52 1.375(6) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C53 C58 1.377(4) . ?
C53 C54 1.385(5) . ?
C54 C55 1.373(5) . ?
C54 H54 0.9300 . ?
C55 C56 1.354(6) . ?
C55 H55 0.9300 . ?
C56 C57 1.363(6) . ?
C56 H56 0.9300 . ?
C57 C58 1.381(5) . ?
C57 H57 0.9300 . ?
C58 H58 0.9300 . ?
C59 C64 1.382(4) . ?
C59 C60 1.388(5) . ?
C60 C61 1.388(6) . ?
C60 H60 0.9300 . ?
C61 C62 1.379(7) . ?
C61 H61 0.9300 . ?
C62 C63 1.365(6) . ?
C62 H62 0.9300 . ?
C63 C64 1.393(5) . ?
C63 H63 0.9300 . ?
C64 H64 0.9300 . ?
C41 C42 1.438(4) . ?
C41 H41 0.9300 . ?
C42 C45 1.392(4) . ?
C45 C44 1.418(5) . ?
C45 C46 1.491(5) . ?
C46 H46C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C44 C43 1.327(6) . ?
C44 H44 0.9300 . ?
C43 H43 0.9300 . ?
C33 C34 1.480(4) . ?
C34 C39 1.386(4) . ?
C34 C35 1.393(4) . ?
C35 C36 1.380(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.392(5) . ?
C36 H36 0.9300 . ?
C37 C38 1.391(5) . ?
C40 H40C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C38 C39 1.383(4) . ?
C38 H38 0.9300 . ?
C39 H39 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
O1 Pd1 N2 78.66(9) . . ?
O1 Pd1 Cl1 172.07(7) . . ?
N2 Pd1 Cl1 94.44(7) . . ?
O1 Pd1 P1 96.17(6) . . ?
N2 Pd1 P1 174.64(6) . . ?
Cl1 Pd1 P1 90.62(3) . . ?
O3 Pd2 N4 78.77(9) . . ?
O3 Pd2 P2 95.68(6) . . ?
N4 Pd2 P2 174.41(7) . . ?
O3 Pd2 Cl2 169.19(7) . . ?
N4 Pd2 Cl2 94.22(7) . . ?
P2 Pd2 Cl2 91.37(3) . . ?
C53 P2 C47 104.52(15) . . ?
C53 P2 C59 103.10(14) . . ?
C47 P2 C59 106.07(14) . . ?
C53 P2 Pd2 113.27(10) . . ?
C47 P2 Pd2 110.45(10) . . ?
C59 P2 Pd2 118.26(10) . . ?
C11 S1 C10 91.61(18) . . ?
C43 S2 C42 91.33(19) . . ?
C21 P1 C27 105.10(14) . . ?
C21 P1 C15 105.63(15) . . ?
C27 P1 C15 104.99(14) . . ?
C21 P1 Pd1 112.81(10) . . ?
C27 P1 Pd1 116.24(10) . . ?
C15 P1 Pd1 111.21(10) . . ?
C1 O1 Pd1 110.77(17) . . ?
C5 O2 C8 118.6(3) . . ?
C33 O3 Pd2 110.57(18) . . ?
C37 O4 C40 118.8(4) . . ?
C1 N1 N2 111.2(2) . . ?
C41 N4 N3 117.9(2) . . ?
C41 N4 Pd2 128.5(2) . . ?
N3 N4 Pd2 113.32(17) . . ?
C33 N3 N4 111.0(2) . . ?
O1 C1 N1 125.7(2) . . ?
O1 C1 C2 117.3(2) . . ?
N1 C1 C2 117.1(2) . . ?
C9 N2 N1 117.5(2) . . ?
C9 N2 Pd1 129.2(2) . . ?
N1 N2 Pd1 113.19(17) . . ?
N2 C9 C10 127.9(3) . . ?
N2 C9 H9 116.1 . . ?
C10 C9 H9 116.1 . . ?
C13 C10 C9 124.1(3) . . ?
C13 C10 S1 110.8(2) . . ?
C9 C10 S1 125.1(2) . . ?
C10 C13 C12 111.3(3) . . ?
C10 C13 C14 125.0(3) . . ?
C12 C13 C14 123.6(3) . . ?
C13 C14 H14C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
H14C C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14C C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C12 C13 113.8(3) . . ?
C11 C12 H12 123.1 . . ?
C13 C12 H12 123.1 . . ?
C12 C11 S1 112.5(3) . . ?
C12 C11 H11 123.8 . . ?
S1 C11 H11 123.8 . . ?
C7 C2 C3 118.4(3) . . ?
C7 C2 C1 121.3(3) . . ?
C3 C2 C1 120.3(3) . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 119.9(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
O2 C5 C4 116.0(3) . . ?
O2 C5 C6 124.1(3) . . ?
C4 C5 C6 119.9(3) . . ?
O2 C8 H8C 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
O2 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
C7 C6 C5 119.4(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C2 C7 C6 121.4(3) . . ?
C2 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C20 C15 C16 118.8(3) . . ?
C20 C15 P1 118.4(3) . . ?
C16 C15 P1 122.7(3) . . ?
C19 C20 C15 120.1(4) . . ?
C19 C20 H20 120.0 . . ?
C15 C20 H20 120.0 . . ?
C18 C19 C20 121.4(4) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C18 C17 119.8(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C15 C16 C17 119.8(4) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C22 C21 C26 119.3(3) . . ?
C22 C21 P1 122.4(2) . . ?
C26 C21 P1 118.2(2) . . ?
C25 C26 C21 120.0(3) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C23 C24 C25 119.7(3) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C23 C22 120.6(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C28 C27 C32 118.9(3) . . ?
C28 C27 P1 122.2(2) . . ?
C32 C27 P1 118.9(2) . . ?
C27 C28 C29 120.0(3) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.4(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 120.3(3) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C32 119.7(4) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C27 120.6(4) . . ?
C31 C32 H32 119.7 . . ?
C27 C32 H32 119.7 . . ?
C48 C47 C52 118.8(3) . . ?
C48 C47 P2 123.5(3) . . ?
C52 C47 P2 117.7(2) . . ?
C47 C48 C49 120.2(3) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 H48 119.9 . . ?
C50 C49 C48 120.5(4) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C51 120.0(4) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C52 C51 C50 119.7(4) . . ?
C52 C51 H51 120.2 . . ?
C50 C51 H51 120.2 . . ?
C51 C52 C47 121.0(3) . . ?
C51 C52 H52 119.5 . . ?
C47 C52 H52 119.5 . . ?
C58 C53 C54 118.4(3) . . ?
C58 C53 P2 122.9(3) . . ?
C54 C53 P2 118.6(3) . . ?
C55 C54 C53 120.7(4) . . ?
C55 C54 H54 119.7 . . ?
C53 C54 H54 119.7 . . ?
C56 C55 C54 120.3(4) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C55 C56 C57 120.1(4) . . ?
C55 C56 H56 120.0 . . ?
C57 C56 H56 120.0 . . ?
C56 C57 C58 120.5(4) . . ?
C56 C57 H57 119.8 . . ?
C58 C57 H57 119.8 . . ?
C53 C58 C57 120.1(3) . . ?
C53 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C64 C59 C60 118.3(3) . . ?
C64 C59 P2 121.5(2) . . ?
C60 C59 P2 120.1(3) . . ?
C61 C60 C59 120.4(4) . . ?
C61 C60 H60 119.8 . . ?
C59 C60 H60 119.8 . . ?
C62 C61 C60 120.5(4) . . ?
C62 C61 H61 119.7 . . ?
C60 C61 H61 119.7 . . ?
C63 C62 C61 119.5(4) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
C62 C63 C64 120.3(4) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 H63 119.9 . . ?
C59 C64 C63 121.0(3) . . ?
C59 C64 H64 119.5 . . ?
C63 C64 H64 119.5 . . ?
N4 C41 C42 128.6(3) . . ?
N4 C41 H41 115.7 . . ?
C42 C41 H41 115.7 . . ?
C45 C42 C41 124.2(3) . . ?
C45 C42 S2 110.9(2) . . ?
C41 C42 S2 124.9(2) . . ?
C42 C45 C44 111.3(3) . . ?
C42 C45 C46 125.4(3) . . ?
C44 C45 C46 123.4(3) . . ?
C45 C46 H46C 109.5 . . ?
C45 C46 H46A 109.5 . . ?
H46C C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46C C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C44 C45 114.1(3) . . ?
C43 C44 H44 122.9 . . ?
C45 C44 H44 122.9 . . ?
C44 C43 S2 112.4(3) . . ?
C44 C43 H43 123.8 . . ?
S2 C43 H43 123.8 . . ?
O3 C33 N3 125.6(3) . . ?
O3 C33 C34 116.6(2) . . ?
N3 C33 C34 117.7(2) . . ?
C39 C34 C35 118.8(3) . . ?
C39 C34 C33 121.2(3) . . ?
C35 C34 C33 120.1(3) . . ?
C36 C35 C34 120.4(3) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C37 120.2(3) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
O4 C37 C38 124.4(3) . . ?
O4 C37 C36 115.7(3) . . ?
C38 C37 C36 119.9(3) . . ?
O4 C40 H40C 109.5 . . ?
O4 C40 H40A 109.5 . . ?
H40C C40 H40A 109.5 . . ?
O4 C40 H40B 109.5 . . ?
H40C C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C38 C37 119.2(3) . . ?
C39 C38 H38 120.4 . . ?
C37 C38 H38 120.4 . . ?
C38 C39 C34 121.5(3) . . ?
C38 C39 H39 119.3 . . ?
C34 C39 H39 119.3 . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        30.11
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.229
