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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H39 As Cl2 N2 Pd'
_chemical_formula_sum            'C39 H39 As Cl2 N2 Pd'
_chemical_formula_weight         787.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
As As 0.0499 2.0058 '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           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.556(7)
_cell_length_b                   13.840(6)
_cell_length_c                   15.138(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.799(7)
_cell_angle_gamma                90.00
_cell_volume                     3674(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6040
_cell_measurement_theta_min      2.2751
_cell_measurement_theta_max      26.6224

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1600
_exptl_absorpt_coefficient_mu    1.573
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7136
_exptl_absorpt_correction_T_max  0.7869
_exptl_absorpt_process_details   SADABS

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17968
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6452
_reflns_number_gt                4825
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0929P)²+0.0000P] 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         6452
_refine_ls_number_parameters     412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1522
_refine_ls_wR_factor_gt          0.1364
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
Pd1 Pd 0.24783(2) 0.42591(3) 0.31508(2) 0.03409(16) Uani 1 1 d . . .
Cl1 Cl 0.35236(9) 0.50736(11) 0.26730(10) 0.0615(4) Uani 1 1 d . . .
Cl2 Cl 0.14770(8) 0.34339(9) 0.37170(9) 0.0481(3) Uani 1 1 d . . .
As1 As 0.24658(3) 0.54431(4) 0.43278(3) 0.03742(18) Uani 1 1 d . . .
N1 N 0.2997(3) 0.2689(3) 0.1886(3) 0.0415(10) Uani 1 1 d . . .
N2 N 0.2002(3) 0.3444(3) 0.1373(3) 0.0446(11) Uani 1 1 d . . .
C1 C 0.2499(3) 0.3386(3) 0.2093(3) 0.0342(11) Uani 1 1 d . . .
C2 C 0.2808(4) 0.2312(4) 0.1049(4) 0.0574(16) Uani 1 1 d . . .
H2 H 0.3063 0.1820 0.0766 0.069 Uiso 1 1 calc R . .
C3 C 0.2195(4) 0.2787(4) 0.0729(4) 0.0569(16) Uani 1 1 d . . .
H3 H 0.1945 0.2695 0.0179 0.068 Uiso 1 1 calc R . .
C4 C 0.3628(3) 0.2346(4) 0.2460(3) 0.0442(13) Uani 1 1 d . . .
C5 C 0.4364(3) 0.2610(4) 0.2264(4) 0.0528(14) Uani 1 1 d . . .
C6 C 0.4946(4) 0.2238(5) 0.2839(5) 0.0680(19) Uani 1 1 d . . .
H6 H 0.5448 0.2394 0.2732 0.082 Uiso 1 1 calc R . .
C7 C 0.4811(4) 0.1654(5) 0.3551(5) 0.0673(19) Uani 1 1 d . . .
C8 C 0.4075(4) 0.1401(4) 0.3683(4) 0.0647(18) Uani 1 1 d . . .
H8 H 0.3975 0.0999 0.4155 0.078 Uiso 1 1 calc R . .
C9 C 0.3472(3) 0.1720(4) 0.3142(4) 0.0493(14) Uani 1 1 d . . .
C10 C 0.4528(4) 0.3249(5) 0.1506(5) 0.078(2) Uani 1 1 d . . .
H10A H 0.4365 0.2938 0.0963 0.116 Uiso 1 1 calc R . .
H10B H 0.5066 0.3373 0.1507 0.116 Uiso 1 1 calc R . .
H10C H 0.4260 0.3849 0.1560 0.116 Uiso 1 1 calc R . .
C11 C 0.2662(4) 0.1365(4) 0.3270(5) 0.0698(19) Uani 1 1 d . . .
H11A H 0.2343 0.1904 0.3405 0.105 Uiso 1 1 calc R . .
H11B H 0.2667 0.0910 0.3749 0.105 Uiso 1 1 calc R . .
H11C H 0.2466 0.1058 0.2738 0.105 Uiso 1 1 calc R . .
C12 C 0.5469(5) 0.1281(7) 0.4143(5) 0.106(3) Uani 1 1 d . . .
H12A H 0.5675 0.0708 0.3887 0.159 Uiso 1 1 calc R . .
H12B H 0.5290 0.1131 0.4716 0.159 Uiso 1 1 calc R . .
H12C H 0.5859 0.1766 0.4200 0.159 Uiso 1 1 calc R . .
C13 C 0.1353(3) 0.4080(4) 0.1298(3) 0.0428(13) Uani 1 1 d . . .
C14 C 0.1464(4) 0.5034(4) 0.1044(4) 0.0544(15) Uani 1 1 d . . .
C15 C 0.0820(5) 0.5632(5) 0.1003(4) 0.0661(19) Uani 1 1 d . . .
H15 H 0.0878 0.6281 0.0862 0.079 Uiso 1 1 calc R . .
C16 C 0.0110(4) 0.5294(5) 0.1164(4) 0.067(2) Uani 1 1 d . . .
C17 C 0.0026(4) 0.4333(5) 0.1392(4) 0.0604(17) Uani 1 1 d . . .
H17 H -0.0457 0.4099 0.1503 0.073 Uiso 1 1 calc R . .
C18 C 0.0644(4) 0.3713(4) 0.1459(3) 0.0513(15) Uani 1 1 d . . .
C19 C 0.2212(4) 0.5418(5) 0.0799(5) 0.076(2) Uani 1 1 d . . .
H19A H 0.2612 0.5086 0.1131 0.115 Uiso 1 1 calc R . .
H19B H 0.2238 0.6096 0.0931 0.115 Uiso 1 1 calc R . .
H19C H 0.2270 0.5321 0.0179 0.115 Uiso 1 1 calc R . .
C20 C 0.0531(4) 0.2659(5) 0.1696(4) 0.0694(18) Uani 1 1 d . . .
H20A H 0.0606 0.2264 0.1187 0.104 Uiso 1 1 calc R . .
H20B H 0.0022 0.2567 0.1887 0.104 Uiso 1 1 calc R . .
H20C H 0.0892 0.2480 0.2164 0.104 Uiso 1 1 calc R . .
C21 C -0.0583(5) 0.5957(6) 0.1085(5) 0.093(3) Uani 1 1 d . . .
H21A H -0.0511 0.6490 0.1485 0.140 Uiso 1 1 calc R . .
H21B H -0.1030 0.5602 0.1229 0.140 Uiso 1 1 calc R . .
H21C H -0.0644 0.6195 0.0490 0.140 Uiso 1 1 calc R . .
C22 C 0.1620(3) 0.5554(4) 0.5097(3) 0.0427(13) Uani 1 1 d . . .
C23 C 0.1556(4) 0.4916(4) 0.5785(4) 0.0623(17) Uani 1 1 d . . .
H23 H 0.1926 0.4441 0.5882 0.075 Uiso 1 1 calc R . .
C24 C 0.0947(4) 0.4969(5) 0.6341(4) 0.0700(19) Uani 1 1 d . . .
H24 H 0.0918 0.4538 0.6810 0.084 Uiso 1 1 calc R . .
C25 C 0.0401(4) 0.5640(5) 0.6201(4) 0.0685(19) Uani 1 1 d . . .
H25 H -0.0009 0.5671 0.6567 0.082 Uiso 1 1 calc R . .
C26 C 0.0453(4) 0.6279(6) 0.5515(5) 0.082(2) Uani 1 1 d . . .
H26 H 0.0077 0.6745 0.5418 0.099 Uiso 1 1 calc R . .
C27 C 0.1054(4) 0.6240(5) 0.4970(4) 0.0678(18) Uani 1 1 d . . .
H27 H 0.1080 0.6682 0.4510 0.081 Uiso 1 1 calc R . .
C28 C 0.3317(3) 0.5289(4) 0.5178(3) 0.0482(14) Uani 1 1 d . . .
C29 C 0.3862(4) 0.4619(5) 0.5005(4) 0.0619(17) Uani 1 1 d . . .
H29 H 0.3847 0.4294 0.4466 0.074 Uiso 1 1 calc R . .
C30 C 0.4444(4) 0.4426(6) 0.5651(6) 0.090(3) Uani 1 1 d . . .
H30 H 0.4819 0.3973 0.5541 0.108 Uiso 1 1 calc R . .
C31 C 0.4459(5) 0.4911(9) 0.6448(7) 0.108(4) Uani 1 1 d . . .
H31 H 0.4846 0.4784 0.6874 0.130 Uiso 1 1 calc R . .
C32 C 0.3917(6) 0.5567(8) 0.6615(6) 0.106(3) Uani 1 1 d . . .
H32 H 0.3928 0.5885 0.7156 0.127 Uiso 1 1 calc R . .
C33 C 0.3347(5) 0.5767(5) 0.5986(4) 0.077(2) Uani 1 1 d . . .
H33 H 0.2979 0.6226 0.6102 0.092 Uiso 1 1 calc R . .
C34 C 0.2503(4) 0.6731(4) 0.3829(4) 0.0507(15) Uani 1 1 d . . .
C35 C 0.2959(4) 0.7457(4) 0.4166(4) 0.0681(19) Uani 1 1 d . . .
H35 H 0.3279 0.7345 0.4663 0.082 Uiso 1 1 calc R . .
C36 C 0.2943(6) 0.8366(5) 0.3764(6) 0.093(3) Uani 1 1 d . . .
H36 H 0.3272 0.8852 0.3970 0.112 Uiso 1 1 calc R . .
C37 C 0.2430(6) 0.8535(5) 0.3054(6) 0.101(3) Uani 1 1 d . . .
H37 H 0.2385 0.9153 0.2818 0.121 Uiso 1 1 calc R . .
C38 C 0.2003(5) 0.7824(6) 0.2707(5) 0.091(3) Uani 1 1 d . . .
H38 H 0.1688 0.7938 0.2207 0.110 Uiso 1 1 calc R . .
C39 C 0.2026(4) 0.6908(5) 0.3090(4) 0.0691(19) Uani 1 1 d . . .
H39 H 0.1721 0.6415 0.2850 0.083 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 C1 2.008(5) . ?
Pd1 Cl2 2.2970(15) . ?
Pd1 Cl1 2.3004(17) . ?
Pd1 As1 2.4216(9) . ?
As1 C28 1.936(5) . ?
As1 C22 1.937(6) . ?
As1 C34 1.938(5) . ?
N1 C1 1.350(6) . ?
N1 C2 1.396(6) . ?
N1 C4 1.453(6) . ?
N2 C1 1.365(6) . ?
N2 C3 1.389(6) . ?
N2 C13 1.440(7) . ?
C2 C3 1.332(8) . ?
C4 C9 1.386(8) . ?
C4 C5 1.388(8) . ?
C5 C6 1.407(8) . ?
C5 C10 1.488(9) . ?
C6 C7 1.376(9) . ?
C7 C8 1.364(10) . ?
C7 C12 1.518(9) . ?
C8 C9 1.378(8) . ?
C9 C11 1.526(9) . ?
C13 C18 1.376(8) . ?
C13 C14 1.392(8) . ?
C14 C15 1.400(9) . ?
C14 C19 1.480(9) . ?
C15 C16 1.364(10) . ?
C16 C17 1.384(9) . ?
C16 C21 1.524(9) . ?
C17 C18 1.383(8) . ?
C18 C20 1.518(8) . ?
C22 C23 1.375(8) . ?
C22 C27 1.381(8) . ?
C23 C24 1.396(9) . ?
C24 C25 1.345(9) . ?
C25 C26 1.370(9) . ?
C26 C27 1.371(9) . ?
C28 C29 1.366(8) . ?
C28 C33 1.388(8) . ?
C29 C30 1.406(10) . ?
C30 C31 1.381(13) . ?
C31 C32 1.348(14) . ?
C32 C33 1.374(11) . ?
C34 C35 1.367(8) . ?
C34 C39 1.386(8) . ?
C35 C36 1.398(9) . ?
C36 C37 1.387(11) . ?
C37 C38 1.329(12) . ?
C38 C39 1.394(9) . ?

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 Pd1 Cl2 92.42(14) . . ?
C1 Pd1 Cl1 89.91(14) . . ?
Cl2 Pd1 Cl1 176.22(6) . . ?
C1 Pd1 As1 174.39(14) . . ?
Cl2 Pd1 As1 91.57(4) . . ?
Cl1 Pd1 As1 86.32(5) . . ?
C28 As1 C22 101.5(2) . . ?
C28 As1 C34 108.7(2) . . ?
C22 As1 C34 101.7(2) . . ?
C28 As1 Pd1 112.35(18) . . ?
C22 As1 Pd1 122.04(15) . . ?
C34 As1 Pd1 109.53(16) . . ?
C1 N1 C2 110.5(5) . . ?
C1 N1 C4 125.4(4) . . ?
C2 N1 C4 124.1(4) . . ?
C1 N2 C3 110.7(4) . . ?
C1 N2 C13 124.9(4) . . ?
C3 N2 C13 124.4(4) . . ?
N1 C1 N2 104.7(4) . . ?
N1 C1 Pd1 130.7(4) . . ?
N2 C1 Pd1 124.4(3) . . ?
C3 C2 N1 107.3(5) . . ?
C2 C3 N2 106.8(5) . . ?
C9 C4 C5 122.9(5) . . ?
C9 C4 N1 118.5(5) . . ?
C5 C4 N1 118.4(5) . . ?
C4 C5 C6 115.3(6) . . ?
C4 C5 C10 122.6(5) . . ?
C6 C5 C10 122.1(6) . . ?
C7 C6 C5 123.5(6) . . ?
C8 C7 C6 117.7(6) . . ?
C8 C7 C12 121.7(8) . . ?
C6 C7 C12 120.5(7) . . ?
C7 C8 C9 122.5(7) . . ?
C8 C9 C4 118.0(6) . . ?
C8 C9 C11 121.0(6) . . ?
C4 C9 C11 121.1(5) . . ?
C18 C13 C14 122.6(5) . . ?
C18 C13 N2 118.6(5) . . ?
C14 C13 N2 118.7(5) . . ?
C13 C14 C15 116.7(6) . . ?
C13 C14 C19 123.2(6) . . ?
C15 C14 C19 120.1(6) . . ?
C16 C15 C14 122.1(6) . . ?
C15 C16 C17 119.0(6) . . ?
C15 C16 C21 120.8(7) . . ?
C17 C16 C21 120.2(8) . . ?
C18 C17 C16 121.3(7) . . ?
C13 C18 C17 118.1(6) . . ?
C13 C18 C20 121.8(5) . . ?
C17 C18 C20 120.1(6) . . ?
C23 C22 C27 117.5(6) . . ?
C23 C22 As1 119.9(4) . . ?
C27 C22 As1 122.6(4) . . ?
C22 C23 C24 121.1(6) . . ?
C25 C24 C23 120.2(6) . . ?
C24 C25 C26 119.5(6) . . ?
C25 C26 C27 120.9(7) . . ?
C26 C27 C22 120.9(6) . . ?
C29 C28 C33 119.7(6) . . ?
C29 C28 As1 118.1(5) . . ?
C33 C28 As1 121.9(5) . . ?
C28 C29 C30 119.2(7) . . ?
C31 C30 C29 119.8(8) . . ?
C32 C31 C30 120.5(8) . . ?
C31 C32 C33 120.1(9) . . ?
C32 C33 C28 120.6(9) . . ?
C35 C34 C39 119.4(6) . . ?
C35 C34 As1 124.1(4) . . ?
C39 C34 As1 116.5(4) . . ?
C34 C35 C36 120.0(7) . . ?
C37 C36 C35 119.1(7) . . ?
C38 C37 C36 120.9(7) . . ?
C37 C38 C39 120.3(7) . . ?
C34 C39 C38 120.0(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.698
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.165
_database_code_depnum_ccdc_archive 'CCDC 1003797'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H39 Cl2 N2 Pd Sb, C H2 Cl2'
_chemical_formula_sum            'C40 H41 Cl4 N2 Pd Sb'
_chemical_formula_weight         919.70

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.8365(19)
_cell_length_b                   13.9429(13)
_cell_length_c                   14.4872(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9250(10)
_cell_angle_gamma                90.00
_cell_volume                     4004.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.2945
_cell_measurement_theta_max      28.3769

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7452
_exptl_absorpt_correction_T_max  0.8260
_exptl_absorpt_process_details   SADABS

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19934
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7054
_reflns_number_gt                6085
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0281P)²+4.2296P] 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         7054
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0687
_refine_ls_wR_factor_gt          0.0641
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.748717(12) 0.973100(17) 0.282988(15) 0.03687(7) Uani 1 1 d . . .
Cl1 Cl 0.80324(7) 0.87486(7) 0.38793(6) 0.0823(4) Uani 1 1 d . . .
Cl2A Cl 0.7056(6) 1.0875(5) 0.1802(5) 0.0644(18) Uani 0.49(5) 1 d P . .
Cl2B Cl 0.6842(16) 1.0677(18) 0.1929(13) 0.103(5) Uani 0.51(5) 1 d P . .
Sb1 Sb 0.718515(10) 1.077252(15) 0.422978(13) 0.03787(7) Uani 1 1 d . . .
N1 N 0.81112(13) 0.87508(19) 0.11785(17) 0.0422(6) Uani 1 1 d . . .
N2 N 0.71833(13) 0.80848(19) 0.15304(17) 0.0425(6) Uani 1 1 d . . .
C1 C 0.76098(15) 0.8805(2) 0.17784(19) 0.0367(6) Uani 1 1 d . . .
C2 C 0.79989(19) 0.8003(3) 0.0559(2) 0.0548(9) Uani 1 1 d . . .
H2 H 0.8275 0.7826 0.0081 0.066 Uiso 1 1 calc R . .
C3 C 0.74208(19) 0.7588(3) 0.0778(2) 0.0555(9) Uani 1 1 d . . .
H3 H 0.7216 0.7066 0.0484 0.067 Uiso 1 1 calc R . .
C4 C 0.86724(15) 0.9405(2) 0.1140(2) 0.0424(7) Uani 1 1 d . . .
C5 C 0.86238(18) 1.0175(3) 0.0531(2) 0.0516(8) Uani 1 1 d . . .
C6 C 0.9171(2) 1.0793(3) 0.0507(3) 0.0634(10) Uani 1 1 d . . .
H6 H 0.9148 1.1317 0.0110 0.076 Uiso 1 1 calc R . .
C7 C 0.9746(2) 1.0660(3) 0.1047(3) 0.0634(11) Uani 1 1 d . . .
C8 C 0.97758(19) 0.9871(3) 0.1614(3) 0.0675(11) Uani 1 1 d . . .
H8 H 1.0167 0.9768 0.1973 0.081 Uiso 1 1 calc R . .
C9 C 0.92492(17) 0.9220(3) 0.1676(2) 0.0527(9) Uani 1 1 d . . .
C10 C 0.8014(2) 1.0325(3) -0.0094(3) 0.0815(13) Uani 1 1 d . . .
H10A H 0.7934 0.9760 -0.0458 0.122 Uiso 1 1 calc R . .
H10B H 0.8090 1.0861 -0.0493 0.122 Uiso 1 1 calc R . .
H10C H 0.7629 1.0452 0.0272 0.122 Uiso 1 1 calc R . .
C11 C 0.9321(2) 0.8351(4) 0.2276(3) 0.0846(14) Uani 1 1 d . . .
H11A H 0.8981 0.8361 0.2733 0.127 Uiso 1 1 calc R . .
H11B H 0.9759 0.8348 0.2576 0.127 Uiso 1 1 calc R . .
H11C H 0.9267 0.7784 0.1903 0.127 Uiso 1 1 calc R . .
C12 C 1.0328(2) 1.1355(4) 0.1002(4) 0.1049(19) Uani 1 1 d . . .
H12A H 1.0528 1.1307 0.0410 0.157 Uiso 1 1 calc R . .
H12B H 1.0660 1.1203 0.1478 0.157 Uiso 1 1 calc R . .
H12C H 1.0167 1.1997 0.1091 0.157 Uiso 1 1 calc R . .
C13 C 0.65591(16) 0.7858(2) 0.1968(2) 0.0420(7) Uani 1 1 d . . .
C14 C 0.59661(18) 0.8293(3) 0.1643(2) 0.0531(8) Uani 1 1 d . . .
C15 C 0.53763(19) 0.8053(3) 0.2072(3) 0.0646(10) Uani 1 1 d . . .
H15 H 0.4977 0.8353 0.1879 0.077 Uiso 1 1 calc R . .
C16 C 0.5358(2) 0.7395(3) 0.2767(3) 0.0622(10) Uani 1 1 d . . .
C17 C 0.5952(2) 0.6967(3) 0.3059(2) 0.0603(10) Uani 1 1 d . . .
H17 H 0.5943 0.6522 0.3538 0.072 Uiso 1 1 calc R . .
C18 C 0.65681(18) 0.7175(2) 0.2664(2) 0.0488(8) Uani 1 1 d . . .
C19 C 0.5958(2) 0.8970(4) 0.0834(3) 0.0859(14) Uani 1 1 d . . .
H19A H 0.5523 0.9267 0.0769 0.129 Uiso 1 1 calc R . .
H19B H 0.6050 0.8620 0.0281 0.129 Uiso 1 1 calc R . .
H19C H 0.6297 0.9454 0.0935 0.129 Uiso 1 1 calc R . .
C20 C 0.7196(2) 0.6656(3) 0.2960(3) 0.0753(12) Uani 1 1 d . . .
H20A H 0.7289 0.6164 0.2519 0.113 Uiso 1 1 calc R . .
H20B H 0.7137 0.6371 0.3555 0.113 Uiso 1 1 calc R . .
H20C H 0.7566 0.7100 0.2997 0.113 Uiso 1 1 calc R . .
C21 C 0.4691(2) 0.7108(4) 0.3174(4) 0.1030(19) Uani 1 1 d . . .
H21A H 0.4460 0.7672 0.3375 0.154 Uiso 1 1 calc R . .
H21B H 0.4775 0.6689 0.3691 0.154 Uiso 1 1 calc R . .
H21C H 0.4418 0.6783 0.2713 0.154 Uiso 1 1 calc R . .
C22 C 0.78311(15) 1.1001(2) 0.5419(2) 0.0414(7) Uani 1 1 d . . .
C23 C 0.79838(19) 1.1915(3) 0.5721(2) 0.0556(9) Uani 1 1 d . . .
H23 H 0.7818 1.2442 0.5393 0.067 Uiso 1 1 calc R . .
C24 C 0.8385(2) 1.2049(3) 0.6515(3) 0.0686(11) Uani 1 1 d . . .
H24 H 0.8494 1.2667 0.6709 0.082 Uiso 1 1 calc R . .
C25 C 0.8618(2) 1.1284(3) 0.7008(3) 0.0697(11) Uani 1 1 d . . .
H25 H 0.8884 1.1378 0.7541 0.084 Uiso 1 1 calc R . .
C26 C 0.8461(2) 1.0368(3) 0.6720(3) 0.0729(12) Uani 1 1 d . . .
H26 H 0.8618 0.9844 0.7061 0.087 Uiso 1 1 calc R . .
C27 C 0.8070(2) 1.0226(3) 0.5921(3) 0.0594(9) Uani 1 1 d . . .
H27 H 0.7969 0.9606 0.5723 0.071 Uiso 1 1 calc R . .
C28 C 0.63988(16) 1.0073(2) 0.4927(2) 0.0419(7) Uani 1 1 d . . .
C29 C 0.62309(19) 1.0327(3) 0.5809(2) 0.0555(9) Uani 1 1 d . . .
H29 H 0.6462 1.0822 0.6111 0.067 Uiso 1 1 calc R . .
C30 C 0.5720(2) 0.9850(3) 0.6250(3) 0.0676(11) Uani 1 1 d . . .
H30 H 0.5605 1.0031 0.6842 0.081 Uiso 1 1 calc R . .
C31 C 0.5387(2) 0.9113(3) 0.5813(3) 0.0675(11) Uani 1 1 d . . .
H31 H 0.5041 0.8797 0.6106 0.081 Uiso 1 1 calc R . .
C32 C 0.5559(2) 0.8840(3) 0.4954(3) 0.0692(11) Uani 1 1 d . . .
H32 H 0.5337 0.8327 0.4668 0.083 Uiso 1 1 calc R . .
C33 C 0.60615(19) 0.9319(3) 0.4498(3) 0.0562(9) Uani 1 1 d . . .
H33 H 0.6172 0.9133 0.3905 0.067 Uiso 1 1 calc R . .
C34 C 0.68221(16) 1.2199(2) 0.4037(2) 0.0422(7) Uani 1 1 d . . .
C35 C 0.70630(19) 1.2739(3) 0.3319(2) 0.0543(9) Uani 1 1 d . . .
H35 H 0.7362 1.2468 0.2913 0.065 Uiso 1 1 calc R . .
C36 C 0.6861(2) 1.3680(3) 0.3203(3) 0.0681(11) Uani 1 1 d . . .
H36 H 0.7026 1.4041 0.2720 0.082 Uiso 1 1 calc R . .
C37 C 0.6417(2) 1.4084(3) 0.3797(3) 0.0696(12) Uani 1 1 d . . .
H37 H 0.6277 1.4716 0.3713 0.083 Uiso 1 1 calc R . .
C38 C 0.6182(2) 1.3563(3) 0.4504(3) 0.0686(11) Uani 1 1 d . . .
H38 H 0.5887 1.3841 0.4910 0.082 Uiso 1 1 calc R . .
C39 C 0.63785(19) 1.2620(3) 0.4627(3) 0.0576(9) Uani 1 1 d . . .
H39 H 0.6210 1.2267 0.5113 0.069 Uiso 1 1 calc R . .
C40 C 0.9397(3) 0.4094(5) 0.9176(6) 0.140(3) Uani 1 1 d . . .
H40A H 0.9366 0.4691 0.8834 0.168 Uiso 1 1 calc R . .
H40B H 0.9172 0.4189 0.9753 0.168 Uiso 1 1 calc R . .
Cl3 Cl 0.89766(9) 0.32354(16) 0.85625(13) 0.1435(7) Uani 1 1 d . . .
Cl4 Cl 1.02192(11) 0.3859(2) 0.9416(2) 0.2084(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.018(3) . ?
Pd1 Cl2B 2.228(10) . ?
Pd1 Cl1 2.2906(10) . ?
Pd1 Cl2A 2.325(7) . ?
Pd1 Sb1 2.5812(3) . ?
Cl2A Cl2B 0.54(4) . ?
Sb1 C28 2.124(3) . ?
Sb1 C34 2.130(3) . ?
Sb1 C22 2.136(3) . ?
N1 C1 1.345(4) . ?
N1 C2 1.389(4) . ?
N1 C4 1.442(4) . ?
N2 C1 1.354(4) . ?
N2 C3 1.387(4) . ?
N2 C13 1.445(4) . ?
C2 C3 1.333(5) . ?
C4 C9 1.385(5) . ?
C4 C5 1.391(5) . ?
C5 C6 1.388(5) . ?
C5 C10 1.500(5) . ?
C6 C7 1.373(6) . ?
C7 C8 1.373(6) . ?
C7 C12 1.511(6) . ?
C8 C9 1.389(5) . ?
C9 C11 1.496(6) . ?
C13 C18 1.385(5) . ?
C13 C14 1.392(5) . ?
C14 C15 1.384(5) . ?
C14 C19 1.504(5) . ?
C15 C16 1.363(6) . ?
C16 C17 1.375(6) . ?
C16 C21 1.520(5) . ?
C17 C18 1.398(5) . ?
C18 C20 1.491(5) . ?
C22 C27 1.377(5) . ?
C22 C23 1.378(5) . ?
C23 C24 1.388(5) . ?
C24 C25 1.357(6) . ?
C25 C26 1.376(6) . ?
C26 C27 1.386(5) . ?
C28 C29 1.377(5) . ?
C28 C33 1.383(5) . ?
C29 C30 1.386(5) . ?
C30 C31 1.366(6) . ?
C31 C32 1.356(6) . ?
C32 C33 1.386(5) . ?
C34 C39 1.379(5) . ?
C34 C35 1.382(5) . ?
C35 C36 1.380(5) . ?
C36 C37 1.374(6) . ?
C37 C38 1.351(6) . ?
C38 C39 1.380(5) . ?
C40 Cl4 1.689(7) . ?
C40 Cl3 1.693(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
C1 Pd1 Cl2B 91.0(2) . . ?
C1 Pd1 Cl1 92.99(9) . . ?
Cl2B Pd1 Cl1 172.5(10) . . ?
C1 Pd1 Cl2A 90.4(2) . . ?
Cl2B Pd1 Cl2A 13.5(9) . . ?
Cl1 Pd1 Cl2A 172.1(3) . . ?
C1 Pd1 Sb1 171.97(9) . . ?
Cl2B Pd1 Sb1 89.0(3) . . ?
Cl1 Pd1 Sb1 86.09(3) . . ?
Cl2A Pd1 Sb1 91.56(19) . . ?
Cl2B Cl2A Pd1 73.1(16) . . ?
Cl2A Cl2B Pd1 93.4(16) . . ?
C28 Sb1 C34 103.92(12) . . ?
C28 Sb1 C22 96.60(12) . . ?
C34 Sb1 C22 99.08(12) . . ?
C28 Sb1 Pd1 108.00(9) . . ?
C34 Sb1 Pd1 120.56(8) . . ?
C22 Sb1 Pd1 124.67(8) . . ?
C1 N1 C2 110.7(3) . . ?
C1 N1 C4 125.3(3) . . ?
C2 N1 C4 123.9(3) . . ?
C1 N2 C3 110.7(3) . . ?
C1 N2 C13 125.7(2) . . ?
C3 N2 C13 123.6(3) . . ?
N1 C1 N2 104.8(2) . . ?
N1 C1 Pd1 129.4(2) . . ?
N2 C1 Pd1 125.8(2) . . ?
C3 C2 N1 107.0(3) . . ?
C2 C3 N2 106.8(3) . . ?
C9 C4 C5 122.5(3) . . ?
C9 C4 N1 119.0(3) . . ?
C5 C4 N1 118.4(3) . . ?
C6 C5 C4 117.2(3) . . ?
C6 C5 C10 120.9(4) . . ?
C4 C5 C10 121.9(3) . . ?
C7 C6 C5 122.5(4) . . ?
C6 C7 C8 117.9(4) . . ?
C6 C7 C12 120.7(4) . . ?
C8 C7 C12 121.4(4) . . ?
C7 C8 C9 123.0(4) . . ?
C4 C9 C8 116.8(4) . . ?
C4 C9 C11 122.4(3) . . ?
C8 C9 C11 120.7(4) . . ?
C18 C13 C14 122.4(3) . . ?
C18 C13 N2 118.6(3) . . ?
C14 C13 N2 118.8(3) . . ?
C15 C14 C13 117.4(3) . . ?
C15 C14 C19 121.0(4) . . ?
C13 C14 C19 121.6(3) . . ?
C16 C15 C14 122.5(4) . . ?
C15 C16 C17 118.5(4) . . ?
C15 C16 C21 120.6(4) . . ?
C17 C16 C21 120.9(4) . . ?
C16 C17 C18 122.3(4) . . ?
C13 C18 C17 116.8(3) . . ?
C13 C18 C20 122.2(3) . . ?
C17 C18 C20 121.0(3) . . ?
C27 C22 C23 119.4(3) . . ?
C27 C22 Sb1 119.7(2) . . ?
C23 C22 Sb1 120.9(2) . . ?
C22 C23 C24 120.1(4) . . ?
C25 C24 C23 120.4(4) . . ?
C24 C25 C26 120.0(4) . . ?
C25 C26 C27 120.1(4) . . ?
C22 C27 C26 120.1(4) . . ?
C29 C28 C33 118.9(3) . . ?
C29 C28 Sb1 121.8(3) . . ?
C33 C28 Sb1 119.2(2) . . ?
C28 C29 C30 120.5(4) . . ?
C31 C30 C29 119.8(4) . . ?
C32 C31 C30 120.3(4) . . ?
C31 C32 C33 120.6(4) . . ?
C28 C33 C32 119.8(4) . . ?
C39 C34 C35 118.5(3) . . ?
C39 C34 Sb1 122.4(2) . . ?
C35 C34 Sb1 118.9(2) . . ?
C36 C35 C34 120.2(4) . . ?
C37 C36 C35 120.2(4) . . ?
C38 C37 C36 119.9(4) . . ?
C37 C38 C39 120.6(4) . . ?
C34 C39 C38 120.5(4) . . ?
Cl4 C40 Cl3 115.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.066
_database_code_depnum_ccdc_archive 'CCDC 1003798'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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#  data retrieval see:
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data_1c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C45 H51 As Cl2 N2 Pd), C H2 Cl2'
_chemical_formula_sum            'C181 H206 As4 Cl10 N8 Pd4'
_chemical_formula_weight         3573.32

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'
N N 0.0061 0.0033 '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'
As As 0.0499 2.0058 '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           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   24.870(6)
_cell_length_b                   19.199(5)
_cell_length_c                   18.773(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.939(5)
_cell_angle_gamma                90.00
_cell_volume                     8770(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4270
_cell_measurement_theta_min      2.2807
_cell_measurement_theta_max      19.2039

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3668
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7546
_exptl_absorpt_correction_T_max  0.8224
_exptl_absorpt_process_details   SADABS

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44371
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_sigmaI/netI    0.1233
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.00
_reflns_number_total             15414
_reflns_number_gt                7894
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0447P)²+0.0000P] 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         15414
_refine_ls_number_parameters     872
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1352
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_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
Pd1 Pd 0.607892(19) 0.14942(2) 0.21073(2) 0.04098(14) Uani 1 1 d . . .
As1 As 0.53655(3) 0.22772(3) 0.14996(4) 0.05007(19) Uani 1 1 d . . .
N1 N 0.6895(2) 0.0677(2) 0.3239(3) 0.0435(12) Uani 1 1 d . . .
N2 N 0.69551(19) 0.0429(2) 0.2150(3) 0.0431(12) Uani 1 1 d . . .
Cl1 Cl 0.54872(7) 0.08636(9) 0.26227(10) 0.0674(5) Uani 1 1 d . . .
Cl2 Cl 0.66871(7) 0.21563(8) 0.16376(9) 0.0585(5) Uani 1 1 d . . .
C1 C 0.6675(2) 0.0835(3) 0.2539(3) 0.0386(14) Uani 1 1 d . . .
C2 C 0.7296(3) 0.0181(3) 0.3278(4) 0.0582(18) Uani 1 1 d . . .
H2 H 0.7504 -0.0009 0.3702 0.070 Uiso 1 1 calc R . .
C3 C 0.7332(3) 0.0019(3) 0.2603(4) 0.0575(18) Uani 1 1 d . . .
H3 H 0.7567 -0.0307 0.2463 0.069 Uiso 1 1 calc R . .
C4 C 0.6763(2) 0.0969(3) 0.3891(3) 0.0415(15) Uani 1 1 d . . .
C5 C 0.6937(2) 0.1643(3) 0.4099(3) 0.0449(16) Uani 1 1 d . . .
C6 C 0.6857(3) 0.1879(3) 0.4762(4) 0.0555(18) Uani 1 1 d . . .
H6 H 0.6964 0.2329 0.4909 0.067 Uiso 1 1 calc R . .
C7 C 0.6626(3) 0.1470(4) 0.5204(4) 0.0618(19) Uani 1 1 d . . .
H7 H 0.6587 0.1638 0.5655 0.074 Uiso 1 1 calc R . .
C8 C 0.6449(3) 0.0810(4) 0.4993(3) 0.0611(19) Uani 1 1 d . . .
H8 H 0.6287 0.0536 0.5299 0.073 Uiso 1 1 calc R . .
C9 C 0.6511(3) 0.0548(3) 0.4326(3) 0.0526(17) Uani 1 1 d . . .
C10 C 0.7212(3) 0.2105(3) 0.3632(4) 0.0651(19) Uani 1 1 d U . .
H10 H 0.7102 0.1939 0.3129 0.078 Uiso 1 1 calc R . .
C11 C 0.7018(4) 0.2855(4) 0.3644(5) 0.122(3) Uani 1 1 d U . .
H11A H 0.7169 0.3057 0.4111 0.183 Uiso 1 1 calc R . .
H11B H 0.6624 0.2865 0.3560 0.183 Uiso 1 1 calc R . .
H11C H 0.7140 0.3116 0.3271 0.183 Uiso 1 1 calc R . .
C12 C 0.7813(3) 0.2061(5) 0.3832(6) 0.144(4) Uani 1 1 d U . .
H12A H 0.7930 0.2108 0.4350 0.216 Uiso 1 1 calc R . .
H12B H 0.7972 0.2428 0.3595 0.216 Uiso 1 1 calc R . .
H12C H 0.7931 0.1619 0.3682 0.216 Uiso 1 1 calc R . .
C13 C 0.6298(4) -0.0170(4) 0.4123(4) 0.084(2) Uani 1 1 d . . .
H13 H 0.6288 -0.0230 0.3602 0.100 Uiso 1 1 calc R . .
C14 C 0.6689(4) -0.0727(4) 0.4529(5) 0.112(3) Uani 1 1 d . . .
H14A H 0.7044 -0.0678 0.4411 0.167 Uiso 1 1 calc R . .
H14B H 0.6545 -0.1182 0.4386 0.167 Uiso 1 1 calc R . .
H14C H 0.6720 -0.0671 0.5045 0.167 Uiso 1 1 calc R . .
C15 C 0.5719(4) -0.0278(5) 0.4237(5) 0.122(4) Uani 1 1 d . . .
H15A H 0.5718 -0.0254 0.4747 0.182 Uiso 1 1 calc R . .
H15B H 0.5587 -0.0726 0.4052 0.182 Uiso 1 1 calc R . .
H15C H 0.5483 0.0079 0.3983 0.182 Uiso 1 1 calc R . .
C16 C 0.6886(3) 0.0417(3) 0.1365(3) 0.0460(16) Uani 1 1 d . . .
C17 C 0.7282(3) 0.0749(3) 0.1056(3) 0.0504(16) Uani 1 1 d U . .
C18 C 0.7202(3) 0.0730(4) 0.0308(4) 0.071(2) Uani 1 1 d . . .
H18 H 0.7454 0.0947 0.0080 0.085 Uiso 1 1 calc R . .
C19 C 0.6760(4) 0.0400(4) -0.0107(4) 0.080(2) Uani 1 1 d . . .
H19 H 0.6717 0.0394 -0.0611 0.096 Uiso 1 1 calc R . .
C20 C 0.6382(3) 0.0079(4) 0.0208(4) 0.072(2) Uani 1 1 d . . .
H20 H 0.6081 -0.0138 -0.0085 0.087 Uiso 1 1 calc R . .
C21 C 0.6437(3) 0.0067(3) 0.0967(4) 0.0526(17) Uani 1 1 d . . .
C22 C 0.7785(3) 0.1098(3) 0.1494(4) 0.0618(18) Uani 1 1 d U . .
H22 H 0.7710 0.1202 0.1975 0.074 Uiso 1 1 calc R . .
C23 C 0.8280(3) 0.0618(4) 0.1608(5) 0.094(3) Uani 1 1 d . . .
H23A H 0.8204 0.0206 0.1859 0.142 Uiso 1 1 calc R . .
H23B H 0.8593 0.0853 0.1893 0.142 Uiso 1 1 calc R . .
H23C H 0.8357 0.0493 0.1145 0.142 Uiso 1 1 calc R . .
C24 C 0.7930(3) 0.1784(4) 0.1170(4) 0.084(2) Uani 1 1 d U . .
H24A H 0.8062 0.1692 0.0733 0.126 Uiso 1 1 calc R . .
H24B H 0.8211 0.2018 0.1515 0.126 Uiso 1 1 calc R . .
H24C H 0.7609 0.2074 0.1057 0.126 Uiso 1 1 calc R . .
C25 C 0.6036(3) -0.0328(3) 0.1311(4) 0.0629(19) Uani 1 1 d . . .
H25 H 0.6049 -0.0126 0.1794 0.075 Uiso 1 1 calc R . .
C26 C 0.6212(4) -0.1083(4) 0.1418(5) 0.111(3) Uani 1 1 d . . .
H26A H 0.6182 -0.1302 0.0952 0.167 Uiso 1 1 calc R . .
H26B H 0.5978 -0.1319 0.1689 0.167 Uiso 1 1 calc R . .
H26C H 0.6586 -0.1105 0.1682 0.167 Uiso 1 1 calc R . .
C27 C 0.5447(3) -0.0272(4) 0.0888(5) 0.106(3) Uani 1 1 d . . .
H27A H 0.5344 0.0210 0.0831 0.159 Uiso 1 1 calc R . .
H27B H 0.5208 -0.0509 0.1149 0.159 Uiso 1 1 calc R . .
H27C H 0.5417 -0.0482 0.0417 0.159 Uiso 1 1 calc R . .
C28 C 0.54130(13) 0.31800(15) 0.19551(18) 0.064(2) Uani 1 1 d GU . .
C29 C 0.59272(14) 0.3490(2) 0.2154(2) 0.106(3) Uani 1 1 d G . .
H29 H 0.6236 0.3265 0.2058 0.127 Uiso 1 1 calc R . .
C30 C 0.59798(17) 0.4137(2) 0.2494(2) 0.117(3) Uani 1 1 d G . .
H30 H 0.6324 0.4345 0.2627 0.141 Uiso 1 1 calc R . .
C31 C 0.55183(19) 0.44730(17) 0.2636(2) 0.107(3) Uani 1 1 d GU . .
H31 H 0.5554 0.4906 0.2864 0.128 Uiso 1 1 calc R . .
C32 C 0.50041(17) 0.41627(16) 0.2438(2) 0.120(4) Uani 1 1 d GU . .
H32 H 0.4695 0.4388 0.2533 0.144 Uiso 1 1 calc R . .
C33 C 0.49514(14) 0.35162(13) 0.20973(16) 0.101(3) Uani 1 1 d GU . .
H33 H 0.4607 0.3309 0.1965 0.121 Uiso 1 1 calc R . .
C34 C 0.45954(13) 0.20429(14) 0.14082(19) 0.0596(19) Uani 1 1 d G . .
C35 C 0.44040(15) 0.19082(16) 0.20424(19) 0.116(4) Uani 1 1 d G . .
H35 H 0.4637 0.1939 0.2498 0.139 Uiso 1 1 calc R . .
C36 C 0.38449(17) 0.1723(2) 0.1971(2) 0.140(4) Uani 1 1 d GU . .
H36 H 0.3712 0.1604 0.2383 0.168 Uiso 1 1 calc R . .
C37 C 0.34946(14) 0.1716(2) 0.1295(3) 0.118(3) Uani 1 1 d GU . .
H37 H 0.3122 0.1625 0.1255 0.142 Uiso 1 1 calc R . .
C38 C 0.36995(16) 0.1844(2) 0.0691(2) 0.127(4) Uani 1 1 d G . .
H38 H 0.3465 0.1829 0.0236 0.152 Uiso 1 1 calc R . .
C39 C 0.42549(17) 0.19983(19) 0.07386(18) 0.095(3) Uani 1 1 d G . .
H39 H 0.4391 0.2070 0.0319 0.114 Uiso 1 1 calc R . .
C40 C 0.5407(2) 0.2444(4) 0.0490(3) 0.0516(17) Uani 1 1 d . . .
C41 C 0.5243(3) 0.3067(4) 0.0152(4) 0.070(2) Uani 1 1 d . . .
H41 H 0.5116 0.3429 0.0402 0.083 Uiso 1 1 calc R . .
C42 C 0.5272(3) 0.3140(5) -0.0581(5) 0.086(3) Uani 1 1 d . . .
H42 H 0.5170 0.3559 -0.0818 0.103 Uiso 1 1 calc R . .
C43 C 0.5446(3) 0.2607(6) -0.0947(5) 0.092(3) Uani 1 1 d . . .
H43 H 0.5461 0.2661 -0.1435 0.111 Uiso 1 1 calc R . .
C44 C 0.5596(3) 0.1996(5) -0.0608(5) 0.092(3) Uani 1 1 d . . .
H44 H 0.5710 0.1630 -0.0866 0.111 Uiso 1 1 calc R . .
C45 C 0.5584(3) 0.1912(4) 0.0110(4) 0.074(2) Uani 1 1 d . . .
H45 H 0.5697 0.1493 0.0342 0.089 Uiso 1 1 calc R . .
C46 C 0.9256(3) 0.9537(3) 0.7238(3) 0.0509(17) Uani 1 1 d . . .
Pd2 Pd 0.86902(2) 0.87910(3) 0.69900(3) 0.05119(16) Uani 1 1 d . . .
As2 As 0.79712(3) 0.79148(4) 0.67398(4) 0.0599(2) Uani 1 1 d . . .
N3 N 0.9808(2) 0.9480(3) 0.7324(3) 0.0549(14) Uani 1 1 d . . .
N4 N 0.9167(2) 1.0220(3) 0.7313(3) 0.0512(14) Uani 1 1 d . . .
Cl3 Cl 0.88948(9) 0.87250(11) 0.58639(11) 0.0909(7) Uani 1 1 d . . .
Cl4 Cl 0.84743(8) 0.88856(10) 0.81059(10) 0.0793(6) Uani 1 1 d . . .
C47 C 1.0052(3) 1.0127(4) 0.7450(4) 0.075(2) Uani 1 1 d . . .
H47 H 1.0427 1.0219 0.7530 0.090 Uiso 1 1 calc R . .
C48 C 0.9660(3) 1.0590(4) 0.7438(4) 0.069(2) Uani 1 1 d . . .
H48 H 0.9703 1.1069 0.7501 0.083 Uiso 1 1 calc R . .
C49 C 1.0117(3) 0.8849(4) 0.7315(4) 0.0618(19) Uani 1 1 d U . .
C50 C 1.0187(3) 0.8427(4) 0.7935(5) 0.082(2) Uani 1 1 d U . .
C51 C 1.0529(4) 0.7858(5) 0.7938(8) 0.130(5) Uani 1 1 d U . .
H51 H 1.0587 0.7561 0.8338 0.156 Uiso 1 1 calc R . .
C52 C 1.0786(5) 0.7715(6) 0.7373(10) 0.151(7) Uani 1 1 d . . .
H52 H 1.1014 0.7328 0.7392 0.182 Uiso 1 1 calc R . .
C53 C 1.0701(4) 0.8148(6) 0.6784(7) 0.127(4) Uani 1 1 d U . .
H53 H 1.0870 0.8047 0.6398 0.153 Uiso 1 1 calc R . .
C54 C 1.0369(3) 0.8736(5) 0.6743(5) 0.088(2) Uani 1 1 d U . .
C55 C 0.9933(4) 0.8590(5) 0.8570(5) 0.113(3) Uani 1 1 d U . .
H55 H 0.9577 0.8809 0.8374 0.135 Uiso 1 1 calc R . .
C56 C 0.9817(5) 0.7960(7) 0.8995(7) 0.200(6) Uani 1 1 d . . .
H56A H 0.9681 0.7589 0.8665 0.299 Uiso 1 1 calc R . .
H56B H 0.9547 0.8077 0.9274 0.299 Uiso 1 1 calc R . .
H56C H 1.0150 0.7814 0.9317 0.299 Uiso 1 1 calc R . .
C57 C 1.0284(4) 0.9135(6) 0.9062(5) 0.156(4) Uani 1 1 d U . .
H57A H 1.0635 0.8936 0.9274 0.233 Uiso 1 1 calc R . .
H57B H 1.0100 0.9273 0.9441 0.233 Uiso 1 1 calc R . .
H57C H 1.0336 0.9535 0.8776 0.233 Uiso 1 1 calc R . .
C58 C 1.0297(4) 0.9195(5) 0.6079(6) 0.109(3) Uani 1 1 d U . .
H58 H 0.9991 0.9515 0.6088 0.131 Uiso 1 1 calc R . .
C59 C 1.0826(4) 0.9634(5) 0.6112(6) 0.148(4) Uani 1 1 d . . .
H59A H 1.0864 0.9960 0.6507 0.222 Uiso 1 1 calc R . .
H59B H 1.0801 0.9882 0.5663 0.222 Uiso 1 1 calc R . .
H59C H 1.1139 0.9331 0.6188 0.222 Uiso 1 1 calc R . .
C60 C 1.0163(4) 0.8777(6) 0.5360(6) 0.164(5) Uani 1 1 d . . .
H60A H 1.0469 0.8482 0.5326 0.247 Uiso 1 1 calc R . .
H60B H 1.0094 0.9093 0.4955 0.247 Uiso 1 1 calc R . .
H60C H 0.9843 0.8495 0.5353 0.247 Uiso 1 1 calc R . .
C61 C 0.86537(16) 1.0538(2) 0.7283(3) 0.0535(17) Uani 1 1 d G . .
C62 C 0.8480(2) 1.0695(3) 0.7923(2) 0.073(2) Uani 1 1 d G . .
C63 C 0.7971(2) 1.1005(3) 0.7893(3) 0.115(3) Uani 1 1 d G . .
H63 H 0.7855 1.1110 0.8321 0.138 Uiso 1 1 calc R . .
C64 C 0.76354(18) 1.1159(3) 0.7223(4) 0.136(4) Uani 1 1 d G . .
H64 H 0.7295 1.1367 0.7202 0.163 Uiso 1 1 calc R . .
C65 C 0.7809(2) 1.1002(3) 0.6583(3) 0.105(3) Uani 1 1 d G . .
H65 H 0.7584 1.1105 0.6135 0.126 Uiso 1 1 calc R . .
C66 C 0.8318(2) 1.0692(3) 0.6613(2) 0.065(2) Uani 1 1 d G . .
C67 C 0.8854(3) 1.0585(4) 0.8669(4) 0.081(2) Uani 1 1 d . . .
H67 H 0.9123 1.0225 0.8619 0.097 Uiso 1 1 calc R . .
C68 C 0.9170(4) 1.1259(4) 0.8921(4) 0.128(4) Uani 1 1 d . . .
H68A H 0.9374 1.1400 0.8564 0.192 Uiso 1 1 calc R . .
H68B H 0.9418 1.1179 0.9378 0.192 Uiso 1 1 calc R . .
H68C H 0.8914 1.1620 0.8978 0.192 Uiso 1 1 calc R . .
C69 C 0.8554(4) 1.0349(5) 0.9249(4) 0.120(3) Uani 1 1 d . . .
H69A H 0.8343 1.0729 0.9379 0.181 Uiso 1 1 calc R . .
H69B H 0.8815 1.0197 0.9670 0.181 Uiso 1 1 calc R . .
H69C H 0.8312 0.9970 0.9064 0.181 Uiso 1 1 calc R . .
C70 C 0.8511(3) 1.0585(4) 0.5912(4) 0.076(2) Uani 1 1 d U . .
H70 H 0.8824 1.0264 0.5999 0.091 Uiso 1 1 calc R . .
C71 C 0.8057(3) 1.0283(5) 0.5315(4) 0.108(3) Uani 1 1 d . . .
H71A H 0.7890 0.9894 0.5506 0.163 Uiso 1 1 calc R . .
H71B H 0.8213 1.0132 0.4913 0.163 Uiso 1 1 calc R . .
H71C H 0.7785 1.0634 0.5151 0.163 Uiso 1 1 calc R . .
C72 C 0.8698(4) 1.1283(5) 0.5671(5) 0.128(4) Uani 1 1 d U . .
H72A H 0.8405 1.1615 0.5632 0.192 Uiso 1 1 calc R . .
H72B H 0.8797 1.1233 0.5206 0.192 Uiso 1 1 calc R . .
H72C H 0.9011 1.1444 0.6022 0.192 Uiso 1 1 calc R . .
C73 C 0.79706(13) 0.73201(12) 0.75618(12) 0.069(2) Uani 1 1 d GU . .
C74 C 0.84689(14) 0.70256(16) 0.78993(15) 0.120(3) Uani 1 1 d GU . .
H74 H 0.8785 0.7118 0.7724 0.144 Uiso 1 1 calc R . .
C75 C 0.84949(19) 0.65934(18) 0.84995(15) 0.142(5) Uani 1 1 d G . .
H75 H 0.8828 0.6396 0.8725 0.170 Uiso 1 1 calc R . .
C76 C 0.8023(2) 0.64558(17) 0.87623(14) 0.131(5) Uani 1 1 d G . .
H76 H 0.8040 0.6167 0.9164 0.157 Uiso 1 1 calc R . .
C77 C 0.75244(19) 0.67502(16) 0.84248(13) 0.132(4) Uani 1 1 d G . .
H77 H 0.7208 0.6658 0.8601 0.158 Uiso 1 1 calc R . .
C78 C 0.74983(15) 0.71824(13) 0.78245(12) 0.096(3) Uani 1 1 d G . .
H78 H 0.7165 0.7379 0.7599 0.115 Uiso 1 1 calc R . .
C79 C 0.79093(10) 0.72330(14) 0.59754(13) 0.064(2) Uani 1 1 d G . .
C80 C 0.77492(12) 0.65559(13) 0.60913(14) 0.101(3) Uani 1 1 d G . .
H80 H 0.7674 0.6431 0.6539 0.121 Uiso 1 1 calc R . .
C81 C 0.77018(15) 0.60648(15) 0.55378(16) 0.115(3) Uani 1 1 d G . .
H81 H 0.7595 0.5612 0.5615 0.138 Uiso 1 1 calc R . .
C82 C 0.78145(17) 0.62509(19) 0.48682(16) 0.104(3) Uani 1 1 d GU . .
H82 H 0.7783 0.5922 0.4498 0.125 Uiso 1 1 calc R . .
C83 C 0.79747(15) 0.6928(2) 0.47522(15) 0.111(3) Uani 1 1 d GU . .
H83 H 0.8050 0.7052 0.4304 0.134 Uiso 1 1 calc R . .
C84 C 0.80221(12) 0.74191(18) 0.53058(15) 0.103(3) Uani 1 1 d G . .
H84 H 0.8129 0.7872 0.5228 0.123 Uiso 1 1 calc R . .
C85 C 0.72530(12) 0.83381(12) 0.65489(13) 0.0616(19) Uani 1 1 d G . .
C86 C 0.67971(10) 0.79712(15) 0.61929(13) 0.082(2) Uani 1 1 d G . .
H86 H 0.6832 0.7519 0.6032 0.099 Uiso 1 1 calc R . .
C87 C 0.62703(11) 0.8302(2) 0.60769(17) 0.097(3) Uani 1 1 d G . .
H87 H 0.5960 0.8054 0.5853 0.117 Uiso 1 1 calc R . .
C88 C 0.62128(15) 0.8980(2) 0.62895(19) 0.097(3) Uani 1 1 d G . .
H88 H 0.5869 0.9190 0.6210 0.116 Uiso 1 1 calc R . .
C89 C 0.66918(18) 0.93522(16) 0.66335(18) 0.100(3) Uani 1 1 d G . .
H89 H 0.6662 0.9814 0.6771 0.120 Uiso 1 1 calc R . .
C90 C 0.72139(16) 0.90239(12) 0.67684(16) 0.076(2) Uani 1 1 d G . .
H90 H 0.7526 0.9264 0.7001 0.092 Uiso 1 1 calc R . .
C91 C 0.9373(17) 0.6957(17) 0.596(2) 0.269(19) Uani 0.50 1 d P . .
H91A H 0.9701 0.7181 0.5864 0.323 Uiso 0.50 1 calc PR . .
H91B H 0.9054 0.7226 0.5727 0.323 Uiso 0.50 1 calc PR . .
Cl5 Cl 0.9401(5) 0.6882(7) 0.6816(8) 0.323(7) Uani 0.50 1 d P . .
Cl6 Cl 0.9322(6) 0.6063(9) 0.5628(11) 0.464(12) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 1.990(6) . ?
Pd1 Cl1 2.2707(17) . ?
Pd1 Cl2 2.2877(16) . ?
Pd1 As1 2.4232(8) . ?
As1 C28 1.926(3) . ?
As1 C34 1.940(3) . ?
As1 C40 1.945(6) . ?
N1 C1 1.350(6) . ?
N1 C2 1.369(7) . ?
N1 C4 1.445(7) . ?
N2 C1 1.355(7) . ?
N2 C3 1.376(7) . ?
N2 C16 1.449(7) . ?
C2 C3 1.327(8) . ?
C4 C9 1.388(8) . ?
C4 C5 1.393(8) . ?
C5 C6 1.377(8) . ?
C5 C10 1.509(8) . ?
C6 C7 1.353(8) . ?
C7 C8 1.373(8) . ?
C8 C9 1.385(8) . ?
C9 C13 1.498(9) . ?
C10 C12 1.466(9) . ?
C10 C11 1.520(9) . ?
C13 C15 1.515(10) . ?
C13 C14 1.537(10) . ?
C16 C21 1.382(8) . ?
C16 C17 1.397(8) . ?
C17 C18 1.377(9) . ?
C17 C22 1.505(8) . ?
C18 C19 1.364(9) . ?
C19 C20 1.357(9) . ?
C20 C21 1.403(9) . ?
C21 C25 1.501(9) . ?
C22 C23 1.517(8) . ?
C22 C24 1.525(8) . ?
C25 C26 1.515(9) . ?
C25 C27 1.518(8) . ?
C28 C29 1.3900 . ?
C28 C33 1.3900 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C34 C39 1.3652 . ?
C34 C35 1.3949 . ?
C35 C36 1.4145 . ?
C36 C37 1.3828 . ?
C37 C38 1.3583 . ?
C38 C39 1.3975 . ?
C40 C45 1.369(9) . ?
C40 C41 1.376(8) . ?
C41 C42 1.398(10) . ?
C42 C43 1.354(11) . ?
C43 C44 1.349(11) . ?
C44 C45 1.365(10) . ?
C46 N4 1.341(7) . ?
C46 N3 1.354(7) . ?
C46 Pd2 1.994(6) . ?
Pd2 Cl4 2.2750(19) . ?
Pd2 Cl3 2.278(2) . ?
Pd2 As2 2.4290(9) . ?
As2 C73 1.920(3) . ?
As2 C79 1.925(2) . ?
As2 C85 1.927(3) . ?
N3 C47 1.381(7) . ?
N3 C49 1.437(8) . ?
N4 C48 1.393(7) . ?
N4 C61 1.407(6) . ?
C47 C48 1.317(8) . ?
C49 C54 1.368(11) . ?
C49 C50 1.399(10) . ?
C50 C51 1.382(12) . ?
C50 C55 1.495(12) . ?
C51 C52 1.375(16) . ?
C52 C53 1.365(16) . ?
C53 C54 1.392(12) . ?
C54 C58 1.506(12) . ?
C55 C56 1.508(12) . ?
C55 C57 1.542(12) . ?
C58 C60 1.547(12) . ?
C58 C59 1.553(11) . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C62 C63 1.3900 . ?
C62 C67 1.527(8) . ?
C63 C64 1.3900 . ?
C64 C65 1.3900 . ?
C65 C66 1.3900 . ?
C66 C70 1.507(8) . ?
C67 C69 1.510(10) . ?
C67 C68 1.537(10) . ?
C70 C72 1.518(10) . ?
C70 C71 1.531(9) . ?
C73 C74 1.3900 . ?
C73 C78 1.3900 . ?
C74 C75 1.3900 . ?
C75 C76 1.3900 . ?
C76 C77 1.3900 . ?
C77 C78 1.3900 . ?
C79 C80 1.3900 . ?
C79 C84 1.3900 . ?
C80 C81 1.3900 . ?
C81 C82 1.3900 . ?
C82 C83 1.3900 . ?
C83 C84 1.3900 . ?
C85 C86 1.3837 . ?
C85 C90 1.3890 . ?
C86 C87 1.4318 . ?
C87 C88 1.3775 . ?
C88 C89 1.4242 . ?
C89 C90 1.4182 . ?
C91 Cl5 1.61(3) . ?
C91 Cl6 1.82(3) . ?

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 Pd1 Cl1 88.95(16) . . ?
C1 Pd1 Cl2 90.78(16) . . ?
Cl1 Pd1 Cl2 177.37(7) . . ?
C1 Pd1 As1 176.04(17) . . ?
Cl1 Pd1 As1 93.18(5) . . ?
Cl2 Pd1 As1 87.24(5) . . ?
C28 As1 C34 102.51(12) . . ?
C28 As1 C40 105.9(2) . . ?
C34 As1 C40 101.7(2) . . ?
C28 As1 Pd1 112.20(10) . . ?
C34 As1 Pd1 120.74(9) . . ?
C40 As1 Pd1 112.3(2) . . ?
C1 N1 C2 110.6(5) . . ?
C1 N1 C4 128.3(5) . . ?
C2 N1 C4 121.1(5) . . ?
C1 N2 C3 110.9(5) . . ?
C1 N2 C16 126.3(5) . . ?
C3 N2 C16 122.8(5) . . ?
N1 C1 N2 104.2(5) . . ?
N1 C1 Pd1 131.1(5) . . ?
N2 C1 Pd1 124.6(4) . . ?
C3 C2 N1 107.8(6) . . ?
C2 C3 N2 106.5(6) . . ?
C9 C4 C5 121.9(6) . . ?
C9 C4 N1 118.8(5) . . ?
C5 C4 N1 119.1(5) . . ?
C6 C5 C4 117.7(6) . . ?
C6 C5 C10 119.9(6) . . ?
C4 C5 C10 122.4(6) . . ?
C7 C6 C5 121.4(6) . . ?
C6 C7 C8 120.7(6) . . ?
C7 C8 C9 120.4(6) . . ?
C8 C9 C4 117.9(6) . . ?
C8 C9 C13 117.7(6) . . ?
C4 C9 C13 124.4(6) . . ?
C12 C10 C5 112.2(6) . . ?
C12 C10 C11 111.1(7) . . ?
C5 C10 C11 111.4(6) . . ?
C9 C13 C15 112.6(7) . . ?
C9 C13 C14 111.2(6) . . ?
C15 C13 C14 110.9(7) . . ?
C21 C16 C17 123.9(6) . . ?
C21 C16 N2 118.1(6) . . ?
C17 C16 N2 118.0(6) . . ?
C18 C17 C16 116.3(6) . . ?
C18 C17 C22 120.0(6) . . ?
C16 C17 C22 123.7(6) . . ?
C19 C18 C17 121.7(7) . . ?
C20 C19 C18 120.6(7) . . ?
C19 C20 C21 121.3(7) . . ?
C16 C21 C20 116.1(6) . . ?
C16 C21 C25 123.2(6) . . ?
C20 C21 C25 120.7(6) . . ?
C17 C22 C23 111.4(6) . . ?
C17 C22 C24 113.9(6) . . ?
C23 C22 C24 109.2(6) . . ?
C21 C25 C26 110.0(6) . . ?
C21 C25 C27 113.3(6) . . ?
C26 C25 C27 110.9(6) . . ?
C29 C28 C33 120.0 . . ?
C29 C28 As1 118.25(9) . . ?
C33 C28 As1 121.74(9) . . ?
C28 C29 C30 120.0 . . ?
C31 C30 C29 120.0 . . ?
C30 C31 C32 120.0 . . ?
C33 C32 C31 120.0 . . ?
C32 C33 C28 120.0 . . ?
C39 C34 C35 121.2 . . ?
C39 C34 As1 120.59(15) . . ?
C35 C34 As1 118.19(15) . . ?
C34 C35 C36 117.9 . . ?
C37 C36 C35 120.6 . . ?
C38 C37 C36 119.4 . . ?
C37 C38 C39 121.5 . . ?
C34 C39 C38 119.2 . . ?
C45 C40 C41 120.2(6) . . ?
C45 C40 As1 118.2(5) . . ?
C41 C40 As1 121.5(6) . . ?
C40 C41 C42 118.1(7) . . ?
C43 C42 C41 120.7(8) . . ?
C44 C43 C42 120.3(8) . . ?
C43 C44 C45 120.5(9) . . ?
C44 C45 C40 120.2(8) . . ?
N4 C46 N3 104.5(5) . . ?
N4 C46 Pd2 127.2(5) . . ?
N3 C46 Pd2 128.2(5) . . ?
C46 Pd2 Cl4 90.95(18) . . ?
C46 Pd2 Cl3 88.56(18) . . ?
Cl4 Pd2 Cl3 178.43(9) . . ?
C46 Pd2 As2 176.47(18) . . ?
Cl4 Pd2 As2 85.92(5) . . ?
Cl3 Pd2 As2 94.52(5) . . ?
C73 As2 C79 100.46(11) . . ?
C73 As2 C85 104.20(13) . . ?
C79 As2 C85 102.71(11) . . ?
C73 As2 Pd2 112.30(8) . . ?
C79 As2 Pd2 123.87(9) . . ?
C85 As2 Pd2 111.15(9) . . ?
C46 N3 C47 110.3(6) . . ?
C46 N3 C49 126.8(5) . . ?
C47 N3 C49 122.9(6) . . ?
C46 N4 C48 111.1(5) . . ?
C46 N4 C61 126.0(5) . . ?
C48 N4 C61 122.9(5) . . ?
C48 C47 N3 107.9(6) . . ?
C47 C48 N4 106.2(6) . . ?
C54 C49 C50 124.2(8) . . ?
C54 C49 N3 118.4(8) . . ?
C50 C49 N3 117.0(7) . . ?
C51 C50 C49 115.6(10) . . ?
C51 C50 C55 121.5(10) . . ?
C49 C50 C55 122.8(8) . . ?
C52 C51 C50 122.6(12) . . ?
C53 C52 C51 118.9(12) . . ?
C52 C53 C54 122.0(13) . . ?
C49 C54 C53 116.7(10) . . ?
C49 C54 C58 124.2(8) . . ?
C53 C54 C58 119.2(10) . . ?
C50 C55 C56 114.4(10) . . ?
C50 C55 C57 109.8(8) . . ?
C56 C55 C57 111.9(9) . . ?
C54 C58 C60 112.7(9) . . ?
C54 C58 C59 109.2(8) . . ?
C60 C58 C59 110.1(8) . . ?
C62 C61 C66 120.0 . . ?
C62 C61 N4 120.1(4) . . ?
C66 C61 N4 119.9(4) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 C67 121.6(5) . . ?
C63 C62 C67 118.2(5) . . ?
C64 C63 C62 120.0 . . ?
C63 C64 C65 120.0 . . ?
C66 C65 C64 120.0 . . ?
C65 C66 C61 120.0 . . ?
C65 C66 C70 118.4(4) . . ?
C61 C66 C70 121.4(4) . . ?
C69 C67 C62 113.9(7) . . ?
C69 C67 C68 109.2(7) . . ?
C62 C67 C68 109.9(6) . . ?
C66 C70 C72 108.2(6) . . ?
C66 C70 C71 111.8(6) . . ?
C72 C70 C71 110.0(7) . . ?
C74 C73 C78 120.0 . . ?
C74 C73 As2 117.34(8) . . ?
C78 C73 As2 122.66(8) . . ?
C75 C74 C73 120.0 . . ?
C74 C75 C76 120.0 . . ?
C75 C76 C77 120.0 . . ?
C78 C77 C76 120.0 . . ?
C77 C78 C73 120.0 . . ?
C80 C79 C84 120.0 . . ?
C80 C79 As2 120.04(8) . . ?
C84 C79 As2 119.96(8) . . ?
C79 C80 C81 120.0 . . ?
C82 C81 C80 120.0 . . ?
C81 C82 C83 120.0 . . ?
C84 C83 C82 120.0 . . ?
C83 C84 C79 120.0 . . ?
C86 C85 C90 121.7 . . ?
C86 C85 As2 120.69(7) . . ?
C90 C85 As2 117.61(7) . . ?
C85 C86 C87 118.7 . . ?
C88 C87 C86 121.5 . . ?
C87 C88 C89 118.6 . . ?
C90 C89 C88 120.5 . . ?
C85 C90 C89 119.1 . . ?
Cl5 C91 Cl6 104.0(19) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 1003799'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C45 H51 Cl2 N2 Pd Sb), C H2 Cl2'
_chemical_formula_sum            'C91 H104 Cl6 N4 Pd2 Sb2'
_chemical_formula_weight         1922.78

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   31.143(6)
_cell_length_b                   13.853(3)
_cell_length_c                   23.658(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.411(3)
_cell_angle_gamma                90.00
_cell_volume                     9294(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9588
_cell_measurement_theta_min      2.2649
_cell_measurement_theta_max      27.5510

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3896
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7505
_exptl_absorpt_correction_T_max  0.7910
_exptl_absorpt_process_details   SADABS

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23266
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8158
_reflns_number_gt                6540
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0268P)²+19.1571P] 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         8158
_refine_ls_number_parameters     495
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0765
_refine_ls_wR_factor_gt          0.0688
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.035
_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
Pd1 Pd 0.340798(9) 0.908692(19) 0.409160(11) 0.04462(8) Uani 1 1 d . . .
Cl1 Cl 0.29701(4) 0.80328(7) 0.33232(4) 0.0749(3) Uani 1 1 d . . .
Cl2 Cl 0.38499(6) 1.00799(11) 0.48837(5) 0.1272(7) Uani 1 1 d . . .
Sb1 Sb 0.356633(8) 0.761869(18) 0.483118(11) 0.05272(8) Uani 1 1 d . . .
N1 N 0.35354(9) 1.03508(17) 0.31232(11) 0.0385(6) Uani 1 1 d . . .
N2 N 0.28871(9) 1.06878(17) 0.31898(11) 0.0392(6) Uani 1 1 d . . .
C1 C 0.32807(11) 1.0137(2) 0.34469(13) 0.0377(7) Uani 1 1 d . . .
C2 C 0.32989(12) 1.1018(2) 0.26627(15) 0.0487(8) Uani 1 1 d . . .
H2 H 0.3402 1.1271 0.2376 0.058 Uiso 1 1 calc R . .
C3 C 0.28979(13) 1.1229(2) 0.27054(15) 0.0491(8) Uani 1 1 d . . .
H3 H 0.2668 1.1659 0.2457 0.059 Uiso 1 1 calc R . .
C4 C 0.40088(11) 1.0010(2) 0.32489(15) 0.0445(8) Uani 1 1 d . . .
C5 C 0.43948(12) 1.0523(3) 0.36765(16) 0.0557(9) Uani 1 1 d . . .
C6 C 0.48375(15) 1.0208(4) 0.3765(2) 0.0837(14) Uani 1 1 d . . .
H6 H 0.5102 1.0529 0.4046 0.100 Uiso 1 1 calc R . .
C7 C 0.48960(16) 0.9429(4) 0.3446(3) 0.0998(17) Uani 1 1 d . . .
H7 H 0.5198 0.9225 0.3516 0.120 Uiso 1 1 calc R . .
C8 C 0.45163(16) 0.8953(3) 0.3029(2) 0.0837(14) Uani 1 1 d . . .
H8 H 0.4564 0.8431 0.2814 0.100 Uiso 1 1 calc R . .
C9 C 0.40580(13) 0.9224(3) 0.29130(18) 0.0546(9) Uani 1 1 d . . .
C10 C 0.43371(14) 1.1414(3) 0.40123(18) 0.0667(11) Uani 1 1 d . . .
H10 H 0.4028 1.1372 0.4029 0.080 Uiso 1 1 calc R . .
C11 C 0.47115(18) 1.1497(4) 0.4681(2) 0.1074(18) Uani 1 1 d . . .
H11A H 0.4727 1.0902 0.4896 0.161 Uiso 1 1 calc R . .
H11B H 0.4629 1.2013 0.4889 0.161 Uiso 1 1 calc R . .
H11C H 0.5013 1.1630 0.4677 0.161 Uiso 1 1 calc R . .
C12 C 0.4341(2) 1.2326(4) 0.3658(3) 0.1049(18) Uani 1 1 d . . .
H12A H 0.4641 1.2390 0.3639 0.157 Uiso 1 1 calc R . .
H12B H 0.4287 1.2876 0.3867 0.157 Uiso 1 1 calc R . .
H12C H 0.4097 1.2288 0.3245 0.157 Uiso 1 1 calc R . .
C13 C 0.36437(14) 0.8692(3) 0.24256(19) 0.0615(10) Uani 1 1 d . . .
H13 H 0.3355 0.8920 0.2454 0.074 Uiso 1 1 calc R . .
C14 C 0.36039(18) 0.8919(3) 0.1775(2) 0.0853(13) Uani 1 1 d . . .
H14A H 0.3564 0.9601 0.1702 0.128 Uiso 1 1 calc R . .
H14B H 0.3337 0.8584 0.1474 0.128 Uiso 1 1 calc R . .
H14C H 0.3886 0.8713 0.1739 0.128 Uiso 1 1 calc R . .
C15 C 0.3677(2) 0.7594(3) 0.2533(3) 0.0903(15) Uani 1 1 d . . .
H15A H 0.3942 0.7345 0.2471 0.135 Uiso 1 1 calc R . .
H15B H 0.3393 0.7292 0.2245 0.135 Uiso 1 1 calc R . .
H15C H 0.3717 0.7459 0.2950 0.135 Uiso 1 1 calc R . .
C16 C 0.25404(11) 1.0819(2) 0.34462(14) 0.0433(7) Uani 1 1 d . . .
C17 C 0.26369(13) 1.1515(3) 0.39087(17) 0.0583(9) Uani 1 1 d . . .
C18 C 0.23074(15) 1.1625(3) 0.41563(19) 0.0709(11) Uani 1 1 d . . .
H18 H 0.2363 1.2075 0.4471 0.085 Uiso 1 1 calc R . .
C19 C 0.19028(14) 1.1091(3) 0.39505(19) 0.0682(11) Uani 1 1 d . . .
H19 H 0.1690 1.1174 0.4130 0.082 Uiso 1 1 calc R . .
C20 C 0.18078(13) 1.0434(3) 0.34799(18) 0.0593(9) Uani 1 1 d . . .
H20 H 0.1529 1.0082 0.3340 0.071 Uiso 1 1 calc R . .
C21 C 0.21227(12) 1.0288(2) 0.32096(15) 0.0464(8) Uani 1 1 d . . .
C22 C 0.30571(17) 1.2192(4) 0.4101(2) 0.0904(16) Uani 1 1 d . . .
H22 H 0.3292 1.1889 0.3982 0.109 Uiso 1 1 calc R . .
C23 C 0.3291(2) 1.2376(6) 0.4798(3) 0.160(3) Uani 1 1 d . . .
H23A H 0.3099 1.2808 0.4912 0.240 Uiso 1 1 calc R . .
H23B H 0.3596 1.2659 0.4906 0.240 Uiso 1 1 calc R . .
H23C H 0.3325 1.1776 0.5016 0.240 Uiso 1 1 calc R . .
C24 C 0.2903(3) 1.3144(4) 0.3737(4) 0.149(3) Uani 1 1 d . . .
H24A H 0.2766 1.3009 0.3300 0.223 Uiso 1 1 calc R . .
H24B H 0.3173 1.3555 0.3836 0.223 Uiso 1 1 calc R . .
H24C H 0.2675 1.3461 0.3848 0.223 Uiso 1 1 calc R . .
C25 C 0.19930(13) 0.9628(3) 0.26536(17) 0.0600(10) Uani 1 1 d . . .
H25 H 0.2284 0.9456 0.2611 0.072 Uiso 1 1 calc R . .
C26 C 0.16756(19) 1.0184(4) 0.2070(2) 0.1049(18) Uani 1 1 d . . .
H26A H 0.1388 1.0358 0.2101 0.157 Uiso 1 1 calc R . .
H26B H 0.1605 0.9784 0.1711 0.157 Uiso 1 1 calc R . .
H26C H 0.1835 1.0757 0.2033 0.157 Uiso 1 1 calc R . .
C27 C 0.17586(19) 0.8695(4) 0.2724(3) 0.1076(19) Uani 1 1 d . . .
H27A H 0.1953 0.8391 0.3110 0.161 Uiso 1 1 calc R . .
H27B H 0.1720 0.8267 0.2387 0.161 Uiso 1 1 calc R . .
H27C H 0.1456 0.8840 0.2719 0.161 Uiso 1 1 calc R . .
C28 C 0.39787(13) 0.6584(3) 0.46136(16) 0.0611(10) Uani 1 1 d . . .
C29 C 0.42651(15) 0.6901(4) 0.4337(2) 0.0853(14) Uani 1 1 d . . .
H29 H 0.4276 0.7554 0.4253 0.102 Uiso 1 1 calc R . .
C30 C 0.45368(19) 0.6243(6) 0.4185(3) 0.116(2) Uani 1 1 d . . .
H30 H 0.4730 0.6459 0.3999 0.139 Uiso 1 1 calc R . .
C31 C 0.4523(2) 0.5279(6) 0.4306(3) 0.118(2) Uani 1 1 d . . .
H31 H 0.4709 0.4845 0.4206 0.142 Uiso 1 1 calc R . .
C32 C 0.4239(2) 0.4960(4) 0.4569(2) 0.1008(17) Uani 1 1 d . . .
H32 H 0.4228 0.4305 0.4647 0.121 Uiso 1 1 calc R . .
C33 C 0.39640(16) 0.5609(4) 0.4724(2) 0.0799(13) Uani 1 1 d . . .
H33 H 0.3768 0.5383 0.4904 0.096 Uiso 1 1 calc R . .
C34 C 0.30089(13) 0.6696(3) 0.47855(17) 0.0559(9) Uani 1 1 d . . .
C35 C 0.27547(16) 0.6198(3) 0.4244(2) 0.0798(13) Uani 1 1 d . . .
H35 H 0.2830 0.6273 0.3905 0.096 Uiso 1 1 calc R . .
C36 C 0.23906(19) 0.5591(4) 0.4198(3) 0.1006(17) Uani 1 1 d . . .
H36 H 0.2225 0.5253 0.3832 0.121 Uiso 1 1 calc R . .
C37 C 0.22730(18) 0.5485(4) 0.4689(3) 0.1014(18) Uani 1 1 d . . .
H37 H 0.2025 0.5082 0.4656 0.122 Uiso 1 1 calc R . .
C38 C 0.25206(17) 0.5975(4) 0.5233(3) 0.0872(15) Uani 1 1 d . . .
H38 H 0.2441 0.5901 0.5568 0.105 Uiso 1 1 calc R . .
C39 C 0.28906(15) 0.6582(3) 0.5282(2) 0.0733(12) Uani 1 1 d . . .
H39 H 0.3058 0.6912 0.5651 0.088 Uiso 1 1 calc R . .
C40 C 0.39430(14) 0.7718(3) 0.58144(17) 0.0637(10) Uani 1 1 d . . .
C41 C 0.4148(2) 0.6910(4) 0.6157(2) 0.132(3) Uani 1 1 d . . .
H41 H 0.4135 0.6324 0.5959 0.158 Uiso 1 1 calc R . .
C42 C 0.4377(3) 0.6970(6) 0.6801(3) 0.147(3) Uani 1 1 d . . .
H42 H 0.4517 0.6422 0.7030 0.176 Uiso 1 1 calc R . .
C43 C 0.4399(2) 0.7807(6) 0.7094(2) 0.109(2) Uani 1 1 d . . .
H43 H 0.4547 0.7833 0.7525 0.131 Uiso 1 1 calc R . .
C44 C 0.42082(19) 0.8603(5) 0.6771(2) 0.1023(17) Uani 1 1 d . . .
H44 H 0.4231 0.9188 0.6975 0.123 Uiso 1 1 calc R . .
C45 C 0.39730(17) 0.8556(4) 0.6120(2) 0.0849(14) Uani 1 1 d . . .
H45 H 0.3836 0.9111 0.5896 0.102 Uiso 1 1 calc R . .
C46 C 0.5552(13) 0.5397(17) 0.3485(14) 0.412(8) Uani 0.50 1 d PDU . .
H46A H 0.5427 0.4959 0.3700 0.494 Uiso 0.50 1 calc PR . .
H46B H 0.5821 0.5136 0.3431 0.494 Uiso 0.50 1 calc PR . .
Cl3 Cl 0.5150(5) 0.5991(9) 0.2869(6) 0.412(6) Uani 0.50 1 d PDU . .
Cl4 Cl 0.5585(4) 0.6497(10) 0.3680(6) 0.386(5) Uani 0.50 1 d PDU . .


_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 C1 2.024(3) . ?
Pd1 Cl2 2.2729(12) . ?
Pd1 Cl1 2.2908(10) . ?
Pd1 Sb1 2.5939(5) . ?
Sb1 C28 2.125(4) . ?
Sb1 C34 2.123(4) . ?
Sb1 C40 2.133(4) . ?
N1 C1 1.344(4) . ?
N1 C2 1.386(4) . ?
N1 C4 1.457(4) . ?
N2 C1 1.356(4) . ?
N2 C3 1.382(4) . ?
N2 C16 1.452(4) . ?
C2 C3 1.327(5) . ?
C4 C9 1.393(5) . ?
C4 C5 1.403(5) . ?
C5 C6 1.377(5) . ?
C5 C10 1.519(5) . ?
C6 C7 1.371(6) . ?
C7 C8 1.357(6) . ?
C8 C9 1.389(5) . ?
C9 C13 1.519(5) . ?
C10 C12 1.519(6) . ?
C10 C11 1.533(6) . ?
C13 C14 1.526(6) . ?
C13 C15 1.539(5) . ?
C16 C21 1.395(5) . ?
C16 C17 1.394(5) . ?
C17 C18 1.384(5) . ?
C17 C22 1.519(6) . ?
C18 C19 1.365(5) . ?
C19 C20 1.372(5) . ?
C20 C21 1.389(5) . ?
C21 C25 1.513(5) . ?
C22 C23 1.525(7) . ?
C22 C24 1.539(8) . ?
C25 C27 1.527(6) . ?
C25 C26 1.532(6) . ?
C28 C29 1.377(6) . ?
C28 C33 1.381(6) . ?
C29 C30 1.389(8) . ?
C30 C31 1.370(9) . ?
C31 C32 1.348(8) . ?
C32 C33 1.392(7) . ?
C34 C39 1.378(5) . ?
C34 C35 1.380(6) . ?
C35 C36 1.380(6) . ?
C36 C37 1.362(7) . ?
C37 C38 1.375(7) . ?
C38 C39 1.392(6) . ?
C40 C45 1.350(6) . ?
C40 C41 1.376(6) . ?
C41 C42 1.391(7) . ?
C42 C43 1.339(8) . ?
C43 C44 1.335(8) . ?
C44 C45 1.407(6) . ?
C46 Cl4 1.583(18) . ?
C46 Cl3 1.692(19) . ?
Cl3 Cl3 1.60(2) 2_655 ?

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 Pd1 Cl2 92.85(9) . . ?
C1 Pd1 Cl1 89.60(9) . . ?
Cl2 Pd1 Cl1 177.54(4) . . ?
C1 Pd1 Sb1 174.20(8) . . ?
Cl2 Pd1 Sb1 92.11(4) . . ?
Cl1 Pd1 Sb1 85.43(3) . . ?
C28 Sb1 C34 98.33(15) . . ?
C28 Sb1 C40 101.12(15) . . ?
C34 Sb1 C40 99.44(15) . . ?
C28 Sb1 Pd1 109.32(11) . . ?
C34 Sb1 Pd1 120.97(9) . . ?
C40 Sb1 Pd1 123.39(12) . . ?
C1 N1 C2 110.4(3) . . ?
C1 N1 C4 126.7(3) . . ?
C2 N1 C4 122.7(2) . . ?
C1 N2 C3 110.5(3) . . ?
C1 N2 C16 125.0(3) . . ?
C3 N2 C16 123.8(3) . . ?
N1 C1 N2 104.9(2) . . ?
N1 C1 Pd1 127.6(2) . . ?
N2 C1 Pd1 127.0(2) . . ?
C3 C2 N1 107.4(3) . . ?
C2 C3 N2 106.8(3) . . ?
C9 C4 C5 123.0(3) . . ?
C9 C4 N1 118.5(3) . . ?
C5 C4 N1 118.4(3) . . ?
C6 C5 C4 117.0(4) . . ?
C6 C5 C10 120.4(4) . . ?
C4 C5 C10 122.5(3) . . ?
C7 C6 C5 121.2(4) . . ?
C8 C7 C6 120.6(4) . . ?
C7 C8 C9 121.8(4) . . ?
C8 C9 C4 116.4(4) . . ?
C8 C9 C13 120.0(3) . . ?
C4 C9 C13 123.6(3) . . ?
C5 C10 C12 111.0(3) . . ?
C5 C10 C11 113.4(4) . . ?
C12 C10 C11 109.3(4) . . ?
C9 C13 C14 110.8(3) . . ?
C9 C13 C15 112.1(4) . . ?
C14 C13 C15 110.0(4) . . ?
C21 C16 C17 122.8(3) . . ?
C21 C16 N2 119.8(3) . . ?
C17 C16 N2 117.3(3) . . ?
C18 C17 C16 116.8(3) . . ?
C18 C17 C22 120.2(3) . . ?
C16 C17 C22 122.7(3) . . ?
C19 C18 C17 121.7(4) . . ?
C18 C19 C20 120.4(3) . . ?
C19 C20 C21 120.9(3) . . ?
C20 C21 C16 117.2(3) . . ?
C20 C21 C25 120.2(3) . . ?
C16 C21 C25 122.5(3) . . ?
C17 C22 C23 113.2(4) . . ?
C17 C22 C24 109.3(4) . . ?
C23 C22 C24 111.1(5) . . ?
C21 C25 C27 112.6(4) . . ?
C21 C25 C26 108.7(3) . . ?
C27 C25 C26 111.4(4) . . ?
C29 C28 C33 118.7(4) . . ?
C29 C28 Sb1 118.3(4) . . ?
C33 C28 Sb1 122.9(3) . . ?
C28 C29 C30 119.8(6) . . ?
C31 C30 C29 120.8(6) . . ?
C32 C31 C30 119.9(6) . . ?
C31 C32 C33 120.2(6) . . ?
C28 C33 C32 120.7(5) . . ?
C39 C34 C35 118.8(4) . . ?
C39 C34 Sb1 121.8(3) . . ?
C35 C34 Sb1 119.4(3) . . ?
C36 C35 C34 121.0(4) . . ?
C37 C36 C35 120.0(5) . . ?
C36 C37 C38 120.0(5) . . ?
C37 C38 C39 120.1(5) . . ?
C34 C39 C38 120.1(5) . . ?
C45 C40 C41 118.2(4) . . ?
C45 C40 Sb1 121.6(3) . . ?
C41 C40 Sb1 120.2(4) . . ?
C40 C41 C42 120.0(6) . . ?
C43 C42 C41 120.9(6) . . ?
C44 C43 C42 120.2(5) . . ?
C43 C44 C45 119.8(5) . . ?
C40 C45 C44 121.0(5) . . ?
Cl4 C46 Cl3 73.7(10) . . ?
Cl3 Cl3 C46 145.9(14) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 1003800'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 As Cl2 N2 Pd'
_chemical_formula_sum            'C39 H41 As Cl2 N2 Pd'
_chemical_formula_weight         789.96

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'
N N 0.0061 0.0033 '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'
As As 0.0499 2.0058 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.317(6)
_cell_length_b                   13.876(5)
_cell_length_c                   15.020(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.337(5)
_cell_angle_gamma                90.00
_cell_volume                     3606(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8899
_cell_measurement_theta_min      2.3477
_cell_measurement_theta_max      28.3330

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    1.603
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6807
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_process_details   SADABS

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18014
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6327
_reflns_number_gt                5362
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0433P)²+1.6779P] 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         6327
_refine_ls_number_parameters     400
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0797
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Pd1 Pd 0.248410(11) 0.428438(15) 0.308299(14) 0.03187(8) Uani 1 1 d . . .
As1 As 0.246722(16) 0.54412(2) 0.427906(19) 0.03624(9) Uani 1 1 d . . .
Cl1 Cl 0.15152(4) 0.34197(6) 0.36856(5) 0.04826(19) Uani 1 1 d . . .
Cl2 Cl 0.35138(5) 0.51345(7) 0.25931(6) 0.0613(2) Uani 1 1 d . . .
N1 N 0.30508(13) 0.28120(18) 0.18003(16) 0.0426(6) Uani 1 1 d . . .
N2 N 0.20151(15) 0.35286(19) 0.13247(16) 0.0475(6) Uani 1 1 d . . .
C1 C 0.25191(15) 0.3450(2) 0.20045(18) 0.0357(6) Uani 1 1 d . . .
C2 C 0.29108(19) 0.2393(3) 0.0908(2) 0.0570(9) Uani 1 1 d . . .
H2A H 0.2814 0.1705 0.0943 0.068 Uiso 1 1 calc R . .
H2B H 0.3345 0.2504 0.0534 0.068 Uiso 1 1 calc R . .
C3 C 0.2206(2) 0.2923(3) 0.0564(2) 0.0745(12) Uani 1 1 d . . .
H3A H 0.2318 0.3312 0.0048 0.089 Uiso 1 1 calc R . .
H3B H 0.1788 0.2482 0.0406 0.089 Uiso 1 1 calc R . .
C4 C 0.36421(16) 0.2439(2) 0.2391(2) 0.0424(7) Uani 1 1 d . . .
C5 C 0.44032(18) 0.2712(2) 0.2286(2) 0.0532(8) Uani 1 1 d . . .
C6 C 0.49600(19) 0.2316(3) 0.2871(3) 0.0652(10) Uani 1 1 d U . .
H6 H 0.5474 0.2485 0.2807 0.078 Uiso 1 1 calc R . .
C7 C 0.4786(2) 0.1693(3) 0.3534(3) 0.0645(10) Uani 1 1 d U . .
C8 C 0.4036(2) 0.1419(3) 0.3594(2) 0.0620(9) Uani 1 1 d . . .
H8 H 0.3910 0.0979 0.4032 0.074 Uiso 1 1 calc R . .
C9 C 0.34528(18) 0.1770(2) 0.3026(2) 0.0486(8) Uani 1 1 d . . .
C10 C 0.4622(2) 0.3383(3) 0.1562(3) 0.0762(12) Uani 1 1 d . . .
H10A H 0.4580 0.3055 0.1000 0.114 Uiso 1 1 calc R . .
H10B H 0.5144 0.3596 0.1671 0.114 Uiso 1 1 calc R . .
H10C H 0.4281 0.3929 0.1550 0.114 Uiso 1 1 calc R . .
C11 C 0.2649(2) 0.1389(3) 0.3077(3) 0.0635(10) Uani 1 1 d . . .
H11A H 0.2309 0.1901 0.3239 0.095 Uiso 1 1 calc R . .
H11B H 0.2639 0.0889 0.3517 0.095 Uiso 1 1 calc R . .
H11C H 0.2482 0.1133 0.2507 0.095 Uiso 1 1 calc R . .
C12 C 0.5411(3) 0.1304(4) 0.4157(3) 0.0965(16) Uani 1 1 d . . .
H12A H 0.5758 0.0914 0.3829 0.145 Uiso 1 1 calc R . .
H12B H 0.5183 0.0920 0.4609 0.145 Uiso 1 1 calc R . .
H12C H 0.5691 0.1830 0.4432 0.145 Uiso 1 1 calc R . .
C13 C 0.13512(19) 0.4152(2) 0.1286(2) 0.0459(7) Uani 1 1 d . . .
C14 C 0.1434(2) 0.5097(3) 0.1030(2) 0.0570(9) Uani 1 1 d . . .
C15 C 0.0777(3) 0.5667(3) 0.1000(2) 0.0681(11) Uani 1 1 d . . .
H15 H 0.0822 0.6314 0.0846 0.082 Uiso 1 1 calc R . .
C16 C 0.0069(2) 0.5318(3) 0.1185(2) 0.0670(11) Uani 1 1 d . . .
C17 C 0.0005(2) 0.4366(3) 0.1408(2) 0.0636(10) Uani 1 1 d . . .
H17 H -0.0479 0.4118 0.1525 0.076 Uiso 1 1 calc R . .
C18 C 0.06394(18) 0.3761(2) 0.1464(2) 0.0509(8) Uani 1 1 d . . .
C19 C 0.2189(3) 0.5508(3) 0.0765(3) 0.0852(13) Uani 1 1 d . . .
H19A H 0.2241 0.6154 0.0988 0.128 Uiso 1 1 calc R . .
H19B H 0.2206 0.5514 0.0127 0.128 Uiso 1 1 calc R . .
H19C H 0.2604 0.5119 0.1010 0.128 Uiso 1 1 calc R . .
C20 C 0.0541(2) 0.2718(3) 0.1699(3) 0.0766(12) Uani 1 1 d . . .
H20A H 0.0617 0.2328 0.1182 0.115 Uiso 1 1 calc R . .
H20B H 0.0030 0.2615 0.1903 0.115 Uiso 1 1 calc R . .
H20C H 0.0914 0.2544 0.2161 0.115 Uiso 1 1 calc R . .
C21 C -0.0633(3) 0.5951(4) 0.1116(3) 0.0976(17) Uani 1 1 d . . .
H21A H -0.0571 0.6478 0.1527 0.146 Uiso 1 1 calc R . .
H21B H -0.1081 0.5583 0.1256 0.146 Uiso 1 1 calc R . .
H21C H -0.0695 0.6198 0.0520 0.146 Uiso 1 1 calc R . .
C22 C 0.33119(17) 0.5236(2) 0.5118(2) 0.0460(7) Uani 1 1 d . . .
C23 C 0.38552(18) 0.4556(3) 0.4919(3) 0.0569(9) Uani 1 1 d . . .
H23 H 0.3835 0.4255 0.4365 0.068 Uiso 1 1 calc R . .
C24 C 0.4434(2) 0.4320(3) 0.5546(4) 0.0817(15) Uani 1 1 d . . .
H24 H 0.4801 0.3857 0.5416 0.098 Uiso 1 1 calc R . .
C25 C 0.4462(3) 0.4769(5) 0.6355(4) 0.0945(18) Uani 1 1 d . . .
H25 H 0.4852 0.4611 0.6774 0.113 Uiso 1 1 calc R . .
C26 C 0.3935(3) 0.5433(4) 0.6553(3) 0.0947(16) Uani 1 1 d . . .
H26 H 0.3961 0.5730 0.7108 0.114 Uiso 1 1 calc R . .
C27 C 0.3355(3) 0.5681(3) 0.5943(3) 0.0738(11) Uani 1 1 d . . .
H27 H 0.2992 0.6145 0.6084 0.089 Uiso 1 1 calc R . .
C28 C 0.16096(11) 0.55560(15) 0.50546(14) 0.0413(7) Uani 1 1 d G . .
C29 C 0.15316(13) 0.48696(15) 0.57190(16) 0.0720(12) Uani 1 1 d G . .
H29 H 0.1894 0.4378 0.5790 0.086 Uiso 1 1 calc R . .
C30 C 0.09116(15) 0.49175(18) 0.62768(16) 0.0794(12) Uani 1 1 d G . .
H30 H 0.0859 0.4458 0.6721 0.095 Uiso 1 1 calc R . .
C31 C 0.03697(12) 0.5652(2) 0.61702(17) 0.0655(10) Uani 1 1 d G . .
H31 H -0.0045 0.5684 0.6543 0.079 Uiso 1 1 calc R . .
C32 C 0.04477(13) 0.63381(18) 0.55058(18) 0.0858(14) Uani 1 1 d G . .
H32 H 0.0085 0.6829 0.5435 0.103 Uiso 1 1 calc R . .
C33 C 0.10676(14) 0.62902(16) 0.49480(15) 0.0691(11) Uani 1 1 d G . .
H33 H 0.1120 0.6749 0.4504 0.083 Uiso 1 1 calc R . .
C34 C 0.25285(19) 0.6732(2) 0.3814(2) 0.0482(8) Uani 1 1 d . . .
C35 C 0.3007(2) 0.7424(3) 0.4169(3) 0.0638(10) Uani 1 1 d . . .
H35 H 0.3333 0.7286 0.4660 0.077 Uiso 1 1 calc R . .
C36 C 0.3002(3) 0.8333(3) 0.3792(4) 0.0896(15) Uani 1 1 d . . .
H36 H 0.3332 0.8807 0.4024 0.108 Uiso 1 1 calc R . .
C37 C 0.2516(4) 0.8536(3) 0.3083(4) 0.0998(18) Uani 1 1 d . . .
H37 H 0.2507 0.9154 0.2844 0.120 Uiso 1 1 calc R . .
C38 C 0.2042(3) 0.7845(4) 0.2717(3) 0.0961(16) Uani 1 1 d . . .
H38 H 0.1716 0.7986 0.2227 0.115 Uiso 1 1 calc R . .
C39 C 0.2051(3) 0.6937(3) 0.3082(3) 0.0704(11) Uani 1 1 d . . .
H39 H 0.1733 0.6458 0.2834 0.085 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 C1 1.994(3) . ?
Pd1 Cl1 2.2799(9) . ?
Pd1 Cl2 2.2846(9) . ?
Pd1 As1 2.4103(7) . ?
As1 C22 1.912(3) . ?
As1 C34 1.927(3) . ?
N1 C1 1.323(3) . ?
N1 C4 1.425(4) . ?
N1 C2 1.472(4) . ?
N2 C1 1.320(4) . ?
N2 C13 1.438(4) . ?
N2 C3 1.467(4) . ?
C2 C3 1.499(5) . ?
C4 C9 1.380(5) . ?
C4 C5 1.386(4) . ?
C5 C6 1.390(5) . ?
C5 C10 1.493(5) . ?
C6 C7 1.362(6) . ?
C7 C8 1.361(5) . ?
C7 C12 1.502(5) . ?
C8 C9 1.383(5) . ?
C9 C11 1.494(5) . ?
C13 C14 1.376(5) . ?
C13 C18 1.383(5) . ?
C14 C15 1.386(5) . ?
C14 C19 1.494(6) . ?
C15 C16 1.358(6) . ?
C16 C17 1.369(6) . ?
C16 C21 1.499(5) . ?
C17 C18 1.382(5) . ?
C18 C20 1.501(5) . ?
C22 C23 1.374(5) . ?
C22 C27 1.384(5) . ?
C23 C24 1.386(5) . ?
C24 C25 1.365(7) . ?
C25 C26 1.340(8) . ?
C26 C27 1.375(6) . ?
C28 C29 1.3900 . ?
C28 C33 1.3900 . ?
C28 As1 1.9311(16) . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C34 C35 1.362(5) . ?
C34 C39 1.378(5) . ?
C35 C36 1.383(6) . ?
C36 C37 1.360(7) . ?
C37 C38 1.363(7) . ?
C38 C39 1.374(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
C1 Pd1 Cl1 93.68(8) . . ?
C1 Pd1 Cl2 89.32(8) . . ?
Cl1 Pd1 Cl2 175.06(3) . . ?
C1 Pd1 As1 173.66(8) . . ?
Cl1 Pd1 As1 91.32(3) . . ?
Cl2 Pd1 As1 85.96(3) . . ?
C22 As1 C34 108.99(14) . . ?
C22 As1 C28 101.62(12) . . ?
C34 As1 C28 101.37(11) . . ?
C22 As1 Pd1 111.06(10) . . ?
C34 As1 Pd1 110.26(9) . . ?
C28 As1 Pd1 122.51(7) . . ?
C1 N1 C4 126.0(2) . . ?
C1 N1 C2 112.7(2) . . ?
C4 N1 C2 120.8(2) . . ?
C1 N2 C13 125.6(2) . . ?
C1 N2 C3 113.1(2) . . ?
C13 N2 C3 121.2(3) . . ?
N2 C1 N1 108.7(2) . . ?
N2 C1 Pd1 122.6(2) . . ?
N1 C1 Pd1 128.4(2) . . ?
N1 C2 C3 102.8(2) . . ?
N2 C3 C2 102.6(3) . . ?
C9 C4 C5 121.0(3) . . ?
C9 C4 N1 119.3(3) . . ?
C5 C4 N1 119.5(3) . . ?
C4 C5 C6 117.3(3) . . ?
C4 C5 C10 121.6(3) . . ?
C6 C5 C10 121.1(3) . . ?
C7 C6 C5 123.0(3) . . ?
C8 C7 C6 117.8(3) . . ?
C8 C7 C12 121.6(4) . . ?
C6 C7 C12 120.6(4) . . ?
C7 C8 C9 122.4(4) . . ?
C4 C9 C8 118.4(3) . . ?
C4 C9 C11 121.4(3) . . ?
C8 C9 C11 120.1(3) . . ?
C14 C13 C18 122.2(3) . . ?
C14 C13 N2 119.5(3) . . ?
C18 C13 N2 118.2(3) . . ?
C13 C14 C15 117.3(4) . . ?
C13 C14 C19 122.7(3) . . ?
C15 C14 C19 120.0(4) . . ?
C16 C15 C14 122.5(4) . . ?
C15 C16 C17 118.5(3) . . ?
C15 C16 C21 120.8(4) . . ?
C17 C16 C21 120.7(4) . . ?
C16 C17 C18 122.0(4) . . ?
C17 C18 C13 117.5(3) . . ?
C17 C18 C20 120.2(3) . . ?
C13 C18 C20 122.3(3) . . ?
C23 C22 C27 119.3(3) . . ?
C23 C22 As1 118.1(3) . . ?
C27 C22 As1 122.3(3) . . ?
C22 C23 C24 119.8(4) . . ?
C25 C24 C23 119.7(5) . . ?
C26 C25 C24 120.8(4) . . ?
C25 C26 C27 120.7(5) . . ?
C26 C27 C22 119.7(5) . . ?
C29 C28 C33 120.0 . . ?
C29 C28 As1 118.44(11) . . ?
C33 C28 As1 121.55(11) . . ?
C30 C29 C28 120.0 . . ?
C31 C30 C29 120.0 . . ?
C30 C31 C32 120.0 . . ?
C33 C32 C31 120.0 . . ?
C32 C33 C28 120.0 . . ?
C35 C34 C39 120.2(3) . . ?
C35 C34 As1 123.7(3) . . ?
C39 C34 As1 116.1(3) . . ?
C34 C35 C36 119.3(4) . . ?
C37 C36 C35 120.2(5) . . ?
C36 C37 C38 120.9(4) . . ?
C37 C38 C39 119.2(5) . . ?
C38 C39 C34 120.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.074
_database_code_depnum_ccdc_archive 'CCDC 1003801'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H41 Cl2 N2 Pd Sb, C H2 Cl2'
_chemical_formula_sum            'C40 H43 Cl4 N2 Pd Sb'
_chemical_formula_weight         921.71

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   19.780(3)
_cell_length_b                   13.9846(17)
_cell_length_c                   14.4282(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.037(2)
_cell_angle_gamma                90.00
_cell_volume                     3988.5(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.2525
_cell_measurement_theta_max      28.4295

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7081
_exptl_absorpt_correction_T_max  0.7936
_exptl_absorpt_process_details   SADABS

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19915
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7009
_reflns_number_gt                6052
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0378P)²+3.3663P] 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         7009
_refine_ls_number_parameters     449
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0730
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.012
_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
Pd1 Pd 0.252005(11) 0.027618(16) 0.721277(15) 0.03496(7) Uani 1 1 d . A 1
Sb1 Sb 0.281995(10) -0.077466(14) 0.580911(13) 0.03667(7) Uani 1 1 d . A 1
N1 N 0.28281(13) 0.19027(19) 0.84784(18) 0.0436(6) Uani 1 1 d . A 1
N2 N 0.18915(13) 0.12280(19) 0.88392(18) 0.0431(6) Uani 1 1 d . A 1
Cl1 Cl 0.20313(7) 0.12989(7) 0.61447(6) 0.0750(3) Uani 1 1 d . A 1
Cl2A Cl 0.2924(5) -0.0862(5) 0.8243(5) 0.0594(16) Uani 0.59(5) 1 d PU A 1
C1 C 0.23986(15) 0.1202(2) 0.8258(2) 0.0366(6) Uani 1 1 d . A 1
C2 C 0.26373(19) 0.2446(3) 0.9302(3) 0.0610(10) Uani 1 1 d . A 1
H2A H 0.2618 0.3127 0.9175 0.073 Uiso 1 1 calc R A 1
H2B H 0.2950 0.2331 0.9823 0.073 Uiso 1 1 calc R A 1
C3 C 0.19419(19) 0.2048(3) 0.9482(3) 0.0575(10) Uani 1 1 d . A 1
H3A H 0.1910 0.1842 1.0121 0.069 Uiso 1 1 calc R A 1
H3B H 0.1591 0.2516 0.9342 0.069 Uiso 1 1 calc R A 1
C4 C 0.34470(15) 0.2126(2) 0.8029(2) 0.0409(7) Uani 1 1 d . A 1
C5 C 0.40447(18) 0.1669(3) 0.8326(2) 0.0516(8) Uani 1 1 d . A 1
C6 C 0.46329(18) 0.1920(3) 0.7896(3) 0.0622(10) Uani 1 1 d . A 1
H6 H 0.5034 0.1612 0.8072 0.075 Uiso 1 1 calc R A 1
C7 C 0.46478(19) 0.2605(3) 0.7221(3) 0.0594(10) Uani 1 1 d . A 1
C8 C 0.4056(2) 0.3042(3) 0.6957(2) 0.0578(10) Uani 1 1 d . A 1
H8 H 0.4063 0.3501 0.6492 0.069 Uiso 1 1 calc R A 1
C9 C 0.34402(17) 0.2831(2) 0.7356(2) 0.0470(8) Uani 1 1 d . A 1
C10 C 0.4062(2) 0.0966(4) 0.9110(3) 0.0817(13) Uani 1 1 d . A 1
H10A H 0.4355 0.0444 0.8967 0.122 Uiso 1 1 calc R A 1
H10B H 0.3613 0.0728 0.9200 0.122 Uiso 1 1 calc R A 1
H10C H 0.4227 0.1277 0.9667 0.122 Uiso 1 1 calc R A 1
C11 C 0.2817(2) 0.3376(3) 0.7092(3) 0.0728(11) Uani 1 1 d . A 1
H11A H 0.2433 0.2957 0.7099 0.109 Uiso 1 1 calc R A 1
H11B H 0.2857 0.3636 0.6480 0.109 Uiso 1 1 calc R A 1
H11C H 0.2758 0.3887 0.7525 0.109 Uiso 1 1 calc R A 1
C12 C 0.5315(2) 0.2904(4) 0.6809(4) 0.1017(18) Uani 1 1 d . A 1
H12A H 0.5549 0.3336 0.7226 0.152 Uiso 1 1 calc R A 1
H12B H 0.5227 0.3215 0.6224 0.152 Uiso 1 1 calc R A 1
H12C H 0.5590 0.2348 0.6718 0.152 Uiso 1 1 calc R A 1
C13 C 0.13335(15) 0.0576(2) 0.8854(2) 0.0413(7) Uani 1 1 d . A 1
C14 C 0.13687(18) -0.0179(2) 0.9482(2) 0.0516(8) Uani 1 1 d . A 1
C15 C 0.0812(2) -0.0792(3) 0.9500(3) 0.0632(10) Uani 1 1 d . A 1
H15 H 0.0827 -0.1308 0.9907 0.076 Uiso 1 1 calc R A 1
C16 C 0.0244(2) -0.0660(3) 0.8938(3) 0.0630(11) Uani 1 1 d . A 1
C17 C 0.02292(19) 0.0111(3) 0.8358(3) 0.0638(10) Uani 1 1 d . A 1
H17 H -0.0155 0.0208 0.7980 0.077 Uiso 1 1 calc R A 1
C18 C 0.07573(17) 0.0755(3) 0.8305(2) 0.0501(8) Uani 1 1 d . A 1
C19 C 0.1967(2) -0.0333(3) 1.0128(3) 0.0789(13) Uani 1 1 d . A 1
H19A H 0.2369 -0.0378 0.9778 0.118 Uiso 1 1 calc R A 1
H19B H 0.1907 -0.0914 1.0469 0.118 Uiso 1 1 calc R A 1
H19C H 0.2007 0.0195 1.0552 0.118 Uiso 1 1 calc R A 1
C20 C 0.0692(2) 0.1615(4) 0.7690(3) 0.0790(13) Uani 1 1 d . A 1
H20A H 0.0564 0.2158 0.8050 0.118 Uiso 1 1 calc R A 1
H20B H 0.0353 0.1498 0.7211 0.118 Uiso 1 1 calc R A 1
H20C H 0.1118 0.1739 0.7413 0.118 Uiso 1 1 calc R A 1
C21 C -0.0343(2) -0.1348(4) 0.8985(4) 0.1011(18) Uani 1 1 d . A 1
H21A H -0.0174 -0.1983 0.9095 0.152 Uiso 1 1 calc R A 1
H21B H -0.0600 -0.1334 0.8408 0.152 Uiso 1 1 calc R A 1
H21C H -0.0627 -0.1164 0.9480 0.152 Uiso 1 1 calc R A 1
C22 C 0.36006(15) -0.0078(2) 0.5096(2) 0.0408(7) Uani 1 1 d . A 1
C23 C 0.39365(18) 0.0682(3) 0.5517(3) 0.0534(9) Uani 1 1 d . A 1
H23 H 0.3829 0.0871 0.6112 0.064 Uiso 1 1 calc R A 1
C24 C 0.4432(2) 0.1159(3) 0.5049(3) 0.0672(11) Uani 1 1 d . A 1
H24 H 0.4655 0.1673 0.5331 0.081 Uiso 1 1 calc R A 1
C25 C 0.4596(2) 0.0885(3) 0.4180(3) 0.0651(11) Uani 1 1 d . A 1
H25 H 0.4935 0.1206 0.3875 0.078 Uiso 1 1 calc R A 1
C26 C 0.4263(2) 0.0139(3) 0.3755(3) 0.0653(11) Uani 1 1 d . A 1
H26 H 0.4375 -0.0047 0.3161 0.078 Uiso 1 1 calc R A 1
C27 C 0.37590(19) -0.0339(3) 0.4207(2) 0.0542(9) Uani 1 1 d . A 1
H27 H 0.3527 -0.0838 0.3912 0.065 Uiso 1 1 calc R A 1
C28 C 0.21676(16) -0.1013(2) 0.4628(2) 0.0417(7) Uani 1 1 d . A 1
C29 C 0.1899(2) -0.0251(3) 0.4138(3) 0.0601(10) Uani 1 1 d . A 1
H29 H 0.1982 0.0368 0.4347 0.072 Uiso 1 1 calc R A 1
C30 C 0.1507(2) -0.0396(3) 0.3338(3) 0.0734(12) Uani 1 1 d . A 1
H30 H 0.1338 0.0125 0.3003 0.088 Uiso 1 1 calc R A 1
C31 C 0.1367(2) -0.1305(3) 0.3040(3) 0.0672(11) Uani 1 1 d . A 1
H31 H 0.1095 -0.1401 0.2510 0.081 Uiso 1 1 calc R A 1
C32 C 0.1624(2) -0.2069(3) 0.3515(3) 0.0667(11) Uani 1 1 d . A 1
H32 H 0.1529 -0.2686 0.3310 0.080 Uiso 1 1 calc R A 1
C33 C 0.20287(19) -0.1926(3) 0.4305(2) 0.0546(9) Uani 1 1 d . A 1
H33 H 0.2210 -0.2450 0.4623 0.065 Uiso 1 1 calc R A 1
C34 C 0.31873(16) -0.2194(2) 0.5998(2) 0.0404(7) Uani 1 1 d . A 1
C35 C 0.36362(19) -0.2605(3) 0.5411(3) 0.0557(9) Uani 1 1 d . A 1
H35 H 0.3814 -0.2246 0.4936 0.067 Uiso 1 1 calc R A 1
C36 C 0.3825(2) -0.3555(3) 0.5526(3) 0.0667(11) Uani 1 1 d . A 1
H36 H 0.4121 -0.3832 0.5119 0.080 Uiso 1 1 calc R A 1
C37 C 0.3581(2) -0.4076(3) 0.6222(3) 0.0671(11) Uani 1 1 d . A 1
H37 H 0.3719 -0.4708 0.6304 0.081 Uiso 1 1 calc R A 1
C38 C 0.3130(2) -0.3681(3) 0.6810(3) 0.0653(11) Uani 1 1 d . A 1
H38 H 0.2956 -0.4050 0.7283 0.078 Uiso 1 1 calc R A 1
C39 C 0.29323(19) -0.2740(3) 0.6706(2) 0.0530(8) Uani 1 1 d . A 1
H39 H 0.2629 -0.2473 0.7110 0.064 Uiso 1 1 calc R A 1
C40 C 0.0591(3) 0.5923(5) 0.0848(6) 0.148(3) Uani 1 1 d . B 1
H40A H 0.0593 0.5341 0.1214 0.178 Uiso 1 1 calc R B 1
H40B H 0.0840 0.5792 0.0295 0.178 Uiso 1 1 calc R B 1
Cl3 Cl 0.10077(10) 0.67727(17) 0.14629(14) 0.1556(8) Uani 1 1 d . B 1
Cl4 Cl -0.02215(11) 0.61796(19) 0.0520(2) 0.2000(13) Uani 1 1 d . B 1
Cl2B Cl 0.3117(18) -0.0720(18) 0.8137(15) 0.093(5) Uani 0.41(5) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C1 2.009(3) . ?
Pd1 Cl1 2.2911(9) . ?
Pd1 Cl2A 2.302(7) . ?
Pd1 Sb1 2.5881(4) . ?
Sb1 C22 2.123(3) . ?
Sb1 C28 2.127(3) . ?
Sb1 C34 2.128(3) . ?
N1 C1 1.328(4) . ?
N1 C4 1.440(4) . ?
N1 C2 1.471(4) . ?
N2 C1 1.330(4) . ?
N2 C13 1.432(4) . ?
N2 C3 1.475(4) . ?
C2 C3 1.515(5) . ?
C4 C9 1.384(5) . ?
C4 C5 1.398(5) . ?
C5 C6 1.384(5) . ?
C5 C10 1.498(5) . ?
C6 C7 1.366(6) . ?
C7 C8 1.363(6) . ?
C7 C12 1.525(5) . ?
C8 C9 1.397(5) . ?
C9 C11 1.488(5) . ?
C13 C18 1.388(5) . ?
C13 C14 1.392(5) . ?
C14 C15 1.396(5) . ?
C14 C19 1.495(5) . ?
C15 C16 1.376(6) . ?
C16 C17 1.365(6) . ?
C16 C21 1.510(5) . ?
C17 C18 1.384(5) . ?
C18 C20 1.496(5) . ?
C22 C27 1.380(5) . ?
C22 C23 1.382(5) . ?
C23 C24 1.381(5) . ?
C24 C25 1.361(6) . ?
C25 C26 1.368(6) . ?
C26 C27 1.382(5) . ?
C28 C29 1.375(5) . ?
C28 C33 1.382(5) . ?
C29 C30 1.382(5) . ?
C30 C31 1.367(6) . ?
C31 C32 1.358(6) . ?
C32 C33 1.383(5) . ?
C34 C35 1.374(5) . ?
C34 C39 1.385(5) . ?
C35 C36 1.388(5) . ?
C36 C37 1.344(6) . ?
C37 C38 1.369(6) . ?
C38 C39 1.380(5) . ?
C40 Cl3 1.681(7) . ?
C40 Cl4 1.698(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
C1 Pd1 Cl1 92.52(9) . . ?
C1 Pd1 Cl2A 90.5(2) . . ?
Cl1 Pd1 Cl2A 174.1(2) . . ?
C1 Pd1 Sb1 172.07(9) . . ?
Cl1 Pd1 Sb1 86.05(3) . . ?
Cl2A Pd1 Sb1 91.65(19) . . ?
C22 Sb1 C28 96.58(12) . . ?
C22 Sb1 C34 103.86(12) . . ?
C28 Sb1 C34 98.68(12) . . ?
C22 Sb1 Pd1 108.03(8) . . ?
C28 Sb1 Pd1 124.52(8) . . ?
C34 Sb1 Pd1 121.07(8) . . ?
C1 N1 C4 126.8(2) . . ?
C1 N1 C2 113.2(2) . . ?
C4 N1 C2 119.9(2) . . ?
C1 N2 C13 126.2(2) . . ?
C1 N2 C3 112.4(3) . . ?
C13 N2 C3 121.3(2) . . ?
N1 C1 N2 108.6(3) . . ?
N1 C1 Pd1 124.2(2) . . ?
N2 C1 Pd1 127.2(2) . . ?
N1 C2 C3 102.0(3) . . ?
N2 C3 C2 102.7(2) . . ?
C9 C4 C5 121.9(3) . . ?
C9 C4 N1 118.9(3) . . ?
C5 C4 N1 119.1(3) . . ?
C6 C5 C4 117.5(3) . . ?
C6 C5 C10 120.6(4) . . ?
C4 C5 C10 121.8(3) . . ?
C7 C6 C5 122.6(4) . . ?
C8 C7 C6 118.2(3) . . ?
C8 C7 C12 121.0(4) . . ?
C6 C7 C12 120.7(4) . . ?
C7 C8 C9 122.9(4) . . ?
C4 C9 C8 116.9(3) . . ?
C4 C9 C11 122.1(3) . . ?
C8 C9 C11 120.9(3) . . ?
C18 C13 C14 122.0(3) . . ?
C18 C13 N2 119.6(3) . . ?
C14 C13 N2 118.2(3) . . ?
C13 C14 C15 117.2(3) . . ?
C13 C14 C19 122.4(3) . . ?
C15 C14 C19 120.4(4) . . ?
C16 C15 C14 122.3(4) . . ?
C17 C16 C15 117.8(4) . . ?
C17 C16 C21 122.1(4) . . ?
C15 C16 C21 120.1(4) . . ?
C16 C17 C18 123.3(4) . . ?
C13 C18 C17 117.2(3) . . ?
C13 C18 C20 122.4(3) . . ?
C17 C18 C20 120.4(4) . . ?
C27 C22 C23 119.4(3) . . ?
C27 C22 Sb1 121.4(2) . . ?
C23 C22 Sb1 119.1(2) . . ?
C24 C23 C22 119.7(4) . . ?
C25 C24 C23 120.7(4) . . ?
C26 C25 C24 120.0(4) . . ?
C25 C26 C27 120.1(4) . . ?
C22 C27 C26 120.1(4) . . ?
C29 C28 C33 118.3(3) . . ?
C29 C28 Sb1 120.2(3) . . ?
C33 C28 Sb1 121.5(2) . . ?
C28 C29 C30 120.7(4) . . ?
C31 C30 C29 120.0(4) . . ?
C32 C31 C30 120.4(4) . . ?
C31 C32 C33 119.8(4) . . ?
C32 C33 C28 120.9(4) . . ?
C35 C34 C39 119.0(3) . . ?
C35 C34 Sb1 122.4(2) . . ?
C39 C34 Sb1 118.5(2) . . ?
C34 C35 C36 120.2(4) . . ?
C37 C36 C35 120.4(4) . . ?
C36 C37 C38 120.2(4) . . ?
C39 C38 C37 120.4(4) . . ?
C38 C39 C34 119.8(4) . . ?
Cl3 C40 Cl4 116.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 1003802'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H53 As Cl2 N2 Pd 0.5(CH2Cl2)'
_chemical_formula_sum            'C45.50 H54 As Cl3 N2 Pd'
_chemical_formula_weight         916.58

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'
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n
_symmetry_space_group_name_Hall  '-P 2ybn'

loop_
_symmetry_equiv_pos_as_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                   10.684(4)
_cell_length_b                   12.179(5)
_cell_length_c                   35.633(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.220(6)
_cell_angle_gamma                90.00
_cell_volume                     4629(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9906
_cell_measurement_theta_min      2.3971
_cell_measurement_theta_max      28.0524

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7520
_exptl_absorpt_correction_T_max  0.8074
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
? 
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 286 49 ' '
2 0.021 0.400 0.797 8 0 ' '
3 0.500 0.500 0.500 286 49 ' '
4 0.479 0.900 0.703 8 0 ' '
5 0.521 0.100 0.297 8 0 ' '
6 0.979 0.600 0.203 8 0 ' '
_platon_squeeze_details          
;
During the refinement, the CH2Cl2 molecule is
seriously disordered. During the final refinement,
the contribution of the solvent molecules to the crystal
structure is treated by using the Platon/SQUEEZE procedure.
Check using platon shows that there are 605.5Å³ volumes
in the unit cell (approximately 98 electrons,
i.e. ca. 2 CH2Cl2 molecules based on the solvents
we have used and each host molecule was
distributed 0.5 CH2Cl2 molecule). So the suitable formula
should be C₄₅H₅₃As₁Cl₂N₂Pd₁.(CH2Cl2)~0.5~. Some related items
have been corrected in the cif file.
;
# start Validation Reply Form
_vrf_CHEMW03_2c                  
;
ALERT_2_C: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: 
This is due to the serious disorders of the CH2Cl2 solvent,
attempts were made to mode this, but we are failed. Then SQUEEZE/PLATON
were used to treated this. But in the cif file some related items were added 
i.e. the Z, formual weight, F000.
;
# end Validation Reply Form

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22942
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8110
_reflns_number_gt                7035
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0218P)²+4.4483P] 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         8110
_refine_ls_number_parameters     468
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.631567(19) 0.504000(17) 0.855637(6) 0.02732(7) Uani 1 1 d . . .
N1 N 0.5575(2) 0.65190(18) 0.78927(6) 0.0308(5) Uani 1 1 d . . .
N2 N 0.5225(2) 0.72718(18) 0.84334(6) 0.0292(5) Uani 1 1 d . . .
Cl1 Cl 0.82428(7) 0.54642(7) 0.83345(2) 0.04430(19) Uani 1 1 d . . .
Cl2 Cl 0.43911(7) 0.46089(7) 0.87822(3) 0.0489(2) Uani 1 1 d . . .
As1 As 0.72507(3) 0.35869(2) 0.896530(8) 0.03020(8) Uani 1 1 d . . .
C1 C 0.5617(2) 0.6350(2) 0.82685(7) 0.0272(6) Uani 1 1 d . . .
C2 C 0.5079(4) 0.7613(3) 0.77871(9) 0.0521(9) Uani 1 1 d . . .
H2A H 0.4254 0.7558 0.7660 0.062 Uiso 1 1 calc R . .
H2B H 0.5636 0.7994 0.7625 0.062 Uiso 1 1 calc R . .
C3 C 0.5021(3) 0.8190(2) 0.81639(8) 0.0401(7) Uani 1 1 d . . .
H3A H 0.5673 0.8741 0.8197 0.048 Uiso 1 1 calc R . .
H3B H 0.4211 0.8533 0.8190 0.048 Uiso 1 1 calc R . .
C4 C 0.5739(3) 0.5687(2) 0.76087(7) 0.0323(6) Uani 1 1 d . . .
C5 C 0.4786(3) 0.4897(3) 0.75414(8) 0.0416(7) Uani 1 1 d . . .
C6 C 0.4959(4) 0.4123(3) 0.72568(9) 0.0533(9) Uani 1 1 d . . .
H6 H 0.4357 0.3581 0.7209 0.064 Uiso 1 1 calc R . .
C7 C 0.6004(4) 0.4151(3) 0.70461(9) 0.0597(10) Uani 1 1 d . . .
H7 H 0.6109 0.3622 0.6862 0.072 Uiso 1 1 calc R . .
C8 C 0.6889(4) 0.4957(3) 0.71077(9) 0.0525(9) Uani 1 1 d . . .
H8 H 0.7574 0.4977 0.6958 0.063 Uiso 1 1 calc R . .
C9 C 0.6795(3) 0.5752(3) 0.73895(8) 0.0384(7) Uani 1 1 d . . .
C10 C 0.3571(3) 0.4879(3) 0.77451(11) 0.0582(10) Uani 1 1 d . . .
H10 H 0.3694 0.5324 0.7973 0.070 Uiso 1 1 calc R . .
C11 C 0.3177(5) 0.3730(4) 0.78611(14) 0.0915(16) Uani 1 1 d . . .
H11A H 0.2981 0.3297 0.7641 0.137 Uiso 1 1 calc R . .
H11B H 0.2451 0.3780 0.8007 0.137 Uiso 1 1 calc R . .
H11C H 0.3850 0.3391 0.8009 0.137 Uiso 1 1 calc R . .
C12 C 0.2524(5) 0.5409(6) 0.74940(19) 0.124(2) Uani 1 1 d . . .
H12A H 0.2740 0.6157 0.7444 0.187 Uiso 1 1 calc R . .
H12B H 0.1753 0.5388 0.7620 0.187 Uiso 1 1 calc R . .
H12C H 0.2424 0.5012 0.7262 0.187 Uiso 1 1 calc R . .
C13 C 0.7782(3) 0.6644(3) 0.74394(9) 0.0450(8) Uani 1 1 d . . .
H13 H 0.7688 0.6990 0.7685 0.054 Uiso 1 1 calc R . .
C14 C 0.7587(4) 0.7541(3) 0.71338(10) 0.0610(10) Uani 1 1 d . . .
H14A H 0.7737 0.7234 0.6892 0.091 Uiso 1 1 calc R . .
H14B H 0.8160 0.8135 0.7187 0.091 Uiso 1 1 calc R . .
H14C H 0.6742 0.7810 0.7133 0.091 Uiso 1 1 calc R . .
C15 C 0.9125(3) 0.6180(3) 0.74353(11) 0.0630(10) Uani 1 1 d . . .
H15A H 0.9220 0.5586 0.7612 0.095 Uiso 1 1 calc R . .
H15B H 0.9717 0.6748 0.7504 0.095 Uiso 1 1 calc R . .
H15C H 0.9274 0.5916 0.7188 0.095 Uiso 1 1 calc R . .
C16 C 0.5055(3) 0.7423(2) 0.88306(7) 0.0277(6) Uani 1 1 d . . .
C17 C 0.3824(3) 0.7397(2) 0.89526(8) 0.0342(7) Uani 1 1 d . . .
C18 C 0.3674(3) 0.7512(3) 0.93369(9) 0.0420(8) Uani 1 1 d . . .
H18 H 0.2873 0.7496 0.9426 0.050 Uiso 1 1 calc R . .
C19 C 0.4702(3) 0.7651(3) 0.95886(9) 0.0476(8) Uani 1 1 d . . .
H19 H 0.4586 0.7701 0.9845 0.057 Uiso 1 1 calc R . .
C20 C 0.5894(3) 0.7715(3) 0.94608(8) 0.0437(8) Uani 1 1 d . . .
H20 H 0.6571 0.7832 0.9632 0.052 Uiso 1 1 calc R . .
C21 C 0.6104(3) 0.7607(2) 0.90782(8) 0.0325(6) Uani 1 1 d . . .
C22 C 0.2658(3) 0.7306(3) 0.86834(9) 0.0459(8) Uani 1 1 d . . .
H22 H 0.2940 0.7142 0.8432 0.055 Uiso 1 1 calc R . .
C23 C 0.1763(3) 0.6393(3) 0.87895(14) 0.0705(12) Uani 1 1 d . . .
H23A H 0.2216 0.5714 0.8818 0.106 Uiso 1 1 calc R . .
H23B H 0.1110 0.6314 0.8595 0.106 Uiso 1 1 calc R . .
H23C H 0.1399 0.6576 0.9022 0.106 Uiso 1 1 calc R . .
C24 C 0.1948(4) 0.8409(3) 0.86613(12) 0.0681(11) Uani 1 1 d . . .
H24A H 0.1694 0.8605 0.8907 0.102 Uiso 1 1 calc R . .
H24B H 0.1220 0.8338 0.8492 0.102 Uiso 1 1 calc R . .
H24C H 0.2487 0.8969 0.8571 0.102 Uiso 1 1 calc R . .
C25 C 0.7433(3) 0.7758(3) 0.89450(9) 0.0410(7) Uani 1 1 d . . .
H25 H 0.7443 0.7481 0.8687 0.049 Uiso 1 1 calc R . .
C26 C 0.8429(3) 0.7125(3) 0.91865(11) 0.0620(10) Uani 1 1 d . . .
H26A H 0.8440 0.7386 0.9441 0.093 Uiso 1 1 calc R . .
H26B H 0.9238 0.7236 0.9088 0.093 Uiso 1 1 calc R . .
H26C H 0.8230 0.6356 0.9181 0.093 Uiso 1 1 calc R . .
C27 C 0.7774(3) 0.8989(3) 0.89398(11) 0.0581(10) Uani 1 1 d . . .
H27A H 0.7755 0.9282 0.9190 0.087 Uiso 1 1 calc R . .
H27B H 0.7180 0.9374 0.8776 0.087 Uiso 1 1 calc R . .
H27C H 0.8599 0.9076 0.8851 0.087 Uiso 1 1 calc R . .
C28 C 0.6223(3) 0.2278(2) 0.90235(8) 0.0354(7) Uani 1 1 d . . .
C29 C 0.5430(3) 0.1929(3) 0.87301(10) 0.0438(8) Uani 1 1 d . . .
H29 H 0.5382 0.2321 0.8506 0.053 Uiso 1 1 calc R . .
C30 C 0.4698(3) 0.0992(3) 0.87664(12) 0.0576(10) Uani 1 1 d . . .
H30 H 0.4178 0.0752 0.8565 0.069 Uiso 1 1 calc R . .
C31 C 0.4740(4) 0.0424(3) 0.90974(13) 0.0664(11) Uani 1 1 d . . .
H31 H 0.4240 -0.0195 0.9121 0.080 Uiso 1 1 calc R . .
C32 C 0.5522(4) 0.0765(3) 0.93966(12) 0.0640(11) Uani 1 1 d . . .
H32 H 0.5553 0.0374 0.9621 0.077 Uiso 1 1 calc R . .
C33 C 0.6265(4) 0.1695(3) 0.93616(10) 0.0499(9) Uani 1 1 d . . .
H33 H 0.6789 0.1927 0.9563 0.060 Uiso 1 1 calc R . .
C34 C 0.8881(3) 0.2964(2) 0.88608(8) 0.0348(7) Uani 1 1 d . . .
C35 C 0.9001(3) 0.1868(3) 0.87618(10) 0.0500(9) Uani 1 1 d . . .
H35 H 0.8313 0.1400 0.8765 0.060 Uiso 1 1 calc R . .
C36 C 1.0152(4) 0.1468(3) 0.86568(13) 0.0744(13) Uani 1 1 d . . .
H36 H 1.0227 0.0739 0.8584 0.089 Uiso 1 1 calc R . .
C37 C 1.1180(4) 0.2150(4) 0.86601(14) 0.0788(13) Uani 1 1 d . . .
H37 H 1.1947 0.1879 0.8590 0.095 Uiso 1 1 calc R . .
C38 C 1.1077(3) 0.3228(3) 0.87660(12) 0.0658(11) Uani 1 1 d . . .
H38 H 1.1778 0.3681 0.8773 0.079 Uiso 1 1 calc R . .
C39 C 0.9932(3) 0.3643(3) 0.88618(10) 0.0483(8) Uani 1 1 d . . .
H39 H 0.9864 0.4379 0.8927 0.058 Uiso 1 1 calc R . .
C40 C 0.7511(3) 0.4107(2) 0.94827(8) 0.0378(7) Uani 1 1 d . . .
C41 C 0.8544(4) 0.3797(3) 0.97126(10) 0.0564(9) Uani 1 1 d . . .
H41 H 0.9145 0.3330 0.9622 0.068 Uiso 1 1 calc R . .
C42 C 0.8676(4) 0.4193(4) 1.00819(11) 0.0727(12) Uani 1 1 d . . .
H42 H 0.9360 0.3978 1.0238 0.087 Uiso 1 1 calc R . .
C43 C 0.7802(5) 0.4894(4) 1.02145(11) 0.0730(13) Uani 1 1 d . . .
H43 H 0.7904 0.5165 1.0458 0.088 Uiso 1 1 calc R . .
C44 C 0.6782(5) 0.5198(3) 0.99900(11) 0.0701(12) Uani 1 1 d . . .
H44 H 0.6189 0.5669 1.0083 0.084 Uiso 1 1 calc R . .
C45 C 0.6620(4) 0.4807(3) 0.96203(9) 0.0525(9) Uani 1 1 d . . .
H45 H 0.5923 0.5015 0.9469 0.063 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 C1 2.017(3) . ?
Pd1 Cl1 2.3052(11) . ?
Pd1 Cl2 2.3101(11) . ?
Pd1 As1 2.4676(7) . ?
N1 C1 1.353(3) . ?
N1 C4 1.450(3) . ?
N1 C2 1.474(4) . ?
N2 C1 1.345(3) . ?
N2 C16 1.448(3) . ?
N2 C3 1.482(3) . ?
As1 C28 1.953(3) . ?
As1 C40 1.954(3) . ?
As1 C34 1.955(3) . ?
C2 C3 1.520(4) . ?
C4 C9 1.409(4) . ?
C4 C5 1.412(4) . ?
C5 C6 1.404(4) . ?
C5 C10 1.522(5) . ?
C6 C7 1.381(5) . ?
C7 C8 1.372(5) . ?
C8 C9 1.402(4) . ?
C9 C13 1.518(5) . ?
C10 C11 1.524(6) . ?
C10 C12 1.535(6) . ?
C13 C15 1.543(5) . ?
C13 C14 1.548(5) . ?
C16 C21 1.404(4) . ?
C16 C17 1.409(4) . ?
C17 C18 1.395(4) . ?
C17 C22 1.533(4) . ?
C18 C19 1.389(5) . ?
C19 C20 1.378(5) . ?
C20 C21 1.400(4) . ?
C21 C25 1.534(4) . ?
C22 C23 1.529(5) . ?
C22 C24 1.542(5) . ?
C25 C26 1.538(5) . ?
C25 C27 1.542(5) . ?
C28 C29 1.376(4) . ?
C28 C33 1.397(4) . ?
C29 C30 1.393(5) . ?
C30 C31 1.366(6) . ?
C31 C32 1.381(6) . ?
C32 C33 1.392(5) . ?
C34 C35 1.389(4) . ?
C34 C39 1.394(4) . ?
C35 C36 1.393(5) . ?
C36 C37 1.375(6) . ?
C37 C38 1.373(6) . ?
C38 C39 1.383(5) . ?
C40 C45 1.388(5) . ?
C40 C41 1.389(5) . ?
C41 C42 1.401(5) . ?
C42 C43 1.369(6) . ?
C43 C44 1.367(6) . ?
C44 C45 1.402(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 Cl1 87.72(8) . . ?
C1 Pd1 Cl2 92.63(8) . . ?
Cl1 Pd1 Cl2 179.61(3) . . ?
C1 Pd1 As1 173.44(8) . . ?
Cl1 Pd1 As1 91.35(3) . . ?
Cl2 Pd1 As1 88.29(3) . . ?
C1 N1 C4 125.9(2) . . ?
C1 N1 C2 112.4(2) . . ?
C4 N1 C2 120.6(2) . . ?
C1 N2 C16 126.3(2) . . ?
C1 N2 C3 112.6(2) . . ?
C16 N2 C3 121.0(2) . . ?
C28 As1 C40 102.44(12) . . ?
C28 As1 C34 102.47(12) . . ?
C40 As1 C34 102.97(13) . . ?
C28 As1 Pd1 115.88(9) . . ?
C40 As1 Pd1 110.85(9) . . ?
C34 As1 Pd1 120.09(9) . . ?
N2 C1 N1 108.2(2) . . ?
N2 C1 Pd1 123.61(18) . . ?
N1 C1 Pd1 127.91(19) . . ?
N1 C2 C3 103.0(2) . . ?
N2 C3 C2 102.2(2) . . ?
C9 C4 C5 122.4(3) . . ?
C9 C4 N1 118.7(3) . . ?
C5 C4 N1 118.7(3) . . ?
C6 C5 C4 117.2(3) . . ?
C6 C5 C10 119.0(3) . . ?
C4 C5 C10 123.7(3) . . ?
C7 C6 C5 121.3(3) . . ?
C8 C7 C6 120.1(3) . . ?
C7 C8 C9 122.1(3) . . ?
C8 C9 C4 116.8(3) . . ?
C8 C9 C13 120.0(3) . . ?
C4 C9 C13 123.2(3) . . ?
C5 C10 C11 113.5(3) . . ?
C5 C10 C12 109.2(4) . . ?
C11 C10 C12 109.9(4) . . ?
C9 C13 C15 112.1(3) . . ?
C9 C13 C14 111.0(3) . . ?
C15 C13 C14 109.9(3) . . ?
C21 C16 C17 122.3(2) . . ?
C21 C16 N2 119.7(2) . . ?
C17 C16 N2 118.0(2) . . ?
C18 C17 C16 117.5(3) . . ?
C18 C17 C22 119.2(3) . . ?
C16 C17 C22 123.2(3) . . ?
C19 C18 C17 121.1(3) . . ?
C20 C19 C18 120.3(3) . . ?
C19 C20 C21 121.2(3) . . ?
C20 C21 C16 117.5(3) . . ?
C20 C21 C25 119.5(3) . . ?
C16 C21 C25 123.0(2) . . ?
C23 C22 C17 113.3(3) . . ?
C23 C22 C24 109.4(3) . . ?
C17 C22 C24 110.4(3) . . ?
C21 C25 C26 113.0(3) . . ?
C21 C25 C27 110.1(3) . . ?
C26 C25 C27 109.7(3) . . ?
C29 C28 C33 119.1(3) . . ?
C29 C28 As1 119.9(2) . . ?
C33 C28 As1 121.0(2) . . ?
C28 C29 C30 120.5(3) . . ?
C31 C30 C29 120.2(4) . . ?
C30 C31 C32 120.2(3) . . ?
C31 C32 C33 119.9(4) . . ?
C32 C33 C28 120.0(4) . . ?
C35 C34 C39 119.0(3) . . ?
C35 C34 As1 121.1(2) . . ?
C39 C34 As1 119.7(2) . . ?
C34 C35 C36 119.9(3) . . ?
C37 C36 C35 120.2(4) . . ?
C38 C37 C36 120.2(4) . . ?
C37 C38 C39 120.2(4) . . ?
C38 C39 C34 120.4(3) . . ?
C45 C40 C41 119.8(3) . . ?
C45 C40 As1 117.9(2) . . ?
C41 C40 As1 122.3(3) . . ?
C40 C41 C42 119.7(4) . . ?
C43 C42 C41 120.3(4) . . ?
C44 C43 C42 120.3(4) . . ?
C43 C44 C45 120.7(4) . . ?
C40 C45 C44 119.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.060
_database_code_depnum_ccdc_archive 'CCDC 1003803'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H53 Cl2 N2 Pd Sb'
_chemical_formula_sum            'C45 H53 Cl2 N2 Pd Sb'
_chemical_formula_weight         920.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P_65
_symmetry_space_group_name_Hall  P_65

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'

_cell_length_a                   25.982(5)
_cell_length_b                   25.982(5)
_cell_length_c                   12.486(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7299(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9874
_cell_measurement_theta_min      2.2624
_cell_measurement_theta_max      26.8868

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2808
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7846
_exptl_absorpt_correction_T_max  0.8400
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
; 
 ? 
;
# start Validation Reply Form
_vrf_PLAT602_2d                  
;
ALERT_2_A: VERY LARGE Solvent Accessible VOID(S) in Structure        ! Info 
RESPONSE: 
The highest peak in the final difference map is just 0.53 e/A3 (0.66A from H45) 
and no suitable model for any solvent could be found in difference Fourier 
syntheses. Attemptsmade to model the solvent molecule were not successful.The 
SQUEEZE option in PLATON (Spek, 2003) indicated there was a solvent cavity of 
volume 1230.4 \%A^3^ containing approximately 350 electrons. In the final cycles 
of refinement, this contribution to the electron density was removed from the 
observed data. The density, the F(000) value, the molecular weight and the formula 
are given without taking into account the results obtained with the SQUEEZE 
option PLATON (Spek, 2003). 
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
;
# end Validation Reply Form

_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 APEX II area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36826
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8505
_reflns_number_gt                7827
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART APEX II'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0428P)²+13.2917P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_number_reflns         8505
_refine_ls_number_parameters     457
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.120
_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
Pd1 Pd 0.329785(18) 0.433167(19) 0.99033(4) 0.03594(11) Uani 1 1 d . . .
Cl1 Cl 0.27748(8) 0.47746(8) 1.04667(15) 0.0550(4) Uani 1 1 d . . .
Cl2 Cl 0.37726(9) 0.38330(8) 0.93462(15) 0.0569(4) Uani 1 1 d . . .
N1 N 0.4166(2) 0.5211(2) 0.8355(4) 0.0398(11) Uani 1 1 d . . .
N2 N 0.3278(2) 0.4764(2) 0.7697(4) 0.0423(12) Uani 1 1 d . . .
Sb1 Sb 0.283795(17) 0.361155(18) 1.15030(3) 0.04111(11) Uani 1 1 d . . .
C1 C 0.3604(3) 0.4830(3) 0.8562(4) 0.0353(13) Uani 1 1 d . . .
C2 C 0.4262(3) 0.5430(4) 0.7239(6) 0.0576(18) Uani 1 1 d . . .
H2A H 0.4521 0.5324 0.6857 0.069 Uiso 1 1 calc R . .
H2B H 0.4431 0.5857 0.7213 0.069 Uiso 1 1 calc R . .
C3 C 0.3636(3) 0.5109(4) 0.6780(5) 0.0573(18) Uani 1 1 d . . .
H3A H 0.3517 0.5389 0.6535 0.069 Uiso 1 1 calc R . .
H3B H 0.3605 0.4852 0.6190 0.069 Uiso 1 1 calc R . .
C4 C 0.4623(3) 0.5481(3) 0.9158(5) 0.0419(14) Uani 1 1 d . . .
C5 C 0.4624(3) 0.5905(3) 0.9855(7) 0.0590(17) Uani 1 1 d . . .
C6 C 0.5079(4) 0.6146(4) 1.0595(7) 0.082(3) Uani 1 1 d . . .
H6 H 0.5081 0.6420 1.1078 0.098 Uiso 1 1 calc R . .
C7 C 0.5515(5) 0.6020(5) 1.0674(9) 0.098(3) Uani 1 1 d . . .
H7 H 0.5797 0.6184 1.1216 0.118 Uiso 1 1 calc R . .
C8 C 0.5534(3) 0.5645(5) 0.9939(9) 0.084(3) Uani 1 1 d . . .
H8 H 0.5854 0.5579 0.9955 0.101 Uiso 1 1 calc R . .
C9 C 0.5085(3) 0.5344(3) 0.9139(7) 0.062(2) Uani 1 1 d . . .
C10 C 0.4152(4) 0.6088(3) 0.9793(7) 0.0639(18) Uani 1 1 d U . .
H10 H 0.3791 0.5756 0.9486 0.077 Uiso 1 1 calc R . .
C11 C 0.3990(5) 0.6241(5) 1.0880(8) 0.093(3) Uani 1 1 d U . .
H11A H 0.3882 0.5918 1.1368 0.139 Uiso 1 1 calc R . .
H11B H 0.3661 0.6308 1.0794 0.139 Uiso 1 1 calc R . .
H11C H 0.4326 0.6594 1.1158 0.139 Uiso 1 1 calc R . .
C12 C 0.4372(5) 0.6625(4) 0.9025(9) 0.091(3) Uani 1 1 d . . .
H12A H 0.4706 0.6965 0.9340 0.136 Uiso 1 1 calc R . .
H12B H 0.4058 0.6710 0.8902 0.136 Uiso 1 1 calc R . .
H12C H 0.4490 0.6532 0.8357 0.136 Uiso 1 1 calc R . .
C13 C 0.5129(3) 0.4936(3) 0.8360(9) 0.069(2) Uani 1 1 d . . .
H13 H 0.4736 0.4702 0.8032 0.083 Uiso 1 1 calc R . .
C14 C 0.5571(4) 0.5295(4) 0.7436(10) 0.087(3) Uani 1 1 d . . .
H14A H 0.5466 0.5571 0.7140 0.130 Uiso 1 1 calc R . .
H14B H 0.5549 0.5026 0.6887 0.130 Uiso 1 1 calc R . .
H14C H 0.5968 0.5508 0.7715 0.130 Uiso 1 1 calc R . .
C15 C 0.5277(4) 0.4496(5) 0.8874(12) 0.109(4) Uani 1 1 d . . .
H15A H 0.5687 0.4699 0.9087 0.164 Uiso 1 1 calc R . .
H15B H 0.5208 0.4190 0.8369 0.164 Uiso 1 1 calc R . .
H15C H 0.5030 0.4322 0.9492 0.164 Uiso 1 1 calc R . .
C16 C 0.2634(3) 0.4405(3) 0.7607(5) 0.0438(14) Uani 1 1 d . . .
C17 C 0.2298(3) 0.4702(3) 0.7732(5) 0.0486(16) Uani 1 1 d . . .
C18 C 0.1695(3) 0.4358(4) 0.7616(6) 0.064(2) Uani 1 1 d . . .
H18 H 0.1462 0.4536 0.7684 0.077 Uiso 1 1 calc R . .
C19 C 0.1414(3) 0.3748(5) 0.7400(7) 0.076(3) Uani 1 1 d . . .
H19 H 0.1003 0.3524 0.7336 0.092 Uiso 1 1 calc R . .
C20 C 0.1755(3) 0.3487(4) 0.7284(7) 0.067(2) Uani 1 1 d . . .
H20 H 0.1569 0.3082 0.7138 0.080 Uiso 1 1 calc R . .
C21 C 0.2381(3) 0.3810(3) 0.7378(5) 0.0521(17) Uani 1 1 d . . .
C22 C 0.2582(3) 0.5360(3) 0.7906(6) 0.0581(19) Uani 1 1 d . . .
H22 H 0.2993 0.5507 0.8131 0.070 Uiso 1 1 calc R . .
C23 C 0.2595(4) 0.5681(4) 0.6866(8) 0.082(3) Uani 1 1 d . . .
H23A H 0.2865 0.5659 0.6368 0.123 Uiso 1 1 calc R . .
H23B H 0.2724 0.6090 0.7019 0.123 Uiso 1 1 calc R . .
H23C H 0.2204 0.5495 0.6560 0.123 Uiso 1 1 calc R . .
C24 C 0.2265(5) 0.5513(5) 0.8802(7) 0.083(3) Uani 1 1 d . . .
H24A H 0.1848 0.5327 0.8647 0.124 Uiso 1 1 calc R . .
H24B H 0.2431 0.5936 0.8835 0.124 Uiso 1 1 calc R . .
H24C H 0.2322 0.5372 0.9478 0.124 Uiso 1 1 calc R . .
C25 C 0.2734(4) 0.3501(4) 0.7180(7) 0.060(2) Uani 1 1 d . . .
H25 H 0.3136 0.3763 0.7455 0.072 Uiso 1 1 calc R . .
C26 C 0.2489(5) 0.2913(4) 0.7767(9) 0.099(3) Uani 1 1 d . . .
H26A H 0.2392 0.2958 0.8490 0.149 Uiso 1 1 calc R . .
H26B H 0.2782 0.2791 0.7772 0.149 Uiso 1 1 calc R . .
H26C H 0.2137 0.2617 0.7410 0.149 Uiso 1 1 calc R . .
C27 C 0.2790(5) 0.3426(5) 0.5977(8) 0.089(3) Uani 1 1 d . . .
H27A H 0.2403 0.3178 0.5676 0.134 Uiso 1 1 calc R . .
H27B H 0.3029 0.3244 0.5864 0.134 Uiso 1 1 calc R . .
H27C H 0.2975 0.3808 0.5635 0.134 Uiso 1 1 calc R . .
C28 C 0.2548(3) 0.3906(4) 1.2856(5) 0.0510(18) Uani 1 1 d . . .
C29 C 0.2888(4) 0.4481(4) 1.3218(7) 0.069(2) Uani 1 1 d . . .
H29 H 0.3241 0.4742 1.2871 0.082 Uiso 1 1 calc R . .
C30 C 0.2705(6) 0.4665(6) 1.4092(7) 0.088(3) Uani 1 1 d . . .
H30 H 0.2939 0.5055 1.4328 0.106 Uiso 1 1 calc R . .
C31 C 0.2200(6) 0.4304(7) 1.4622(7) 0.100(4) Uani 1 1 d . . .
H31 H 0.2087 0.4447 1.5207 0.120 Uiso 1 1 calc R . .
C32 C 0.1849(5) 0.3722(6) 1.4296(7) 0.088(3) Uani 1 1 d . . .
H32 H 0.1502 0.3470 1.4665 0.105 Uiso 1 1 calc R . .
C33 C 0.2022(4) 0.3512(5) 1.3393(7) 0.077(3) Uani 1 1 d . . .
H33 H 0.1791 0.3121 1.3163 0.093 Uiso 1 1 calc R . .
C34 C 0.3262(3) 0.3190(3) 1.2282(5) 0.0454(15) Uani 1 1 d . . .
C35 C 0.3164(4) 0.3051(4) 1.3342(6) 0.075(2) Uani 1 1 d . . .
H35 H 0.2888 0.3108 1.3721 0.090 Uiso 1 1 calc R . .
C36 C 0.3488(5) 0.2819(5) 1.3853(7) 0.090(3) Uani 1 1 d . . .
H36 H 0.3437 0.2737 1.4583 0.108 Uiso 1 1 calc R . .
C37 C 0.3872(4) 0.2715(4) 1.3297(9) 0.078(2) Uani 1 1 d . . .
H37 H 0.4079 0.2558 1.3646 0.094 Uiso 1 1 calc R . .
C38 C 0.3960(4) 0.2838(4) 1.2227(8) 0.078(3) Uani 1 1 d . . .
H38 H 0.4227 0.2768 1.1848 0.094 Uiso 1 1 calc R . .
C39 C 0.3650(4) 0.3067(4) 1.1716(7) 0.074(3) Uani 1 1 d . . .
H39 H 0.3700 0.3141 1.0984 0.089 Uiso 1 1 calc R . .
C40 C 0.2022(2) 0.2888(3) 1.1025(5) 0.070(2) Uani 1 1 d GU . .
C41 C 0.1812(4) 0.2319(3) 1.1430(7) 0.142(4) Uani 1 1 d GU . .
H41 H 0.2031 0.2251 1.1941 0.171 Uiso 1 1 calc R . .
C42 C 0.1274(4) 0.1852(3) 1.1070(10) 0.164(5) Uani 1 1 d GU . .
H42 H 0.1133 0.1471 1.1340 0.196 Uiso 1 1 calc R . .
C43 C 0.0946(3) 0.1954(3) 1.0305(9) 0.178(7) Uani 1 1 d GU . .
H43 H 0.0586 0.1641 1.0064 0.213 Uiso 1 1 calc R . .
C44 C 0.1156(3) 0.2523(4) 0.9900(7) 0.132(5) Uani 1 1 d GU . .
H44 H 0.0937 0.2591 0.9389 0.158 Uiso 1 1 calc R . .
C45 C 0.1694(3) 0.2990(3) 1.0261(6) 0.089(3) Uani 1 1 d GU . .
H45 H 0.1835 0.3371 0.9990 0.106 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 C1 2.021(6) . ?
Pd1 Cl1 2.2869(17) . ?
Pd1 Cl2 2.2982(17) . ?
Pd1 Sb1 2.5849(7) . ?
N1 C1 1.317(8) . ?
N1 C4 1.441(8) . ?
N1 C2 1.478(8) . ?
N2 C1 1.329(7) . ?
N2 C16 1.457(8) . ?
N2 C3 1.465(8) . ?
Sb1 C34 2.139(6) . ?
Sb1 C28 2.141(7) . ?
C2 C3 1.521(10) . ?
C4 C5 1.403(10) . ?
C4 C9 1.410(10) . ?
C5 C6 1.379(11) . ?
C5 C10 1.524(11) . ?
C6 C7 1.331(14) . ?
C7 C8 1.359(15) . ?
C8 C9 1.434(12) . ?
C9 C13 1.486(13) . ?
C10 C11 1.530(12) . ?
C10 C12 1.548(12) . ?
C13 C15 1.517(11) . ?
C13 C14 1.565(12) . ?
C16 C21 1.376(10) . ?
C16 C17 1.433(9) . ?
C17 C18 1.369(10) . ?
C17 C22 1.500(10) . ?
C18 C19 1.402(13) . ?
C19 C20 1.365(12) . ?
C20 C21 1.412(10) . ?
C21 C25 1.510(10) . ?
C22 C23 1.534(11) . ?
C22 C24 1.554(10) . ?
C25 C26 1.519(13) . ?
C25 C27 1.532(11) . ?
C28 C29 1.377(11) . ?
C28 C33 1.403(11) . ?
C29 C30 1.369(12) . ?
C30 C31 1.346(16) . ?
C31 C32 1.380(16) . ?
C32 C33 1.419(13) . ?
C34 C35 1.362(10) . ?
C34 C39 1.393(10) . ?
C35 C36 1.410(11) . ?
C36 C37 1.349(13) . ?
C37 C38 1.367(13) . ?
C38 C39 1.373(11) . ?
C40 C41 1.3900 . ?
C40 C45 1.3900 . ?
C40 Sb1 2.098(5) . ?
C41 C42 1.3900 . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C44 C45 1.3900 . ?

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 Pd1 Cl1 94.30(16) . . ?
C1 Pd1 Cl2 87.72(16) . . ?
Cl1 Pd1 Cl2 176.60(7) . . ?
C1 Pd1 Sb1 174.54(18) . . ?
Cl1 Pd1 Sb1 87.17(5) . . ?
Cl2 Pd1 Sb1 90.57(5) . . ?
C1 N1 C4 124.3(5) . . ?
C1 N1 C2 112.7(5) . . ?
C4 N1 C2 122.0(5) . . ?
C1 N2 C16 126.8(5) . . ?
C1 N2 C3 112.8(5) . . ?
C16 N2 C3 120.4(5) . . ?
C40 Sb1 C34 102.7(3) . . ?
C40 Sb1 C28 99.6(3) . . ?
C34 Sb1 C28 100.8(2) . . ?
C40 Sb1 Pd1 108.86(19) . . ?
C34 Sb1 Pd1 123.52(18) . . ?
C28 Sb1 Pd1 117.97(19) . . ?
N1 C1 N2 109.4(5) . . ?
N1 C1 Pd1 125.3(4) . . ?
N2 C1 Pd1 124.7(4) . . ?
N1 C2 C3 102.4(5) . . ?
N2 C3 C2 102.7(5) . . ?
C5 C4 C9 122.7(6) . . ?
C5 C4 N1 119.3(6) . . ?
C9 C4 N1 117.7(6) . . ?
C6 C5 C4 116.0(7) . . ?
C6 C5 C10 122.1(8) . . ?
C4 C5 C10 121.9(7) . . ?
C7 C6 C5 125.3(10) . . ?
C6 C7 C8 117.9(9) . . ?
C7 C8 C9 123.4(8) . . ?
C4 C9 C8 114.5(8) . . ?
C4 C9 C13 124.8(7) . . ?
C8 C9 C13 120.8(7) . . ?
C5 C10 C11 113.9(8) . . ?
C5 C10 C12 108.7(7) . . ?
C11 C10 C12 109.9(7) . . ?
C9 C13 C15 113.6(9) . . ?
C9 C13 C14 110.6(7) . . ?
C15 C13 C14 112.0(8) . . ?
C21 C16 C17 123.4(6) . . ?
C21 C16 N2 119.1(6) . . ?
C17 C16 N2 117.5(6) . . ?
C18 C17 C16 116.3(7) . . ?
C18 C17 C22 120.6(7) . . ?
C16 C17 C22 122.9(6) . . ?
C17 C18 C19 122.4(7) . . ?
C20 C19 C18 118.9(7) . . ?
C19 C20 C21 122.4(8) . . ?
C16 C21 C20 116.5(7) . . ?
C16 C21 C25 123.8(6) . . ?
C20 C21 C25 119.7(7) . . ?
C17 C22 C23 111.2(6) . . ?
C17 C22 C24 112.0(7) . . ?
C23 C22 C24 109.9(7) . . ?
C21 C25 C26 113.3(7) . . ?
C21 C25 C27 110.5(7) . . ?
C26 C25 C27 111.3(9) . . ?
C29 C28 C33 119.8(7) . . ?
C29 C28 Sb1 119.8(6) . . ?
C33 C28 Sb1 120.3(6) . . ?
C30 C29 C28 119.6(10) . . ?
C31 C30 C29 122.4(11) . . ?
C30 C31 C32 119.9(9) . . ?
C31 C32 C33 119.6(9) . . ?
C28 C33 C32 118.6(10) . . ?
C35 C34 C39 119.6(6) . . ?
C35 C34 Sb1 120.1(5) . . ?
C39 C34 Sb1 120.3(5) . . ?
C34 C35 C36 118.7(7) . . ?
C37 C36 C35 120.8(8) . . ?
C36 C37 C38 120.6(7) . . ?
C37 C38 C39 119.3(8) . . ?
C38 C39 C34 120.8(7) . . ?
C41 C40 C45 120.0 . . ?
C41 C40 Sb1 122.2(4) . . ?
C45 C40 Sb1 117.8(4) . . ?
C42 C41 C40 120.0 . . ?
C41 C42 C43 120.0 . . ?
C44 C43 C42 120.0 . . ?
C43 C44 C45 120.0 . . ?
C44 C45 C40 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.083
######################################################END                                                                     
_database_code_depnum_ccdc_archive 'CCDC 1003804'
