# Electronic Supplementary MAterial for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Michael Mastalerz'
_publ_contact_author_email       MICHAEL.MASTALERZ@UNI-ULM.DE

_publ_section_title              
;
Structural Diversity of Pyridoxycalix[4]arene
Palladium(II)-Complexes in the Crystalline State
;
loop_
_publ_author_name
'Michael Mastalerz'
'Gerald Dyker'
'Wiebke Huggenberg'
'Klaus Merz'
'Iris M. Oppel'
'Hebert Jesus Estevez Rivera'

# Attachment '2b_revised.cif'

data_md1291t
_database_code_depnum_ccdc_archive 'CCDC 682872'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H38 Cl6 N2 O4 Pd'
_chemical_formula_weight         953.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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                   12.118(3)
_cell_length_b                   23.052(7)
_cell_length_c                   14.590(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.792(13)
_cell_angle_gamma                90.00
_cell_volume                     4061.6(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1936
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8410
_exptl_absorpt_correction_T_max  0.9157
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(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 axs CCD 1000'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15016
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.1295
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25.06
_reflns_number_total             5773
_reflns_number_gt                3374
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Siemens, 1996)'
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'

_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)+(0.0389P)²+29.5940P] 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         5773
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1401
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.1639
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd -0.00614(6) 0.16495(3) 0.74197(5) 0.0234(2) Uani 1 1 d . . .
Cl1 Cl 0.0949(2) 0.08339(11) 0.7134(2) 0.0489(8) Uani 1 1 d . . .
N1 N -0.1420(6) 0.1125(3) 0.7431(5) 0.0265(19) Uani 1 1 d . . .
O1 O -0.1574(5) 0.2354(3) 0.5708(5) 0.048(2) Uani 1 1 d . . .
H1B H -0.1884 0.2035 0.5742 0.072 Uiso 1 1 calc R . .
C1 C -0.1691(8) 0.0876(4) 0.8227(7) 0.038(3) Uani 1 1 d . . .
H1A H -0.1265 0.0968 0.8776 0.046 Uiso 1 1 calc R . .
Cl2 Cl -0.1026(2) 0.24404(11) 0.7875(2) 0.0453(7) Uani 1 1 d . . .
N2 N 0.1315(6) 0.2157(3) 0.7402(5) 0.0265(19) Uani 1 1 d . . .
C2 C -0.2544(8) 0.0502(4) 0.8265(7) 0.038(3) Uani 1 1 d . . .
H2A H -0.2699 0.0345 0.8834 0.045 Uiso 1 1 calc R . .
O2 O 0.0245(6) 0.1533(3) 0.5278(5) 0.046(2) Uani 1 1 d . . .
H2B H 0.0509 0.1864 0.5348 0.069 Uiso 1 1 calc R . .
O3 O 0.0592(5) 0.2566(2) 0.6087(4) 0.0262(15) Uani 1 1 d . . .
C3 C -0.3198(8) 0.0347(4) 0.7474(7) 0.031(2) Uani 1 1 d . . .
Cl3 Cl 0.1107(7) -0.0271(3) 0.9235(6) 0.265(5) Uani 1 1 d . . .
O4 O -0.1705(5) 0.1216(3) 0.5896(4) 0.0288(16) Uani 1 1 d . . .
Cl4 Cl 0.3482(7) -0.0272(3) 0.9264(4) 0.209(4) Uani 1 1 d . . .
C4 C -0.2925(7) 0.0592(4) 0.6676(7) 0.027(2) Uani 1 1 d . . .
H4A H -0.3343 0.0503 0.6122 0.033 Uiso 1 1 calc R . .
C5 C -0.2040(7) 0.0971(4) 0.6668(7) 0.024(2) Uani 1 1 d . . .
Cl5 Cl 0.4106(4) 0.0610(3) 0.5021(4) 0.138(2) Uani 1 1 d . . .
C6 C -0.4130(8) -0.0077(5) 0.7527(8) 0.048(3) Uani 1 1 d . . .
H6A H -0.4601 -0.0068 0.6955 0.073 Uiso 1 1 calc R . .
H6B H -0.4561 0.0027 0.8033 0.073 Uiso 1 1 calc R . .
H6C H -0.3830 -0.0464 0.7625 0.073 Uiso 1 1 calc R . .
Cl6 Cl 0.3772(3) 0.11898(19) 0.6681(3) 0.1017(15) Uani 1 1 d . . .
C7 C 0.2124(7) 0.2116(4) 0.8095(7) 0.027(2) Uani 1 1 d . . .
H7A H 0.2018 0.1869 0.8592 0.032 Uiso 1 1 calc R . .
C8 C 0.3085(7) 0.2421(4) 0.8101(6) 0.027(2) Uani 1 1 d . . .
H8A H 0.3625 0.2383 0.8598 0.033 Uiso 1 1 calc R . .
C9 C 0.3273(7) 0.2788(4) 0.7373(7) 0.030(2) Uani 1 1 d . . .
C10 C 0.2437(7) 0.2845(4) 0.6668(7) 0.029(2) Uani 1 1 d . . .
H10A H 0.2524 0.3093 0.6169 0.035 Uiso 1 1 calc R . .
C11 C 0.1472(7) 0.2529(4) 0.6714(6) 0.025(2) Uani 1 1 d . . .
C12 C 0.4345(8) 0.3111(4) 0.7344(7) 0.039(3) Uani 1 1 d . . .
H12A H 0.4253 0.3421 0.6896 0.059 Uiso 1 1 calc R . .
H12B H 0.4915 0.2846 0.7172 0.059 Uiso 1 1 calc R . .
H12C H 0.4561 0.3273 0.7946 0.059 Uiso 1 1 calc R . .
C13 C -0.2334(4) 0.1200(3) 0.5059(3) 0.025(2) Uani 1 1 d G . .
C14 C -0.3284(5) 0.1532(2) 0.4874(4) 0.028(2) Uani 1 1 d G . .
C15 C -0.3846(4) 0.1519(2) 0.4005(4) 0.036(3) Uani 1 1 d G . .
H15A H -0.4489 0.1743 0.3880 0.044 Uiso 1 1 calc R . .
C16 C -0.3459(5) 0.1174(3) 0.3319(3) 0.039(3) Uani 1 1 d G . .
H16A H -0.3839 0.1165 0.2731 0.047 Uiso 1 1 calc R . .
C17 C -0.2509(5) 0.0842(2) 0.3503(4) 0.038(3) Uani 1 1 d G . .
H17A H -0.2247 0.0609 0.3040 0.046 Uiso 1 1 calc R . .
C18 C -0.1946(4) 0.0855(2) 0.4373(4) 0.028(2) Uani 1 1 d G . .
C19 C -0.0858(7) 0.0516(4) 0.4522(7) 0.034(3) Uani 1 1 d . . .
H19A H -0.0973 0.0128 0.4258 0.041 Uiso 1 1 calc R . .
H19B H -0.0673 0.0470 0.5184 0.041 Uiso 1 1 calc R . .
C20 C 0.0136(4) 0.0800(2) 0.4098(4) 0.029(2) Uani 1 1 d G . .
C21 C 0.0541(5) 0.0584(2) 0.3302(4) 0.039(3) Uani 1 1 d G . .
H21A H 0.0219 0.0253 0.3015 0.047 Uiso 1 1 calc R . .
C22 C 0.1423(5) 0.0859(3) 0.2930(4) 0.046(3) Uani 1 1 d G . .
H22A H 0.1697 0.0713 0.2392 0.055 Uiso 1 1 calc R . .
C23 C 0.1899(4) 0.1349(3) 0.3355(5) 0.038(3) Uani 1 1 d G . .
H23A H 0.2495 0.1535 0.3104 0.046 Uiso 1 1 calc R . .
C24 C 0.1493(5) 0.1564(2) 0.4151(4) 0.029(2) Uani 1 1 d G . .
C25 C 0.0612(5) 0.1290(3) 0.4522(4) 0.028(2) Uani 1 1 d G . .
C26 C 0.2018(7) 0.2084(4) 0.4681(7) 0.032(2) Uani 1 1 d . . .
H26A H 0.2749 0.2160 0.4465 0.038 Uiso 1 1 calc R . .
H26B H 0.2126 0.1985 0.5336 0.038 Uiso 1 1 calc R . .
C27 C 0.1305(5) 0.2645(2) 0.4567(5) 0.030(2) Uani 1 1 d G . .
C28 C 0.1275(5) 0.2927(3) 0.3723(4) 0.038(3) Uani 1 1 d G . .
H28A H 0.1718 0.2794 0.3267 0.046 Uiso 1 1 calc R . .
C29 C 0.0592(5) 0.3406(3) 0.3554(4) 0.042(3) Uani 1 1 d G . .
H29A H 0.0573 0.3597 0.2983 0.051 Uiso 1 1 calc R . .
C30 C -0.0061(5) 0.3603(2) 0.4228(5) 0.039(3) Uani 1 1 d G . .
H30A H -0.0523 0.3927 0.4114 0.047 Uiso 1 1 calc R . .
C31 C -0.0032(5) 0.3321(3) 0.5072(4) 0.034(2) Uani 1 1 d G . .
C32 C 0.0651(5) 0.2842(3) 0.5241(4) 0.029(2) Uani 1 1 d G . .
C33 C -0.0817(8) 0.3536(4) 0.5767(8) 0.049(3) Uani 1 1 d . . .
H33A H -0.0784 0.3961 0.5789 0.058 Uiso 1 1 calc R . .
H33B H -0.0553 0.3392 0.6378 0.058 Uiso 1 1 calc R . .
C34 C -0.2047(4) 0.3349(3) 0.5556(5) 0.033(2) Uani 1 1 d G . .
C35 C -0.2863(6) 0.3764(2) 0.5357(5) 0.044(3) Uani 1 1 d G . .
H35A H -0.2672 0.4159 0.5338 0.052 Uiso 1 1 calc R . .
C36 C -0.3963(5) 0.3596(3) 0.5186(5) 0.051(3) Uani 1 1 d G . .
H36A H -0.4515 0.3876 0.5052 0.061 Uiso 1 1 calc R . .
C37 C -0.4245(4) 0.3012(3) 0.5215(5) 0.047(3) Uani 1 1 d G . .
H37A H -0.4989 0.2898 0.5099 0.057 Uiso 1 1 calc R . .
C38 C -0.3428(5) 0.2597(2) 0.5414(5) 0.035(3) Uani 1 1 d G . .
C39 C -0.2329(4) 0.2765(2) 0.5585(5) 0.033(3) Uani 1 1 d G . .
C40 C -0.3698(8) 0.1960(4) 0.5585(7) 0.035(3) Uani 1 1 d . . .
H40A H -0.4503 0.1920 0.5586 0.041 Uiso 1 1 calc R . .
H40B H -0.3371 0.1852 0.6198 0.041 Uiso 1 1 calc R . .
C41 C 0.225(2) -0.0008(9) 0.8776(11) 0.174(11) Uani 1 1 d . . .
H41A H 0.2251 0.0415 0.8836 0.209 Uiso 1 1 calc R . .
H41B H 0.2191 -0.0100 0.8118 0.209 Uiso 1 1 calc R . .
C42 C 0.3220(9) 0.0721(5) 0.5844(8) 0.062(4) Uani 1 1 d . . .
H42A H 0.3053 0.0349 0.6127 0.074 Uiso 1 1 calc R . .
H42B H 0.2524 0.0882 0.5560 0.074 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 N2 2.038(7) . ?
Pd1 N1 2.044(7) . ?
Pd1 Cl2 2.293(3) . ?
Pd1 Cl1 2.301(3) . ?
N1 C5 1.338(11) . ?
N1 C1 1.360(12) . ?
O1 C39 1.320(7) . ?
C1 C2 1.351(13) . ?
N2 C11 1.347(11) . ?
N2 C7 1.351(11) . ?
C2 C3 1.390(13) . ?
O2 C25 1.346(8) . ?
O3 C11 1.349(10) . ?
O3 C32 1.396(7) . ?
C3 C4 1.360(12) . ?
C3 C6 1.500(12) . ?
Cl3 C41 1.70(3) . ?
O4 C5 1.352(10) . ?
O4 C13 1.386(7) . ?
Cl4 C41 1.71(2) . ?
C4 C5 1.384(12) . ?
Cl5 C42 1.696(12) . ?
Cl6 C42 1.723(12) . ?
C7 C8 1.360(12) . ?
C8 C9 1.391(13) . ?
C9 C10 1.388(12) . ?
C9 C12 1.501(12) . ?
C10 C11 1.383(12) . ?
C13 C14 1.3900 . ?
C13 C18 1.3900 . ?
C14 C15 1.3900 . ?
C14 C40 1.546(10) . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.532(10) . ?
C19 C20 1.545(10) . ?
C20 C21 1.3900 . ?
C20 C25 1.3900 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C23 C24 1.3900 . ?
C24 C25 1.3900 . ?
C24 C26 1.535(10) . ?
C26 C27 1.557(10) . ?
C27 C28 1.3900 . ?
C27 C32 1.3900 . ?
C28 C29 1.3900 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 C32 1.3900 . ?
C31 C33 1.530(12) . ?
C33 C34 1.558(11) . ?
C34 C35 1.3900 . ?
C34 C39 1.3900 . ?
C35 C36 1.3900 . ?
C36 C37 1.3900 . ?
C37 C38 1.3900 . ?
C38 C39 1.3900 . ?
C38 C40 1.528(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Pd1 N1 178.7(3) . . ?
N2 Pd1 Cl2 89.1(2) . . ?
N1 Pd1 Cl2 92.2(2) . . ?
N2 Pd1 Cl1 91.0(2) . . ?
N1 Pd1 Cl1 87.7(2) . . ?
Cl2 Pd1 Cl1 173.62(11) . . ?
C5 N1 C1 116.1(8) . . ?
C5 N1 Pd1 123.2(6) . . ?
C1 N1 Pd1 120.6(7) . . ?
C2 C1 N1 122.9(10) . . ?
C11 N2 C7 117.5(8) . . ?
C11 N2 Pd1 122.8(6) . . ?
C7 N2 Pd1 119.6(6) . . ?
C1 C2 C3 121.1(10) . . ?
C11 O3 C32 122.2(6) . . ?
C4 C3 C2 116.1(9) . . ?
C4 C3 C6 123.5(10) . . ?
C2 C3 C6 120.4(9) . . ?
C5 O4 C13 122.8(6) . . ?
C3 C4 C5 120.9(9) . . ?
N1 C5 O4 113.2(8) . . ?
N1 C5 C4 122.8(9) . . ?
O4 C5 C4 123.9(9) . . ?
N2 C7 C8 122.5(9) . . ?
C7 C8 C9 120.3(9) . . ?
C10 C9 C8 117.8(8) . . ?
C10 C9 C12 120.9(9) . . ?
C8 C9 C12 121.3(9) . . ?
C11 C10 C9 118.9(9) . . ?
N2 C11 O3 113.1(8) . . ?
N2 C11 C10 123.0(9) . . ?
O3 C11 C10 123.9(8) . . ?
O4 C13 C14 122.8(5) . . ?
O4 C13 C18 117.1(5) . . ?
C14 C13 C18 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C40 122.2(5) . . ?
C15 C14 C40 117.6(5) . . ?
C14 C15 C16 120.0 . . ?
C17 C16 C15 120.0 . . ?
C16 C17 C18 120.0 . . ?
C17 C18 C13 120.0 . . ?
C17 C18 C19 118.0(5) . . ?
C13 C18 C19 121.9(5) . . ?
C18 C19 C20 114.7(6) . . ?
C21 C20 C25 120.0 . . ?
C21 C20 C19 121.7(6) . . ?
C25 C20 C19 118.3(6) . . ?
C20 C21 C22 120.0 . . ?
C21 C22 C23 120.0 . . ?
C24 C23 C22 120.0 . . ?
C23 C24 C25 120.0 . . ?
C23 C24 C26 122.6(6) . . ?
C25 C24 C26 117.3(6) . . ?
O2 C25 C24 116.6(5) . . ?
O2 C25 C20 123.4(5) . . ?
C24 C25 C20 120.0 . . ?
C24 C26 C27 113.0(6) . . ?
C28 C27 C32 120.0 . . ?
C28 C27 C26 117.2(6) . . ?
C32 C27 C26 122.7(6) . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C30 120.0 . . ?
C31 C30 C29 120.0 . . ?
C30 C31 C32 120.0 . . ?
C30 C31 C33 117.7(6) . . ?
C32 C31 C33 122.3(6) . . ?
C31 C32 C27 120.0 . . ?
C31 C32 O3 116.5(5) . . ?
C27 C32 O3 123.5(5) . . ?
C31 C33 C34 114.6(8) . . ?
C35 C34 C39 120.0 . . ?
C35 C34 C33 120.2(6) . . ?
C39 C34 C33 119.8(6) . . ?
C36 C35 C34 120.0 . . ?
C35 C36 C37 120.0 . . ?
C36 C37 C38 120.0 . . ?
C37 C38 C39 120.0 . . ?
C37 C38 C40 122.5(5) . . ?
C39 C38 C40 117.0(5) . . ?
O1 C39 C38 117.8(5) . . ?
O1 C39 C34 122.0(5) . . ?
C38 C39 C34 120.0 . . ?
C38 C40 C14 114.7(7) . . ?
Cl3 C41 Cl4 114.9(12) . . ?
Cl5 C42 Cl6 111.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.801
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.801
_refine_diff_density_max         0.996
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.120


# Attachment '3b.CIF'

data_p21c
_database_code_depnum_ccdc_archive 'CCDC 682873'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H33.50 Cl2 N2 O4.75 Pd'
_chemical_formula_weight         783.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   19.4585(18)
_cell_length_b                   20.414(2)
_cell_length_c                   17.2783(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.127(8)
_cell_angle_gamma                90.00
_cell_volume                     6853.3(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    7395
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.045
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3196
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      113(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  '560 frames in ω and 30 sec'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56369
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_sigmaI/netI    0.1323
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         25.00
_reflns_number_total             12041
_reflns_number_gt                6469
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD Oxford diffraction'
_computing_cell_refinement       'CrysAlis RED Oxford diffraction'
_computing_data_reduction        'CrysAlis RED Oxford diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97

_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)+(0.0485P)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         12041
_refine_ls_number_parameters     886
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1210
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_restrained_S_all      0.916
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

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 0.31569(3) 0.62949(2) 0.84951(3) 0.02469(13) Uani 1 1 d . . .
Cl11 Cl 0.23067(10) 0.55216(8) 0.86327(11) 0.0465(5) Uani 1 1 d . . .
Cl12 Cl 0.40766(8) 0.70009(7) 0.85138(9) 0.0338(4) Uani 1 1 d . . .
O11 O 0.3673(2) 0.61873(16) 0.6878(2) 0.0257(10) Uani 1 1 d . . .
O12 O 0.2320(2) 0.6055(2) 0.6894(2) 0.0435(12) Uani 1 1 d . . .
H12 H 0.2131 0.6295 0.7216 0.065 Uiso 1 1 calc R . .
O13 O 0.1999(2) 0.71311(18) 0.7814(2) 0.0329(11) Uani 1 1 d . . .
O14 O 0.3147(2) 0.74122(19) 0.7099(3) 0.0430(12) Uani 1 1 d . . .
H14 H 0.3395 0.7083 0.7027 0.064 Uiso 1 1 calc R . .
N11 N 0.3793(2) 0.5641(2) 0.8002(3) 0.0244(12) Uani 1 1 d . . .
N12 N 0.2550(2) 0.6989(2) 0.8980(3) 0.0248(12) Uani 1 1 d . . .
C101 C 0.4072(3) 0.6777(3) 0.5790(4) 0.0310(16) Uani 1 1 d . . .
C102 C 0.4424(4) 0.7284(3) 0.6315(4) 0.0348(17) Uani 1 1 d . . .
H10A H 0.4886 0.7380 0.6130 0.042 Uiso 1 1 calc R . .
H10B H 0.4484 0.7106 0.6847 0.042 Uiso 1 1 calc R . .
C103 C 0.4007(4) 0.7917(3) 0.6330(4) 0.0369(17) Uani 1 1 d . . .
C104 C 0.4176(4) 0.8477(3) 0.5918(4) 0.050(2) Uani 1 1 d . . .
H104 H 0.4565 0.8469 0.5608 0.060 Uiso 1 1 calc R . .
C105 C 0.3799(5) 0.9032(3) 0.5950(5) 0.054(2) Uani 1 1 d . . .
H105 H 0.3925 0.9405 0.5661 0.065 Uiso 1 1 calc R . .
C106 C 0.3225(5) 0.9066(3) 0.6402(5) 0.056(2) Uani 1 1 d . . .
H106 H 0.2970 0.9461 0.6427 0.067 Uiso 1 1 calc R . .
C107 C 0.3028(4) 0.8516(3) 0.6817(4) 0.0391(18) Uani 1 1 d . . .
C108 C 0.2443(4) 0.8506(3) 0.7359(4) 0.044(2) Uani 1 1 d . . .
H10C H 0.2306 0.8962 0.7468 0.053 Uiso 1 1 calc R . .
H10D H 0.2608 0.8304 0.7856 0.053 Uiso 1 1 calc R . .
C109 C 0.1815(3) 0.8130(3) 0.7033(4) 0.0370(18) Uani 1 1 d . . .
C110 C 0.1419(4) 0.8430(3) 0.6437(4) 0.052(2) Uani 1 1 d . . .
H110 H 0.1539 0.8859 0.6276 0.063 Uiso 1 1 calc R . .
C111 C 0.0859(4) 0.8121(3) 0.6073(4) 0.052(2) Uani 1 1 d . . .
H111 H 0.0588 0.8342 0.5680 0.062 Uiso 1 1 calc R . .
C112 C 0.0698(3) 0.7499(3) 0.6280(4) 0.0418(19) Uani 1 1 d . . .
H112 H 0.0318 0.7287 0.6018 0.050 Uiso 1 1 calc R . .
C113 C 0.1074(3) 0.7163(3) 0.6864(4) 0.0330(16) Uani 1 1 d . . .
C114 C 0.0904(3) 0.6451(3) 0.7006(4) 0.0330(16) Uani 1 1 d . . .
H11A H 0.0399 0.6401 0.7033 0.040 Uiso 1 1 calc R . .
H11B H 0.1123 0.6310 0.7509 0.040 Uiso 1 1 calc R . .
C115 C 0.1156(3) 0.6017(3) 0.6362(4) 0.0313(16) Uani 1 1 d . . .
C116 C 0.0709(4) 0.5788(3) 0.5757(4) 0.0397(18) Uani 1 1 d . . .
H116 H 0.0233 0.5897 0.5746 0.048 Uiso 1 1 calc R . .
C117 C 0.0966(4) 0.5398(3) 0.5166(4) 0.0429(18) Uani 1 1 d . . .
H117 H 0.0665 0.5243 0.4755 0.051 Uiso 1 1 calc R . .
C118 C 0.1657(4) 0.5241(3) 0.5186(4) 0.0398(18) Uani 1 1 d . . .
H118 H 0.1825 0.4977 0.4785 0.048 Uiso 1 1 calc R . .
C119 C 0.2110(3) 0.5457(3) 0.5773(4) 0.0293(15) Uani 1 1 d . . .
C120 C 0.2856(3) 0.5277(3) 0.5837(4) 0.0331(16) Uani 1 1 d . . .
H12A H 0.2929 0.4881 0.5521 0.040 Uiso 1 1 calc R . .
H12B H 0.2989 0.5169 0.6384 0.040 Uiso 1 1 calc R . .
C121 C 0.3318(3) 0.5827(3) 0.5569(4) 0.0295(15) Uani 1 1 d . . .
C122 C 0.3346(4) 0.5950(3) 0.4778(4) 0.0395(17) Uani 1 1 d . . .
H122 H 0.3092 0.5675 0.4424 0.047 Uiso 1 1 calc R . .
C123 C 0.3723(4) 0.6449(3) 0.4490(4) 0.0423(18) Uani 1 1 d . . .
H123 H 0.3741 0.6509 0.3947 0.051 Uiso 1 1 calc R . .
C124 C 0.4074(4) 0.6863(3) 0.4997(4) 0.0401(18) Uani 1 1 d . . .
H124 H 0.4325 0.7219 0.4797 0.048 Uiso 1 1 calc R . .
C125 C 0.3705(3) 0.6246(3) 0.6065(3) 0.0281(15) Uani 1 1 d . . .
C126 C 0.1842(3) 0.5847(3) 0.6350(3) 0.0270(15) Uani 1 1 d . . .
C127 C 0.1615(4) 0.7500(3) 0.7244(4) 0.0350(17) Uani 1 1 d . . .
C128 C 0.3417(4) 0.7948(3) 0.6741(4) 0.0364(18) Uani 1 1 d . . .
C129 C 0.4000(3) 0.5705(3) 0.7281(3) 0.0274(15) Uani 1 1 d . . .
C130 C 0.4521(3) 0.5335(3) 0.6998(4) 0.0302(15) Uani 1 1 d . . .
H130 H 0.4647 0.5395 0.6479 0.036 Uiso 1 1 calc R . .
C131 C 0.4862(3) 0.4875(3) 0.7464(4) 0.0328(16) Uani 1 1 d . . .
C132 C 0.4629(4) 0.4797(3) 0.8204(4) 0.0393(18) Uani 1 1 d . . .
H132 H 0.4834 0.4474 0.8538 0.047 Uiso 1 1 calc R . .
C133 C 0.4106(3) 0.5180(3) 0.8461(4) 0.0304(16) Uani 1 1 d . . .
H133 H 0.3961 0.5120 0.8973 0.036 Uiso 1 1 calc R . .
C134 C 0.5462(4) 0.4502(3) 0.7198(5) 0.052(2) Uani 1 1 d . . .
H13A H 0.5888 0.4685 0.7437 0.078 Uiso 1 1 calc R . .
H13B H 0.5472 0.4532 0.6632 0.078 Uiso 1 1 calc R . .
H13C H 0.5421 0.4041 0.7349 0.078 Uiso 1 1 calc R . .
C135 C 0.2075(3) 0.7326(3) 0.8568(3) 0.0269(15) Uani 1 1 d . . .
C136 C 0.1669(3) 0.7800(3) 0.8889(4) 0.0354(17) Uani 1 1 d . . .
H136 H 0.1318 0.8018 0.8582 0.043 Uiso 1 1 calc R . .
C137 C 0.1783(4) 0.7948(3) 0.9654(4) 0.0416(18) Uani 1 1 d . . .
H137 H 0.1525 0.8282 0.9888 0.050 Uiso 1 1 calc R . .
C138 C 0.2288(4) 0.7598(3) 1.0089(4) 0.0408(18) Uani 1 1 d . . .
H138 H 0.2371 0.7686 1.0625 0.049 Uiso 1 1 calc R . .
C139 C 0.2655(3) 0.7132(3) 0.9739(4) 0.0310(16) Uani 1 1 d . . .
H139 H 0.2998 0.6898 1.0038 0.037 Uiso 1 1 calc R . .
O1 O 0.5000 0.5000 0.5000 0.0560(19) Uiso 1 2 d S . .
O2A O 0.0647(7) 0.5393(5) 0.0102(7) 0.093(4) Uani 0.50 1 d P A 1
O2B O 0.0742(6) 0.6409(6) -0.0964(7) 0.092(4) Uani 0.50 1 d P B 2
Pd2 Pd 0.81049(3) 0.59900(2) 0.65032(3) 0.03131(15) Uani 1 1 d . . .
Cl21 Cl 0.90998(9) 0.65340(8) 0.62599(10) 0.0468(5) Uani 1 1 d . . .
Cl22 Cl 0.71596(10) 0.53259(8) 0.66093(11) 0.0492(5) Uani 1 1 d . . .
O21 O 0.8715(2) 0.62338(18) 0.8103(2) 0.0291(10) Uani 1 1 d . . .
O22 O 0.8259(3) 0.7384(2) 0.7357(3) 0.0559(15) Uani 1 1 d . . .
H22 H 0.8526 0.7082 0.7510 0.084 Uiso 1 1 calc R . .
O23 O 0.6991(2) 0.69869(19) 0.6802(2) 0.0343(11) Uani 1 1 d . . .
O24 O 0.7352(2) 0.6207(2) 0.8050(2) 0.0475(13) Uani 1 1 d . . .
H24 H 0.7160 0.6398 0.7665 0.071 Uiso 1 1 calc R . .
N21 N 0.8694(3) 0.5414(2) 0.7227(3) 0.0318(13) Uani 1 1 d . . .
N22 N 0.7555(3) 0.6612(2) 0.5791(3) 0.0320(13) Uani 1 1 d . . .
C201 C 0.8391(3) 0.6104(3) 0.9441(4) 0.0273(15) Uani 1 1 d . . .
C202 C 0.7890(3) 0.5544(3) 0.9269(4) 0.0301(16) Uani 1 1 d . . .
H20A H 0.7993 0.5343 0.8767 0.036 Uiso 1 1 calc R . .
H20B H 0.7962 0.5204 0.9675 0.036 Uiso 1 1 calc R . .
C203 C 0.7143(3) 0.5753(2) 0.9237(4) 0.0265(15) Uani 1 1 d . . .
C204 C 0.6708(4) 0.5650(3) 0.9828(4) 0.0371(17) Uani 1 1 d . . .
H204 H 0.6882 0.5457 1.0298 0.044 Uiso 1 1 calc R . .
C205 C 0.6020(4) 0.5825(3) 0.9748(4) 0.0401(18) Uani 1 1 d . . .
H205 H 0.5727 0.5758 1.0162 0.048 Uiso 1 1 calc R . .
C206 C 0.5768(3) 0.6095(3) 0.9061(4) 0.0368(17) Uani 1 1 d . . .
H206 H 0.5294 0.6207 0.9004 0.044 Uiso 1 1 calc R . .
C207 C 0.6185(3) 0.6207(3) 0.8452(4) 0.0304(15) Uani 1 1 d . . .
C208 C 0.5907(3) 0.6519(3) 0.7689(4) 0.0330(16) Uani 1 1 d . . .
H20C H 0.6093 0.6280 0.7249 0.040 Uiso 1 1 calc R . .
H20D H 0.5399 0.6476 0.7648 0.040 Uiso 1 1 calc R . .
C209 C 0.6098(3) 0.7238(3) 0.7636(4) 0.0311(16) Uani 1 1 d . . .
C210 C 0.5735(4) 0.7680(3) 0.8063(4) 0.0411(18) Uani 1 1 d . . .
H210 H 0.5362 0.7535 0.8350 0.049 Uiso 1 1 calc R . .
C211 C 0.5919(4) 0.8337(3) 0.8071(5) 0.053(2) Uani 1 1 d . . .
H211 H 0.5665 0.8641 0.8358 0.064 Uiso 1 1 calc R . .
C212 C 0.6463(4) 0.8553(3) 0.7668(4) 0.0418(18) Uani 1 1 d . . .
H212 H 0.6582 0.9004 0.7686 0.050 Uiso 1 1 calc R . .
C213 C 0.6842(3) 0.8130(3) 0.7236(4) 0.0304(16) Uani 1 1 d . . .
C214 C 0.7477(3) 0.8409(3) 0.6874(4) 0.0333(16) Uani 1 1 d . . .
H21A H 0.7621 0.8107 0.6465 0.040 Uiso 1 1 calc R . .
H21B H 0.7356 0.8834 0.6626 0.040 Uiso 1 1 calc R . .
C215 C 0.8075(3) 0.8511(3) 0.7461(4) 0.0304(16) Uani 1 1 d . . .
C216 C 0.8252(4) 0.9105(3) 0.7775(4) 0.0373(17) Uani 1 1 d . . .
H216 H 0.7989 0.9482 0.7630 0.045 Uiso 1 1 calc R . .
C217 C 0.8813(4) 0.9162(3) 0.8306(4) 0.0447(19) Uani 1 1 d . . .
H217 H 0.8930 0.9578 0.8523 0.054 Uiso 1 1 calc R . .
C218 C 0.9198(3) 0.8621(3) 0.8518(4) 0.0386(17) Uani 1 1 d . . .
H218 H 0.9574 0.8666 0.8887 0.046 Uiso 1 1 calc R . .
C219 C 0.9048(3) 0.8004(3) 0.8201(4) 0.0274(15) Uani 1 1 d . . .
C220 C 0.9469(3) 0.7400(3) 0.8432(4) 0.0347(16) Uani 1 1 d . . .
H22A H 0.9522 0.7122 0.7970 0.042 Uiso 1 1 calc R . .
H22B H 0.9935 0.7537 0.8630 0.042 Uiso 1 1 calc R . .
C221 C 0.9131(3) 0.7001(3) 0.9053(4) 0.0310(16) Uani 1 1 d . . .
C222 C 0.9163(3) 0.7224(3) 0.9801(4) 0.0344(16) Uani 1 1 d . . .
H222 H 0.9419 0.7609 0.9929 0.041 Uiso 1 1 calc R . .
C223 C 0.8829(3) 0.6899(3) 1.0378(4) 0.0345(17) Uani 1 1 d . . .
H223 H 0.8859 0.7057 1.0895 0.041 Uiso 1 1 calc R . .
C224 C 0.8456(3) 0.6349(3) 1.0192(3) 0.0277(15) Uani 1 1 d . . .
H224 H 0.8232 0.6126 1.0590 0.033 Uiso 1 1 calc R . .
C225 C 0.8758(3) 0.6437(3) 0.8883(3) 0.0260(15) Uani 1 1 d . . .
C226 C 0.8473(3) 0.7964(3) 0.7688(4) 0.0329(16) Uani 1 1 d . . .
C227 C 0.6633(3) 0.7476(3) 0.7203(4) 0.0319(16) Uani 1 1 d . . .
C228 C 0.6872(3) 0.6058(3) 0.8572(4) 0.0296(15) Uani 1 1 d . . .
C229 C 0.8972(3) 0.5644(3) 0.7901(4) 0.0288(15) Uani 1 1 d . . .
C230 C 0.9491(4) 0.5321(3) 0.8323(4) 0.0395(18) Uani 1 1 d . . .
H230 H 0.9675 0.5502 0.8797 0.047 Uiso 1 1 calc R . .
C231 C 0.9740(4) 0.4739(4) 0.8056(4) 0.049(2) Uani 1 1 d . . .
C232 C 0.9429(4) 0.4488(3) 0.7382(4) 0.049(2) Uani 1 1 d . . .
H232 H 0.9567 0.4073 0.7197 0.059 Uiso 1 1 calc R . .
C233 C 0.8927(4) 0.4828(3) 0.6980(4) 0.0429(19) Uani 1 1 d . . .
H233 H 0.8733 0.4650 0.6509 0.051 Uiso 1 1 calc R . .
C234 C 1.0331(5) 0.4408(4) 0.8492(5) 0.082(3) Uani 1 1 d . . .
H23A H 1.0313 0.3936 0.8390 0.124 Uiso 1 1 calc R . .
H23B H 1.0300 0.4486 0.9049 0.124 Uiso 1 1 calc R . .
H23C H 1.0766 0.4586 0.8323 0.124 Uiso 1 1 calc R . .
C235 C 0.7091(3) 0.7035(3) 0.6019(4) 0.0335(16) Uani 1 1 d . . .
C236 C 0.6736(4) 0.7474(3) 0.5530(4) 0.0420(18) Uani 1 1 d . . .
H236 H 0.6402 0.7763 0.5722 0.050 Uiso 1 1 calc R . .
C237 C 0.6878(4) 0.7477(3) 0.4777(4) 0.0460(19) Uani 1 1 d . . .
H237 H 0.6644 0.7771 0.4427 0.055 Uiso 1 1 calc R . .
C238 C 0.7363(4) 0.7054(3) 0.4517(4) 0.0437(19) Uani 1 1 d . . .
H238 H 0.7472 0.7063 0.3988 0.052 Uiso 1 1 calc R . .
C239 C 0.7690(4) 0.6617(3) 0.5017(4) 0.0418(18) Uani 1 1 d . . .
H239 H 0.8012 0.6315 0.4826 0.050 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 N11 2.038(5) . ?
Pd1 N12 2.053(5) . ?
Pd1 Cl12 2.2967(16) . ?
Pd1 Cl11 2.3084(18) . ?
O11 C129 1.346(6) . ?
O11 C125 1.415(7) . ?
O12 C126 1.354(7) . ?
O13 C135 1.364(7) . ?
O13 C127 1.419(7) . ?
O14 C128 1.375(7) . ?
N11 C129 1.337(7) . ?
N11 C133 1.353(7) . ?
N12 C135 1.326(7) . ?
N12 C139 1.349(7) . ?
C101 C124 1.382(8) . ?
C101 C125 1.395(8) . ?
C101 C102 1.515(8) . ?
C102 C103 1.526(9) . ?
C103 C128 1.384(9) . ?
C103 C104 1.397(9) . ?
C104 C105 1.353(10) . ?
C105 C106 1.398(11) . ?
C106 C107 1.397(9) . ?
C107 C128 1.395(9) . ?
C107 C108 1.512(10) . ?
C108 C109 1.526(9) . ?
C109 C110 1.394(9) . ?
C109 C127 1.398(9) . ?
C110 C111 1.381(9) . ?
C111 C112 1.361(8) . ?
C112 C113 1.394(8) . ?
C113 C127 1.391(9) . ?
C113 C114 1.514(8) . ?
C114 C115 1.525(8) . ?
C115 C126 1.381(8) . ?
C115 C116 1.402(9) . ?
C116 C117 1.409(9) . ?
C117 C118 1.380(9) . ?
C118 C119 1.379(8) . ?
C119 C126 1.400(8) . ?
C119 C120 1.495(9) . ?
C120 C121 1.525(8) . ?
C121 C122 1.393(8) . ?
C121 C125 1.401(8) . ?
C122 C123 1.364(9) . ?
C123 C124 1.373(9) . ?
C129 C130 1.376(8) . ?
C130 C131 1.382(8) . ?
C131 C132 1.390(9) . ?
C131 C134 1.488(9) . ?
C132 C133 1.377(8) . ?
C135 C136 1.385(8) . ?
C136 C137 1.362(9) . ?
C137 C138 1.401(9) . ?
C138 C139 1.351(8) . ?
Pd2 N21 2.026(5) . ?
Pd2 N22 2.031(5) . ?
Pd2 Cl21 2.2904(18) . ?
Pd2 Cl22 2.3004(18) . ?
O21 C229 1.357(7) . ?
O21 C225 1.408(7) . ?
O22 C226 1.371(7) . ?
O23 C235 1.381(7) . ?
O23 C227 1.420(7) . ?
O24 C228 1.368(7) . ?
N21 C229 1.341(8) . ?
N21 C233 1.356(7) . ?
N22 C235 1.326(8) . ?
N22 C239 1.377(8) . ?
C201 C224 1.389(8) . ?
C201 C225 1.406(8) . ?
C201 C202 1.522(8) . ?
C202 C203 1.514(8) . ?
C203 C204 1.377(8) . ?
C203 C228 1.386(8) . ?
C204 C205 1.383(9) . ?
C205 C206 1.374(9) . ?
C206 C207 1.382(9) . ?
C207 C228 1.375(8) . ?
C207 C208 1.536(8) . ?
C208 C209 1.518(8) . ?
C209 C210 1.384(9) . ?
C209 C227 1.401(9) . ?
C210 C211 1.387(9) . ?
C211 C212 1.372(9) . ?
C212 C213 1.380(8) . ?
C213 C227 1.396(8) . ?
C213 C214 1.525(8) . ?
C214 C215 1.516(9) . ?
C215 C216 1.364(8) . ?
C215 C226 1.401(8) . ?
C216 C217 1.393(9) . ?
C217 C218 1.374(9) . ?
C218 C219 1.397(8) . ?
C219 C226 1.392(8) . ?
C219 C220 1.522(8) . ?
C220 C221 1.525(8) . ?
C221 C222 1.368(8) . ?
C221 C225 1.386(8) . ?
C222 C223 1.387(8) . ?
C223 C224 1.365(8) . ?
C229 C230 1.380(9) . ?
C230 C231 1.373(8) . ?
C231 C232 1.382(10) . ?
C231 C234 1.500(10) . ?
C232 C233 1.358(9) . ?
C235 C236 1.389(8) . ?
C236 C237 1.345(9) . ?
C237 C238 1.373(10) . ?
C238 C239 1.374(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
N11 Pd1 N12 177.22(19) . . ?
N11 Pd1 Cl12 85.80(14) . . ?
N12 Pd1 Cl12 91.52(14) . . ?
N11 Pd1 Cl11 92.86(14) . . ?
N12 Pd1 Cl11 89.90(14) . . ?
Cl12 Pd1 Cl11 171.89(7) . . ?
C129 O11 C125 122.1(4) . . ?
C135 O13 C127 122.3(4) . . ?
C129 N11 C133 117.8(5) . . ?
C129 N11 Pd1 123.1(4) . . ?
C133 N11 Pd1 118.3(4) . . ?
C135 N12 C139 118.3(5) . . ?
C135 N12 Pd1 122.6(4) . . ?
C139 N12 Pd1 119.1(4) . . ?
C124 C101 C125 117.8(6) . . ?
C124 C101 C102 118.7(6) . . ?
C125 C101 C102 123.4(5) . . ?
C101 C102 C103 111.5(5) . . ?
C128 C103 C104 116.7(6) . . ?
C128 C103 C102 120.3(6) . . ?
C104 C103 C102 123.0(7) . . ?
C105 C104 C103 121.4(8) . . ?
C104 C105 C106 121.0(7) . . ?
C105 C106 C107 119.9(7) . . ?
C128 C107 C106 116.9(8) . . ?
C128 C107 C108 118.6(6) . . ?
C106 C107 C108 124.5(6) . . ?
C107 C108 C109 113.2(6) . . ?
C110 C109 C127 116.6(6) . . ?
C110 C109 C108 116.8(6) . . ?
C127 C109 C108 126.6(6) . . ?
C111 C110 C109 121.7(6) . . ?
C112 C111 C110 119.6(6) . . ?
C111 C112 C113 122.0(6) . . ?
C127 C113 C112 116.9(6) . . ?
C127 C113 C114 124.4(6) . . ?
C112 C113 C114 118.6(6) . . ?
C113 C114 C115 110.9(5) . . ?
C126 C115 C116 117.9(6) . . ?
C126 C115 C114 120.4(6) . . ?
C116 C115 C114 121.7(6) . . ?
C117 C116 C115 119.8(7) . . ?
C118 C117 C116 119.8(7) . . ?
C117 C118 C119 121.8(6) . . ?
C118 C119 C126 117.2(6) . . ?
C118 C119 C120 123.8(6) . . ?
C126 C119 C120 119.0(6) . . ?
C119 C120 C121 112.5(5) . . ?
C122 C121 C125 116.1(6) . . ?
C122 C121 C120 119.1(6) . . ?
C125 C121 C120 124.7(6) . . ?
C123 C122 C121 122.9(6) . . ?
C122 C123 C124 119.1(6) . . ?
C123 C124 C101 121.7(6) . . ?
C101 C125 C121 122.3(6) . . ?
C101 C125 O11 117.1(5) . . ?
C121 C125 O11 120.3(5) . . ?
O12 C126 C115 122.6(5) . . ?
O12 C126 C119 113.9(6) . . ?
C115 C126 C119 123.4(6) . . ?
C113 C127 C109 123.1(6) . . ?
C113 C127 O13 115.0(5) . . ?
C109 C127 O13 121.6(6) . . ?
O14 C128 C103 122.9(6) . . ?
O14 C128 C107 113.3(7) . . ?
C103 C128 C107 123.8(6) . . ?
N11 C129 O11 113.3(5) . . ?
N11 C129 C130 122.9(5) . . ?
O11 C129 C130 123.7(6) . . ?
C129 C130 C131 120.4(6) . . ?
C130 C131 C132 116.3(6) . . ?
C130 C131 C134 121.9(6) . . ?
C132 C131 C134 121.8(6) . . ?
C133 C132 C131 121.1(6) . . ?
N11 C133 C132 121.5(6) . . ?
N12 C135 O13 113.4(5) . . ?
N12 C135 C136 123.0(6) . . ?
O13 C135 C136 123.5(6) . . ?
C137 C136 C135 118.5(6) . . ?
C136 C137 C138 118.6(6) . . ?
C139 C138 C137 119.5(6) . . ?
N12 C139 C138 122.1(6) . . ?
N21 Pd2 N22 176.5(2) . . ?
N21 Pd2 Cl21 86.50(15) . . ?
N22 Pd2 Cl21 90.47(15) . . ?
N21 Pd2 Cl22 92.12(15) . . ?
N22 Pd2 Cl22 91.13(15) . . ?
Cl21 Pd2 Cl22 171.06(7) . . ?
C229 O21 C225 120.2(4) . . ?
C235 O23 C227 121.8(5) . . ?
C229 N21 C233 117.1(6) . . ?
C229 N21 Pd2 121.4(4) . . ?
C233 N21 Pd2 120.3(4) . . ?
C235 N22 C239 116.9(6) . . ?
C235 N22 Pd2 124.9(4) . . ?
C239 N22 Pd2 118.2(4) . . ?
C224 C201 C225 116.3(5) . . ?
C224 C201 C202 118.5(6) . . ?
C225 C201 C202 125.0(5) . . ?
C203 C202 C201 113.6(4) . . ?
C204 C203 C228 117.5(6) . . ?
C204 C203 C202 123.9(6) . . ?
C228 C203 C202 118.6(6) . . ?
C203 C204 C205 121.1(6) . . ?
C206 C205 C204 119.2(6) . . ?
C205 C206 C207 121.8(6) . . ?
C228 C207 C206 117.1(6) . . ?
C228 C207 C208 121.0(6) . . ?
C206 C207 C208 121.9(6) . . ?
C209 C208 C207 112.2(5) . . ?
C210 C209 C227 118.3(6) . . ?
C210 C209 C208 117.7(6) . . ?
C227 C209 C208 124.0(6) . . ?
C209 C210 C211 119.8(7) . . ?
C212 C211 C210 120.7(7) . . ?
C211 C212 C213 121.6(6) . . ?
C212 C213 C227 117.2(6) . . ?
C212 C213 C214 117.1(5) . . ?
C227 C213 C214 125.6(6) . . ?
C215 C214 C213 112.8(5) . . ?
C216 C215 C226 118.3(6) . . ?
C216 C215 C214 123.7(6) . . ?
C226 C215 C214 118.0(5) . . ?
C215 C216 C217 120.6(6) . . ?
C218 C217 C216 120.2(6) . . ?
C217 C218 C219 121.5(6) . . ?
C226 C219 C218 116.4(6) . . ?
C226 C219 C220 121.5(5) . . ?
C218 C219 C220 122.0(6) . . ?
C221 C220 C219 111.7(5) . . ?
C222 C221 C225 118.2(6) . . ?
C222 C221 C220 119.3(6) . . ?
C225 C221 C220 122.4(6) . . ?
C221 C222 C223 121.4(6) . . ?
C224 C223 C222 119.2(6) . . ?
C223 C224 C201 122.4(6) . . ?
C221 C225 C201 122.4(6) . . ?
C221 C225 O21 116.8(5) . . ?
C201 C225 O21 120.6(5) . . ?
O22 C226 C219 122.1(6) . . ?
O22 C226 C215 114.9(6) . . ?
C219 C226 C215 123.0(6) . . ?
C213 C227 C209 122.3(6) . . ?
C213 C227 O23 122.9(6) . . ?
C209 C227 O23 114.5(5) . . ?
O24 C228 C207 123.1(6) . . ?
O24 C228 C203 113.8(6) . . ?
C207 C228 C203 123.1(6) . . ?
N21 C229 O21 113.4(5) . . ?
N21 C229 C230 122.7(6) . . ?
O21 C229 C230 123.8(6) . . ?
C231 C230 C229 119.8(7) . . ?
C230 C231 C232 117.2(7) . . ?
C230 C231 C234 119.7(7) . . ?
C232 C231 C234 123.0(7) . . ?
C233 C232 C231 120.7(7) . . ?
C232 C233 N21 122.2(7) . . ?
N22 C235 O23 112.3(5) . . ?
N22 C235 C236 124.3(6) . . ?
O23 C235 C236 123.4(6) . . ?
C237 C236 C235 118.0(7) . . ?
C236 C237 C238 119.7(7) . . ?
C239 C238 C237 120.4(7) . . ?
C238 C239 N22 120.7(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N12 Pd1 N11 C129 -55(4) . . . . ?
Cl12 Pd1 N11 C129 -70.3(5) . . . . ?
Cl11 Pd1 N11 C129 117.8(5) . . . . ?
N12 Pd1 N11 C133 114(4) . . . . ?
Cl12 Pd1 N11 C133 99.0(4) . . . . ?
Cl11 Pd1 N11 C133 -73.0(4) . . . . ?
N11 Pd1 N12 C135 88(4) . . . . ?
Cl12 Pd1 N12 C135 102.8(5) . . . . ?
Cl11 Pd1 N12 C135 -85.2(5) . . . . ?
N11 Pd1 N12 C139 -89(4) . . . . ?
Cl12 Pd1 N12 C139 -74.1(4) . . . . ?
Cl11 Pd1 N12 C139 97.9(4) . . . . ?
C124 C101 C102 C103 73.1(8) . . . . ?
C125 C101 C102 C103 -102.4(7) . . . . ?
C101 C102 C103 C128 75.1(7) . . . . ?
C101 C102 C103 C104 -102.4(7) . . . . ?
C128 C103 C104 C105 3.1(10) . . . . ?
C102 C103 C104 C105 -179.4(6) . . . . ?
C103 C104 C105 C106 0.3(11) . . . . ?
C104 C105 C106 C107 -1.2(11) . . . . ?
C105 C106 C107 C128 -1.4(10) . . . . ?
C105 C106 C107 C108 176.4(7) . . . . ?
C128 C107 C108 C109 -74.7(8) . . . . ?
C106 C107 C108 C109 107.6(7) . . . . ?
C107 C108 C109 C110 -73.2(8) . . . . ?
C107 C108 C109 C127 103.1(8) . . . . ?
C127 C109 C110 C111 0.1(11) . . . . ?
C108 C109 C110 C111 176.7(7) . . . . ?
C109 C110 C111 C112 -2.3(12) . . . . ?
C110 C111 C112 C113 1.4(12) . . . . ?
C111 C112 C113 C127 1.6(10) . . . . ?
C111 C112 C113 C114 -174.3(6) . . . . ?
C127 C113 C114 C115 -102.4(7) . . . . ?
C112 C113 C114 C115 73.2(8) . . . . ?
C113 C114 C115 C126 78.3(7) . . . . ?
C113 C114 C115 C116 -100.3(7) . . . . ?
C126 C115 C116 C117 0.2(9) . . . . ?
C114 C115 C116 C117 178.9(6) . . . . ?
C115 C116 C117 C118 0.1(10) . . . . ?
C116 C117 C118 C119 -0.1(10) . . . . ?
C117 C118 C119 C126 -0.3(9) . . . . ?
C117 C118 C119 C120 177.4(6) . . . . ?
C118 C119 C120 C121 102.2(7) . . . . ?
C126 C119 C120 C121 -80.1(7) . . . . ?
C119 C120 C121 C122 -74.6(7) . . . . ?
C119 C120 C121 C125 102.5(7) . . . . ?
C125 C121 C122 C123 -0.3(9) . . . . ?
C120 C121 C122 C123 177.1(6) . . . . ?
C121 C122 C123 C124 -2.1(10) . . . . ?
C122 C123 C124 C101 1.9(11) . . . . ?
C125 C101 C124 C123 0.7(10) . . . . ?
C102 C101 C124 C123 -175.2(6) . . . . ?
C124 C101 C125 C121 -3.2(9) . . . . ?
C102 C101 C125 C121 172.5(6) . . . . ?
C124 C101 C125 O11 -176.2(5) . . . . ?
C102 C101 C125 O11 -0.6(9) . . . . ?
C122 C121 C125 C101 2.9(9) . . . . ?
C120 C121 C125 C101 -174.3(6) . . . . ?
C122 C121 C125 O11 175.8(5) . . . . ?
C120 C121 C125 O11 -1.4(9) . . . . ?
C129 O11 C125 C101 -110.7(6) . . . . ?
C129 O11 C125 C121 76.2(7) . . . . ?
C116 C115 C126 O12 178.2(5) . . . . ?
C114 C115 C126 O12 -0.5(9) . . . . ?
C116 C115 C126 C119 -0.6(9) . . . . ?
C114 C115 C126 C119 -179.3(5) . . . . ?
C118 C119 C126 O12 -178.3(5) . . . . ?
C120 C119 C126 O12 3.9(8) . . . . ?
C118 C119 C126 C115 0.6(9) . . . . ?
C120 C119 C126 C115 -177.1(5) . . . . ?
C112 C113 C127 C109 -4.0(10) . . . . ?
C114 C113 C127 C109 171.7(6) . . . . ?
C112 C113 C127 O13 -177.7(6) . . . . ?
C114 C113 C127 O13 -2.1(9) . . . . ?
C110 C109 C127 C113 3.1(10) . . . . ?
C108 C109 C127 C113 -173.1(7) . . . . ?
C110 C109 C127 O13 176.5(6) . . . . ?
C108 C109 C127 O13 0.2(10) . . . . ?
C135 O13 C127 C113 -122.3(6) . . . . ?
C135 O13 C127 C109 63.8(8) . . . . ?
C104 C103 C128 O14 172.4(6) . . . . ?
C102 C103 C128 O14 -5.2(9) . . . . ?
C104 C103 C128 C107 -5.9(10) . . . . ?
C102 C103 C128 C107 176.5(6) . . . . ?
C106 C107 C128 O14 -173.4(5) . . . . ?
C108 C107 C128 O14 8.7(8) . . . . ?
C106 C107 C128 C103 5.1(10) . . . . ?
C108 C107 C128 C103 -172.8(6) . . . . ?
C133 N11 C129 O11 -178.2(5) . . . . ?
Pd1 N11 C129 O11 -8.9(7) . . . . ?
C133 N11 C129 C130 -1.4(9) . . . . ?
Pd1 N11 C129 C130 168.0(4) . . . . ?
C125 O11 C129 N11 -166.2(5) . . . . ?
C125 O11 C129 C130 17.0(9) . . . . ?
N11 C129 C130 C131 -0.6(9) . . . . ?
O11 C129 C130 C131 175.9(6) . . . . ?
C129 C130 C131 C132 2.6(9) . . . . ?
C129 C130 C131 C134 -175.3(6) . . . . ?
C130 C131 C132 C133 -2.7(10) . . . . ?
C134 C131 C132 C133 175.2(6) . . . . ?
C129 N11 C133 C132 1.2(9) . . . . ?
Pd1 N11 C133 C132 -168.6(5) . . . . ?
C131 C132 C133 N11 0.9(10) . . . . ?
C139 N12 C135 O13 -178.5(5) . . . . ?
Pd1 N12 C135 O13 4.6(7) . . . . ?
C139 N12 C135 C136 -2.3(9) . . . . ?
Pd1 N12 C135 C136 -179.2(5) . . . . ?
C127 O13 C135 N12 -168.3(5) . . . . ?
C127 O13 C135 C136 15.5(9) . . . . ?
N12 C135 C136 C137 3.0(10) . . . . ?
O13 C135 C136 C137 178.9(6) . . . . ?
C135 C136 C137 C138 -2.3(10) . . . . ?
C136 C137 C138 C139 1.1(10) . . . . ?
C135 N12 C139 C138 0.9(9) . . . . ?
Pd1 N12 C139 C138 178.0(5) . . . . ?
C137 C138 C139 N12 -0.3(10) . . . . ?
N22 Pd2 N21 C229 42(4) . . . . ?
Cl21 Pd2 N21 C229 70.6(5) . . . . ?
Cl22 Pd2 N21 C229 -118.2(5) . . . . ?
N22 Pd2 N21 C233 -125(3) . . . . ?
Cl21 Pd2 N21 C233 -96.7(5) . . . . ?
Cl22 Pd2 N21 C233 74.5(5) . . . . ?
N21 Pd2 N22 C235 -85(4) . . . . ?
Cl21 Pd2 N22 C235 -113.7(5) . . . . ?
Cl22 Pd2 N22 C235 75.1(5) . . . . ?
N21 Pd2 N22 C239 92(3) . . . . ?
Cl21 Pd2 N22 C239 63.5(4) . . . . ?
Cl22 Pd2 N22 C239 -107.7(4) . . . . ?
C224 C201 C202 C203 74.1(7) . . . . ?
C225 C201 C202 C203 -100.1(7) . . . . ?
C201 C202 C203 C204 -102.2(7) . . . . ?
C201 C202 C203 C228 78.8(7) . . . . ?
C228 C203 C204 C205 2.3(9) . . . . ?
C202 C203 C204 C205 -176.8(5) . . . . ?
C203 C204 C205 C206 1.0(9) . . . . ?
C204 C205 C206 C207 -1.0(10) . . . . ?
C205 C206 C207 C228 -2.3(9) . . . . ?
C205 C206 C207 C208 -178.9(6) . . . . ?
C228 C207 C208 C209 -74.6(7) . . . . ?
C206 C207 C208 C209 101.9(7) . . . . ?
C207 C208 C209 C210 -76.1(7) . . . . ?
C207 C208 C209 C227 101.5(7) . . . . ?
C227 C209 C210 C211 -1.8(10) . . . . ?
C208 C209 C210 C211 176.0(6) . . . . ?
C209 C210 C211 C212 -0.9(11) . . . . ?
C210 C211 C212 C213 0.7(11) . . . . ?
C211 C212 C213 C227 2.3(10) . . . . ?
C211 C212 C213 C214 -174.4(7) . . . . ?
C212 C213 C214 C215 75.2(7) . . . . ?
C227 C213 C214 C215 -101.1(7) . . . . ?
C213 C214 C215 C216 -101.0(7) . . . . ?
C213 C214 C215 C226 79.5(7) . . . . ?
C226 C215 C216 C217 0.0(9) . . . . ?
C214 C215 C216 C217 -179.4(6) . . . . ?
C215 C216 C217 C218 0.3(10) . . . . ?
C216 C217 C218 C219 1.1(10) . . . . ?
C217 C218 C219 C226 -2.7(9) . . . . ?
C217 C218 C219 C220 -179.8(6) . . . . ?
C226 C219 C220 C221 -79.9(7) . . . . ?
C218 C219 C220 C221 97.1(7) . . . . ?
C219 C220 C221 C222 -75.2(7) . . . . ?
C219 C220 C221 C225 101.1(7) . . . . ?
C225 C221 C222 C223 -0.4(9) . . . . ?
C220 C221 C222 C223 176.1(6) . . . . ?
C221 C222 C223 C224 -0.6(10) . . . . ?
C222 C223 C224 C201 -0.7(9) . . . . ?
C225 C201 C224 C223 2.7(8) . . . . ?
C202 C201 C224 C223 -172.0(6) . . . . ?
C222 C221 C225 C201 2.6(9) . . . . ?
C220 C221 C225 C201 -173.8(5) . . . . ?
C222 C221 C225 O21 177.8(5) . . . . ?
C220 C221 C225 O21 1.4(9) . . . . ?
C224 C201 C225 C221 -3.7(9) . . . . ?
C202 C201 C225 C221 170.6(6) . . . . ?
C224 C201 C225 O21 -178.7(5) . . . . ?
C202 C201 C225 O21 -4.4(9) . . . . ?
C229 O21 C225 C221 118.7(6) . . . . ?
C229 O21 C225 C201 -66.1(7) . . . . ?
C218 C219 C226 O22 -177.9(6) . . . . ?
C220 C219 C226 O22 -0.7(9) . . . . ?
C218 C219 C226 C215 3.1(9) . . . . ?
C220 C219 C226 C215 -179.8(6) . . . . ?
C216 C215 C226 O22 179.1(5) . . . . ?
C214 C215 C226 O22 -1.4(8) . . . . ?
C216 C215 C226 C219 -1.8(9) . . . . ?
C214 C215 C226 C219 177.6(6) . . . . ?
C212 C213 C227 C209 -5.1(9) . . . . ?
C214 C213 C227 C209 171.2(6) . . . . ?
C212 C213 C227 O23 -177.8(6) . . . . ?
C214 C213 C227 O23 -1.4(9) . . . . ?
C210 C209 C227 C213 4.9(9) . . . . ?
C208 C209 C227 C213 -172.7(6) . . . . ?
C210 C209 C227 O23 178.1(5) . . . . ?
C208 C209 C227 O23 0.5(9) . . . . ?
C235 O23 C227 C213 -58.7(8) . . . . ?
C235 O23 C227 C209 128.2(6) . . . . ?
C206 C207 C228 O24 -173.0(5) . . . . ?
C208 C207 C228 O24 3.6(9) . . . . ?
C206 C207 C228 C203 5.9(9) . . . . ?
C208 C207 C228 C203 -177.4(5) . . . . ?
C204 C203 C228 O24 173.1(5) . . . . ?
C202 C203 C228 O24 -7.8(7) . . . . ?
C204 C203 C228 C207 -5.9(9) . . . . ?
C202 C203 C228 C207 173.2(5) . . . . ?
C233 N21 C229 O21 179.5(5) . . . . ?
Pd2 N21 C229 O21 11.8(7) . . . . ?
C233 N21 C229 C230 2.4(9) . . . . ?
Pd2 N21 C229 C230 -165.3(5) . . . . ?
C225 O21 C229 N21 157.7(5) . . . . ?
C225 O21 C229 C230 -25.2(9) . . . . ?
N21 C229 C230 C231 -0.3(10) . . . . ?
O21 C229 C230 C231 -177.1(6) . . . . ?
C229 C230 C231 C232 -2.9(11) . . . . ?
C229 C230 C231 C234 176.6(7) . . . . ?
C230 C231 C232 C233 4.0(11) . . . . ?
C234 C231 C232 C233 -175.4(7) . . . . ?
C231 C232 C233 N21 -2.0(12) . . . . ?
C229 N21 C233 C232 -1.2(10) . . . . ?
Pd2 N21 C233 C232 166.6(6) . . . . ?
C239 N22 C235 O23 179.5(5) . . . . ?
Pd2 N22 C235 O23 -3.2(7) . . . . ?
C239 N22 C235 C236 0.4(9) . . . . ?
Pd2 N22 C235 C236 177.7(5) . . . . ?
C227 O23 C235 N22 166.5(5) . . . . ?
C227 O23 C235 C236 -14.5(9) . . . . ?
N22 C235 C236 C237 -1.1(11) . . . . ?
O23 C235 C236 C237 179.9(6) . . . . ?
C235 C236 C237 C238 0.0(10) . . . . ?
C236 C237 C238 C239 1.6(11) . . . . ?
C237 C238 C239 N22 -2.3(10) . . . . ?
C235 N22 C239 C238 1.3(9) . . . . ?
Pd2 N22 C239 C238 -176.2(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.101

# Attachment '3c.cif'

data_060119t
_database_code_depnum_ccdc_archive 'CCDC 682874'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H31 Cl4 N2 O4 Pd2'
_chemical_formula_weight         946.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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                   18.184(4)
_cell_length_b                   19.203(4)
_cell_length_c                   13.458(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.49(3)
_cell_angle_gamma                90.00
_cell_volume                     4342.0(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8082
_exptl_absorpt_correction_T_max  0.8969
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      213(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 axs CCD 1000'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10953
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_sigmaI/netI    0.2090
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.24
_reflns_number_total             3853
_reflns_number_gt                1721
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Siemens, 1996)'
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'

_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)+(0.0705P)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         3853
_refine_ls_number_parameters     211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.1875
_refine_ls_wR_factor_gt          0.1603
_refine_ls_goodness_of_fit_ref   0.840
_refine_ls_restrained_S_all      0.840
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.01739(5) 0.42329(4) 0.14278(6) 0.0419(3) Uani 1 1 d . . .
Cl1 Cl -0.05989(16) 0.39389(14) -0.0311(2) 0.0511(7) Uani 1 1 d . . .
O1 O 0.0917(4) 0.2821(3) 0.1551(5) 0.0430(18) Uani 1 1 d . . .
C1 C 0.1584(7) 0.4406(5) 0.0924(10) 0.056(3) Uani 1 1 d . . .
H1A H 0.1402 0.4869 0.0824 0.067 Uiso 1 1 calc R . .
N1 N 0.1153(5) 0.3922(4) 0.1209(6) 0.044(2) Uani 1 1 d . . .
Cl2 Cl 0.09140(15) 0.45828(13) 0.3193(2) 0.0505(7) Uani 1 1 d . . .
C2 C 0.2223(9) 0.4262(7) 0.0785(12) 0.089(5) Uani 1 1 d . . .
H2B H 0.2492 0.4623 0.0594 0.107 Uiso 1 1 calc R . .
O2 O 0.0718(4) 0.2546(3) 0.3612(5) 0.0453(18) Uani 1 1 d . . .
H2A H 0.0874 0.2541 0.3107 0.068 Uiso 1 1 calc R . .
C3 C 0.2548(7) 0.3571(6) 0.0910(11) 0.064(4) Uani 1 1 d . . .
C4 C 0.2084(6) 0.3065(5) 0.1152(8) 0.046(3) Uani 1 1 d . . .
H4A H 0.2233 0.2593 0.1205 0.055 Uiso 1 1 calc R . .
C5 C 0.1413(6) 0.3263(5) 0.1310(8) 0.045(3) Uani 1 1 d . . .
C6 C 0.3225(15) 0.3417(11) 0.085(2) 0.063(7) Uani 0.50 1 d P . .
H6A H 0.3322 0.2921 0.0963 0.094 Uiso 0.50 1 calc PR . .
H6B H 0.3648 0.3673 0.1392 0.094 Uiso 0.50 1 calc PR . .
H6C H 0.3209 0.3542 0.0141 0.094 Uiso 0.50 1 calc PR . .
C7 C 0.1046(4) 0.2095(2) 0.1523(5) 0.038(2) Uani 1 1 d G . .
C8 C 0.0573(3) 0.1733(3) 0.0607(4) 0.042(3) Uani 1 1 d G . .
C9 C 0.0719(4) 0.1032(3) 0.0498(5) 0.055(3) Uani 1 1 d G . .
H9A H 0.0399 0.0787 -0.0122 0.066 Uiso 1 1 calc R . .
C10 C 0.1338(4) 0.0694(2) 0.1304(6) 0.064(3) Uani 1 1 d G . .
H10A H 0.1436 0.0220 0.1230 0.077 Uiso 1 1 calc R . .
C11 C 0.1811(3) 0.1056(3) 0.2220(5) 0.053(3) Uani 1 1 d G . .
H11A H 0.2229 0.0827 0.2765 0.063 Uiso 1 1 calc R . .
C12 C 0.1665(3) 0.1756(3) 0.2329(4) 0.038(2) Uani 1 1 d G . .
C13 C -0.0205(7) 0.2087(6) -0.0297(9) 0.061(3) Uani 1 1 d . . .
H13A H -0.0172 0.2594 -0.0207 0.073 Uiso 1 1 calc R . .
H13B H -0.0213 0.1980 -0.1013 0.073 Uiso 1 1 calc R . .
C14 C 0.2104(5) 0.2109(5) 0.3373(8) 0.045(3) Uani 1 1 d . . .
H14A H 0.2003 0.2611 0.3282 0.054 Uiso 1 1 calc R . .
H14B H 0.2676 0.2036 0.3571 0.054 Uiso 1 1 calc R . .
C15 C 0.1866(4) 0.1841(3) 0.4326(5) 0.053(3) Uani 1 1 d G . .
C16 C 0.2343(3) 0.1362(3) 0.5069(6) 0.056(3) Uani 1 1 d G . .
H16A H 0.2816 0.1203 0.5019 0.067 Uiso 1 1 calc R . .
C17 C 0.2121(4) 0.1121(3) 0.5887(5) 0.058(3) Uani 1 1 d G . .
H17A H 0.2443 0.0797 0.6390 0.070 Uiso 1 1 calc R . .
C18 C 0.1421(4) 0.1357(3) 0.5962(5) 0.053(3) Uani 1 1 d G . .
H18A H 0.1271 0.1194 0.6515 0.064 Uiso 1 1 calc R . .
C19 C 0.0944(3) 0.1835(3) 0.5219(5) 0.044(3) Uani 1 1 d G . .
C20 C 0.1167(4) 0.2077(3) 0.4401(5) 0.041(3) Uani 1 1 d G . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.003(9) . ?
Pd1 Cl1 2.292(3) . ?
Pd1 Cl2 2.323(3) 2 ?
Pd1 Cl2 2.337(3) . ?
Pd1 Pd1 3.1819(19) 2 ?
O1 C5 1.366(12) . ?
O1 C7 1.417(7) . ?
C1 C2 1.274(17) . ?
C1 N1 1.363(13) . ?
N1 C5 1.340(12) . ?
Cl2 Pd1 2.323(3) 2 ?
C2 C3 1.436(17) . ?
O2 C20 1.393(7) . ?
C3 C6 1.30(2) . ?
C3 C4 1.404(14) . ?
C4 C5 1.371(14) . ?
C7 C8 1.3900 . ?
C7 C12 1.3900 . ?
C8 C9 1.3900 . ?
C8 C13 1.621(11) . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C14 1.486(11) . ?
C13 C19 1.47(3) 2 ?
C14 C15 1.589(11) . ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C19 C13 1.470(13) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 Cl1 90.5(2) . . ?
N1 Pd1 Cl2 176.1(2) . 2 ?
Cl1 Pd1 Cl2 93.12(10) . 2 ?
N1 Pd1 Cl2 92.1(2) . . ?
Cl1 Pd1 Cl2 176.88(10) . . ?
Cl2 Pd1 Cl2 84.33(10) 2 . ?
N1 Pd1 Pd1 129.0(2) . 2 ?
Cl1 Pd1 Pd1 132.00(9) . 2 ?
Cl2 Pd1 Pd1 47.12(7) 2 2 ?
Cl2 Pd1 Pd1 46.75(7) . 2 ?
C5 O1 C7 118.3(7) . . ?
C2 C1 N1 123.3(10) . . ?
C5 N1 C1 116.9(9) . . ?
C5 N1 Pd1 124.5(7) . . ?
C1 N1 Pd1 118.6(7) . . ?
Pd1 Cl2 Pd1 86.13(9) 2 . ?
C1 C2 C3 122.7(12) . . ?
C6 C3 C4 121.6(15) . . ?
C6 C3 C2 124.1(15) . . ?
C4 C3 C2 114.2(11) . . ?
C5 C4 C3 119.5(10) . . ?
N1 C5 O1 111.8(9) . . ?
N1 C5 C4 123.2(10) . . ?
O1 C5 C4 125.0(8) . . ?
C8 C7 C12 120.0 . . ?
C8 C7 O1 117.6(4) . . ?
C12 C7 O1 122.2(4) . . ?
C9 C8 C7 120.0 . . ?
C9 C8 C13 118.3(5) . . ?
C7 C8 C13 121.5(5) . . ?
C8 C9 C10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C12 120.0 . . ?
C11 C12 C7 120.0 . . ?
C11 C12 C14 119.0(5) . . ?
C7 C12 C14 120.4(5) . . ?
C19 C13 C8 111.6(10) 2 . ?
C12 C14 C15 113.7(7) . . ?
C16 C15 C20 120.0 . . ?
C16 C15 C14 120.5(5) . . ?
C20 C15 C14 119.5(5) . . ?
C15 C16 C17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C17 C18 C19 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C13 120.1(6) . 2 ?
C20 C19 C13 119.9(6) . 2 ?
C19 C20 C15 120.0 . . ?
C19 C20 O2 123.8(5) . . ?
C15 C20 O2 116.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.143


