# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009 


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Chun-ying Duan'
_publ_contact_author_email       DUANCY@NJU.EDU.CN

_publ_section_title              
;
A Palladium(II) triangle as Building Blocks of
Microporous Molecular Materials: Structures and Catalytic Performance
;
loop_
_publ_author_name
'Chun-ying Duan'
'Dongbin Dang'
'Cheng He'
'Yang Liu'
'Rong Zhang'

# Attachment 'pd1-squeeze.txt'

data_pd1-squeeze
_database_code_depnum_ccdc_archive 'CCDC 718744'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C157 H260 N30 O72 Pd3'
_chemical_formula_weight         4039.15

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

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   P-43m

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

_cell_length_a                   30.749(3)
_cell_length_b                   30.749(3)
_cell_length_c                   30.749(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     29073(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8504
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            22514
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_sigmaI/netI    0.2437
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7968
_reflns_number_gt                1920
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding mode'
_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   0.53(7)
_refine_ls_number_reflns         7968
_refine_ls_number_parameters     493
_refine_ls_number_restraints     734
_refine_ls_R_factor_all          0.2670
_refine_ls_R_factor_gt           0.0900
_refine_ls_wR_factor_ref         0.2307
_refine_ls_wR_factor_gt          0.1978
_refine_ls_goodness_of_fit_ref   0.817
_refine_ls_restrained_S_all      0.915
_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
C33 C 1.0000 0.691(2) 1.0000 0.41(4) Uiso 0.67 4 d SPDU . 1
O13 O 0.9680(9) 0.672(2) 0.9680(9) 0.34(3) Uiso 0.33 2 d SPDU A 1
O14 O 0.7542(15) 0.2458(15) 1.0108(18) 0.302(18) Uiso 0.33 2 d SPDU B 1
C34 C 0.770(2) 0.230(2) 1.054(2) 0.32(2) Uiso 0.33 2 d SPDU B 1
O14' O 0.7536(8) 0.2464(8) 1.021(4) 0.304(18) Uiso 0.33 2 d SPDU C 2
C34' C 0.7860(13) 0.2140(13) 1.004(3) 0.33(2) Uiso 0.33 2 d SPDU C 2
O15' O 0.8496(8) 0.319(6) 0.8496(8) 0.43(3) Uiso 0.17 2 d SPDU D 2
C35' C 0.8152(13) 0.314(10) 0.8152(13) 0.44(2) Uiso 0.17 2 d SPDU D 2
O16 O 0.6898(10) 0.6255(11) 1.1986(13) 0.216(16) Uiso 0.25 1 d PDU E 2
C36 C 0.6572(12) 0.6572(12) 1.1802(18) 0.25(2) Uiso 0.50 2 d SPDU E 2
O16' O 0.6227(4) 0.3773(4) 0.8130(9) 0.228(10) Uiso 0.50 2 d SPDU F 1
C36' C 0.6712(7) 0.372(2) 0.818(3) 0.201(18) Uiso 0.25 1 d PDU F 1
O17 O 0.6120(6) 0.6120(6) 1.8265(17) 0.310(17) Uiso 0.33 2 d SPDU G 1
C37 C 0.589(2) 0.589(2) 1.790(3) 0.322(19) Uiso 0.33 2 d SPDU G 1
O2W O 0.757(2) 0.243(2) 1.019(5) 0.310(18) Uiso 0.33 2 d SPU H 3
O17' O 0.6240(6) 0.6240(6) 1.8337(18) 0.308(18) Uiso 0.33 2 d SPDU I 3
C37' C 0.6483(17) 0.6483(17) 1.799(2) 0.33(2) Uiso 0.33 2 d SPDU I 3
O18 O 0.7048(12) 0.0877(9) 1.0877(9) 0.195(13) Uiso 0.33 2 d SPDU J 3
C38 C 0.7431(17) 0.0650(14) 1.0650(14) 0.24(2) Uiso 0.33 2 d SPDU J 3
O6W O 0.5946(14) 0.5946(14) 1.8003(18) 0.323(13) Uiso 0.50 2 d SPU K 2
O18' O 0.6859(6) 0.0563(11) 1.0563(11) 0.207(13) Uiso 0.33 2 d SPDU L 2
C38' C 0.6427(13) 0.0726(14) 1.0726(14) 0.23(2) Uiso 0.33 2 d SPDU L 2
O19 O 0.7120(5) 0.3342(8) 1.1006(8) 0.152(8) Uiso 0.33 1 d PDU M 1
C39 C 0.6691(7) 0.3309(7) 1.1241(11) 0.249(11) Uiso 0.67 2 d SPDU M 1
O19' O 0.6953(7) 0.3606(9) 1.0856(9) 0.197(10) Uiso 0.33 1 d PDU N 2
C39' C 0.6635(10) 0.3365(10) 1.0572(11) 0.243(12) Uiso 0.67 2 d SPDU N 2
O19" O 0.7194(13) 0.3320(18) 1.0750(18) 0.176(15) Uiso 0.17 1 d PDU O 3
C39" C 0.6693(14) 0.3307(14) 1.077(3) 0.238(14) Uiso 0.33 2 d SPDU O 3
C40 C 0.6887(8) 0.6887(8) 1.6887(8) 0.30(2) Uiso 1 6 d SDU P 2
O40 O 0.6565(6) 0.6565(6) 1.7065(13) 0.219(15) Uiso 0.33 2 d SPDU P 2
O22' O 0.9415(10) 0.3339(16) 0.9415(10) 0.275(17) Uiso 0.33 2 d SPDU Q 2
C42' C 0.9204(17) 0.295(2) 0.9204(17) 0.29(2) Uiso 0.33 2 d SPDU Q 2
O23 O 0.5291(5) -0.0704(8) 1.4709(5) 0.201(9) Uiso 0.50 2 d SPDU R 1
C43 C 0.5000 -0.0975(12) 1.5000 0.245(11) Uiso 1 4 d SDU . 1
O1W O 0.5000 -0.0510(13) 1.5000 0.250(10) Uiso 0.67 4 d SPU S 2
O21 O 0.4764(4) -0.1201(14) 1.5236(4) 0.200(11) Uiso 0.33 2 d SPDU . 2
C41 C 0.5105(5) -0.129(2) 1.4895(5) 0.221(13) Uiso 0.33 2 d SPDU . 2
C44 C 0.6029(19) 0.3971(19) 0.739(2) 0.26(3) Uiso 0.25 2 d SPDU T 2
O24 O 0.593(2) 0.407(2) 0.691(2) 0.36(4) Uiso 0.25 2 d SPDU T 2
O25 O 0.5142(11) -0.0108(9) 1.2062(12) 0.176(11) Uiso 0.25 1 d PDU . 3
C45 C 0.5119(18) 0.0358(10) 1.1919(17) 0.172(12) Uiso 0.25 1 d PDU . 3
O25' O 0.4591(9) -0.0201(9) 1.2515(8) 0.257(9) Uiso 0.50 1 d PDU U 2
C45' C 0.4452(14) -0.0504(13) 1.2875(12) 0.313(16) Uiso 0.50 1 d PDU U 2
O26 O 0.5280(7) -0.0113(7) 1.2637(7) 0.217(8) Uiso 0.50 1 d PDU . 1
C46 C 0.4981(12) -0.0137(11) 1.2253(9) 0.188(11) Uiso 0.50 1 d PDU . 1
O27 O 0.6659(12) 0.2372(8) 1.2372(8) 0.204(13) Uiso 0.33 2 d SPDU V 1
C47 C 0.650(3) 0.2700(10) 1.2700(10) 0.28(2) Uiso 0.33 2 d SPDU V 1
O27' O 0.6515(5) 0.1831(3) 1.1831(3) 0.135(5) Uiso 0.67 2 d SPDU W 2
C47' C 0.6931(6) 0.2013(5) 1.2013(5) 0.141(8) Uiso 0.67 2 d SPDU W 2
O27" O 0.6822(7) 0.1766(8) 1.2192(7) 0.042(6) Uiso 0.17 1 d PDU . 3
C47" C 0.7141(13) 0.1827(12) 1.1827(12) 0.193(17) Uiso 0.33 2 d SPDU . 3
O7W O 0.7365(19) 0.4618(16) 0.7365(19) 0.366(17) Uiso 0.50 2 d SPU X 1
O3W O 0.628(2) 0.558(2) 1.763(2) 0.348(17) Uiso 0.25 1 d PU Y 4
O15 O 0.745(2) 0.4205(13) 0.745(2) 0.38(2) Uiso 0.25 2 d SPDU Z 4
O4W O 0.5914(12) 0.2862(8) 1.2862(8) 0.274(14) Uiso 0.50 2 d SPU A 4
C35 C 0.743(6) 0.4694(15) 0.743(6) 0.37(2) Uiso 0.25 2 d SPDU Z 4
O22 O 0.9492(9) 0.279(2) 0.9492(9) 0.32(2) Uiso 0.33 2 d SPDU B 1
C42 C 0.9185(13) 0.256(3) 0.9185(13) 0.31(3) Uiso 0.33 2 d SPDU B 1
N8 N 0.7157(8) 0.5195(12) 0.7157(8) 0.362(19) Uiso 0.25 2 d SPDU C 3
O81 O 0.6899(9) 0.5054(16) 0.6899(9) 0.40(2) Uiso 0.25 2 d SPDU C 3
O82 O 0.7197(14) 0.5576(13) 0.7197(14) 0.36(3) Uiso 0.25 2 d SPDU C 3
O83 O 0.7368(11) 0.495(2) 0.7368(11) 0.37(2) Uiso 0.25 2 d SPDU C 3
N9 N 0.8049(7) 0.3594(9) 0.8049(7) 0.44(2) Uiso 0.50 2 d SPDU D 4
O93 O 0.8325(7) 0.3604(14) 0.8325(7) 0.47(2) Uiso 0.50 2 d SPDU D 4
O92 O 0.7920(9) 0.3246(11) 0.7920(9) 0.44(2) Uiso 0.50 2 d SPDU D 4
O91 O 0.7903(9) 0.3921(11) 0.7903(9) 0.411(18) Uiso 0.50 2 d SPDU D 4
N7 N 0.9029(4) 0.4532(5) 0.9029(4) 0.188(6) Uiso 1 2 d SD . .
O73' O 0.9017(7) 0.4150(6) 0.9017(7) 0.243(13) Uiso 0.50 2 d SPD E 1
O72' O 0.8813(5) 0.4744(9) 0.8813(5) 0.219(12) Uiso 0.50 2 d SPD E 1
O71' O 0.9270(5) 0.4699(8) 0.9270(5) 0.197(11) Uiso 0.50 2 d SPD E 1
O71 O 0.9273(4) 0.4383(8) 0.9273(4) 0.162(8) Uiso 0.50 2 d SPD E 2
O73 O 0.8990(8) 0.4901(7) 0.8990(8) 0.32(2) Uiso 0.50 2 d SPD E 2
O72 O 0.8816(6) 0.4291(10) 0.8816(6) 0.263(15) Uiso 0.50 2 d SPD E 2
N6 N 0.9790(5) 0.5240(8) 0.9790(5) 0.283(18) Uiso 0.25 2 d SPDU . 3
O61 O 0.9832(8) 0.5612(8) 0.9832(8) 0.295(18) Uiso 0.25 2 d SPDU . 3
O62 O 1.0000 0.5000 1.0000 0.333(16) Uiso 1 8 d SDU . 3
O63 O 0.9540(5) 0.5100(13) 0.9540(5) 0.34(2) Uiso 0.25 2 d SPDU F 3
Pd1 Pd 0.14691(3) 0.85309(3) 0.43902(5) 0.1597(6) Uani 1 2 d SU . .
O1 O 0.3382(2) 0.9372(3) 0.5039(2) 0.146(2) Uani 1 1 d U . .
O2 O 0.2311(2) 1.0618(3) 0.3965(3) 0.176(3) Uani 1 1 d U . .
N2 N 0.3647(3) 0.8735(3) 0.4840(3) 0.155(2) Uani 1 1 d DU . .
H2A H 0.3832 0.8595 0.4685 0.186 Uiso 1 1 calc R . .
N3 N 0.2139(3) 1.0496(3) 0.3308(4) 0.188(3) Uani 1 1 d DU . .
H3A H 0.2202 1.0504 0.3035 0.225 Uiso 1 1 calc R . .
N1 N 0.2086(3) 0.8550(3) 0.4623(3) 0.156(2) Uani 1 1 d DU . .
C1 C 0.2416(3) 0.8422(3) 0.4356(3) 0.153(3) Uani 1 1 d DU . .
H1A H 0.2362 0.8356 0.4066 0.184 Uiso 1 1 calc R . .
C2 C 0.2831(3) 0.8391(3) 0.4525(3) 0.158(2) Uani 1 1 d DU . .
H2B H 0.3056 0.8292 0.4349 0.189 Uiso 1 1 calc R . .
C3 C 0.2918(2) 0.8504(4) 0.4945(3) 0.153(2) Uani 1 1 d DU . .
C4 C 0.2587(3) 0.8642(3) 0.5218(3) 0.158(2) Uani 1 1 d DU . .
H4A H 0.2643 0.8712 0.5507 0.190 Uiso 1 1 calc R . .
C5 C 0.2165(3) 0.8673(3) 0.5044(3) 0.158(3) Uani 1 1 d DU . .
H5A H 0.1939 0.8778 0.5216 0.190 Uiso 1 1 calc R . .
C6 C 0.3353(3) 0.8512(4) 0.5115(4) 0.159(3) Uani 1 1 d DU . .
H6A H 0.3351 0.8652 0.5398 0.191 Uiso 1 1 calc R . .
H6B H 0.3454 0.8216 0.5155 0.191 Uiso 1 1 calc R . .
C7 C 0.3628(4) 0.9174(4) 0.4826(4) 0.133(3) Uani 1 1 d DU . .
C8 C 0.4228(3) 0.9177(4) 0.4228(3) 0.126(3) Uani 1 2 d SDU . .
H8A H 0.4264 0.8879 0.4264 0.151 Uiso 1 2 calc SR . .
C9 C 0.3912(3) 0.9379(3) 0.4495(3) 0.118(2) Uani 1 1 d DU . .
C10 C 0.3842(3) 0.9817(3) 0.4384(3) 0.124(2) Uani 1 1 d DU . .
H10A H 0.3601 0.9951 0.4507 0.148 Uiso 1 1 calc R . .
C11 C 0.4102(3) 1.0076(5) 0.4102(3) 0.125(3) Uani 1 2 d SDU . .
C12 C 0.3988(4) 1.0530(5) 0.3988(4) 0.137(3) Uani 1 2 d SU . .
H12A H 0.3893 1.0672 0.4258 0.165 Uiso 0.50 1 d PR . .
C13 C 0.3655(3) 1.0575(5) 0.3655(3) 0.137(3) Uani 1 2 d SDU . .
C14 C 0.3217(3) 1.0577(4) 0.3774(3) 0.148(3) Uani 1 1 d DU . .
H14A H 0.3139 1.0546 0.4065 0.177 Uiso 1 1 calc R . .
C15 C 0.2894(3) 1.0626(4) 0.3455(3) 0.151(3) Uani 1 1 d DU . .
C16 C 0.3018(4) 1.0616(5) 0.3018(4) 0.150(3) Uani 1 2 d SDU . .
H16A H 0.2804 1.0601 0.2804 0.180 Uiso 1 2 calc SR . .
C17 C 0.2445(4) 1.0613(5) 0.3602(5) 0.169(3) Uani 1 1 d DU . .
C18 C 0.1707(4) 1.0356(4) 0.3443(5) 0.195(3) Uani 1 1 d DU . .
H18A H 0.1535 1.0338 0.3179 0.234 Uiso 1 1 calc R . .
H18B H 0.1587 1.0596 0.3609 0.234 Uiso 1 1 calc R . .
C19 C 0.1740(4) 0.9183(3) 0.3702(4) 0.193(3) Uani 1 1 d DU . .
H19A H 0.1847 0.8937 0.3561 0.232 Uiso 1 1 calc R . .
C20 C 0.1789(4) 0.9591(4) 0.3503(4) 0.200(3) Uani 1 1 d DU . .
H20A H 0.1945 0.9619 0.3245 0.240 Uiso 1 1 calc R . .
C21 C 0.1602(4) 0.9952(3) 0.3697(4) 0.196(3) Uani 1 1 d DU . .
C22 C 0.1434(4) 0.9907(3) 0.4122(4) 0.195(3) Uani 1 1 d DU . .
H22A H 0.1383 1.0152 0.4292 0.234 Uiso 1 1 calc R . .
C23 C 0.1345(4) 0.9497(3) 0.4284(3) 0.194(3) Uani 1 1 d DU . .
H23A H 0.1155 0.9467 0.4517 0.233 Uiso 1 1 calc R . .
N4 N 0.1535(3) 0.9133(3) 0.4104(4) 0.183(3) Uani 1 1 d DU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.1207(6) 0.1207(6) 0.2377(14) -0.0162(7) 0.0162(7) -0.0287(8)
O1 0.147(5) 0.152(5) 0.138(5) 0.003(4) 0.006(4) -0.048(4)
O2 0.145(5) 0.198(5) 0.184(5) -0.003(5) 0.030(5) -0.029(5)
N2 0.127(5) 0.142(5) 0.196(5) 0.024(5) 0.008(4) -0.052(4)
N3 0.161(5) 0.187(5) 0.214(5) 0.002(5) 0.010(5) -0.033(5)
N1 0.130(4) 0.139(4) 0.200(4) -0.011(4) 0.009(4) -0.037(4)
C1 0.115(4) 0.148(4) 0.197(5) -0.005(4) 0.012(4) -0.045(4)
C2 0.124(4) 0.147(4) 0.201(5) -0.002(5) 0.005(5) -0.037(4)
C3 0.121(4) 0.139(4) 0.199(5) 0.007(4) 0.002(4) -0.043(4)
C4 0.124(5) 0.149(5) 0.202(5) 0.005(4) 0.010(5) -0.044(4)
C5 0.127(5) 0.147(5) 0.200(5) 0.001(5) 0.002(5) -0.040(5)
C6 0.129(5) 0.148(5) 0.200(5) 0.017(5) 0.001(5) -0.046(5)
C7 0.115(5) 0.124(5) 0.161(5) 0.011(5) -0.014(4) -0.029(5)
C8 0.128(4) 0.122(6) 0.128(4) -0.018(4) -0.030(6) -0.018(4)
C9 0.097(4) 0.119(5) 0.138(5) 0.006(4) -0.012(4) -0.038(4)
C10 0.111(4) 0.125(5) 0.135(5) -0.012(5) -0.015(4) -0.030(4)
C11 0.127(4) 0.120(6) 0.127(4) -0.018(4) -0.007(5) -0.018(4)
C12 0.141(4) 0.130(6) 0.141(4) -0.021(4) -0.004(5) -0.021(4)
C13 0.143(4) 0.126(5) 0.143(4) -0.016(4) 0.005(5) -0.016(4)
C14 0.141(5) 0.140(5) 0.163(5) -0.008(5) 0.003(5) -0.024(5)
C15 0.145(5) 0.148(5) 0.161(5) -0.004(5) 0.005(5) -0.024(5)
C16 0.152(4) 0.145(6) 0.152(4) -0.016(4) 0.008(6) -0.016(4)
C17 0.156(5) 0.166(5) 0.184(5) -0.004(5) 0.006(5) -0.025(5)
C18 0.169(5) 0.183(5) 0.234(5) 0.007(5) 0.021(5) -0.039(5)
C19 0.160(5) 0.166(5) 0.254(6) 0.006(5) 0.030(5) -0.047(5)
C20 0.166(5) 0.177(5) 0.257(5) 0.000(5) 0.030(5) -0.035(5)
C21 0.165(5) 0.175(5) 0.248(5) 0.006(5) 0.028(5) -0.044(5)
C22 0.165(5) 0.169(5) 0.252(5) 0.001(5) 0.033(5) -0.035(5)
C23 0.154(5) 0.170(5) 0.257(6) 0.007(5) 0.037(5) -0.043(5)
N4 0.140(5) 0.162(5) 0.248(5) -0.012(5) 0.028(5) -0.033(4)

_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
C33 O13 1.513(12) . ?
C33 O13 1.513(12) 3_757 ?
O14 C34 1.503(13) . ?
O14' C34' 1.506(13) . ?
O15' C35' 1.506(13) . ?
O16 C36 1.507(12) . ?
C36 O16 1.507(12) 13 ?
O16' C36' 1.507(8) . ?
O16' C36' 1.507(8) 14_665 ?
C36' C36' 1.88(12) 14_665 ?
O17 C37 1.506(8) . ?
O17' C37' 1.507(8) . ?
O18 C38 1.54(2) . ?
O18' C38' 1.507(8) . ?
O19 C39 1.508(7) . ?
C39 O19 1.508(7) 14_665 ?
O19' C39' 1.505(7) . ?
C39' O19' 1.505(7) 14_665 ?
O19" C39" 1.54(2) . ?
C39" O19" 1.54(2) 14_665 ?
C40 O40 1.504(12) 9_546 ?
C40 O40 1.504(12) . ?
C40 O40 1.504(12) 5_456 ?
O22' C42' 1.503(13) . ?
O23 C43 1.514(12) . ?
C43 O23 1.514(12) 3_658 ?
O21 C41 0.63(6) 3_658 ?
O21 C41 1.507(8) . ?
C41 O21 0.63(6) 3_658 ?
C41 C41 0.91(5) 3_658 ?
C44 O24 1.543(11) . ?
O25 O25 1.10(6) 2_655 ?
O25 C45 1.20(5) 2_655 ?
O25 C45 1.502(12) . ?
C45 O25 1.20(5) 2_655 ?
O25' C45' 1.508(12) . ?
O26 C46 1.498(12) . ?
O26 C46 1.62(4) 2_655 ?
C46 C46 0.85(7) 2_655 ?
C46 O26 1.62(4) 2_655 ?
O27 C47 1.510(12) . ?
O27' C47' 1.502(11) . ?
O27" C47" 1.502(12) . ?
C47" O27" 1.502(12) 17_546 ?
O15 C35 1.507(13) . ?
O22 C42 1.507(13) . ?
N8 O82 1.19(2) . ?
N8 O83 1.19(2) . ?
N8 O81 1.20(2) . ?
N9 O91 1.190(16) . ?
N9 O93 1.20(2) . ?
N9 O92 1.21(2) . ?
N7 O72' 1.141(18) . ?
N7 O73 1.146(19) . ?
N7 O71 1.156(16) . ?
N7 O71' 1.170(17) . ?
N7 O73' 1.175(18) . ?
N7 O72 1.184(19) . ?
N6 O61 1.16(2) . ?
N6 O63 1.17(2) . ?
N6 O62 1.17(2) . ?
N6 N6 1.82(5) 3_757 ?
O61 O61 1.46(7) 3_757 ?
O62 N6 1.17(2) 3_757 ?
O62 N6 1.17(2) 4_567 ?
O62 N6 1.17(2) 2_765 ?
Pd1 N1 2.027(8) . ?
Pd1 N1 2.027(8) 14_665 ?
Pd1 N4 2.061(10) 14_665 ?
Pd1 N4 2.061(10) . ?
O1 C7 1.173(11) . ?
O2 C17 1.188(13) . ?
N2 C7 1.352(9) . ?
N2 C6 1.415(8) . ?
N3 C17 1.353(9) . ?
N3 C18 1.459(9) . ?
N1 C1 1.361(8) . ?
N1 C5 1.372(8) . ?
C1 C2 1.383(8) . ?
C2 C3 1.363(8) . ?
C3 C4 1.385(8) . ?
C3 C6 1.436(8) . ?
C4 C5 1.408(9) . ?
C7 C9 1.480(9) . ?
C8 C9 1.416(7) 21 ?
C8 C9 1.416(7) . ?
C9 C10 1.407(7) . ?
C10 C11 1.421(7) . ?
C11 C10 1.421(7) 21 ?
C11 C12 1.482(19) . ?
C12 C13 1.454(18) . ?
C13 C14 1.396(7) 21 ?
C13 C14 1.396(7) . ?
C14 C15 1.407(7) . ?
C15 C16 1.396(7) . ?
C15 C17 1.456(9) . ?
C16 C15 1.396(7) 21 ?
C18 C21 1.502(9) . ?
C19 N4 1.395(8) . ?
C19 C20 1.406(9) . ?
C20 C21 1.386(8) . ?
C21 C22 1.411(9) . ?
C22 C23 1.382(9) . ?
C23 N4 1.378(8) . ?

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
O13 C33 O13 134(8) . 3_757 ?
O16 C36 O16 136(5) 13 . ?
C36' O16' C36' 77(6) . 14_665 ?
O16' C36' C36' 51(3) . 14_665 ?
O19 C39 O19 84(2) . 14_665 ?
O19' C39' O19' 108(3) . 14_665 ?
O19" C39" O19" 93(5) . 14_665 ?
O40 C40 O40 92(3) 9_546 . ?
O40 C40 O40 92(3) 9_546 5_456 ?
O40 C40 O40 92(3) . 5_456 ?
O23 C43 O23 113(3) 3_658 . ?
C41 O21 C41 15(4) 3_658 . ?
O21 C41 C41 155(7) 3_658 3_658 ?
O21 C41 O21 144(10) 3_658 . ?
C41 C41 O21 10(4) 3_658 . ?
O25 O25 C45 82(4) 2_655 2_655 ?
O25 O25 C45 52(3) 2_655 . ?
C45 O25 C45 118(4) 2_655 . ?
O25 C45 O25 46(3) 2_655 . ?
C46 O26 C46 31(2) . 2_655 ?
C46 C46 O26 82(3) 2_655 . ?
C46 C46 O26 66(3) 2_655 2_655 ?
O26 C46 O26 73(2) . 2_655 ?
O27" C47" O27" 76(2) 17_546 . ?
O82 N8 O83 121(2) . . ?
O82 N8 O81 119.5(19) . . ?
O83 N8 O81 120(2) . . ?
O91 N9 O93 120.8(19) . . ?
O91 N9 O92 120.0(19) . . ?
O93 N9 O92 119.2(17) . . ?
O72' N7 O73 46.7(17) . . ?
O72' N7 O71 168.5(17) . . ?
O73 N7 O71 121.8(17) . . ?
O72' N7 O71' 119.2(15) . . ?
O73 N7 O71' 72.5(17) . . ?
O71 N7 O71' 49.3(12) . . ?
O72' N7 O73' 122.3(16) . . ?
O73 N7 O73' 169.0(18) . . ?
O71 N7 O73' 69.1(14) . . ?
O71' N7 O73' 118.5(15) . . ?
O72' N7 O72 73.5(17) . . ?
O73 N7 O72 120.2(17) . . ?
O71 N7 O72 118.0(15) . . ?
O71' N7 O72 167.3(17) . . ?
O73' N7 O72 48.9(15) . . ?
O61 N6 O63 121(2) . . ?
O61 N6 O62 120.0(19) . . ?
O63 N6 O62 119.4(19) . . ?
O61 N6 N6 81.0(16) . 3_757 ?
O63 N6 N6 158.4(17) . 3_757 ?
O62 N6 N6 39.0(13) . 3_757 ?
N6 O61 O61 99.0(16) . 3_757 ?
N6 O62 N6 113.3(14) 3_757 4_567 ?
N6 O62 N6 102(3) 3_757 . ?
N6 O62 N6 113.3(14) 4_567 . ?
N6 O62 N6 113.3(14) 3_757 2_765 ?
N6 O62 N6 102(3) 4_567 2_765 ?
N6 O62 N6 113.3(14) . 2_765 ?
N1 Pd1 N1 85.9(5) . 14_665 ?
N1 Pd1 N4 173.8(4) . 14_665 ?
N1 Pd1 N4 91.9(4) 14_665 14_665 ?
N1 Pd1 N4 91.9(4) . . ?
N1 Pd1 N4 173.8(4) 14_665 . ?
N4 Pd1 N4 89.7(6) 14_665 . ?
C7 N2 C6 118.5(10) . . ?
C17 N3 C18 121.3(12) . . ?
C1 N1 C5 121.0(8) . . ?
C1 N1 Pd1 118.5(7) . . ?
C5 N1 Pd1 120.5(7) . . ?
N1 C1 C2 118.8(7) . . ?
C3 C2 C1 121.4(7) . . ?
C2 C3 C4 120.4(6) . . ?
C2 C3 C6 122.2(9) . . ?
C4 C3 C6 117.3(9) . . ?
C3 C4 C5 118.0(7) . . ?
N1 C5 C4 120.3(7) . . ?
N2 C6 C3 112.6(9) . . ?
O1 C7 N2 121.8(11) . . ?
O1 C7 C9 123.1(10) . . ?
N2 C7 C9 114.9(10) . . ?
C9 C8 C9 127.1(13) 21 . ?
C10 C9 C8 112.5(11) . . ?
C10 C9 C7 119.0(8) . . ?
C8 C9 C7 128.1(9) . . ?
C9 C10 C11 126.8(11) . . ?
C10 C11 C10 111.8(13) 21 . ?
C10 C11 C12 122.6(7) 21 . ?
C10 C11 C12 122.6(7) . . ?
C13 C12 C11 114.9(13) . . ?
C14 C13 C14 120.4(14) 21 . ?
C14 C13 C12 119.7(7) 21 . ?
C14 C13 C12 119.7(7) . . ?
C13 C14 C15 120.0(11) . . ?
C16 C15 C14 118.5(12) . . ?
C16 C15 C17 123.9(10) . . ?
C14 C15 C17 116.7(9) . . ?
C15 C16 C15 121.6(15) 21 . ?
O2 C17 N3 113.0(11) . . ?
O2 C17 C15 128.4(12) . . ?
N3 C17 C15 117.2(12) . . ?
N3 C18 C21 126.0(11) . . ?
N4 C19 C20 122.1(7) . . ?
C21 C20 C19 118.9(7) . . ?
C20 C21 C22 118.1(6) . . ?
C20 C21 C18 110.4(10) . . ?
C22 C21 C18 129.9(10) . . ?
C23 C22 C21 119.7(8) . . ?
N4 C23 C22 120.7(8) . . ?
C23 N4 C19 117.3(9) . . ?
C23 N4 Pd1 121.1(8) . . ?
C19 N4 Pd1 121.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.051


# Attachment 'PD1.txt'

data_pd1
_database_code_depnum_ccdc_archive 'CCDC 752539'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C157 H260 N30 O72 Pd3'
_chemical_formula_weight         4039.15

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

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   P-43m

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

_cell_length_a                   30.749(3)
_cell_length_b                   30.749(3)
_cell_length_c                   30.749(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     29073(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8504
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_reflns_number            22514
_diffrn_reflns_av_R_equivalents  0.1226
_diffrn_reflns_av_sigmaI/netI    0.2466
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7968
_reflns_number_gt                1926
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    'riding mode'
_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   0.48(7)
_refine_ls_number_reflns         7968
_refine_ls_number_parameters     493
_refine_ls_number_restraints     747
_refine_ls_R_factor_all          0.3223
_refine_ls_R_factor_gt           0.0897
_refine_ls_wR_factor_ref         0.2450
_refine_ls_wR_factor_gt          0.1920
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_restrained_S_all      0.968
_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
C33 C 1.0000 0.6928(19) 1.0000 0.43(4) Uiso 0.67 4 d SPDU . 1
O13 O 0.9698(11) 0.667(2) 0.9698(11) 0.35(3) Uiso 0.33 2 d SPDU A 1
O14 O 0.7543(19) 0.2457(19) 1.0165(18) 0.325(19) Uiso 0.33 2 d SPDU B 1
C34 C 0.766(2) 0.234(2) 1.063(2) 0.31(2) Uiso 0.33 2 d SPDU B 1
O14' O 0.7531(8) 0.2469(8) 1.017(4) 0.323(19) Uiso 0.33 2 d SPDU C 2
C34' C 0.7858(14) 0.2142(14) 0.999(4) 0.34(2) Uiso 0.33 2 d SPDU C 2
O15' O 0.8433(11) 0.335(4) 0.8433(11) 0.41(2) Uiso 0.17 2 d SPDU D 2
C35' C 0.817(5) 0.367(7) 0.817(5) 0.43(2) Uiso 0.17 2 d SPDU D 2
O16 O 0.6888(10) 0.6238(12) 1.1996(14) 0.222(19) Uiso 0.25 1 d PDU E 2
C36 C 0.6570(11) 0.6570(11) 1.1805(18) 0.23(2) Uiso 0.50 2 d SPDU E 2
O16' O 0.6252(5) 0.3748(5) 0.8131(11) 0.251(13) Uiso 0.50 2 d SPDU F 1
C36' C 0.6741(7) 0.373(2) 0.822(2) 0.17(2) Uiso 0.25 1 d PDU F 1
O17 O 0.6195(5) 0.6195(5) 1.8298(19) 0.292(17) Uiso 0.33 2 d SPDU G 1
C37 C 0.592(2) 0.592(2) 1.798(4) 0.302(19) Uiso 0.33 2 d SPDU G 1
O2W O 0.759(2) 0.241(2) 1.016(5) 0.330(19) Uiso 0.33 2 d SPU H 3
O17' O 0.6268(5) 0.6268(5) 1.829(2) 0.299(17) Uiso 0.33 2 d SPDU I 3
C37' C 0.6549(15) 0.6549(15) 1.799(2) 0.30(2) Uiso 0.33 2 d SPDU I 3
O18 O 0.7019(12) 0.0870(9) 1.0870(9) 0.182(13) Uiso 0.33 2 d SPDU J 3
C38 C 0.735(2) 0.0605(14) 1.0605(14) 0.25(2) Uiso 0.33 2 d SPDU J 3
O6W O 0.5964(14) 0.5964(14) 1.803(2) 0.307(13) Uiso 0.50 2 d SPU K 2
O18' O 0.6825(6) 0.0562(11) 1.0562(11) 0.210(14) Uiso 0.33 2 d SPDU L 2
C38' C 0.6389(13) 0.0729(14) 1.0729(14) 0.22(2) Uiso 0.33 2 d SPDU L 2
O19 O 0.7116(5) 0.3349(8) 1.1023(8) 0.146(9) Uiso 0.33 1 d PDU M 1
C39 C 0.6689(8) 0.3311(8) 1.1274(12) 0.258(12) Uiso 0.67 2 d SPDU M 1
O19' O 0.6971(7) 0.3587(10) 1.0821(9) 0.199(11) Uiso 0.33 1 d PDU N 2
C39' C 0.6613(11) 0.3387(11) 1.0541(11) 0.251(12) Uiso 0.67 2 d SPDU N 2
O19" O 0.7206(14) 0.332(2) 1.078(2) 0.179(16) Uiso 0.17 1 d PDU O 3
C39" C 0.6706(15) 0.3294(15) 1.078(3) 0.243(14) Uiso 0.33 2 d SPDU O 3
C40 C 0.6901(8) 0.6901(8) 1.6901(8) 0.29(2) Uiso 1 6 d SDU P 2
O40 O 0.6569(6) 0.6569(6) 1.7059(14) 0.225(17) Uiso 0.33 2 d SPDU P 2
O22' O 0.9453(8) 0.3330(18) 0.9453(8) 0.273(18) Uiso 0.33 2 d SPDU Q 2
C42' C 0.9149(13) 0.308(3) 0.9149(13) 0.30(3) Uiso 0.33 2 d SPDU Q 2
O23 O 0.5307(4) -0.0695(8) 1.4693(4) 0.190(9) Uiso 0.50 2 d SPDU R 1
C43 C 0.5000 -0.0934(13) 1.5000 0.250(12) Uiso 1 4 d SDU . 1
O1W O 0.5000 -0.0491(14) 1.5000 0.249(11) Uiso 0.67 4 d SPU S 2
O21 O 0.4760(4) -0.1186(15) 1.5240(4) 0.202(12) Uiso 0.33 2 d SPDU . 2
C41 C 0.5103(6) -0.129(2) 1.4897(6) 0.232(13) Uiso 0.33 2 d SPDU . 2
C44 C 0.6212(12) 0.3788(12) 0.724(3) 0.32(3) Uiso 0.25 2 d SPDU T 2
O24 O 0.598(2) 0.402(2) 0.687(3) 0.34(3) Uiso 0.25 2 d SPDU T 2
O25 O 0.5145(10) -0.0099(8) 1.2052(11) 0.147(10) Uiso 0.25 1 d PDU . 3
C45 C 0.5109(16) 0.0372(9) 1.1905(15) 0.142(13) Uiso 0.25 1 d PDU . 3
O25' O 0.4587(8) -0.0201(8) 1.2524(8) 0.229(9) Uiso 0.50 1 d PDU U 2
C45' C 0.4439(15) -0.0497(13) 1.2892(12) 0.314(17) Uiso 0.50 1 d PDU U 2
O26 O 0.5303(7) -0.0119(8) 1.2658(7) 0.213(8) Uiso 0.50 1 d PDU . 1
C46 C 0.4987(11) -0.0157(9) 1.2281(9) 0.173(10) Uiso 0.50 1 d PDU . 1
O27 O 0.6622(14) 0.2401(8) 1.2401(8) 0.225(15) Uiso 0.33 2 d SPDU V 1
C47 C 0.647(3) 0.2737(10) 1.2737(10) 0.27(2) Uiso 0.33 2 d SPDU V 1
O27' O 0.6496(5) 0.1830(3) 1.1830(3) 0.134(5) Uiso 0.67 2 d SPDU W 2
C47' C 0.6922(7) 0.2005(6) 1.2005(6) 0.159(10) Uiso 0.67 2 d SPDU W 2
O27" O 0.6833(8) 0.1775(10) 1.2188(9) 0.066(8) Uiso 0.17 1 d PDU . 3
C47" C 0.7168(13) 0.1828(12) 1.1828(12) 0.169(14) Uiso 0.33 2 d SPDU . 3
O7W O 0.7384(19) 0.4649(17) 0.7384(19) 0.359(15) Uiso 0.50 2 d SPU X 1
O3W O 0.620(2) 0.575(2) 1.767(2) 0.322(16) Uiso 0.25 1 d PU Y 4
O15 O 0.740(3) 0.4384(15) 0.740(3) 0.38(2) Uiso 0.25 2 d SPDU Z 4
O4W O 0.5928(11) 0.2867(8) 1.2867(8) 0.249(13) Uiso 0.50 2 d SPU A 4
C35 C 0.743(5) 0.4878(16) 0.743(5) 0.36(2) Uiso 0.25 2 d SPDU Z 4
O22 O 0.9447(8) 0.282(2) 0.9447(8) 0.33(2) Uiso 0.33 2 d SPDU B 1
C42 C 0.9115(12) 0.265(3) 0.9115(12) 0.30(3) Uiso 0.33 2 d SPDU B 1
N8 N 0.7155(8) 0.5112(12) 0.7155(8) 0.368(18) Uiso 0.25 2 d SPDU C 3
O81 O 0.6883(9) 0.5033(17) 0.6883(9) 0.38(2) Uiso 0.25 2 d SPDU C 3
O82 O 0.7241(13) 0.5480(14) 0.7241(13) 0.35(2) Uiso 0.25 2 d SPDU C 3
O83 O 0.7336(12) 0.4817(18) 0.7336(12) 0.36(2) Uiso 0.25 2 d SPDU C 3
N9 N 0.7996(7) 0.3677(10) 0.7996(7) 0.43(2) Uiso 0.50 2 d SPDU D 4
O93 O 0.8267(7) 0.3732(14) 0.8267(7) 0.44(2) Uiso 0.50 2 d SPDU D 4
O92 O 0.7895(10) 0.3311(11) 0.7895(10) 0.427(19) Uiso 0.50 2 d SPDU D 4
O91 O 0.7825(9) 0.3979(12) 0.7825(9) 0.419(19) Uiso 0.50 2 d SPDU D 4
N7 N 0.9050(4) 0.4521(5) 0.9050(4) 0.193(7) Uiso 1 2 d SD . .
O73' O 0.9018(7) 0.4138(7) 0.9018(7) 0.242(14) Uiso 0.50 2 d SPD E 1
O72' O 0.8839(5) 0.4744(8) 0.8839(5) 0.196(11) Uiso 0.50 2 d SPD E 1
O71' O 0.9295(5) 0.4664(9) 0.9295(5) 0.209(12) Uiso 0.50 2 d SPD E 1
O71 O 0.9283(5) 0.4348(9) 0.9283(5) 0.198(11) Uiso 0.50 2 d SPD E 2
O73 O 0.9038(9) 0.4896(7) 0.9038(9) 0.33(2) Uiso 0.50 2 d SPD E 2
O72 O 0.8825(6) 0.4318(12) 0.8825(6) 0.278(17) Uiso 0.50 2 d SPD E 2
N6 N 0.9789(5) 0.5248(8) 0.9789(5) 0.285(19) Uiso 0.25 2 d SPDU . 3
O61 O 0.9835(9) 0.5620(8) 0.9835(9) 0.289(18) Uiso 0.25 2 d SPDU . 3
O62 O 1.0000 0.5000 1.0000 0.340(16) Uiso 1 8 d SDU . 3
O63 O 0.9537(5) 0.5110(14) 0.9537(5) 0.34(2) Uiso 0.25 2 d SPDU F 3
Pd1 Pd 0.14690(4) 0.85310(4) 0.43903(6) 0.1572(6) Uani 1 2 d SU . .
O1 O 0.3372(2) 0.9379(3) 0.5033(2) 0.143(2) Uani 1 1 d U . .
O2 O 0.2313(3) 1.0609(3) 0.3959(3) 0.178(3) Uani 1 1 d U . .
N2 N 0.3652(3) 0.8736(3) 0.4839(3) 0.157(3) Uani 1 1 d DU . .
H2A H 0.3840 0.8598 0.4684 0.188 Uiso 1 1 calc R . .
N3 N 0.2141(3) 1.0482(4) 0.3315(4) 0.187(3) Uani 1 1 d DU . .
H3A H 0.2209 1.0476 0.3044 0.224 Uiso 1 1 calc R . .
N1 N 0.2085(3) 0.8549(3) 0.4627(3) 0.152(2) Uani 1 1 d DU . .
C1 C 0.2411(3) 0.8423(3) 0.4352(3) 0.153(3) Uani 1 1 d DU . .
H1A H 0.2354 0.8361 0.4062 0.183 Uiso 1 1 calc R . .
C2 C 0.2830(3) 0.8391(3) 0.4517(3) 0.154(3) Uani 1 1 d DU . .
H2B H 0.3053 0.8288 0.4341 0.185 Uiso 1 1 calc R . .
C3 C 0.2919(2) 0.8509(4) 0.4938(3) 0.152(2) Uani 1 1 d DU . .
C4 C 0.2589(3) 0.8641(4) 0.5212(3) 0.156(3) Uani 1 1 d DU . .
H4A H 0.2646 0.8711 0.5501 0.187 Uiso 1 1 calc R . .
C5 C 0.2163(3) 0.8666(4) 0.5047(3) 0.154(3) Uani 1 1 d DU . .
H5A H 0.1936 0.8763 0.5223 0.185 Uiso 1 1 calc R . .
C6 C 0.3353(3) 0.8508(4) 0.5113(4) 0.159(3) Uani 1 1 d DU . .
H6A H 0.3350 0.8643 0.5398 0.191 Uiso 1 1 calc R . .
H6B H 0.3450 0.8210 0.5148 0.191 Uiso 1 1 calc R . .
C7 C 0.3629(4) 0.9178(4) 0.4833(4) 0.134(3) Uani 1 1 d DU . .
C8 C 0.4227(3) 0.9175(5) 0.4227(3) 0.122(3) Uani 1 2 d SDU . .
H8A H 0.4259 0.8876 0.4259 0.147 Uiso 1 2 calc SR . .
C9 C 0.3913(3) 0.9375(3) 0.4497(3) 0.121(2) Uani 1 1 d DU . .
C10 C 0.3842(3) 0.9816(3) 0.4396(3) 0.124(2) Uani 1 1 d DU . .
H10A H 0.3609 0.9956 0.4528 0.149 Uiso 1 1 calc R . .
C11 C 0.4105(3) 1.0058(5) 0.4105(3) 0.125(3) Uani 1 2 d SDU . .
C12 C 0.3997(4) 1.0510(5) 0.3997(4) 0.136(3) Uani 1 2 d SU . .
H12A H 0.3901 1.0652 0.4258 0.164 Uiso 0.50 1 d PR . .
C13 C 0.3656(3) 1.0574(5) 0.3656(3) 0.137(3) Uani 1 2 d SDU . .
C14 C 0.3216(3) 1.0570(4) 0.3776(4) 0.147(3) Uani 1 1 d DU . .
H14A H 0.3138 1.0531 0.4065 0.176 Uiso 1 1 calc R . .
C15 C 0.2895(4) 1.0624(4) 0.3457(3) 0.151(3) Uani 1 1 d DU . .
C16 C 0.3019(4) 1.0630(5) 0.3019(4) 0.149(3) Uani 1 2 d SDU . .
H16A H 0.2805 1.0637 0.2805 0.179 Uiso 1 2 calc SR . .
C17 C 0.2448(4) 1.0608(5) 0.3604(5) 0.166(3) Uani 1 1 d DU . .
C18 C 0.1697(4) 1.0356(4) 0.3438(5) 0.193(3) Uani 1 1 d DU . .
H18A H 0.1530 1.0334 0.3171 0.231 Uiso 1 1 calc R . .
H18B H 0.1575 1.0595 0.3603 0.231 Uiso 1 1 calc R . .
C19 C 0.1734(4) 0.9177(3) 0.3699(4) 0.191(3) Uani 1 1 d DU . .
H19A H 0.1833 0.8929 0.3558 0.229 Uiso 1 1 calc R . .
C20 C 0.1791(4) 0.9584(4) 0.3499(4) 0.196(3) Uani 1 1 d DU . .
H20A H 0.1948 0.9608 0.3242 0.236 Uiso 1 1 calc R . .
C21 C 0.1610(4) 0.9949(3) 0.3693(4) 0.194(3) Uani 1 1 d DU . .
C22 C 0.1448(4) 0.9913(4) 0.4118(4) 0.193(3) Uani 1 1 d DU . .
H22A H 0.1405 1.0160 0.4287 0.231 Uiso 1 1 calc R . .
C23 C 0.1353(4) 0.9502(4) 0.4286(4) 0.190(3) Uani 1 1 d DU . .
H23A H 0.1166 0.9476 0.4522 0.228 Uiso 1 1 calc R . .
N4 N 0.1534(3) 0.9137(3) 0.4105(4) 0.179(3) Uani 1 1 d DU . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.1191(6) 0.1191(6) 0.2334(15) -0.0174(8) 0.0174(8) -0.0287(9)
O1 0.147(5) 0.148(5) 0.135(5) 0.005(4) 0.004(4) -0.044(4)
O2 0.144(5) 0.202(6) 0.186(6) -0.003(5) 0.030(5) -0.028(5)
N2 0.126(5) 0.149(5) 0.196(5) 0.024(5) -0.002(4) -0.054(4)
N3 0.158(5) 0.186(5) 0.217(5) 0.001(5) 0.012(5) -0.028(5)
N1 0.122(4) 0.137(4) 0.198(5) -0.001(4) 0.003(4) -0.037(4)
C1 0.115(4) 0.147(5) 0.196(5) 0.006(4) 0.005(5) -0.040(4)
C2 0.117(4) 0.145(5) 0.200(5) 0.008(5) 0.000(5) -0.036(4)
C3 0.117(4) 0.140(4) 0.198(5) 0.013(4) -0.002(4) -0.041(4)
C4 0.120(5) 0.148(5) 0.200(5) 0.013(5) 0.001(5) -0.042(5)
C5 0.118(5) 0.145(5) 0.198(5) 0.010(5) 0.000(5) -0.040(5)
C6 0.127(5) 0.151(5) 0.199(5) 0.022(5) -0.003(5) -0.044(5)
C7 0.113(5) 0.128(5) 0.161(5) 0.008(5) -0.020(4) -0.031(5)
C8 0.124(4) 0.118(6) 0.124(4) -0.017(4) -0.032(5) -0.017(4)
C9 0.102(4) 0.125(5) 0.136(5) 0.007(5) -0.018(4) -0.038(4)
C10 0.114(4) 0.126(5) 0.131(5) -0.011(4) -0.015(4) -0.028(4)
C11 0.126(4) 0.123(5) 0.126(4) -0.017(4) -0.014(5) -0.017(4)
C12 0.138(4) 0.134(6) 0.138(4) -0.016(4) -0.001(5) -0.016(4)
C13 0.140(4) 0.131(5) 0.140(4) -0.013(4) 0.007(5) -0.013(4)
C14 0.141(5) 0.143(5) 0.158(5) -0.004(5) 0.007(5) -0.018(5)
C15 0.144(5) 0.151(5) 0.160(5) -0.004(5) 0.008(5) -0.019(5)
C16 0.150(4) 0.146(6) 0.150(4) -0.010(4) 0.012(6) -0.010(4)
C17 0.153(5) 0.164(5) 0.180(5) -0.003(5) 0.008(5) -0.021(5)
C18 0.160(5) 0.182(5) 0.235(5) 0.010(5) 0.020(5) -0.035(5)
C19 0.152(5) 0.163(5) 0.256(6) 0.011(5) 0.027(5) -0.042(5)
C20 0.159(5) 0.175(5) 0.256(5) 0.004(5) 0.027(5) -0.031(5)
C21 0.159(5) 0.172(5) 0.250(5) 0.008(5) 0.025(5) -0.038(5)
C22 0.158(5) 0.167(5) 0.253(6) 0.006(5) 0.030(5) -0.030(5)
C23 0.148(5) 0.166(6) 0.257(6) 0.010(6) 0.032(5) -0.041(5)
N4 0.137(5) 0.157(5) 0.244(5) -0.008(5) 0.027(5) -0.026(4)

_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
C33 O13 1.529(12) . ?
C33 O13 1.529(12) 3_757 ?
O14 C34 1.525(12) . ?
O14' C34' 1.525(12) . ?
O15' C35' 1.527(13) . ?
O16 C36 1.531(12) . ?
C36 O16 1.531(12) 13 ?
O16' C36' 1.526(8) 14_665 ?
O16' C36' 1.526(8) . ?
O17 C37 1.525(8) . ?
O17' C37' 1.525(8) . ?
O18 C38 1.53(2) . ?
O18' C38' 1.524(8) . ?
O19 C39 1.527(7) . ?
C39 O19 1.527(7) 14_665 ?
O19' C39' 1.525(7) . ?
C39' O19' 1.525(7) 14_665 ?
O19" C39" 1.54(2) . ?
C39" O19" 1.54(2) 14_665 ?
C40 O40 1.522(12) 9_546 ?
C40 O40 1.522(12) 5_456 ?
C40 O40 1.522(12) . ?
O22' C42' 1.524(12) . ?
O23 C43 1.522(12) . ?
C43 O23 1.522(12) 3_658 ?
O21 C41 0.68(7) 3_658 ?
O21 C41 1.527(8) . ?
C41 O21 0.68(7) 3_658 ?
C41 C41 0.89(5) 3_658 ?
C44 O24 1.540(11) . ?
O25 O25 1.08(5) 2_655 ?
O25 C45 1.23(5) 2_655 ?
O25 C45 1.521(12) . ?
C45 O25 1.23(5) 2_655 ?
O25' C45' 1.521(12) . ?
O26 C46 1.517(12) . ?
O26 C46 1.69(4) 2_655 ?
C46 C46 0.97(6) 2_655 ?
C46 O26 1.69(4) 2_655 ?
O27 C47 1.531(12) . ?
O27' C47' 1.515(12) . ?
O27" C47" 1.521(12) . ?
O27" O27" 1.79(6) 17_546 ?
C47" O27" 1.521(12) 17_546 ?
O15 C35 1.525(13) . ?
O22 C42 1.528(12) . ?
N8 O82 1.19(2) . ?
N8 O83 1.20(2) . ?
N8 O81 1.21(2) . ?
N9 O91 1.187(16) . ?
N9 O93 1.19(2) . ?
N9 O92 1.21(2) . ?
N7 O71 1.141(18) . ?
N7 O72' 1.146(18) . ?
N7 O71' 1.151(18) . ?
N7 O73 1.154(19) . ?
N7 O72 1.161(19) . ?
N7 O73' 1.183(18) . ?
N6 O61 1.16(2) . ?
N6 O63 1.17(2) . ?
N6 O62 1.19(2) . ?
N6 N6 1.83(5) 3_757 ?
O61 O61 1.44(7) 3_757 ?
O62 N6 1.19(2) 4_567 ?
O62 N6 1.19(2) 2_765 ?
O62 N6 1.19(2) 3_757 ?
Pd1 N1 2.030(9) . ?
Pd1 N1 2.030(9) 14_665 ?
Pd1 N4 2.070(10) 14_665 ?
Pd1 N4 2.070(10) . ?
O1 C7 1.175(12) . ?
O2 C17 1.167(13) . ?
N2 C7 1.364(9) . ?
N2 C6 1.430(8) . ?
N3 C17 1.354(9) . ?
N3 C18 1.470(9) . ?
N1 C5 1.359(8) . ?
N1 C1 1.370(8) . ?
C1 C2 1.388(8) . ?
C2 C3 1.370(8) . ?
C3 C4 1.381(8) . ?
C3 C6 1.439(8) . ?
C4 C5 1.407(9) . ?
C7 C9 1.483(9) . ?
C8 C9 1.415(7) 21 ?
C8 C9 1.415(7) . ?
C9 C10 1.407(7) . ?
C10 C11 1.417(7) . ?
C11 C10 1.417(7) 21 ?
C11 C12 1.47(2) . ?
C12 C13 1.496(19) . ?
C13 C14 1.402(7) 21 ?
C13 C14 1.402(7) . ?
C14 C15 1.401(7) . ?
C15 C16 1.402(7) . ?
C15 C17 1.448(9) . ?
C16 C15 1.402(7) 21 ?
C18 C21 1.498(9) . ?
C19 N4 1.397(9) . ?
C19 C20 1.404(9) . ?
C20 C21 1.388(9) . ?
C21 C22 1.404(9) . ?
C22 C23 1.395(9) . ?
C23 N4 1.372(8) . ?

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
O13 C33 O13 118(7) . 3_757 ?
O16 C36 O16 135(5) 13 . ?
C36' O16' C36' 84(5) 14_665 . ?
O19 C39 O19 83(2) 14_665 . ?
O19' C39' O19' 105(3) 14_665 . ?
O19" C39" O19" 95(6) 14_665 . ?
O40 C40 O40 89(3) 9_546 5_456 ?
O40 C40 O40 89(3) 9_546 . ?
O40 C40 O40 89(3) 5_456 . ?
O23 C43 O23 122(3) . 3_658 ?
C41 O21 C41 16(3) 3_658 . ?
O21 C41 C41 151(6) 3_658 3_658 ?
O21 C41 O21 138(10) 3_658 . ?
C41 C41 O21 13(4) 3_658 . ?
O25 O25 C45 82(3) 2_655 2_655 ?
O25 O25 C45 53(3) 2_655 . ?
C45 O25 C45 119(4) 2_655 . ?
O25 C45 O25 45(3) 2_655 . ?
C46 O26 C46 35(2) . 2_655 ?
C46 C46 O26 83(3) 2_655 . ?
C46 C46 O26 63(2) 2_655 2_655 ?
O26 C46 O26 77(2) . 2_655 ?
C47" O27" O27" 53.9(15) . 17_546 ?
O27" C47" O27" 72(3) 17_546 . ?
O82 N8 O83 121(2) . . ?
O82 N8 O81 119.9(19) . . ?
O83 N8 O81 119.4(19) . . ?
O91 N9 O93 120.4(19) . . ?
O91 N9 O92 120.2(19) . . ?
O93 N9 O92 119.4(17) . . ?
O71 N7 O72' 171.0(18) . . ?
O71 N7 O71' 50.2(14) . . ?
O72' N7 O71' 120.7(16) . . ?
O71 N7 O73 120.4(17) . . ?
O72' N7 O73 50.5(18) . . ?
O71' N7 O73 70.2(18) . . ?
O71 N7 O72 119.8(17) . . ?
O72' N7 O72 69.3(17) . . ?
O71' N7 O72 170.0(19) . . ?
O73 N7 O72 119.8(17) . . ?
O71 N7 O73' 69.0(15) . . ?
O72' N7 O73' 120.0(16) . . ?
O71' N7 O73' 119.3(16) . . ?
O73 N7 O73' 170.5(19) . . ?
O72 N7 O73' 50.7(16) . . ?
O61 N6 O63 121(2) . . ?
O61 N6 O62 119.8(19) . . ?
O63 N6 O62 119.2(19) . . ?
O61 N6 N6 80.1(16) . 3_757 ?
O63 N6 N6 158.8(18) . 3_757 ?
O62 N6 N6 39.7(13) . 3_757 ?
N6 O61 O61 99.9(16) . 3_757 ?
N6 O62 N6 101(3) 4_567 2_765 ?
N6 O62 N6 114.1(14) 4_567 . ?
N6 O62 N6 114.1(14) 2_765 . ?
N6 O62 N6 114.1(14) 4_567 3_757 ?
N6 O62 N6 114.1(14) 2_765 3_757 ?
N6 O62 N6 101(3) . 3_757 ?
N1 Pd1 N1 85.6(5) . 14_665 ?
N1 Pd1 N4 174.3(4) . 14_665 ?
N1 Pd1 N4 92.2(4) 14_665 14_665 ?
N1 Pd1 N4 92.2(4) . . ?
N1 Pd1 N4 174.3(5) 14_665 . ?
N4 Pd1 N4 89.6(6) 14_665 . ?
C7 N2 C6 117.5(10) . . ?
C17 N3 C18 123.7(12) . . ?
C5 N1 C1 122.1(8) . . ?
C5 N1 Pd1 120.8(7) . . ?
C1 N1 Pd1 117.0(7) . . ?
N1 C1 C2 118.3(7) . . ?
C3 C2 C1 120.8(7) . . ?
C2 C3 C4 120.5(6) . . ?
C2 C3 C6 122.5(10) . . ?
C4 C3 C6 117.0(10) . . ?
C3 C4 C5 118.7(7) . . ?
N1 C5 C4 119.5(7) . . ?
N2 C6 C3 112.1(9) . . ?
O1 C7 N2 123.6(11) . . ?
O1 C7 C9 123.1(11) . . ?
N2 C7 C9 112.7(11) . . ?
C9 C8 C9 127.6(14) 21 . ?
C10 C9 C8 113.3(11) . . ?
C10 C9 C7 117.1(8) . . ?
C8 C9 C7 129.3(10) . . ?
C9 C10 C11 123.8(12) . . ?
C10 C11 C10 116.4(15) 21 . ?
C10 C11 C12 120.8(8) 21 . ?
C10 C11 C12 120.8(8) . . ?
C11 C12 C13 116.3(14) . . ?
C14 C13 C14 120.5(14) 21 . ?
C14 C13 C12 119.4(7) 21 . ?
C14 C13 C12 119.4(7) . . ?
C15 C14 C13 119.7(12) . . ?
C14 C15 C16 118.9(13) . . ?
C14 C15 C17 116.6(9) . . ?
C16 C15 C17 123.9(11) . . ?
C15 C16 C15 121.4(16) 21 . ?
O2 C17 N3 111.5(12) . . ?
O2 C17 C15 128.9(12) . . ?
N3 C17 C15 117.9(12) . . ?
N3 C18 C21 121.5(11) . . ?
N4 C19 C20 121.6(7) . . ?
C21 C20 C19 118.9(8) . . ?
C20 C21 C22 118.5(6) . . ?
C20 C21 C18 112.3(11) . . ?
C22 C21 C18 128.1(11) . . ?
C23 C22 C21 119.4(8) . . ?
N4 C23 C22 120.3(8) . . ?
C23 N4 C19 118.0(9) . . ?
C23 N4 Pd1 121.7(8) . . ?
C19 N4 Pd1 120.1(8) . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.049