Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge      186

_publ_requested_journal       'Dalton Transactions'

loop_
_publ_author_name
'James Darkwa'
'Galina A. Bikzhanova'
'Ilia A. Guzei'
'Kelin Li'
'Selwyn F. Mapolie'

_publ_contact_author_name     	'Prof James Darkwa'  
_publ_contact_author_address 
;
Department of Chemistry
University of the Western Cape
Private Bag X17
Bellville 7535
SOUTH AFRICA
;

_publ_contact_author_email       'JDARKWA@UWC.AC.ZA'

_publ_section_title		
;
Benzenedicarbonyl and Benzenetricarbonyl Linker
Pyrazolyl Complexes of Palladium(II): Synthesis, X-ray Structures and
Evaluation as Ethylene Polymerisation Catalysts
;

data_1
_database_code_CSD                  185333

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C30 H42 N4 O2' 
_chemical_formula_weight          490.68 

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' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

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                    11.0518(8) 
_cell_length_b                    25.9439(19) 
_cell_length_c                    10.0002(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  92.3630(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      2864.9(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.40 
_exptl_crystal_size_mid           0.30 
_exptl_crystal_size_min           0.30 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.138 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1064 
_exptl_absorpt_coefficient_mu     0.072 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.9718 
_exptl_absorpt_correction_T_max   0.9788 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       173(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   ? 
_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             5851 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0189 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        32 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          2.57 
_diffrn_reflns_theta_max          26.37 
_reflns_number_total              5851 
_reflns_number_gt                 4889 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.0910P)^2^+0.6030P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5851 
_refine_ls_number_parameters      337 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0537 
_refine_ls_R_factor_gt            0.0447 
_refine_ls_wR_factor_ref          0.1297 
_refine_ls_wR_factor_gt           0.1241 
_refine_ls_goodness_of_fit_ref    0.928 
_refine_ls_restrained_S_all       0.928 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_adp_type 
_atom_site_occupancy 
_atom_site_symmetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
O1 O 1.16413(11) 0.60884(5) -0.20345(10) 0.0484(3) Uani 1 1 d . . . 
O2 O 0.69652(11) 0.66498(4) 0.08552(14) 0.0523(3) Uani 1 1 d . . . 
N1 N 1.10856(9) 0.61967(4) 0.13548(10) 0.0250(2) Uani 1 1 d . . . 
N2 N 1.13636(9) 0.59499(4) 0.01738(10) 0.0241(2) Uani 1 1 d . . . 
N3 N 0.65153(10) 0.74826(4) 0.03022(11) 0.0271(2) Uani 1 1 d . . . 
N4 N 0.71246(10) 0.79482(4) 0.02797(11) 0.0289(3) Uani 1 1 d . . . 
C1 C 1.06164(14) 0.55916(6) 0.44088(14) 0.0378(3) Uani 1 1 d . . . 
H1A H 0.9807 0.5587 0.3971 0.057 Uiso 1 1 calc R . . 
H1B H 1.0548 0.5661 0.5366 0.057 Uiso 1 1 calc R . . 
H1C H 1.1008 0.5257 0.4289 0.057 Uiso 1 1 calc R . . 
C2 C 1.26343(14) 0.60167(7) 0.44998(14) 0.0435(4) Uani 1 1 d . . . 
H2A H 1.3031 0.5684 0.4364 0.065 Uiso 1 1 calc R . . 
H2B H 1.2548 0.6075 0.5459 0.065 Uiso 1 1 calc R . . 
H2C H 1.3126 0.6293 0.4132 0.065 Uiso 1 1 calc R . . 
C3 C 1.07612(17) 0.65352(6) 0.39518(15) 0.0455(4) Uani 1 1 d . . . 
H3A H 1.1259 0.6806 0.3570 0.068 Uiso 1 1 calc R . . 
H3B H 1.0666 0.6604 0.4906 0.068 Uiso 1 1 calc R . . 
H3C H 0.9963 0.6530 0.3487 0.068 Uiso 1 1 calc R . . 
C4 C 1.13759(12) 0.60145(5) 0.37848(12) 0.0284(3) Uani 1 1 d . . . 
C5 C 1.15126(11) 0.58916(5) 0.23156(12) 0.0244(3) Uani 1 1 d . . . 
C6 C 1.20680(12) 0.54495(5) 0.17806(13) 0.0276(3) Uani 1 1 d . . . 
H6 H 1.2435 0.5176 0.2282 0.033 Uiso 1 1 calc R . . 
C7 C 1.19828(11) 0.54851(5) 0.04243(12) 0.0248(3) Uani 1 1 d . . . 
C8 C 1.23926(12) 0.50893(5) -0.05874(14) 0.0302(3) Uani 1 1 d . . . 
C9 C 1.27812(18) 0.46032(6) 0.01985(17) 0.0481(4) Uani 1 1 d . . . 
H9A H 1.3462 0.4687 0.0819 0.072 Uiso 1 1 calc R . . 
H9B H 1.3029 0.4336 -0.0427 0.072 Uiso 1 1 calc R . . 
H9C H 1.2100 0.4477 0.0704 0.072 Uiso 1 1 calc R . . 
C10 C 1.35007(13) 0.52763(6) -0.13279(16) 0.0387(3) Uani 1 1 d . . . 
H10A H 1.3271 0.5571 -0.1897 0.058 Uiso 1 1 calc R . . 
H10B H 1.3799 0.4996 -0.1884 0.058 Uiso 1 1 calc R . . 
H10C H 1.4139 0.5381 -0.0675 0.058 Uiso 1 1 calc R . . 
C11 C 1.13540(15) 0.49360(7) -0.15711(17) 0.0461(4) Uani 1 1 d . . . 
H11A H 1.0658 0.4822 -0.1071 0.069 Uiso 1 1 calc R . . 
H11B H 1.1620 0.4654 -0.2143 0.069 Uiso 1 1 calc R . . 
H11C H 1.1120 0.5233 -0.2128 0.069 Uiso 1 1 calc R . . 
C12 C 1.11234(12) 0.62108(5) -0.10403(13) 0.0286(3) Uani 1 1 d . . . 
C13 C 1.02082(12) 0.66354(5) -0.11077(12) 0.0257(3) Uani 1 1 d . . . 
C14 C 1.03370(13) 0.69863(5) -0.21527(13) 0.0303(3) Uani 1 1 d . . . 
H14 H 1.1028 0.6968 -0.2685 0.036 Uiso 1 1 calc R . . 
C15 C 0.94702(14) 0.73592(6) -0.24183(14) 0.0351(3) Uani 1 1 d . . . 
H15 H 0.9571 0.7596 -0.3130 0.042 Uiso 1 1 calc R . . 
C16 C 0.84549(13) 0.73908(5) -0.16560(14) 0.0321(3) Uani 1 1 d . . . 
H16 H 0.7854 0.7645 -0.1851 0.038 Uiso 1 1 calc R . . 
C17 C 0.83211(12) 0.70468(5) -0.06002(13) 0.0266(3) Uani 1 1 d . . . 
C18 C 0.91923(11) 0.66662(5) -0.03341(12) 0.0253(3) Uani 1 1 d . . . 
H18 H 0.9091 0.6428 0.0375 0.030 Uiso 1 1 calc R . . 
C19 C 0.72318(12) 0.70302(5) 0.02396(14) 0.0314(3) Uani 1 1 d . . . 
C20 C 0.43870(17) 0.67668(6) -0.05199(16) 0.0455(4) Uani 1 1 d . . . 
H20A H 0.4333 0.6970 -0.1347 0.068 Uiso 1 1 calc R . . 
H20B H 0.3705 0.6525 -0.0509 0.068 Uiso 1 1 calc R . . 
H20C H 0.5150 0.6574 -0.0477 0.068 Uiso 1 1 calc R . . 
C21 C 0.44665(16) 0.68189(6) 0.19920(16) 0.0441(4) Uani 1 1 d . . . 
H21A H 0.5256 0.6646 0.2045 0.066 Uiso 1 1 calc R . . 
H21B H 0.3821 0.6560 0.2007 0.066 Uiso 1 1 calc R . . 
H21C H 0.4402 0.7052 0.2757 0.066 Uiso 1 1 calc R . . 
C22 C 0.31038(14) 0.73940(7) 0.0649(2) 0.0485(4) Uani 1 1 d . . . 
H22A H 0.3055 0.7626 0.1418 0.073 Uiso 1 1 calc R . . 
H22B H 0.2465 0.7133 0.0685 0.073 Uiso 1 1 calc R . . 
H22C H 0.2998 0.7592 -0.0182 0.073 Uiso 1 1 calc R . . 
C23 C 0.43439(12) 0.71287(5) 0.06886(14) 0.0306(3) Uani 1 1 d . . . 
C24 C 0.53106(11) 0.75468(5) 0.06344(12) 0.0258(3) Uani 1 1 d . . . 
C25 C 0.51827(12) 0.80651(5) 0.07967(13) 0.0267(3) Uani 1 1 d . . . 
H25 H 0.4461 0.8240 0.1015 0.032 Uiso 1 1 calc R . . 
C26 C 0.63160(12) 0.82961(5) 0.05825(12) 0.0256(3) Uani 1 1 d . . . 
C27 C 0.66652(12) 0.88628(5) 0.06378(13) 0.0291(3) Uani 1 1 d . . . 
C28 C 0.79154(14) 0.89190(6) 0.13404(18) 0.0407(4) Uani 1 1 d . . . 
H28A H 0.7886 0.8790 0.2259 0.061 Uiso 1 1 calc R . . 
H28B H 0.8151 0.9283 0.1357 0.061 Uiso 1 1 calc R . . 
H28C H 0.8510 0.8720 0.0855 0.061 Uiso 1 1 calc R . . 
C29 C 0.57395(14) 0.91661(6) 0.14166(18) 0.0432(4) Uani 1 1 d . . . 
H29A H 0.4940 0.9138 0.0960 0.065 Uiso 1 1 calc R . . 
H29B H 0.5981 0.9529 0.1465 0.065 Uiso 1 1 calc R . . 
H29C H 0.5704 0.9026 0.2324 0.065 Uiso 1 1 calc R . . 
C30 C 0.6697(2) 0.90718(6) -0.07915(17) 0.0575(5) Uani 1 1 d . . . 
H30A H 0.7266 0.8868 -0.1300 0.086 Uiso 1 1 calc R . . 
H30B H 0.6960 0.9433 -0.0767 0.086 Uiso 1 1 calc R . . 
H30C H 0.5887 0.9049 -0.1223 0.086 Uiso 1 1 calc R . . 

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 
O1 0.0590(7) 0.0597(7) 0.0274(5) 0.0092(5) 0.0138(5) 0.0287(6) 
O2 0.0455(6) 0.0304(6) 0.0827(9) 0.0146(6) 0.0242(6) 0.0086(5) 
N1 0.0263(5) 0.0280(5) 0.0207(5) -0.0016(4) 0.0011(4) 0.0006(4) 
N2 0.0244(5) 0.0271(5) 0.0208(5) -0.0009(4) 0.0009(4) 0.0018(4) 
N3 0.0273(6) 0.0225(5) 0.0316(6) -0.0012(4) 0.0021(4) 0.0006(4) 
N4 0.0292(6) 0.0228(5) 0.0346(6) -0.0027(4) 0.0012(5) -0.0004(4) 
C1 0.0403(8) 0.0445(8) 0.0291(7) 0.0014(6) 0.0070(6) -0.0094(7) 
C2 0.0370(8) 0.0694(11) 0.0239(7) -0.0002(7) -0.0029(6) -0.0125(7) 
C3 0.0691(11) 0.0393(8) 0.0284(7) -0.0059(6) 0.0049(7) 0.0051(8) 
C4 0.0313(7) 0.0326(7) 0.0212(6) 0.0002(5) 0.0005(5) -0.0039(5) 
C5 0.0230(6) 0.0267(6) 0.0236(6) 0.0014(5) -0.0002(5) -0.0037(5) 
C6 0.0290(7) 0.0269(6) 0.0268(6) 0.0023(5) -0.0020(5) 0.0006(5) 
C7 0.0211(6) 0.0262(6) 0.0272(6) -0.0003(5) 0.0004(5) -0.0014(5) 
C8 0.0305(7) 0.0287(7) 0.0316(7) -0.0049(5) 0.0025(5) 0.0011(5) 
C9 0.0700(11) 0.0292(8) 0.0458(9) -0.0026(6) 0.0094(8) 0.0097(7) 
C10 0.0312(7) 0.0418(8) 0.0436(8) -0.0046(7) 0.0086(6) 0.0061(6) 
C11 0.0406(9) 0.0559(10) 0.0417(9) -0.0209(7) 0.0019(7) -0.0076(7) 
C12 0.0288(7) 0.0352(7) 0.0218(6) 0.0013(5) 0.0013(5) 0.0040(5) 
C13 0.0288(6) 0.0271(6) 0.0209(6) -0.0019(5) -0.0034(5) 0.0005(5) 
C14 0.0337(7) 0.0345(7) 0.0227(6) 0.0004(5) 0.0023(5) 0.0006(6) 
C15 0.0489(9) 0.0307(7) 0.0256(7) 0.0044(5) 0.0012(6) 0.0039(6) 
C16 0.0395(8) 0.0280(7) 0.0283(7) -0.0008(5) -0.0032(6) 0.0083(6) 
C17 0.0290(6) 0.0228(6) 0.0276(6) -0.0050(5) -0.0020(5) 0.0006(5) 
C18 0.0296(6) 0.0227(6) 0.0233(6) -0.0020(5) -0.0018(5) -0.0002(5) 
C19 0.0311(7) 0.0240(7) 0.0392(8) -0.0010(5) 0.0021(6) 0.0016(5) 
C20 0.0545(10) 0.0395(9) 0.0426(9) -0.0068(7) 0.0018(7) -0.0150(7) 
C21 0.0491(9) 0.0423(9) 0.0418(8) 0.0115(7) 0.0109(7) -0.0049(7) 
C22 0.0286(8) 0.0427(9) 0.0744(12) 0.0058(8) 0.0031(7) -0.0038(6) 
C23 0.0306(7) 0.0286(7) 0.0326(7) 0.0025(5) 0.0027(5) -0.0034(5) 
C24 0.0266(6) 0.0293(7) 0.0215(6) 0.0014(5) 0.0010(5) 0.0021(5) 
C25 0.0273(6) 0.0270(6) 0.0260(6) 0.0004(5) 0.0016(5) 0.0029(5) 
C26 0.0290(6) 0.0249(6) 0.0226(6) -0.0002(5) -0.0012(5) 0.0025(5) 
C27 0.0338(7) 0.0237(6) 0.0297(7) -0.0014(5) -0.0001(5) 0.0004(5) 
C28 0.0329(8) 0.0305(7) 0.0587(10) -0.0048(7) -0.0001(7) -0.0034(6) 
C29 0.0353(8) 0.0294(7) 0.0646(10) -0.0143(7) 0.0001(7) 0.0024(6) 
C30 0.1046(16) 0.0300(8) 0.0376(9) 0.0047(6) -0.0032(9) -0.0122(9) 

_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 
O1 C12 1.2098(16) . ? 
O2 C19 1.2060(17) . ? 
N1 C5 1.3172(16) . ? 
N1 N2 1.3889(14) . ? 
N2 C7 1.4040(16) . ? 
N2 C12 1.4057(16) . ? 
N3 N4 1.3837(15) . ? 
N3 C24 1.3955(17) . ? 
N3 C19 1.4186(17) . ? 
N4 C26 1.3140(17) . ? 
C1 C4 1.5299(19) . ? 
C2 C4 1.537(2) . ? 
C3 C4 1.524(2) . ? 
C4 C5 1.5170(18) . ? 
C5 C6 1.4162(18) . ? 
C6 C7 1.3589(18) . ? 
C7 C8 1.5235(18) . ? 
C8 C11 1.533(2) . ? 
C8 C10 1.536(2) . ? 
C8 C9 1.538(2) . ? 
C12 C13 1.4952(18) . ? 
C13 C18 1.3918(18) . ? 
C13 C14 1.3977(18) . ? 
C14 C15 1.380(2) . ? 
C15 C16 1.385(2) . ? 
C16 C17 1.3950(19) . ? 
C17 C18 1.3971(18) . ? 
C17 C19 1.4966(19) . ? 
C20 C23 1.533(2) . ? 
C21 C23 1.532(2) . ? 
C22 C23 1.533(2) . ? 
C23 C24 1.5250(18) . ? 
C24 C25 1.3626(18) . ? 
C25 C26 1.4128(18) . ? 
C26 C27 1.5205(18) . ? 
C27 C29 1.529(2) . ? 
C27 C30 1.531(2) . ? 
C27 C28 1.531(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 
C5 N1 N2 104.96(10) . . ? 
N1 N2 C7 111.56(10) . . ? 
N1 N2 C12 118.16(10) . . ? 
C7 N2 C12 129.86(11) . . ? 
N4 N3 C24 111.68(10) . . ? 
N4 N3 C19 116.67(10) . . ? 
C24 N3 C19 130.46(11) . . ? 
C26 N4 N3 105.06(10) . . ? 
C5 C4 C3 110.79(11) . . ? 
C5 C4 C1 108.82(11) . . ? 
C3 C4 C1 109.65(12) . . ? 
C5 C4 C2 109.08(11) . . ? 
C3 C4 C2 110.14(13) . . ? 
C1 C4 C2 108.30(12) . . ? 
N1 C5 C6 111.04(11) . . ? 
N1 C5 C4 122.22(11) . . ? 
C6 C5 C4 126.73(12) . . ? 
C7 C6 C5 107.98(11) . . ? 
C6 C7 N2 104.46(11) . . ? 
C6 C7 C8 127.36(12) . . ? 
N2 C7 C8 128.06(11) . . ? 
C7 C8 C11 111.46(12) . . ? 
C7 C8 C10 111.84(11) . . ? 
C11 C8 C10 111.31(12) . . ? 
C7 C8 C9 107.32(11) . . ? 
C11 C8 C9 107.53(13) . . ? 
C10 C8 C9 107.10(12) . . ? 
O1 C12 N2 120.30(12) . . ? 
O1 C12 C13 119.90(12) . . ? 
N2 C12 C13 119.80(11) . . ? 
C18 C13 C14 119.18(12) . . ? 
C18 C13 C12 125.24(12) . . ? 
C14 C13 C12 115.09(11) . . ? 
C15 C14 C13 120.62(13) . . ? 
C14 C15 C16 120.50(13) . . ? 
C15 C16 C17 119.50(12) . . ? 
C16 C17 C18 120.17(12) . . ? 
C16 C17 C19 123.78(12) . . ? 
C18 C17 C19 115.90(12) . . ? 
C13 C18 C17 120.01(12) . . ? 
O2 C19 N3 120.39(12) . . ? 
O2 C19 C17 121.95(12) . . ? 
N3 C19 C17 117.66(11) . . ? 
C24 C23 C21 111.45(12) . . ? 
C24 C23 C20 111.29(11) . . ? 
C21 C23 C20 110.18(12) . . ? 
C24 C23 C22 107.85(12) . . ? 
C21 C23 C22 107.77(13) . . ? 
C20 C23 C22 108.14(13) . . ? 
C25 C24 N3 104.52(11) . . ? 
C25 C24 C23 128.43(12) . . ? 
N3 C24 C23 126.89(11) . . ? 
C24 C25 C26 107.67(11) . . ? 
N4 C26 C25 111.05(11) . . ? 
N4 C26 C27 119.90(12) . . ? 
C25 C26 C27 129.04(12) . . ? 
C26 C27 C29 110.00(11) . . ? 
C26 C27 C30 108.92(11) . . ? 
C29 C27 C30 109.58(13) . . ? 
C26 C27 C28 109.37(11) . . ? 
C29 C27 C28 109.11(12) . . ? 
C30 C27 C28 109.85(14) . . ? 

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 
C5 N1 N2 C7 -0.44(13) . . . . ? 
C5 N1 N2 C12 -173.80(11) . . . . ? 
C24 N3 N4 C26 -0.40(14) . . . . ? 
C19 N3 N4 C26 -169.24(11) . . . . ? 
N2 N1 C5 C6 0.12(14) . . . . ? 
N2 N1 C5 C4 -178.76(11) . . . . ? 
C3 C4 C5 N1 -3.08(18) . . . . ? 
C1 C4 C5 N1 117.54(14) . . . . ? 
C2 C4 C5 N1 -124.49(14) . . . . ? 
C3 C4 C5 C6 178.22(13) . . . . ? 
C1 C4 C5 C6 -61.16(17) . . . . ? 
C2 C4 C5 C6 56.81(17) . . . . ? 
N1 C5 C6 C7 0.24(15) . . . . ? 
C4 C5 C6 C7 179.06(12) . . . . ? 
C5 C6 C7 N2 -0.48(14) . . . . ? 
C5 C6 C7 C8 -176.69(12) . . . . ? 
N1 N2 C7 C6 0.58(13) . . . . ? 
C12 N2 C7 C6 172.95(12) . . . . ? 
N1 N2 C7 C8 176.76(12) . . . . ? 
C12 N2 C7 C8 -10.9(2) . . . . ? 
C6 C7 C8 C11 124.60(15) . . . . ? 
N2 C7 C8 C11 -50.74(18) . . . . ? 
C6 C7 C8 C10 -110.08(15) . . . . ? 
N2 C7 C8 C10 74.59(17) . . . . ? 
C6 C7 C8 C9 7.11(19) . . . . ? 
N2 C7 C8 C9 -168.23(13) . . . . ? 
N1 N2 C12 O1 158.94(13) . . . . ? 
C7 N2 C12 O1 -13.0(2) . . . . ? 
N1 N2 C12 C13 -22.09(17) . . . . ? 
C7 N2 C12 C13 165.97(12) . . . . ? 
O1 C12 C13 C18 148.55(14) . . . . ? 
N2 C12 C13 C18 -30.42(19) . . . . ? 
O1 C12 C13 C14 -23.31(19) . . . . ? 
N2 C12 C13 C14 157.72(12) . . . . ? 
C18 C13 C14 C15 -0.02(19) . . . . ? 
C12 C13 C14 C15 172.37(12) . . . . ? 
C13 C14 C15 C16 -0.2(2) . . . . ? 
C14 C15 C16 C17 1.0(2) . . . . ? 
C15 C16 C17 C18 -1.4(2) . . . . ? 
C15 C16 C17 C19 -176.76(13) . . . . ? 
C14 C13 C18 C17 -0.46(18) . . . . ? 
C12 C13 C18 C17 -172.01(12) . . . . ? 
C16 C17 C18 C13 1.19(19) . . . . ? 
C19 C17 C18 C13 176.88(11) . . . . ? 
N4 N3 C19 O2 144.16(14) . . . . ? 
C24 N3 C19 O2 -22.2(2) . . . . ? 
N4 N3 C19 C17 -35.31(17) . . . . ? 
C24 N3 C19 C17 158.35(12) . . . . ? 
C16 C17 C19 O2 157.45(15) . . . . ? 
C18 C17 C19 O2 -18.1(2) . . . . ? 
C16 C17 C19 N3 -23.09(19) . . . . ? 
C18 C17 C19 N3 161.40(11) . . . . ? 
N4 N3 C24 C25 0.93(14) . . . . ? 
C19 N3 C24 C25 167.80(13) . . . . ? 
N4 N3 C24 C23 176.61(11) . . . . ? 
C19 N3 C24 C23 -16.5(2) . . . . ? 
C21 C23 C24 C25 -105.50(16) . . . . ? 
C20 C23 C24 C25 131.07(15) . . . . ? 
C22 C23 C24 C25 12.60(19) . . . . ? 
C21 C23 C24 N3 79.84(16) . . . . ? 
C20 C23 C24 N3 -43.59(18) . . . . ? 
C22 C23 C24 N3 -162.06(13) . . . . ? 
N3 C24 C25 C26 -1.06(13) . . . . ? 
C23 C24 C25 C26 -176.65(12) . . . . ? 
N3 N4 C26 C25 -0.30(14) . . . . ? 
N3 N4 C26 C27 -179.31(11) . . . . ? 
C24 C25 C26 N4 0.89(15) . . . . ? 
C24 C25 C26 C27 179.80(12) . . . . ? 
N4 C26 C27 C29 -162.25(12) . . . . ? 
C25 C26 C27 C29 18.92(18) . . . . ? 
N4 C26 C27 C30 77.63(17) . . . . ? 
C25 C26 C27 C30 -101.19(17) . . . . ? 
N4 C26 C27 C28 -42.43(16) . . . . ? 
C25 C26 C27 C28 138.74(14) . . . . ? 

_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              26.37 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.438 
_refine_diff_density_min   -0.326 
_refine_diff_density_rms    0.038 



data_darj 
_database_code_CSD                  185334

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C42 H60 N6 O3' 
_chemical_formula_weight          696.96 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'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' 
'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' 

_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    Pbca 

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

_cell_length_a                    19.3167(13) 
_cell_length_b                    14.3940(11) 
_cell_length_c                    29.844(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      8297.8(11) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.116 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3024 
_exptl_absorpt_coefficient_mu     0.071 
_exptl_absorpt_correction_type    'Empirical with SADABS'
_exptl_absorpt_correction_T_min   0.9654 
_exptl_absorpt_correction_T_max   0.9860 
_exptl_absorpt_process_details    ? 


_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7311 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0248 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        35 
_diffrn_reflns_theta_min          1.72 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              7311 
_reflns_number_gt                 5507 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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^)+(0.1243P)^2^+6.1531P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7311 
_refine_ls_number_parameters      508 
_refine_ls_number_restraints      57 
_refine_ls_R_factor_all           0.0878 
_refine_ls_R_factor_gt            0.0657 
_refine_ls_wR_factor_ref          0.2078 
_refine_ls_wR_factor_gt           0.1930 
_refine_ls_goodness_of_fit_ref    0.995 
_refine_ls_restrained_S_all       1.010 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 

loop_ 
_atom_site_label 
_atom_site_type_symbol 
_atom_site_fract_x 
_atom_site_fract_y 
_atom_site_fract_z 
_atom_site_U_iso_or_equiv 
_atom_site_adp_type 
_atom_site_occupancy 
_atom_site_symmetry_multiplicity 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
O1 O 0.96820(12) 0.49382(16) 0.05754(7) 0.0610(6) Uani 1 1 d . . . 
O2 O 1.25178(11) 0.60530(17) 0.14271(9) 0.0731(8) Uani 1 1 d . . . 
O3 O 1.15382(10) 0.41763(14) 0.25932(6) 0.0480(5) Uani 1 1 d . . . 
N1 N 0.93089(11) 0.37022(14) 0.09872(7) 0.0349(5) Uani 1 1 d . . . 
N2 N 0.95698(12) 0.29447(15) 0.12199(7) 0.0405(5) Uani 1 1 d . . . 
N3 N 1.11682(11) 0.71295(13) 0.08584(7) 0.0326(5) Uani 1 1 d . . . 
N4 N 1.18489(10) 0.68925(13) 0.09484(6) 0.0301(5) Uani 1 1 d . . . 
N5 N 1.04154(10) 0.36967(14) 0.26113(6) 0.0310(5) Uani 1 1 d . . . 
N6 N 0.97692(10) 0.40860(15) 0.25455(7) 0.0337(5) Uani 1 1 d . . . 
C1 C 1.03317(13) 0.46475(16) 0.12296(8) 0.0315(5) Uani 1 1 d . . . 
C2 C 1.08385(13) 0.52761(16) 0.10879(8) 0.0333(6) Uani 1 1 d . . . 
H2 H 1.0828 0.5511 0.0790 0.040 Uiso 1 1 calc R . . 
C3 C 1.13591(12) 0.55600(16) 0.13812(8) 0.0329(6) Uani 1 1 d . . . 
C4 C 1.13779(13) 0.51989(17) 0.18112(9) 0.0338(6) Uani 1 1 d . . . 
H4 H 1.1742 0.5373 0.2008 0.041 Uiso 1 1 calc R . . 
C5 C 1.08692(12) 0.45826(16) 0.19599(8) 0.0299(5) Uani 1 1 d . . . 
C6 C 1.03448(13) 0.43163(16) 0.16689(8) 0.0311(5) Uani 1 1 d . . . 
H6 H 0.9993 0.3906 0.1770 0.037 Uiso 1 1 calc R . . 
C7 C 0.97689(14) 0.44525(18) 0.08994(8) 0.0380(6) Uani 1 1 d . . . 
C8 C 0.90447(15) 0.23607(18) 0.12545(8) 0.0396(6) Uani 1 1 d . A . 
C9 C 0.91176(14) 0.14530(18) 0.15051(8) 0.0503(8) Uani 1 1 d D . . 
C10A C 0.9525(4) 0.1612(7) 0.1940(2) 0.0594(9) Uiso 0.347(6) 1 d PD A 1 
H10A H 0.9997 0.1814 0.1867 0.089 Uiso 0.347(6) 1 calc PR A 1 
H10B H 0.9545 0.1031 0.2111 0.089 Uiso 0.347(6) 1 calc PR A 1 
H10C H 0.9295 0.2092 0.2119 0.089 Uiso 0.347(6) 1 calc PR A 1 
C11A C 0.8414(3) 0.1035(7) 0.1635(3) 0.0594(9) Uiso 0.347(6) 1 d PD A 1 
H11A H 0.8158 0.1480 0.1820 0.089 Uiso 0.347(6) 1 calc PR A 1 
H11B H 0.8487 0.0460 0.1805 0.089 Uiso 0.347(6) 1 calc PR A 1 
H11C H 0.8149 0.0897 0.1363 0.089 Uiso 0.347(6) 1 calc PR A 1 
C12A C 0.9510(5) 0.0737(5) 0.1223(3) 0.0594(9) Uiso 0.347(6) 1 d PD A 1 
H12A H 0.9300 0.0698 0.0924 0.089 Uiso 0.347(6) 1 calc PR A 1 
H12B H 0.9486 0.0128 0.1369 0.089 Uiso 0.347(6) 1 calc PR A 1 
H12C H 0.9995 0.0927 0.1194 0.089 Uiso 0.347(6) 1 calc PR A 1 
C10B C 0.9730(3) 0.1451(6) 0.1830(2) 0.0594(9) Uiso 0.410(6) 1 d PD A 2 
H10D H 1.0159 0.1561 0.1664 0.089 Uiso 0.410(6) 1 calc PR A 2 
H10E H 0.9756 0.0848 0.1981 0.089 Uiso 0.410(6) 1 calc PR A 2 
H10F H 0.9666 0.1943 0.2053 0.089 Uiso 0.410(6) 1 calc PR A 2 
C11B C 0.8440(3) 0.1319(6) 0.1772(3) 0.0594(9) Uiso 0.410(6) 1 d PD A 2 
H11D H 0.8378 0.1842 0.1979 0.089 Uiso 0.410(6) 1 calc PR A 2 
H11E H 0.8465 0.0738 0.1942 0.089 Uiso 0.410(6) 1 calc PR A 2 
H11F H 0.8048 0.1293 0.1564 0.089 Uiso 0.410(6) 1 calc PR A 2 
C12B C 0.9180(5) 0.0661(4) 0.1165(2) 0.0594(9) Uiso 0.410(6) 1 d PD A 2 
H12D H 0.8790 0.0688 0.0956 0.089 Uiso 0.410(6) 1 calc PR A 2 
H12E H 0.9174 0.0064 0.1323 0.089 Uiso 0.410(6) 1 calc PR A 2 
H12F H 0.9615 0.0723 0.0999 0.089 Uiso 0.410(6) 1 calc PR A 2 
C10C C 0.9895(2) 0.1228(9) 0.1522(4) 0.0594(9) Uiso 0.243(4) 1 d PD A 3 
H10G H 1.0061 0.1080 0.1220 0.089 Uiso 0.243(4) 1 calc PR A 3 
H10H H 0.9972 0.0693 0.1719 0.089 Uiso 0.243(4) 1 calc PR A 3 
H10I H 1.0149 0.1766 0.1638 0.089 Uiso 0.243(4) 1 calc PR A 3 
C12C C 0.8739(5) 0.0662(7) 0.1264(4) 0.0594(9) Uiso 0.243(4) 1 d PD A 3 
H12G H 0.8239 0.0771 0.1277 0.089 Uiso 0.243(4) 1 calc PR A 3 
H12H H 0.8847 0.0071 0.1412 0.089 Uiso 0.243(4) 1 calc PR A 3 
H12I H 0.8889 0.0637 0.0951 0.089 Uiso 0.243(4) 1 calc PR A 3 
C11C C 0.8841(5) 0.1557(10) 0.19832(18) 0.0594(9) Uiso 0.243(4) 1 d PD A 3 
H11G H 0.9126 0.2005 0.2147 0.089 Uiso 0.243(4) 1 calc PR A 3 
H11H H 0.8858 0.0954 0.2135 0.089 Uiso 0.243(4) 1 calc PR A 3 
H11I H 0.8361 0.1777 0.1973 0.089 Uiso 0.243(4) 1 calc PR A 3 
C13 C 0.84491(15) 0.27332(19) 0.10474(8) 0.0402(6) Uani 1 1 d . . . 
H13 H 0.8008 0.2443 0.1032 0.048 Uiso 1 1 calc R A . 
C14 C 0.86156(14) 0.35811(18) 0.08734(8) 0.0352(6) Uani 1 1 d . A . 
C15 C 0.81491(15) 0.42561(19) 0.06289(9) 0.0406(6) Uani 1 1 d . . . 
C16 C 0.74009(16) 0.3897(3) 0.06636(11) 0.0598(8) Uani 1 1 d . A . 
H16A H 0.7370 0.3282 0.0525 0.090 Uiso 1 1 calc R . . 
H16B H 0.7089 0.4327 0.0508 0.090 Uiso 1 1 calc R . . 
H16C H 0.7267 0.3854 0.0980 0.090 Uiso 1 1 calc R . . 
C17 C 0.83354(16) 0.4312(2) 0.01259(9) 0.0464(7) Uani 1 1 d . A . 
H17A H 0.8804 0.4563 0.0092 0.070 Uiso 1 1 calc R . . 
H17B H 0.8005 0.4718 -0.0028 0.070 Uiso 1 1 calc R . . 
H17C H 0.8316 0.3689 -0.0006 0.070 Uiso 1 1 calc R . . 
C18 C 0.8166(2) 0.5236(2) 0.08414(11) 0.0601(9) Uani 1 1 d . A . 
H18A H 0.8066 0.5188 0.1162 0.090 Uiso 1 1 calc R . . 
H18B H 0.7818 0.5630 0.0697 0.090 Uiso 1 1 calc R . . 
H18C H 0.8626 0.5509 0.0799 0.090 Uiso 1 1 calc R . . 
C19 C 1.19565(14) 0.61705(19) 0.12571(9) 0.0412(6) Uani 1 1 d . . . 
C20 C 1.12023(14) 0.78479(17) 0.05883(8) 0.0352(6) Uani 1 1 d . B . 
C21 C 1.05492(14) 0.82899(17) 0.04067(8) 0.0453(7) Uani 1 1 d D . . 
C22A C 1.0670(7) 0.8699(7) -0.00604(17) 0.0587(9) Uiso 0.267(4) 1 d PD B 1 
H22A H 1.1024 0.9186 -0.0043 0.088 Uiso 0.267(4) 1 calc PR B 1 
H22B H 1.0237 0.8966 -0.0173 0.088 Uiso 0.267(4) 1 calc PR B 1 
H22C H 1.0827 0.8208 -0.0264 0.088 Uiso 0.267(4) 1 calc PR B 1 
C23A C 1.0308(6) 0.9062(5) 0.0724(3) 0.0587(9) Uiso 0.267(4) 1 d PD B 1 
H23A H 1.0199 0.8794 0.1018 0.088 Uiso 0.267(4) 1 calc PR B 1 
H23B H 0.9895 0.9362 0.0601 0.088 Uiso 0.267(4) 1 calc PR B 1 
H23C H 1.0678 0.9523 0.0758 0.088 Uiso 0.267(4) 1 calc PR B 1 
C24A C 0.9975(5) 0.7554(7) 0.0377(4) 0.0587(9) Uiso 0.267(4) 1 d PD B 1 
H24A H 1.0102 0.7083 0.0155 0.088 Uiso 0.267(4) 1 calc PR B 1 
H24B H 0.9540 0.7851 0.0288 0.088 Uiso 0.267(4) 1 calc PR B 1 
H24C H 0.9916 0.7257 0.0671 0.088 Uiso 0.267(4) 1 calc PR B 1 
C22B C 1.0509(5) 0.8160(8) -0.01017(11) 0.0587(9) Uiso 0.381(7) 1 d PD B 2 
H22D H 1.0938 0.8384 -0.0240 0.088 Uiso 0.381(7) 1 calc PR B 2 
H22E H 1.0115 0.8514 -0.0220 0.088 Uiso 0.381(7) 1 calc PR B 2 
H22F H 1.0447 0.7500 -0.0171 0.088 Uiso 0.381(7) 1 calc PR B 2 
C23B C 1.0573(5) 0.9333(3) 0.0514(4) 0.0587(9) Uiso 0.381(7) 1 d PD B 2 
H23D H 1.0604 0.9420 0.0839 0.088 Uiso 0.381(7) 1 calc PR B 2 
H23E H 1.0152 0.9632 0.0402 0.088 Uiso 0.381(7) 1 calc PR B 2 
H23F H 1.0979 0.9612 0.0370 0.088 Uiso 0.381(7) 1 calc PR B 2 
C24B C 0.9900(3) 0.7868(7) 0.0624(3) 0.0587(9) Uiso 0.381(7) 1 d PD B 2 
H24D H 0.9872 0.7206 0.0549 0.088 Uiso 0.381(7) 1 calc PR B 2 
H24E H 0.9488 0.8188 0.0511 0.088 Uiso 0.381(7) 1 calc PR B 2 
H24F H 0.9927 0.7940 0.0950 0.088 Uiso 0.381(7) 1 calc PR B 2 
C22C C 1.0382(5) 0.7786(7) -0.0034(2) 0.0587(9) Uiso 0.351(8) 1 d PD B 3 
H22G H 1.0774 0.7846 -0.0240 0.088 Uiso 0.351(8) 1 calc PR B 3 
H22H H 0.9969 0.8064 -0.0170 0.088 Uiso 0.351(8) 1 calc PR B 3 
H22I H 1.0295 0.7128 0.0028 0.088 Uiso 0.351(8) 1 calc PR B 3 
C23C C 1.0697(5) 0.9319(3) 0.0311(4) 0.0587(9) Uiso 0.351(8) 1 d PD B 3 
H23G H 1.0866 0.9620 0.0585 0.088 Uiso 0.351(8) 1 calc PR B 3 
H23H H 1.0270 0.9625 0.0212 0.088 Uiso 0.351(8) 1 calc PR B 3 
H23I H 1.1048 0.9370 0.0075 0.088 Uiso 0.351(8) 1 calc PR B 3 
C24C C 0.9944(4) 0.8197(7) 0.0734(3) 0.0587(9) Uiso 0.351(8) 1 d PD B 3 
H24G H 0.9800 0.7545 0.0751 0.088 Uiso 0.351(8) 1 calc PR B 3 
H24H H 0.9555 0.8576 0.0629 0.088 Uiso 0.351(8) 1 calc PR B 3 
H24I H 1.0088 0.8410 0.1032 0.088 Uiso 0.351(8) 1 calc PR B 3 
C25 C 1.19011(14) 0.80877(17) 0.05006(8) 0.0379(6) Uani 1 1 d . . . 
H25 H 1.2054 0.8581 0.0314 0.045 Uiso 1 1 calc R B . 
C26 C 1.23157(13) 0.74872(17) 0.07315(8) 0.0332(6) Uani 1 1 d . B . 
C27 C 1.31023(14) 0.74591(19) 0.07488(9) 0.0391(6) Uani 1 1 d . . . 
C28 C 1.33799(18) 0.8177(3) 0.04117(12) 0.0646(10) Uani 1 1 d . B . 
H28A H 1.3207 0.8028 0.0111 0.097 Uiso 1 1 calc R . . 
H28B H 1.3887 0.8160 0.0411 0.097 Uiso 1 1 calc R . . 
H28C H 1.3222 0.8798 0.0498 0.097 Uiso 1 1 calc R . . 
C29 C 1.33724(16) 0.7743(2) 0.12129(10) 0.0504(7) Uani 1 1 d . B . 
H29A H 1.3198 0.8362 0.1289 0.076 Uiso 1 1 calc R . . 
H29B H 1.3880 0.7753 0.1209 0.076 Uiso 1 1 calc R . . 
H29C H 1.3212 0.7294 0.1437 0.076 Uiso 1 1 calc R . . 
C30 C 1.33873(16) 0.6506(2) 0.06124(11) 0.0552(8) Uani 1 1 d . B . 
H30A H 1.3235 0.6037 0.0829 0.083 Uiso 1 1 calc R . . 
H30B H 1.3894 0.6528 0.0607 0.083 Uiso 1 1 calc R . . 
H30C H 1.3215 0.6343 0.0314 0.083 Uiso 1 1 calc R . . 
C31 C 1.09798(13) 0.41554(17) 0.24100(8) 0.0334(6) Uani 1 1 d . . . 
C32 C 1.03879(13) 0.29477(17) 0.29054(8) 0.0337(6) Uani 1 1 d . . . 
C33 C 1.09841(14) 0.23037(19) 0.30265(9) 0.0406(6) Uani 1 1 d . . . 
C34 C 1.13940(17) 0.2014(2) 0.26065(11) 0.0562(8) Uani 1 1 d . . . 
H34A H 1.1075 0.1759 0.2383 0.084 Uiso 1 1 calc R . . 
H34B H 1.1737 0.1542 0.2688 0.084 Uiso 1 1 calc R . . 
H34C H 1.1630 0.2558 0.2482 0.084 Uiso 1 1 calc R . . 
C35 C 1.14652(16) 0.2745(2) 0.33754(11) 0.0544(8) Uani 1 1 d . . . 
H35A H 1.1681 0.3302 0.3248 0.082 Uiso 1 1 calc R . . 
H35B H 1.1826 0.2299 0.3460 0.082 Uiso 1 1 calc R . . 
H35C H 1.1197 0.2917 0.3641 0.082 Uiso 1 1 calc R . . 
C36 C 1.06679(16) 0.1418(2) 0.32317(11) 0.0514(8) Uani 1 1 d . . . 
H36A H 1.0401 0.1582 0.3500 0.077 Uiso 1 1 calc R . . 
H36B H 1.1039 0.0987 0.3314 0.077 Uiso 1 1 calc R . . 
H36C H 1.0362 0.1121 0.3012 0.077 Uiso 1 1 calc R . . 
C37 C 0.97107(13) 0.28791(18) 0.30239(8) 0.0363(6) Uani 1 1 d . . . 
H37 H 0.9517 0.2435 0.3224 0.044 Uiso 1 1 calc R . . 
C38 C 0.93444(13) 0.35899(18) 0.27955(8) 0.0350(6) Uani 1 1 d . C . 
C39 C 0.85843(13) 0.38146(17) 0.28098(8) 0.0495(7) Uani 1 1 d D . . 
C40A C 0.8491(4) 0.4713(4) 0.3079(2) 0.0550(8) Uiso 0.421(7) 1 d PD C 1 
H40A H 0.8635 0.4608 0.3390 0.083 Uiso 0.421(7) 1 calc PR C 1 
H40B H 0.8004 0.4899 0.3072 0.083 Uiso 0.421(7) 1 calc PR C 1 
H40C H 0.8776 0.5205 0.2947 0.083 Uiso 0.421(7) 1 calc PR C 1 
C41A C 0.8132(4) 0.3040(5) 0.3001(2) 0.0550(8) Uiso 0.421(7) 1 d PD C 1 
H41A H 0.8202 0.2471 0.2826 0.083 Uiso 0.421(7) 1 calc PR C 1 
H41B H 0.7645 0.3225 0.2984 0.083 Uiso 0.421(7) 1 calc PR C 1 
H41C H 0.8260 0.2927 0.3314 0.083 Uiso 0.421(7) 1 calc PR C 1 
C42A C 0.8361(5) 0.4006(5) 0.23220(14) 0.0550(8) Uiso 0.421(7) 1 d PD C 1 
H42A H 0.8630 0.4527 0.2202 0.083 Uiso 0.421(7) 1 calc PR C 1 
H42B H 0.7867 0.4161 0.2315 0.083 Uiso 0.421(7) 1 calc PR C 1 
H42C H 0.8444 0.3451 0.2139 0.083 Uiso 0.421(7) 1 calc PR C 1 
C40B C 0.8455(4) 0.4425(6) 0.3223(2) 0.0550(8) Uiso 0.440(7) 1 d PD C 2 
H40D H 0.8597 0.4089 0.3493 0.083 Uiso 0.440(7) 1 calc PR C 2 
H40E H 0.7961 0.4575 0.3242 0.083 Uiso 0.440(7) 1 calc PR C 2 
H40F H 0.8723 0.5000 0.3197 0.083 Uiso 0.440(7) 1 calc PR C 2 
C41B C 0.8205(4) 0.2881(4) 0.2872(3) 0.0550(8) Uiso 0.440(7) 1 d PD C 2 
H41D H 0.8310 0.2472 0.2618 0.083 Uiso 0.440(7) 1 calc PR C 2 
H41E H 0.7705 0.2990 0.2886 0.083 Uiso 0.440(7) 1 calc PR C 2 
H41F H 0.8360 0.2587 0.3151 0.083 Uiso 0.440(7) 1 calc PR C 2 
C42B C 0.8336(5) 0.4291(6) 0.23804(19) 0.0550(8) Uiso 0.440(7) 1 d PD C 2 
H42D H 0.8640 0.4817 0.2312 0.083 Uiso 0.440(7) 1 calc PR C 2 
H42E H 0.7862 0.4515 0.2422 0.083 Uiso 0.440(7) 1 calc PR C 2 
H42F H 0.8348 0.3846 0.2132 0.083 Uiso 0.440(7) 1 calc PR C 2 
C40C C 0.8437(12) 0.4014(15) 0.3307(2) 0.0550(8) Uiso 0.139(5) 1 d PD C 3 
H40G H 0.8513 0.3448 0.3482 0.083 Uiso 0.139(5) 1 calc PR C 3 
H40H H 0.7956 0.4218 0.3342 0.083 Uiso 0.139(5) 1 calc PR C 3 
H40I H 0.8749 0.4503 0.3413 0.083 Uiso 0.139(5) 1 calc PR C 3 
C41C C 0.8078(10) 0.3045(12) 0.2672(7) 0.0550(8) Uiso 0.139(5) 1 d PD C 3 
H41G H 0.8130 0.2917 0.2351 0.083 Uiso 0.139(5) 1 calc PR C 3 
H41H H 0.7603 0.3247 0.2733 0.083 Uiso 0.139(5) 1 calc PR C 3 
H41I H 0.8179 0.2480 0.2843 0.083 Uiso 0.139(5) 1 calc PR C 3 
C42C C 0.8368(12) 0.4690(9) 0.2553(7) 0.0550(8) Uiso 0.139(5) 1 d PD C 3 
H42G H 0.8568 0.5238 0.2699 0.083 Uiso 0.139(5) 1 calc PR C 3 
H42H H 0.7863 0.4740 0.2552 0.083 Uiso 0.139(5) 1 calc PR C 3 
H42I H 0.8537 0.4652 0.2244 0.083 Uiso 0.139(5) 1 calc PR C 3 

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 
O1 0.0693(15) 0.0682(14) 0.0454(11) 0.0232(11) -0.0136(10) -0.0288(12) 
O2 0.0303(12) 0.0814(17) 0.1076(18) 0.0612(15) -0.0091(12) -0.0093(11) 
O3 0.0311(11) 0.0581(12) 0.0549(12) 0.0153(9) -0.0068(9) -0.0096(9) 
N1 0.0399(13) 0.0325(11) 0.0324(10) 0.0015(8) -0.0029(9) -0.0075(9) 
N2 0.0500(14) 0.0319(11) 0.0394(12) 0.0013(9) -0.0058(10) -0.0040(10) 
N3 0.0324(12) 0.0293(10) 0.0360(11) 0.0008(9) -0.0012(9) 0.0031(9) 
N4 0.0277(12) 0.0299(10) 0.0328(10) 0.0036(8) 0.0005(8) -0.0010(8) 
N5 0.0246(11) 0.0338(11) 0.0345(11) 0.0039(8) 0.0014(8) 0.0000(9) 
N6 0.0269(11) 0.0407(12) 0.0334(11) 0.0023(9) 0.0014(8) 0.0022(9) 
C1 0.0321(14) 0.0266(12) 0.0358(13) -0.0025(10) 0.0050(10) -0.0002(10) 
C2 0.0351(14) 0.0286(12) 0.0363(13) 0.0037(10) 0.0081(10) 0.0032(10) 
C3 0.0261(13) 0.0281(12) 0.0446(14) 0.0051(10) 0.0049(10) 0.0009(10) 
C4 0.0269(13) 0.0286(12) 0.0459(14) 0.0025(10) 0.0006(10) 0.0003(10) 
C5 0.0272(13) 0.0268(12) 0.0358(12) 0.0012(10) 0.0053(10) 0.0011(10) 
C6 0.0303(13) 0.0276(12) 0.0354(12) -0.0009(10) 0.0064(10) -0.0022(10) 
C7 0.0441(16) 0.0361(13) 0.0338(13) 0.0014(11) 0.0025(11) -0.0083(12) 
C8 0.0514(17) 0.0354(14) 0.0320(13) -0.0019(10) -0.0043(11) -0.0107(12) 
C9 0.070(2) 0.0360(15) 0.0451(16) 0.0057(12) -0.0075(14) -0.0120(14) 
C13 0.0416(16) 0.0429(15) 0.0362(13) -0.0012(11) 0.0003(11) -0.0120(12) 
C14 0.0388(15) 0.0383(14) 0.0285(12) -0.0026(10) 0.0024(10) -0.0051(11) 
C15 0.0458(17) 0.0407(15) 0.0354(14) -0.0010(11) -0.0004(11) -0.0014(12) 
C16 0.0455(19) 0.072(2) 0.0617(19) 0.0118(17) -0.0027(15) 0.0010(16) 
C17 0.0573(19) 0.0478(16) 0.0342(14) 0.0029(12) -0.0068(12) -0.0017(14) 
C18 0.078(2) 0.0488(18) 0.0538(18) -0.0097(14) -0.0033(16) 0.0114(17) 
C19 0.0299(15) 0.0370(14) 0.0567(17) 0.0140(12) 0.0010(12) 0.0005(12) 
C20 0.0436(16) 0.0305(13) 0.0314(12) -0.0020(10) -0.0009(11) 0.0031(11) 
C21 0.0496(18) 0.0435(15) 0.0428(15) 0.0046(12) -0.0040(12) 0.0140(13) 
C25 0.0489(17) 0.0282(13) 0.0366(13) 0.0056(10) 0.0005(11) -0.0030(11) 
C26 0.0378(15) 0.0292(12) 0.0327(12) -0.0008(10) 0.0016(10) -0.0052(11) 
C27 0.0353(15) 0.0407(14) 0.0414(14) 0.0043(12) 0.0037(11) -0.0095(12) 
C28 0.048(2) 0.078(2) 0.068(2) 0.0262(18) 0.0089(16) -0.0197(17) 
C29 0.0412(17) 0.0571(18) 0.0529(17) -0.0010(14) -0.0051(13) -0.0106(14) 
C30 0.0385(17) 0.0608(19) 0.066(2) -0.0097(16) 0.0020(14) 0.0041(15) 
C31 0.0278(14) 0.0323(13) 0.0400(14) 0.0004(10) 0.0015(10) -0.0025(10) 
C32 0.0352(15) 0.0352(13) 0.0306(12) 0.0016(10) -0.0011(10) -0.0036(11) 
C33 0.0372(15) 0.0417(15) 0.0428(14) 0.0110(12) -0.0005(11) 0.0022(12) 
C34 0.0484(19) 0.0541(18) 0.066(2) 0.0071(15) 0.0084(15) 0.0159(15) 
C35 0.0456(18) 0.0603(19) 0.0572(18) 0.0148(15) -0.0161(14) -0.0011(15) 
C36 0.0520(19) 0.0402(16) 0.0620(19) 0.0157(14) -0.0045(14) 0.0021(14) 
C37 0.0335(15) 0.0415(14) 0.0337(13) 0.0059(11) 0.0021(10) -0.0057(11) 
C38 0.0318(14) 0.0421(14) 0.0310(12) -0.0014(10) 0.0042(10) -0.0033(11) 
C39 0.0319(16) 0.0640(19) 0.0527(17) 0.0058(14) 0.0060(12) 0.0062(14) 

_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 
O1 C7 1.205(3) . ? 
O2 C19 1.209(3) . ? 
O3 C31 1.210(3) . ? 
N1 N2 1.387(3) . ? 
N1 C14 1.393(3) . ? 
N1 C7 1.423(3) . ? 
N2 C8 1.321(3) . ? 
N3 C20 1.313(3) . ? 
N3 N4 1.385(3) . ? 
N4 C26 1.402(3) . ? 
N4 C19 1.404(3) . ? 
N5 N6 1.382(3) . ? 
N5 C32 1.391(3) . ? 
N5 C31 1.409(3) . ? 
N6 C38 1.319(3) . ? 
C1 C6 1.395(3) . ? 
C1 C2 1.399(3) . ? 
C1 C7 1.494(4) . ? 
C2 C3 1.394(4) . ? 
C3 C4 1.385(4) . ? 
C3 C19 1.497(4) . ? 
C4 C5 1.396(3) . ? 
C5 C6 1.388(3) . ? 
C5 C31 1.493(3) . ? 
C8 C13 1.412(4) . ? 
C8 C9 1.512(4) . ? 
C9 C10B 1.529(2) . ? 
C9 C12B 1.531(2) . ? 
C9 C11C 1.531(2) . ? 
C9 C12C 1.532(2) . ? 
C9 C12A 1.532(2) . ? 
C9 C10A 1.535(2) . ? 
C9 C11A 1.536(2) . ? 
C9 C10C 1.538(2) . ? 
C9 C11B 1.544(2) . ? 
C13 C14 1.365(4) . ? 
C14 C15 1.513(4) . ? 
C15 C16 1.538(4) . ? 
C15 C17 1.546(4) . ? 
C15 C18 1.546(4) . ? 
C20 C25 1.418(4) . ? 
C20 C21 1.513(4) . ? 
C21 C24C 1.530(2) . ? 
C21 C22B 1.531(2) . ? 
C21 C22A 1.531(2) . ? 
C21 C23A 1.533(2) . ? 
C21 C22C 1.535(2) . ? 
C21 C23C 1.535(2) . ? 
C21 C23B 1.536(2) . ? 
C21 C24B 1.536(2) . ? 
C21 C24A 1.537(2) . ? 
C25 C26 1.365(4) . ? 
C26 C27 1.521(4) . ? 
C27 C30 1.533(4) . ? 
C27 C29 1.535(4) . ? 
C27 C28 1.538(4) . ? 
C32 C37 1.359(4) . ? 
C32 C33 1.522(4) . ? 
C33 C35 1.534(4) . ? 
C33 C34 1.540(4) . ? 
C33 C36 1.541(4) . ? 
C37 C38 1.419(4) . ? 
C38 C39 1.504(4) . ? 
C39 C41A 1.526(2) . ? 
C39 C42B 1.530(2) . ? 
C39 C40A 1.532(2) . ? 
C39 C42C 1.532(2) . ? 
C39 C41C 1.533(2) . ? 
C39 C40B 1.534(2) . ? 
C39 C40C 1.537(2) . ? 
C39 C41B 1.542(2) . ? 
C39 C42A 1.543(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 
N2 N1 C14 111.9(2) . . ? 
N2 N1 C7 117.5(2) . . ? 
C14 N1 C7 130.6(2) . . ? 
C8 N2 N1 105.1(2) . . ? 
C20 N3 N4 105.4(2) . . ? 
N3 N4 C26 111.76(19) . . ? 
N3 N4 C19 116.77(19) . . ? 
C26 N4 C19 131.3(2) . . ? 
N6 N5 C32 111.68(19) . . ? 
N6 N5 C31 116.63(19) . . ? 
C32 N5 C31 131.4(2) . . ? 
C38 N6 N5 105.2(2) . . ? 
C6 C1 C2 119.5(2) . . ? 
C6 C1 C7 124.7(2) . . ? 
C2 C1 C7 115.6(2) . . ? 
C3 C2 C1 120.3(2) . . ? 
C4 C3 C2 119.4(2) . . ? 
C4 C3 C19 115.4(2) . . ? 
C2 C3 C19 124.9(2) . . ? 
C3 C4 C5 121.0(2) . . ? 
C6 C5 C4 119.3(2) . . ? 
C6 C5 C31 123.6(2) . . ? 
C4 C5 C31 116.6(2) . . ? 
C5 C6 C1 120.4(2) . . ? 
O1 C7 N1 120.1(2) . . ? 
O1 C7 C1 121.4(2) . . ? 
N1 C7 C1 118.4(2) . . ? 
N2 C8 C13 110.5(2) . . ? 
N2 C8 C9 121.1(2) . . ? 
C13 C8 C9 128.4(2) . . ? 
C8 C9 C10B 112.8(4) . . ? 
C8 C9 C12B 108.9(4) . . ? 
C10B C9 C12B 111.0(3) . . ? 
C8 C9 C11C 110.1(6) . . ? 
C10B C9 C11C 71.3(5) . . ? 
C12B C9 C11C 135.8(6) . . ? 
C8 C9 C12C 111.5(6) . . ? 
C10B C9 C12C 131.7(6) . . ? 
C12B C9 C12C 34.2(4) . . ? 
C11C C9 C12C 110.0(4) . . ? 
C8 C9 C12A 110.8(4) . . ? 
C10B C9 C12A 88.0(4) . . ? 
C12B C9 C12A 25.3(4) . . ? 
C11C C9 C12A 138.7(7) . . ? 
C12C C9 C12A 58.5(5) . . ? 
C8 C9 C10A 109.7(4) . . ? 
C10B C9 C10A 21.2(4) . . ? 
C12B C9 C10A 129.1(5) . . ? 
C11C C9 C10A 51.5(5) . . ? 
C12C C9 C10A 138.7(7) . . ? 
C12A C9 C10A 108.1(3) . . ? 
C8 C9 C11A 112.4(4) . . ? 
C10B C9 C11A 121.6(5) . . ? 
C12B C9 C11A 86.8(4) . . ? 
C11C C9 C11A 59.6(5) . . ? 
C12C C9 C11A 53.5(5) . . ? 
C12A C9 C11A 108.2(3) . . ? 
C10A C9 C11A 107.4(3) . . ? 
C8 C9 C10C 106.8(6) . . ? 
C10B C9 C10C 39.0(4) . . ? 
C12B C9 C10C 77.8(5) . . ? 
C11C C9 C10C 109.3(4) . . ? 
C12C C9 C10C 109.0(4) . . ? 
C12A C9 C10C 52.6(5) . . ? 
C10A C9 C10C 60.1(5) . . ? 
C11A C9 C10C 140.6(7) . . ? 
C8 C9 C11B 106.5(4) . . ? 
C10B C9 C11B 109.2(3) . . ? 
C12B C9 C11B 108.4(3) . . ? 
C11C C9 C11B 40.1(4) . . ? 
C12C C9 C11B 75.2(5) . . ? 
C12A C9 C11B 128.3(5) . . ? 
C10A C9 C11B 91.0(4) . . ? 
C11A C9 C11B 21.7(4) . . ? 
C10C C9 C11B 141.7(6) . . ? 
C14 C13 C8 108.3(2) . . ? 
C13 C14 N1 104.2(2) . . ? 
C13 C14 C15 128.1(2) . . ? 
N1 C14 C15 127.6(2) . . ? 
C14 C15 C16 108.2(2) . . ? 
C14 C15 C17 111.3(2) . . ? 
C16 C15 C17 107.5(2) . . ? 
C14 C15 C18 112.0(2) . . ? 
C16 C15 C18 107.4(3) . . ? 
C17 C15 C18 110.2(2) . . ? 
O2 C19 N4 120.8(2) . . ? 
O2 C19 C3 120.3(2) . . ? 
N4 C19 C3 118.9(2) . . ? 
N3 C20 C25 110.7(2) . . ? 
N3 C20 C21 120.6(2) . . ? 
C25 C20 C21 128.7(2) . . ? 
C20 C21 C24C 111.8(4) . . ? 
C20 C21 C22B 110.3(4) . . ? 
C24C C21 C22B 125.7(5) . . ? 
C20 C21 C22A 111.2(5) . . ? 
C24C C21 C22A 137.0(6) . . ? 
C22B C21 C22A 32.1(4) . . ? 
C20 C21 C23A 109.6(5) . . ? 
C24C C21 C23A 55.7(5) . . ? 
C22B C21 C23A 133.3(6) . . ? 
C22A C21 C23A 109.3(4) . . ? 
C20 C21 C22C 106.5(4) . . ? 
C24C C21 C22C 110.1(3) . . ? 
C22B C21 C22C 23.5(4) . . ? 
C22A C21 C22C 55.6(5) . . ? 
C23A C21 C22C 143.9(6) . . ? 
C20 C21 C23C 108.5(4) . . ? 
C24C C21 C23C 110.2(3) . . ? 
C22B C21 C23C 86.7(4) . . ? 
C22A C21 C23C 55.3(5) . . ? 
C23A C21 C23C 58.1(5) . . ? 
C22C C21 C23C 109.6(3) . . ? 
C20 C21 C23B 108.1(4) . . ? 
C24C C21 C23B 88.6(4) . . ? 
C22B C21 C23B 109.1(3) . . ? 
C22A C21 C23B 79.0(5) . . ? 
C23A C21 C23B 34.0(4) . . ? 
C22C C21 C23B 130.3(5) . . ? 
C23C C21 C23B 24.5(4) . . ? 
C20 C21 C24B 111.3(4) . . ? 
C24C C21 C24B 21.9(4) . . ? 
C22B C21 C24B 109.1(3) . . ? 
C22A C21 C24B 131.3(6) . . ? 
C23A C21 C24B 77.2(5) . . ? 
C22C C21 C24B 90.1(4) . . ? 
C23C C21 C24B 127.7(5) . . ? 
C23B C21 C24B 108.8(3) . . ? 
C20 C21 C24A 109.4(5) . . ? 
C24C C21 C24A 54.8(5) . . ? 
C22B C21 C24A 79.8(5) . . ? 
C22A C21 C24A 108.9(4) . . ? 
C23A C21 C24A 108.4(4) . . ? 
C22C C21 C24A 58.2(5) . . ? 
C23C C21 C24A 142.1(6) . . ? 
C23B C21 C24A 135.0(6) . . ? 
C24B C21 C24A 33.1(4) . . ? 
C26 C25 C20 108.1(2) . . ? 
C25 C26 N4 104.0(2) . . ? 
C25 C26 C27 128.3(2) . . ? 
N4 C26 C27 127.6(2) . . ? 
C26 C27 C30 111.9(2) . . ? 
C26 C27 C29 111.3(2) . . ? 
C30 C27 C29 110.8(2) . . ? 
C26 C27 C28 107.9(2) . . ? 
C30 C27 C28 107.6(3) . . ? 
C29 C27 C28 107.0(2) . . ? 
O3 C31 N5 120.6(2) . . ? 
O3 C31 C5 121.6(2) . . ? 
N5 C31 C5 117.8(2) . . ? 
C37 C32 N5 104.9(2) . . ? 
C37 C32 C33 128.5(2) . . ? 
N5 C32 C33 126.4(2) . . ? 
C32 C33 C35 111.6(2) . . ? 
C32 C33 C34 111.1(2) . . ? 
C35 C33 C34 110.7(3) . . ? 
C32 C33 C36 107.4(2) . . ? 
C35 C33 C36 108.3(2) . . ? 
C34 C33 C36 107.7(2) . . ? 
C32 C37 C38 107.6(2) . . ? 
N6 C38 C37 110.6(2) . . ? 
N6 C38 C39 120.5(2) . . ? 
C37 C38 C39 128.9(2) . . ? 
C38 C39 C41A 114.3(4) . . ? 
C38 C39 C42B 112.2(4) . . ? 
C41A C39 C42B 117.4(6) . . ? 
C38 C39 C40A 108.1(4) . . ? 
C41A C39 C40A 110.7(3) . . ? 
C42B C39 C40A 91.4(4) . . ? 
C38 C39 C42C 115.3(9) . . ? 
C41A C39 C42C 129.1(10) . . ? 
C42B C39 C42C 29.3(7) . . ? 
C40A C39 C42C 62.4(9) . . ? 
C38 C39 C41C 117.3(9) . . ? 
C41A C39 C41C 37.6(8) . . ? 
C42B C39 C41C 84.2(7) . . ? 
C40A C39 C41C 132.5(10) . . ? 
C42C C39 C41C 106.6(7) . . ? 
C38 C39 C40B 107.8(4) . . ? 
C41A C39 C40B 91.5(4) . . ? 
C42B C39 C40B 111.4(3) . . ? 
C40A C39 C40B 22.6(3) . . ? 
C42C C39 C40B 83.5(8) . . ? 
C41C C39 C40B 121.7(9) . . ? 
C38 C39 C40C 104.4(9) . . ? 
C41A C39 C40C 70.8(8) . . ? 
C42B C39 C40C 131.8(9) . . ? 
C40A C39 C40C 46.8(8) . . ? 
C42C C39 C40C 106.2(7) . . ? 
C41C C39 C40C 106.1(7) . . ? 
C40B C39 C40C 24.2(7) . . ? 
C38 C39 C41B 106.2(4) . . ? 
C41A C39 C41B 17.6(4) . . ? 
C42B C39 C41B 110.0(3) . . ? 
C40A C39 C41B 128.1(4) . . ? 
C42C C39 C41B 130.4(8) . . ? 
C41C C39 C41B 25.9(7) . . ? 
C40B C39 C41B 109.0(3) . . ? 
C40C C39 C41B 87.7(7) . . ? 
C38 C39 C42A 106.5(4) . . ? 
C41A C39 C42A 108.8(3) . . ? 
C42B C39 C42A 16.8(4) . . ? 
C40A C39 C42A 108.1(3) . . ? 
C42C C39 C42A 46.0(9) . . ? 
C41C C39 C42A 72.4(8) . . ? 
C40B C39 C42A 127.6(4) . . ? 
C40C C39 C42A 145.6(10) . . ? 
C41B C39 C42A 97.8(5) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
C14 N1 N2 C8 -0.5(3) . . . . ? 
C7 N1 N2 C8 -179.9(2) . . . . ? 
C20 N3 N4 C26 0.6(3) . . . . ? 
C20 N3 N4 C19 176.0(2) . . . . ? 
C32 N5 N6 C38 0.2(3) . . . . ? 
C31 N5 N6 C38 -174.5(2) . . . . ? 
C6 C1 C2 C3 0.9(4) . . . . ? 
C7 C1 C2 C3 175.3(2) . . . . ? 
C1 C2 C3 C4 1.3(4) . . . . ? 
C1 C2 C3 C19 175.1(2) . . . . ? 
C2 C3 C4 C5 -2.4(4) . . . . ? 
C19 C3 C4 C5 -176.8(2) . . . . ? 
C3 C4 C5 C6 1.2(4) . . . . ? 
C3 C4 C5 C31 173.5(2) . . . . ? 
C4 C5 C6 C1 1.1(3) . . . . ? 
C31 C5 C6 C1 -170.7(2) . . . . ? 
C2 C1 C6 C5 -2.1(3) . . . . ? 
C7 C1 C6 C5 -176.0(2) . . . . ? 
N2 N1 C7 O1 151.8(3) . . . . ? 
C14 N1 C7 O1 -27.5(4) . . . . ? 
N2 N1 C7 C1 -31.3(3) . . . . ? 
C14 N1 C7 C1 149.4(2) . . . . ? 
C6 C1 C7 O1 159.7(3) . . . . ? 
C2 C1 C7 O1 -14.3(4) . . . . ? 
C6 C1 C7 N1 -17.1(4) . . . . ? 
C2 C1 C7 N1 168.9(2) . . . . ? 
N1 N2 C8 C13 0.0(3) . . . . ? 
N1 N2 C8 C9 -177.8(2) . . . . ? 
N2 C8 C9 C10B 19.7(5) . . . . ? 
C13 C8 C9 C10B -157.5(4) . . . . ? 
N2 C8 C9 C12B -103.9(4) . . . . ? 
C13 C8 C9 C12B 78.8(5) . . . . ? 
N2 C8 C9 C11C 97.2(5) . . . . ? 
C13 C8 C9 C11C -80.1(5) . . . . ? 
N2 C8 C9 C12C -140.3(5) . . . . ? 
C13 C8 C9 C12C 42.4(5) . . . . ? 
N2 C8 C9 C12A -77.1(5) . . . . ? 
C13 C8 C9 C12A 105.6(5) . . . . ? 
N2 C8 C9 C10A 42.2(5) . . . . ? 
C13 C8 C9 C10A -135.1(5) . . . . ? 
N2 C8 C9 C11A 161.6(4) . . . . ? 
C13 C8 C9 C11A -15.6(5) . . . . ? 
N2 C8 C9 C10C -21.4(5) . . . . ? 
C13 C8 C9 C10C 161.3(5) . . . . ? 
N2 C8 C9 C11B 139.4(4) . . . . ? 
C13 C8 C9 C11B -37.8(4) . . . . ? 
N2 C8 C13 C14 0.6(3) . . . . ? 
C9 C8 C13 C14 178.1(2) . . . . ? 
C8 C13 C14 N1 -0.9(3) . . . . ? 
C8 C13 C14 C15 -178.6(2) . . . . ? 
N2 N1 C14 C13 0.9(3) . . . . ? 
C7 N1 C14 C13 -179.8(2) . . . . ? 
N2 N1 C14 C15 178.7(2) . . . . ? 
C7 N1 C14 C15 -2.0(4) . . . . ? 
C13 C14 C15 C16 8.3(4) . . . . ? 
N1 C14 C15 C16 -169.0(2) . . . . ? 
C13 C14 C15 C17 -109.7(3) . . . . ? 
N1 C14 C15 C17 73.1(3) . . . . ? 
C13 C14 C15 C18 126.4(3) . . . . ? 
N1 C14 C15 C18 -50.9(4) . . . . ? 
N3 N4 C19 O2 -163.9(3) . . . . ? 
C26 N4 C19 O2 10.4(5) . . . . ? 
N3 N4 C19 C3 14.7(3) . . . . ? 
C26 N4 C19 C3 -171.1(2) . . . . ? 
C4 C3 C19 O2 29.0(4) . . . . ? 
C2 C3 C19 O2 -145.1(3) . . . . ? 
C4 C3 C19 N4 -149.6(2) . . . . ? 
C2 C3 C19 N4 36.4(4) . . . . ? 
N4 N3 C20 C25 -0.2(3) . . . . ? 
N4 N3 C20 C21 178.5(2) . . . . ? 
N3 C20 C21 C24C 30.4(5) . . . . ? 
C25 C20 C21 C24C -151.2(5) . . . . ? 
N3 C20 C21 C22B -114.4(5) . . . . ? 
C25 C20 C21 C22B 64.0(6) . . . . ? 
N3 C20 C21 C22A -148.7(5) . . . . ? 
C25 C20 C21 C22A 29.7(5) . . . . ? 
N3 C20 C21 C23A 90.3(5) . . . . ? 
C25 C20 C21 C23A -91.3(5) . . . . ? 
N3 C20 C21 C22C -89.9(5) . . . . ? 
C25 C20 C21 C22C 88.5(5) . . . . ? 
N3 C20 C21 C23C 152.2(5) . . . . ? 
C25 C20 C21 C23C -29.4(5) . . . . ? 
N3 C20 C21 C23B 126.3(5) . . . . ? 
C25 C20 C21 C23B -55.3(5) . . . . ? 
N3 C20 C21 C24B 6.9(5) . . . . ? 
C25 C20 C21 C24B -174.7(5) . . . . ? 
N3 C20 C21 C24A -28.5(5) . . . . ? 
C25 C20 C21 C24A 149.9(5) . . . . ? 
N3 C20 C25 C26 -0.4(3) . . . . ? 
C21 C20 C25 C26 -178.9(2) . . . . ? 
C20 C25 C26 N4 0.7(3) . . . . ? 
C20 C25 C26 C27 -179.7(2) . . . . ? 
N3 N4 C26 C25 -0.8(3) . . . . ? 
C19 N4 C26 C25 -175.4(3) . . . . ? 
N3 N4 C26 C27 179.6(2) . . . . ? 
C19 N4 C26 C27 5.1(4) . . . . ? 
C25 C26 C27 C30 -124.4(3) . . . . ? 
N4 C26 C27 C30 55.0(3) . . . . ? 
C25 C26 C27 C29 110.9(3) . . . . ? 
N4 C26 C27 C29 -69.6(3) . . . . ? 
C25 C26 C27 C28 -6.2(4) . . . . ? 
N4 C26 C27 C28 173.2(3) . . . . ? 
N6 N5 C31 O3 145.1(2) . . . . ? 
C32 N5 C31 O3 -28.3(4) . . . . ? 
N6 N5 C31 C5 -36.9(3) . . . . ? 
C32 N5 C31 C5 149.8(2) . . . . ? 
C6 C5 C31 O3 156.4(2) . . . . ? 
C4 C5 C31 O3 -15.5(3) . . . . ? 
C6 C5 C31 N5 -21.6(3) . . . . ? 
C4 C5 C31 N5 166.5(2) . . . . ? 
N6 N5 C32 C37 -0.3(3) . . . . ? 
C31 N5 C32 C37 173.4(2) . . . . ? 
N6 N5 C32 C33 174.6(2) . . . . ? 
C31 N5 C32 C33 -11.8(4) . . . . ? 
C37 C32 C33 C35 -106.6(3) . . . . ? 
N5 C32 C33 C35 79.7(3) . . . . ? 
C37 C32 C33 C34 129.3(3) . . . . ? 
N5 C32 C33 C34 -44.3(4) . . . . ? 
C37 C32 C33 C36 11.8(4) . . . . ? 
N5 C32 C33 C36 -161.8(2) . . . . ? 
N5 C32 C37 C38 0.2(3) . . . . ? 
C33 C32 C37 C38 -174.5(2) . . . . ? 
N5 N6 C38 C37 0.0(3) . . . . ? 
N5 N6 C38 C39 179.9(2) . . . . ? 
C32 C37 C38 N6 -0.2(3) . . . . ? 
C32 C37 C38 C39 179.9(2) . . . . ? 
N6 C38 C39 C41A 163.6(4) . . . . ? 
C37 C38 C39 C41A -16.5(4) . . . . ? 
N6 C38 C39 C42B 26.7(5) . . . . ? 
C37 C38 C39 C42B -153.4(4) . . . . ? 
N6 C38 C39 C40A -72.6(4) . . . . ? 
C37 C38 C39 C40A 107.3(4) . . . . ? 
N6 C38 C39 C42C -5.3(10) . . . . ? 
C37 C38 C39 C42C 174.6(9) . . . . ? 
N6 C38 C39 C41C 121.7(9) . . . . ? 
C37 C38 C39 C41C -58.4(9) . . . . ? 
N6 C38 C39 C40B -96.4(4) . . . . ? 
C37 C38 C39 C40B 83.5(5) . . . . ? 
N6 C38 C39 C40C -121.3(8) . . . . ? 
C37 C38 C39 C40C 58.6(9) . . . . ? 
N6 C38 C39 C41B 147.0(4) . . . . ? 
C37 C38 C39 C41B -33.1(5) . . . . ? 
N6 C38 C39 C42A 43.4(4) . . . . ? 
C37 C38 C39 C42A -136.7(4) . . . . ? 

_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.477 
_refine_diff_density_min   -0.540 
_refine_diff_density_rms    0.049 

data_darm 
_database_code_CSD                  185335

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C16 H14 N4 O2' 
_chemical_formula_weight          294.31 

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' 

_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                    18.538(2) 
_cell_length_b                    7.2850(7) 
_cell_length_c                    11.3601(13) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  100.922(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1506.4(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 


_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.45 
_exptl_crystal_size_mid           0.43 
_exptl_crystal_size_min           0.41 
_exptl_crystal_density_meas       0 
_exptl_crystal_density_diffrn     1.298 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              616 
_exptl_absorpt_coefficient_mu     0.089 
_exptl_absorpt_correction_type    'Empirical with SADABS'
_exptl_absorpt_correction_T_min   0.9609 
_exptl_absorpt_correction_T_max   0.9643 
_exptl_absorpt_process_details    ? 
_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             1442 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0154 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.24 
_diffrn_reflns_theta_max          26.35 
_reflns_number_total              1442 
_reflns_number_gt                 1204 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Bruker SMART' 
_computing_cell_refinement        'Bruker SMART' 
_computing_data_reduction         'Bruker SAINT' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_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^)+(0.0608P)^2^+0.6307P] 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     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0098(17) 
_refine_ls_extinction_expression 
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          1442 
_refine_ls_number_parameters      103 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0475 
_refine_ls_R_factor_gt            0.0386 
_refine_ls_wR_factor_ref          0.1141 
_refine_ls_wR_factor_gt           0.1077 
_refine_ls_goodness_of_fit_ref    1.022 
_refine_ls_restrained_S_all       1.022 
_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 
O1 O 0.05636(7) 0.19246(19) -0.02770(9) 0.0704(4) Uani 1 1 d . . . 
N1 N 0.11045(6) -0.01462(17) 0.10760(10) 0.0462(3) Uani 1 1 d . . . 
N2 N 0.13174(7) -0.06946(19) 0.22449(10) 0.0523(4) Uani 1 1 d . . . 
C1 C 0.0000 0.1356(3) 0.2500 0.0389(4) Uani 1 2 d S . . 
H1 H 0.0000 0.0080 0.2500 0.047 Uiso 1 2 calc SR . . 
C2 C 0.03284(7) 0.2323(2) 0.16876(11) 0.0429(4) Uani 1 1 d . . . 
C3 C 0.03057(10) 0.4229(2) 0.16684(14) 0.0583(4) Uani 1 1 d . . . 
H3 H 0.0498 0.4868 0.1090 0.070 Uiso 1 1 calc R . . 
C4 C 0.0000 0.5177(3) 0.2500 0.0706(7) Uani 1 2 d S . . 
H4 H 0.0000 0.6454 0.2500 0.085 Uiso 1 2 calc SR . . 
C5 C 0.06605(8) 0.1397(2) 0.07486(12) 0.0467(4) Uani 1 1 d . . . 
C6 C 0.13896(8) -0.1261(2) 0.03093(14) 0.0564(4) Uani 1 1 d . . . 
H6 H 0.1323 -0.1150 -0.0520 0.068 Uiso 1 1 calc R . . 
C7 C 0.17848(9) -0.2548(3) 0.09913(16) 0.0645(5) Uani 1 1 d . . . 
H7 H 0.2046 -0.3507 0.0729 0.077 Uiso 1 1 calc R . . 
C8 C 0.17255(9) -0.2157(3) 0.21859(15) 0.0602(5) Uani 1 1 d . . . 
C9 C 0.20555(13) -0.3165(4) 0.33007(19) 0.0968(8) Uani 1 1 d . . . 
H9A H 0.2575 -0.2934 0.3486 0.145 Uiso 1 1 calc R . . 
H9B H 0.1970 -0.4457 0.3182 0.145 Uiso 1 1 calc R . . 
H9C H 0.1834 -0.2751 0.3952 0.145 Uiso 1 1 calc R . . 

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 
O1 0.0920(9) 0.0790(9) 0.0447(7) 0.0147(6) 0.0242(6) 0.0089(7) 
N1 0.0445(6) 0.0563(8) 0.0402(6) -0.0009(5) 0.0136(5) -0.0030(5) 
N2 0.0488(7) 0.0655(9) 0.0442(7) 0.0048(6) 0.0131(5) 0.0071(6) 
C1 0.0416(9) 0.0358(10) 0.0391(9) 0.000 0.0074(7) 0.000 
C2 0.0449(7) 0.0435(8) 0.0391(7) 0.0016(5) 0.0046(5) -0.0032(6) 
C3 0.0770(11) 0.0459(10) 0.0522(9) 0.0072(7) 0.0128(8) -0.0096(7) 
C4 0.110(2) 0.0363(13) 0.0651(15) 0.000 0.0167(14) 0.000 
C5 0.0483(8) 0.0512(9) 0.0422(8) 0.0043(6) 0.0126(6) -0.0073(6) 
C6 0.0512(8) 0.0700(11) 0.0517(9) -0.0101(7) 0.0192(7) -0.0046(7) 
C7 0.0581(9) 0.0675(12) 0.0733(11) -0.0095(9) 0.0263(8) 0.0050(8) 
C8 0.0514(8) 0.0692(11) 0.0634(10) 0.0061(8) 0.0190(7) 0.0109(8) 
C9 0.0945(15) 0.115(2) 0.0834(14) 0.0251(13) 0.0231(12) 0.0526(14) 

_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 
O1 C5 1.2077(17) . ? 
N1 C6 1.3682(19) . ? 
N1 N2 1.3711(16) . ? 
N1 C5 1.401(2) . ? 
N2 C8 1.316(2) . ? 
C1 C2 1.3898(16) . ? 
C1 C2 1.3898(16) 2 ? 
C2 C3 1.389(2) . ? 
C2 C5 1.490(2) . ? 
C3 C4 1.376(2) . ? 
C4 C3 1.376(2) 2 ? 
C6 C7 1.342(3) . ? 
C7 C8 1.411(2) . ? 
C8 C9 1.491(3) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
C6 N1 N2 111.63(13) . . ? 
C6 N1 C5 125.85(13) . . ? 
N2 N1 C5 122.52(11) . . ? 
C8 N2 N1 104.44(12) . . ? 
C2 C1 C2 119.09(18) . 2 ? 
C3 C2 C1 120.08(14) . . ? 
C3 C2 C5 117.19(13) . . ? 
C1 C2 C5 122.55(14) . . ? 
C4 C3 C2 120.41(15) . . ? 
C3 C4 C3 119.7(2) . 2 ? 
O1 C5 N1 118.95(13) . . ? 
O1 C5 C2 122.70(15) . . ? 
N1 C5 C2 118.35(12) . . ? 
C7 C6 N1 106.36(14) . . ? 
C6 C7 C8 106.30(15) . . ? 
N2 C8 C7 111.27(15) . . ? 
N2 C8 C9 120.17(16) . . ? 
C7 C8 C9 128.56(17) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
C6 N1 N2 C8 -0.69(16) . . . . ? 
C5 N1 N2 C8 -179.56(13) . . . . ? 
C2 C1 C2 C3 -2.04(11) 2 . . . ? 
C2 C1 C2 C5 -176.96(14) 2 . . . ? 
C1 C2 C3 C4 4.1(2) . . . . ? 
C5 C2 C3 C4 179.31(11) . . . . ? 
C2 C3 C4 C3 -2.06(11) . . . 2 ? 
C6 N1 C5 O1 -7.2(2) . . . . ? 
N2 N1 C5 O1 171.55(14) . . . . ? 
C6 N1 C5 C2 173.03(13) . . . . ? 
N2 N1 C5 C2 -8.26(19) . . . . ? 
C3 C2 C5 O1 -39.4(2) . . . . ? 
C1 C2 C5 O1 135.70(15) . . . . ? 
C3 C2 C5 N1 140.44(14) . . . . ? 
C1 C2 C5 N1 -44.50(17) . . . . ? 
N2 N1 C6 C7 0.49(17) . . . . ? 
C5 N1 C6 C7 179.32(14) . . . . ? 
N1 C6 C7 C8 -0.10(18) . . . . ? 
N1 N2 C8 C7 0.61(18) . . . . ? 
N1 N2 C8 C9 -179.39(18) . . . . ? 
C6 C7 C8 N2 -0.3(2) . . . . ? 
C6 C7 C8 C9 179.7(2) . . . . ? 

_diffrn_measured_fraction_theta_max    0.936 
_diffrn_reflns_theta_full              26.35 
_diffrn_measured_fraction_theta_full   0.936 
_refine_diff_density_max    0.156 
_refine_diff_density_min   -0.126 
_refine_diff_density_rms    0.029 

data_darn 
_database_code_CSD                  185336


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C18 H18 N4 O2' 
_chemical_formula_weight          322.36 

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' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

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

_cell_length_a                    8.6173(9) 
_cell_length_b                    9.7287(9) 
_cell_length_c                    11.6949(12) 
_cell_angle_alpha                 68.665(3) 
_cell_angle_beta                  73.638(2) 
_cell_angle_gamma                 63.788(2) 
_cell_volume                      810.70(14) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.37 
_exptl_crystal_size_min           0.32 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.321 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              340 
_exptl_absorpt_coefficient_mu     0.089 
_exptl_absorpt_correction_type    'Empirical with SADABS' 
_exptl_absorpt_correction_T_min   0.9568 
_exptl_absorpt_correction_T_max   0.9720 
_exptl_absorpt_process_details    ? 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_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             2930 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0285 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          1.89 
_diffrn_reflns_theta_max          26.38 
_reflns_number_total              2930 
_reflns_number_gt                 2264 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.0617P)^2^+0.1434P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2930 
_refine_ls_number_parameters      221 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0565 
_refine_ls_R_factor_gt            0.0417 
_refine_ls_wR_factor_ref          0.1221 
_refine_ls_wR_factor_gt           0.1135 
_refine_ls_goodness_of_fit_ref    1.045 
_refine_ls_restrained_S_all       1.045 
_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 
O1 O 0.06314(17) 0.31637(17) 0.98139(12) 0.0634(4) Uani 1 1 d . . . 
O2 O 0.2298(2) 0.72369(18) 0.43450(14) 0.0880(5) Uani 1 1 d . . . 
N1 N 0.32481(18) 0.21727(17) 1.04920(13) 0.0493(4) Uani 1 1 d . . . 
N2 N 0.49661(18) 0.20567(18) 1.01688(13) 0.0533(4) Uani 1 1 d . . . 
N3 N 0.23007(18) 0.48048(17) 0.46957(13) 0.0491(4) Uani 1 1 d . . . 
N4 N 0.25716(19) 0.32656(17) 0.54489(13) 0.0526(4) Uani 1 1 d . . . 
C1 C 0.2316(2) 0.4528(2) 0.74187(15) 0.0461(4) Uani 1 1 d . . . 
H1 H 0.1781 0.3915 0.7358 0.055 Uiso 1 1 calc R . . 
C2 C 0.2635(2) 0.4376(2) 0.85681(15) 0.0458(4) Uani 1 1 d . . . 
C3 C 0.3396(2) 0.5320(2) 0.86668(18) 0.0528(4) Uani 1 1 d . . . 
H3 H 0.3610 0.5220 0.9435 0.063 Uiso 1 1 calc R . . 
C4 C 0.3832(2) 0.6402(2) 0.76209(18) 0.0550(5) Uani 1 1 d . . . 
H4 H 0.4325 0.7044 0.7686 0.066 Uiso 1 1 calc R . . 
C5 C 0.3539(2) 0.6535(2) 0.64781(18) 0.0527(4) Uani 1 1 d . . . 
H5 H 0.3843 0.7265 0.5777 0.063 Uiso 1 1 calc R . . 
C6 C 0.2793(2) 0.55916(19) 0.63617(16) 0.0466(4) Uani 1 1 d . . . 
C7 C 0.2042(2) 0.3234(2) 0.96593(15) 0.0480(4) Uani 1 1 d . . . 
C8 C 0.1325(3) 0.0835(3) 1.21555(19) 0.0719(6) Uani 1 1 d . . . 
H8A H 0.0465 0.1547 1.1614 0.108 Uiso 0.50 1 calc PR . . 
H8B H 0.0958 0.1095 1.2931 0.108 Uiso 0.50 1 calc PR . . 
H8C H 0.1452 -0.0243 1.2299 0.108 Uiso 0.50 1 calc PR . . 
H8D H 0.1452 0.0053 1.2949 0.108 Uiso 0.50 1 calc PR . . 
H8E H 0.0958 0.0504 1.1632 0.108 Uiso 0.50 1 calc PR . . 
H8F H 0.0465 0.1843 1.2264 0.108 Uiso 0.50 1 calc PR . . 
C9 C 0.3028(2) 0.1000(2) 1.15709(16) 0.0530(4) Uani 1 1 d . . . 
C10 C 0.4638(3) 0.0151(2) 1.19221(17) 0.0593(5) Uani 1 1 d . . . 
H10 H 0.4932 -0.0719 1.2615 0.071 Uiso 1 1 calc R . . 
C11 C 0.5793(2) 0.0838(2) 1.10354(17) 0.0556(5) Uani 1 1 d . . . 
C12 C 0.7707(3) 0.0354(3) 1.0988(2) 0.0742(6) Uani 1 1 d . . . 
H12A H 0.8110 0.1094 1.0307 0.111 Uiso 0.50 1 calc PR . . 
H12B H 0.8318 -0.0697 1.0876 0.111 Uiso 0.50 1 calc PR . . 
H12C H 0.7923 0.0353 1.1750 0.111 Uiso 0.50 1 calc PR . . 
H12D H 0.8124 -0.0594 1.1648 0.111 Uiso 0.50 1 calc PR . . 
H12E H 0.7916 0.1197 1.1079 0.111 Uiso 0.50 1 calc PR . . 
H12F H 0.8311 0.0147 1.0205 0.111 Uiso 0.50 1 calc PR . . 
C13 C 0.2448(2) 0.5948(2) 0.50751(17) 0.0548(4) Uani 1 1 d . . . 
C14 C 0.2493(3) 0.0863(2) 0.5287(2) 0.0698(6) Uani 1 1 d . . . 
H14A H 0.3037 0.0371 0.6024 0.105 Uiso 1 1 calc R . . 
H14B H 0.3191 0.0299 0.4677 0.105 Uiso 1 1 calc R . . 
H14C H 0.1350 0.0828 0.5482 0.105 Uiso 1 1 calc R . . 
C15 C 0.2341(2) 0.2555(2) 0.47846(17) 0.0537(4) Uani 1 1 d . . . 
C16 C 0.1932(2) 0.3602(2) 0.35998(17) 0.0559(5) Uani 1 1 d . . . 
H16 H 0.1710 0.3361 0.2977 0.067 Uiso 1 1 calc R . . 
C17 C 0.1926(2) 0.5016(2) 0.35468(16) 0.0513(4) Uani 1 1 d . . . 
C18 C 0.1639(3) 0.6498(3) 0.24973(17) 0.0662(5) Uani 1 1 d . . . 
H18A H 0.1366 0.6352 0.1819 0.099 Uiso 1 1 calc R . . 
H18B H 0.2680 0.6729 0.2234 0.099 Uiso 1 1 calc R . . 
H18C H 0.0686 0.7370 0.2762 0.099 Uiso 1 1 calc R . . 

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 
O1 0.0598(8) 0.0758(9) 0.0587(8) -0.0058(7) -0.0173(6) -0.0343(7) 
O2 0.1506(15) 0.0529(9) 0.0637(9) 0.0103(8) -0.0401(9) -0.0477(9) 
N1 0.0547(8) 0.0487(9) 0.0453(8) -0.0096(7) -0.0150(6) -0.0185(7) 
N2 0.0508(8) 0.0555(9) 0.0529(8) -0.0179(7) -0.0142(7) -0.0133(7) 
N3 0.0531(8) 0.0428(8) 0.0442(7) -0.0058(7) -0.0106(6) -0.0148(6) 
N4 0.0610(9) 0.0427(8) 0.0490(8) -0.0084(7) -0.0096(7) -0.0179(7) 
C1 0.0458(9) 0.0413(9) 0.0518(9) -0.0093(8) -0.0137(7) -0.0159(7) 
C2 0.0434(8) 0.0429(9) 0.0485(9) -0.0105(8) -0.0126(7) -0.0122(7) 
C3 0.0507(10) 0.0521(11) 0.0606(11) -0.0201(9) -0.0159(8) -0.0155(8) 
C4 0.0518(10) 0.0478(11) 0.0723(12) -0.0223(10) -0.0087(9) -0.0207(8) 
C5 0.0520(10) 0.0392(10) 0.0615(11) -0.0117(9) -0.0042(8) -0.0168(8) 
C6 0.0469(9) 0.0370(9) 0.0499(9) -0.0078(8) -0.0103(7) -0.0122(7) 
C7 0.0544(10) 0.0480(10) 0.0443(9) -0.0124(8) -0.0133(7) -0.0185(8) 
C8 0.0891(15) 0.0745(15) 0.0579(11) 0.0018(11) -0.0195(10) -0.0467(12) 
C9 0.0714(12) 0.0466(10) 0.0463(9) -0.0114(8) -0.0166(8) -0.0234(9) 
C10 0.0766(12) 0.0487(11) 0.0504(10) -0.0127(9) -0.0235(9) -0.0141(9) 
C11 0.0606(11) 0.0513(11) 0.0539(10) -0.0237(9) -0.0188(8) -0.0069(8) 
C12 0.0615(12) 0.0744(14) 0.0764(14) -0.0296(12) -0.0242(10) -0.0017(10) 
C13 0.0643(11) 0.0426(11) 0.0532(10) -0.0058(10) -0.0133(8) -0.0195(8) 
C14 0.0876(15) 0.0559(13) 0.0674(12) -0.0180(11) -0.0085(11) -0.0294(11) 
C15 0.0519(10) 0.0528(11) 0.0542(10) -0.0175(9) -0.0047(8) -0.0177(8) 
C16 0.0549(10) 0.0627(12) 0.0504(10) -0.0162(9) -0.0108(8) -0.0204(9) 
C17 0.0463(9) 0.0555(11) 0.0456(9) -0.0108(9) -0.0094(7) -0.0147(8) 
C18 0.0727(13) 0.0665(13) 0.0497(10) -0.0027(10) -0.0192(9) -0.0225(10) 

_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 
O1 C7 1.207(2) . ? 
O2 C13 1.208(2) . ? 
N1 N2 1.3840(19) . ? 
N1 C9 1.392(2) . ? 
N1 C7 1.409(2) . ? 
N2 C11 1.314(2) . ? 
N3 N4 1.386(2) . ? 
N3 C17 1.392(2) . ? 
N3 C13 1.402(2) . ? 
N4 C15 1.311(2) . ? 
C1 C6 1.388(2) . ? 
C1 C2 1.390(2) . ? 
C2 C3 1.392(2) . ? 
C2 C7 1.492(2) . ? 
C3 C4 1.378(3) . ? 
C4 C5 1.379(3) . ? 
C5 C6 1.391(2) . ? 
C6 C13 1.501(2) . ? 
C8 C9 1.487(3) . ? 
C9 C10 1.356(3) . ? 
C10 C11 1.419(3) . ? 
C11 C12 1.492(3) . ? 
C14 C15 1.491(3) . ? 
C15 C16 1.419(3) . ? 
C16 C17 1.352(3) . ? 
C17 C18 1.488(3) . ? 

loop_ 
_geom_angle_atom_site_label_1 
_geom_angle_atom_site_label_2 
_geom_angle_atom_site_label_3 
_geom_angle 
_geom_angle_site_symmetry_1 
_geom_angle_site_symmetry_3 
_geom_angle_publ_flag 
N2 N1 C9 111.74(14) . . ? 
N2 N1 C7 119.40(14) . . ? 
C9 N1 C7 128.16(15) . . ? 
C11 N2 N1 104.75(15) . . ? 
N4 N3 C17 111.36(14) . . ? 
N4 N3 C13 122.33(14) . . ? 
C17 N3 C13 126.29(15) . . ? 
C15 N4 N3 104.85(14) . . ? 
C6 C1 C2 120.14(15) . . ? 
C1 C2 C3 120.06(16) . . ? 
C1 C2 C7 116.65(14) . . ? 
C3 C2 C7 123.22(15) . . ? 
C4 C3 C2 119.69(17) . . ? 
C3 C4 C5 120.25(16) . . ? 
C4 C5 C6 120.79(17) . . ? 
C1 C6 C5 119.04(16) . . ? 
C1 C6 C13 126.15(15) . . ? 
C5 C6 C13 114.60(16) . . ? 
O1 C7 N1 120.62(16) . . ? 
O1 C7 C2 122.68(15) . . ? 
N1 C7 C2 116.64(14) . . ? 
C10 C9 N1 105.02(16) . . ? 
C10 C9 C8 130.84(18) . . ? 
N1 C9 C8 124.12(16) . . ? 
C9 C10 C11 107.26(17) . . ? 
N2 C11 C10 111.22(16) . . ? 
N2 C11 C12 119.82(19) . . ? 
C10 C11 C12 128.95(18) . . ? 
O2 C13 N3 118.84(17) . . ? 
O2 C13 C6 119.96(16) . . ? 
N3 C13 C6 121.20(16) . . ? 
N4 C15 C16 111.31(16) . . ? 
N4 C15 C14 121.34(17) . . ? 
C16 C15 C14 127.35(17) . . ? 
C17 C16 C15 107.10(16) . . ? 
C16 C17 N3 105.37(15) . . ? 
C16 C17 C18 129.02(17) . . ? 
N3 C17 C18 125.59(17) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
C9 N1 N2 C11 -0.24(17) . . . . ? 
C7 N1 N2 C11 -171.45(14) . . . . ? 
C17 N3 N4 C15 -0.95(18) . . . . ? 
C13 N3 N4 C15 -179.35(15) . . . . ? 
C6 C1 C2 C3 1.6(2) . . . . ? 
C6 C1 C2 C7 178.59(15) . . . . ? 
C1 C2 C3 C4 0.0(2) . . . . ? 
C7 C2 C3 C4 -176.85(15) . . . . ? 
C2 C3 C4 C5 -0.9(3) . . . . ? 
C3 C4 C5 C6 0.4(3) . . . . ? 
C2 C1 C6 C5 -2.1(2) . . . . ? 
C2 C1 C6 C13 -176.48(16) . . . . ? 
C4 C5 C6 C1 1.2(2) . . . . ? 
C4 C5 C6 C13 176.16(15) . . . . ? 
N2 N1 C7 O1 167.02(15) . . . . ? 
C9 N1 C7 O1 -2.6(3) . . . . ? 
N2 N1 C7 C2 -10.3(2) . . . . ? 
C9 N1 C7 C2 -179.94(15) . . . . ? 
C1 C2 C7 O1 -44.1(2) . . . . ? 
C3 C2 C7 O1 132.84(18) . . . . ? 
C1 C2 C7 N1 133.23(16) . . . . ? 
C3 C2 C7 N1 -49.9(2) . . . . ? 
N2 N1 C9 C10 0.29(18) . . . . ? 
C7 N1 C9 C10 170.54(16) . . . . ? 
N2 N1 C9 C8 179.17(16) . . . . ? 
C7 N1 C9 C8 -10.6(3) . . . . ? 
N1 C9 C10 C11 -0.22(18) . . . . ? 
C8 C9 C10 C11 -178.99(18) . . . . ? 
N1 N2 C11 C10 0.09(18) . . . . ? 
N1 N2 C11 C12 -179.96(15) . . . . ? 
C9 C10 C11 N2 0.1(2) . . . . ? 
C9 C10 C11 C12 -179.85(17) . . . . ? 
N4 N3 C13 O2 175.58(17) . . . . ? 
C17 N3 C13 O2 -2.6(3) . . . . ? 
N4 N3 C13 C6 -4.1(2) . . . . ? 
C17 N3 C13 C6 177.71(15) . . . . ? 
C1 C6 C13 O2 152.04(19) . . . . ? 
C5 C6 C13 O2 -22.5(3) . . . . ? 
C1 C6 C13 N3 -28.3(3) . . . . ? 
C5 C6 C13 N3 157.15(16) . . . . ? 
N3 N4 C15 C16 0.35(19) . . . . ? 
N3 N4 C15 C14 -178.98(16) . . . . ? 
N4 C15 C16 C17 0.4(2) . . . . ? 
C14 C15 C16 C17 179.65(18) . . . . ? 
C15 C16 C17 N3 -0.90(19) . . . . ? 
C15 C16 C17 C18 177.50(18) . . . . ? 
N4 N3 C17 C16 1.17(18) . . . . ? 
C13 N3 C17 C16 179.51(16) . . . . ? 
N4 N3 C17 C18 -177.30(16) . . . . ? 
C13 N3 C17 C18 1.0(3) . . . . ? 

_diffrn_measured_fraction_theta_max    0.881 
_diffrn_reflns_theta_full              26.38 
_diffrn_measured_fraction_theta_full   0.881 
_refine_diff_density_max    0.202 
_refine_diff_density_min   -0.204 
_refine_diff_density_rms    0.031 

data_daro
_database_code_CSD                  185337


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C24.50 H25 Cl1.50 N6 O3' 
_chemical_formula_weight          504.68 

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' 

_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    ? 

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                    23.360(2) 
_cell_length_b                    17.3164(15) 
_cell_length_c                    16.6335(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  128.1070(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      5294.3(8) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     296(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.38 
_exptl_crystal_size_mid           0.32 
_exptl_crystal_size_min           0.29 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.266 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2108 
_exptl_absorpt_coefficient_mu     0.231 
_exptl_absorpt_correction_type    'Empirical with SADABS' 
_exptl_absorpt_correction_T_min   0.9173 
_exptl_absorpt_correction_T_max   0.9360 
_exptl_absorpt_process_details    ?

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       296(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_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             4148 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0478 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        21 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.70 
_diffrn_reflns_theta_max          23.99 
_reflns_number_total              4148 
_reflns_number_gt                 3185 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.0587P)^2^+5.9411P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4148 
_refine_ls_number_parameters      308 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0731 
_refine_ls_R_factor_gt            0.0550 
_refine_ls_wR_factor_ref          0.1311 
_refine_ls_wR_factor_gt           0.1246 
_refine_ls_goodness_of_fit_ref    1.019 
_refine_ls_restrained_S_all       1.019 
_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 
O1 O 1.06156(9) 0.44196(10) 0.21575(13) 0.0344(4) Uani 1 1 d . . . 
O2 O 1.08397(10) 0.14795(10) 0.02846(15) 0.0445(5) Uani 1 1 d . . . 
O3 O 0.88915(9) 0.16008(10) 0.16572(14) 0.0349(4) Uani 1 1 d . . . 
N1 N 1.07477(10) 0.44492(11) 0.09227(14) 0.0234(5) Uani 1 1 d . . . 
N2 N 1.06335(11) 0.40956(12) 0.00900(15) 0.0288(5) Uani 1 1 d . . . 
N3 N 0.97390(10) 0.09020(11) -0.07014(15) 0.0284(5) Uani 1 1 d . . . 
N4 N 0.90379(11) 0.08412(13) -0.10173(17) 0.0362(5) Uani 1 1 d . . . 
N5 N 0.83496(10) 0.27772(11) 0.11694(14) 0.0253(5) Uani 1 1 d . . . 
N6 N 0.82181(10) 0.34529(11) 0.06303(15) 0.0268(5) Uani 1 1 d . . . 
C1 C 1.01716(12) 0.33157(13) 0.11063(17) 0.0228(5) Uani 1 1 d . . . 
C2 C 1.03294(12) 0.27362(13) 0.06935(17) 0.0257(6) Uani 1 1 d . . . 
H2 H 1.0669 0.2827 0.0584 0.031 Uiso 1 1 calc R . . 
C3 C 0.99862(12) 0.20189(13) 0.04399(18) 0.0243(6) Uani 1 1 d . . . 
C4 C 0.94969(12) 0.18791(14) 0.06375(17) 0.0250(5) Uani 1 1 d . . . 
H4 H 0.9277 0.1397 0.0492 0.030 Uiso 1 1 calc R . . 
C5 C 0.93350(12) 0.24563(13) 0.10523(17) 0.0236(5) Uani 1 1 d . . . 
C6 C 0.96698(12) 0.31752(13) 0.12799(17) 0.0225(5) Uani 1 1 d . . . 
H6 H 0.9557 0.3563 0.1549 0.027 Uiso 1 1 calc R . . 
C7 C 1.05296(12) 0.40956(14) 0.14484(18) 0.0249(5) Uani 1 1 d . . . 
C8 C 1.12394(15) 0.57157(15) 0.1921(2) 0.0396(7) Uani 1 1 d . . . 
H8A H 1.1481 0.6163 0.1919 0.059 Uiso 1 1 calc R . . 
H8B H 1.1551 0.5464 0.2573 0.059 Uiso 1 1 calc R . . 
H8C H 1.0797 0.5871 0.1799 0.059 Uiso 1 1 calc R . . 
C9 C 1.10665(12) 0.51724(14) 0.11031(18) 0.0274(6) Uani 1 1 d . . . 
C10 C 1.11621(13) 0.52613(14) 0.03873(19) 0.0307(6) Uani 1 1 d . . . 
H10 H 1.1367 0.5686 0.0309 0.037 Uiso 1 1 calc R . . 
C11 C 1.08907(13) 0.45840(14) -0.02252(19) 0.0292(6) Uani 1 1 d . . . 
C12 C 1.08657(16) 0.43802(18) -0.1115(2) 0.0449(7) Uani 1 1 d . . . 
H12A H 1.1344 0.4240 -0.0879 0.067 Uiso 1 1 calc R . . 
H12B H 1.0696 0.4816 -0.1565 0.067 Uiso 1 1 calc R . . 
H12C H 1.0541 0.3953 -0.1474 0.067 Uiso 1 1 calc R . . 
C13 C 1.02270(13) 0.14515(14) 0.0024(2) 0.0299(6) Uani 1 1 d . . . 
C14 C 1.05645(15) 0.02868(16) -0.1039(2) 0.0399(7) Uani 1 1 d . . . 
H14A H 1.0526 -0.0129 -0.1452 0.060 Uiso 1 1 calc R . . 
H14B H 1.0955 0.0183 -0.0333 0.060 Uiso 1 1 calc R . . 
H14C H 1.0661 0.0760 -0.1237 0.060 Uiso 1 1 calc R . . 
C15 C 0.98690(13) 0.03602(14) -0.11876(19) 0.0299(6) Uani 1 1 d . . . 
C16 C 0.92483(14) -0.00460(16) -0.1798(2) 0.0362(6) Uani 1 1 d . . . 
H16 H 0.9163 -0.0454 -0.2223 0.043 Uiso 1 1 calc R . . 
C17 C 0.87510(14) 0.02646(16) -0.1670(2) 0.0392(7) Uani 1 1 d . . . 
C18 C 0.79907(16) -0.0002(2) -0.2168(3) 0.0646(10) Uani 1 1 d . . . 
H18A H 0.8004 -0.0490 -0.1883 0.097 Uiso 1 1 calc R . . 
H18B H 0.7735 -0.0058 -0.2889 0.097 Uiso 1 1 calc R . . 
H18C H 0.7745 0.0371 -0.2051 0.097 Uiso 1 1 calc R . . 
C19 C 0.88536(12) 0.22334(14) 0.13178(17) 0.0248(5) Uani 1 1 d . . . 
C20 C 0.78929(15) 0.20490(17) 0.2008(2) 0.0408(7) Uani 1 1 d . . . 
H20A H 0.7580 0.2165 0.2183 0.061 Uiso 1 1 calc R . . 
H20B H 0.8377 0.1952 0.2620 0.061 Uiso 1 1 calc R . . 
H20C H 0.7715 0.1600 0.1579 0.061 Uiso 1 1 calc R . . 
C21 C 0.79038(13) 0.27162(15) 0.14534(18) 0.0293(6) Uani 1 1 d . . . 
C22 C 0.74965(14) 0.33656(15) 0.1099(2) 0.0338(6) Uani 1 1 d . . . 
H22 H 0.7145 0.3501 0.1172 0.041 Uiso 1 1 calc R . . 
C23 C 0.77039(13) 0.38014(14) 0.05970(19) 0.0296(6) Uani 1 1 d . . . 
C24 C 0.74047(14) 0.45628(15) 0.0060(2) 0.0412(7) Uani 1 1 d . . . 
H24A H 0.7661 0.4727 -0.0191 0.062 Uiso 1 1 calc R . . 
H24B H 0.7465 0.4940 0.0530 0.062 Uiso 1 1 calc R . . 
H24C H 0.6897 0.4507 -0.0502 0.062 Uiso 1 1 calc R . . 

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 
O1 0.0457(11) 0.0302(10) 0.0377(11) -0.0102(8) 0.0309(9) -0.0093(8) 
O2 0.0364(11) 0.0367(11) 0.0726(14) -0.0203(10) 0.0397(11) -0.0080(9) 
O3 0.0388(10) 0.0269(10) 0.0477(11) 0.0079(9) 0.0310(9) 0.0001(8) 
N1 0.0272(11) 0.0201(11) 0.0289(11) -0.0007(9) 0.0204(10) -0.0020(8) 
N2 0.0315(12) 0.0292(12) 0.0303(12) 0.0011(9) 0.0214(10) 0.0006(9) 
N3 0.0275(11) 0.0261(11) 0.0364(12) -0.0086(9) 0.0222(10) -0.0034(9) 
N4 0.0304(12) 0.0386(14) 0.0415(13) -0.0125(11) 0.0231(11) -0.0029(10) 
N5 0.0261(11) 0.0238(11) 0.0296(11) 0.0000(9) 0.0191(10) -0.0015(9) 
N6 0.0258(11) 0.0231(11) 0.0339(12) 0.0005(9) 0.0197(10) 0.0013(9) 
C1 0.0244(13) 0.0200(13) 0.0225(12) 0.0028(10) 0.0136(11) 0.0014(10) 
C2 0.0254(13) 0.0247(13) 0.0323(14) 0.0034(11) 0.0205(12) 0.0028(10) 
C3 0.0235(13) 0.0216(13) 0.0269(13) 0.0007(10) 0.0151(11) 0.0034(10) 
C4 0.0249(13) 0.0208(13) 0.0266(13) -0.0008(10) 0.0146(11) -0.0008(10) 
C5 0.0249(13) 0.0223(13) 0.0237(12) 0.0034(10) 0.0151(11) 0.0027(10) 
C6 0.0242(13) 0.0213(13) 0.0215(12) 0.0022(10) 0.0139(11) 0.0053(10) 
C7 0.0248(13) 0.0224(13) 0.0282(13) 0.0002(11) 0.0167(11) 0.0022(10) 
C8 0.0390(16) 0.0270(15) 0.0551(18) -0.0063(13) 0.0302(15) -0.0089(12) 
C9 0.0202(12) 0.0225(14) 0.0353(14) 0.0030(11) 0.0151(12) 0.0008(10) 
C10 0.0244(13) 0.0274(14) 0.0414(15) 0.0083(12) 0.0207(12) 0.0001(11) 
C11 0.0266(13) 0.0313(15) 0.0337(14) 0.0074(12) 0.0206(12) 0.0035(11) 
C12 0.0513(18) 0.0517(19) 0.0436(17) 0.0055(14) 0.0353(16) -0.0008(15) 
C13 0.0295(14) 0.0243(14) 0.0424(15) -0.0015(12) 0.0254(13) -0.0009(11) 
C14 0.0452(17) 0.0341(16) 0.0550(18) -0.0071(13) 0.0382(16) 0.0018(13) 
C15 0.0356(15) 0.0248(14) 0.0337(14) -0.0025(11) 0.0237(13) 0.0023(11) 
C16 0.0414(16) 0.0335(15) 0.0353(15) -0.0110(12) 0.0244(14) -0.0032(13) 
C17 0.0338(15) 0.0426(17) 0.0410(16) -0.0132(14) 0.0230(14) -0.0032(13) 
C18 0.0389(18) 0.071(2) 0.076(2) -0.041(2) 0.0320(18) -0.0166(17) 
C19 0.0257(13) 0.0241(14) 0.0253(13) -0.0010(11) 0.0161(11) -0.0032(11) 
C20 0.0412(16) 0.0508(19) 0.0458(17) 0.0005(14) 0.0346(15) -0.0053(14) 
C21 0.0278(13) 0.0346(15) 0.0311(14) -0.0062(12) 0.0210(12) -0.0069(12) 
C22 0.0294(14) 0.0406(16) 0.0421(16) -0.0108(13) 0.0274(13) -0.0042(12) 
C23 0.0243(13) 0.0273(14) 0.0379(15) -0.0077(11) 0.0196(12) -0.0037(11) 
C24 0.0342(15) 0.0315(16) 0.0608(19) -0.0004(14) 0.0309(15) 0.0044(12) 

_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 
O1 C7 1.206(3) . ? 
O2 C13 1.214(3) . ? 
O3 C19 1.210(3) . ? 
N1 N2 1.381(3) . ? 
N1 C9 1.392(3) . ? 
N1 C7 1.396(3) . ? 
N2 C11 1.319(3) . ? 
N3 N4 1.381(3) . ? 
N3 C15 1.389(3) . ? 
N3 C13 1.401(3) . ? 
N4 C17 1.314(3) . ? 
N5 C21 1.388(3) . ? 
N5 N6 1.388(3) . ? 
N5 C19 1.405(3) . ? 
N6 C23 1.315(3) . ? 
C1 C2 1.388(3) . ? 
C1 C6 1.391(3) . ? 
C1 C7 1.503(3) . ? 
C2 C3 1.395(3) . ? 
C3 C4 1.392(3) . ? 
C3 C13 1.497(3) . ? 
C4 C5 1.393(3) . ? 
C5 C6 1.393(3) . ? 
C5 C19 1.490(3) . ? 
C8 C9 1.491(4) . ? 
C9 C10 1.349(3) . ? 
C10 C11 1.421(3) . ? 
C11 C12 1.487(4) . ? 
C14 C15 1.490(3) . ? 
C15 C16 1.346(3) . ? 
C16 C17 1.411(4) . ? 
C17 C18 1.496(4) . ? 
C20 C21 1.489(4) . ? 
C21 C22 1.351(4) . ? 
C22 C23 1.415(4) . ? 
C23 C24 1.501(4) . ? 

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 N1 C9 111.20(18) . . ? 
N2 N1 C7 120.95(18) . . ? 
C9 N1 C7 127.8(2) . . ? 
C11 N2 N1 105.12(19) . . ? 
N4 N3 C15 111.17(19) . . ? 
N4 N3 C13 121.53(19) . . ? 
C15 N3 C13 127.3(2) . . ? 
C17 N4 N3 104.65(19) . . ? 
C21 N5 N6 111.76(19) . . ? 
C21 N5 C19 127.8(2) . . ? 
N6 N5 C19 120.37(18) . . ? 
C23 N6 N5 104.26(19) . . ? 
C2 C1 C6 119.4(2) . . ? 
C2 C1 C7 125.5(2) . . ? 
C6 C1 C7 115.0(2) . . ? 
C1 C2 C3 121.0(2) . . ? 
C4 C3 C2 119.1(2) . . ? 
C4 C3 C13 126.4(2) . . ? 
C2 C3 C13 114.5(2) . . ? 
C3 C4 C5 120.4(2) . . ? 
C6 C5 C4 119.8(2) . . ? 
C6 C5 C19 123.4(2) . . ? 
C4 C5 C19 116.5(2) . . ? 
C1 C6 C5 120.3(2) . . ? 
O1 C7 N1 120.2(2) . . ? 
O1 C7 C1 120.4(2) . . ? 
N1 C7 C1 119.3(2) . . ? 
C10 C9 N1 105.7(2) . . ? 
C10 C9 C8 129.4(2) . . ? 
N1 C9 C8 124.9(2) . . ? 
C9 C10 C11 107.2(2) . . ? 
N2 C11 C10 110.8(2) . . ? 
N2 C11 C12 119.7(2) . . ? 
C10 C11 C12 129.5(2) . . ? 
O2 C13 N3 119.2(2) . . ? 
O2 C13 C3 120.4(2) . . ? 
N3 C13 C3 120.4(2) . . ? 
C16 C15 N3 105.7(2) . . ? 
C16 C15 C14 129.6(2) . . ? 
N3 C15 C14 124.7(2) . . ? 
C15 C16 C17 106.9(2) . . ? 
N4 C17 C16 111.5(2) . . ? 
N4 C17 C18 121.2(2) . . ? 
C16 C17 C18 127.3(2) . . ? 
O3 C19 N5 120.0(2) . . ? 
O3 C19 C5 121.4(2) . . ? 
N5 C19 C5 118.5(2) . . ? 
C22 C21 N5 105.2(2) . . ? 
C22 C21 C20 129.7(2) . . ? 
N5 C21 C20 125.0(2) . . ? 
C21 C22 C23 107.2(2) . . ? 
N6 C23 C22 111.5(2) . . ? 
N6 C23 C24 120.4(2) . . ? 
C22 C23 C24 128.0(2) . . ? 

loop_ 
_geom_torsion_atom_site_label_1 
_geom_torsion_atom_site_label_2 
_geom_torsion_atom_site_label_3 
_geom_torsion_atom_site_label_4 
_geom_torsion 
_geom_torsion_site_symmetry_1 
_geom_torsion_site_symmetry_2 
_geom_torsion_site_symmetry_3 
_geom_torsion_site_symmetry_4 
_geom_torsion_publ_flag 
C9 N1 N2 C11 1.2(2) . . . . ? 
C7 N1 N2 C11 179.1(2) . . . . ? 
C15 N3 N4 C17 1.1(3) . . . . ? 
C13 N3 N4 C17 -178.6(2) . . . . ? 
C21 N5 N6 C23 0.6(2) . . . . ? 
C19 N5 N6 C23 177.1(2) . . . . ? 
C6 C1 C2 C3 0.7(3) . . . . ? 
C7 C1 C2 C3 177.2(2) . . . . ? 
C1 C2 C3 C4 -2.1(3) . . . . ? 
C1 C2 C3 C13 -178.8(2) . . . . ? 
C2 C3 C4 C5 2.0(3) . . . . ? 
C13 C3 C4 C5 178.3(2) . . . . ? 
C3 C4 C5 C6 -0.6(3) . . . . ? 
C3 C4 C5 C19 -175.1(2) . . . . ? 
C2 C1 C6 C5 0.7(3) . . . . ? 
C7 C1 C6 C5 -176.1(2) . . . . ? 
C4 C5 C6 C1 -0.8(3) . . . . ? 
C19 C5 C6 C1 173.2(2) . . . . ? 
N2 N1 C7 O1 -178.1(2) . . . . ? 
C9 N1 C7 O1 -0.6(4) . . . . ? 
N2 N1 C7 C1 0.6(3) . . . . ? 
C9 N1 C7 C1 178.0(2) . . . . ? 
C2 C1 C7 O1 -147.4(2) . . . . ? 
C6 C1 C7 O1 29.2(3) . . . . ? 
C2 C1 C7 N1 34.0(3) . . . . ? 
C6 C1 C7 N1 -149.4(2) . . . . ? 
N2 N1 C9 C10 -1.1(2) . . . . ? 
C7 N1 C9 C10 -178.8(2) . . . . ? 
N2 N1 C9 C8 177.9(2) . . . . ? 
C7 N1 C9 C8 0.2(4) . . . . ? 
N1 C9 C10 C11 0.4(3) . . . . ? 
C8 C9 C10 C11 -178.4(2) . . . . ? 
N1 N2 C11 C10 -0.9(3) . . . . ? 
N1 N2 C11 C12 179.1(2) . . . . ? 
C9 C10 C11 N2 0.3(3) . . . . ? 
C9 C10 C11 C12 -179.7(3) . . . . ? 
N4 N3 C13 O2 179.4(2) . . . . ? 
C15 N3 C13 O2 -0.2(4) . . . . ? 
N4 N3 C13 C3 -3.1(3) . . . . ? 
C15 N3 C13 C3 177.3(2) . . . . ? 
C4 C3 C13 O2 -146.9(3) . . . . ? 
C2 C3 C13 O2 29.4(3) . . . . ? 
C4 C3 C13 N3 35.6(4) . . . . ? 
C2 C3 C13 N3 -148.0(2) . . . . ? 
N4 N3 C15 C16 -0.8(3) . . . . ? 
C13 N3 C15 C16 178.8(2) . . . . ? 
N4 N3 C15 C14 178.2(2) . . . . ? 
C13 N3 C15 C14 -2.1(4) . . . . ? 
N3 C15 C16 C17 0.3(3) . . . . ? 
C14 C15 C16 C17 -178.7(3) . . . . ? 
N3 N4 C17 C16 -0.9(3) . . . . ? 
N3 N4 C17 C18 178.2(3) . . . . ? 
C15 C16 C17 N4 0.4(3) . . . . ? 
C15 C16 C17 C18 -178.6(3) . . . . ? 
C21 N5 C19 O3 6.4(4) . . . . ? 
N6 N5 C19 O3 -169.5(2) . . . . ? 
C21 N5 C19 C5 -173.4(2) . . . . ? 
N6 N5 C19 C5 10.8(3) . . . . ? 
C6 C5 C19 O3 -137.8(2) . . . . ? 
C4 C5 C19 O3 36.4(3) . . . . ? 
C6 C5 C19 N5 41.9(3) . . . . ? 
C4 C5 C19 N5 -143.8(2) . . . . ? 
N6 N5 C21 C22 -0.8(3) . . . . ? 
C19 N5 C21 C22 -177.0(2) . . . . ? 
N6 N5 C21 C20 177.9(2) . . . . ? 
C19 N5 C21 C20 1.7(4) . . . . ? 
N5 C21 C22 C23 0.6(3) . . . . ? 
C20 C21 C22 C23 -178.0(3) . . . . ? 
N5 N6 C23 C22 -0.2(3) . . . . ? 
N5 N6 C23 C24 -179.5(2) . . . . ? 
C21 C22 C23 N6 -0.3(3) . . . . ? 
C21 C22 C23 C24 179.0(2) . . . . ? 

_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              23.99 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    0.207 
_refine_diff_density_min   -0.172 
_refine_diff_density_rms    0.045 

data_darr 
_database_code_CSD                  185338


_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C30 H42 N4 O2' 
_chemical_formula_weight          490.68 

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' 

_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                    11.2718(11) 
_cell_length_b                    18.6937(18) 
_cell_length_c                    13.9240(15) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.554(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2920.2(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.44 
_exptl_crystal_size_mid           0.42 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.116 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1064 
_exptl_absorpt_coefficient_mu     0.070 
_exptl_absorpt_correction_type    'Empirical with SADABS' 
_exptl_absorpt_correction_T_min   0.9696 
_exptl_absorpt_correction_T_max   0.9860 
_exptl_absorpt_process_details    ?

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       173(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   ? 
_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             11835 
_diffrn_reflns_av_R_equivalents   0.0364 
_diffrn_reflns_av_sigmaI/netI     0.0624 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.83 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              5094 
_reflns_number_gt                 3903 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 

_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^)+(0.0424P)^2^+0.5568P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5094 
_refine_ls_number_parameters      337 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0645 
_refine_ls_R_factor_gt            0.0464 
_refine_ls_wR_factor_ref          0.1210 
_refine_ls_wR_factor_gt           0.1142 
_refine_ls_goodness_of_fit_ref    1.042 
_refine_ls_restrained_S_all       1.042 
_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 
O1 O 0.85321(11) 0.23388(7) 0.23901(9) 0.0407(3) Uani 1 1 d . . . 
O2 O 0.97183(11) 0.10011(8) 0.11090(9) 0.0462(4) Uani 1 1 d . . . 
N1 N 0.79419(11) 0.23656(7) 0.39073(9) 0.0283(3) Uani 1 1 d . . . 
N2 N 0.79953(12) 0.20008(7) 0.47798(9) 0.0293(3) Uani 1 1 d . . . 
N3 N 0.79593(12) 0.09037(8) 0.17991(9) 0.0315(3) Uani 1 1 d . . . 
N4 N 0.75207(12) 0.07721(7) 0.26721(9) 0.0300(3) Uani 1 1 d . . . 
C1 C 0.61428(18) 0.30437(12) 0.21837(14) 0.0478(5) Uani 1 1 d . . . 
H1A H 0.6708 0.2714 0.1926 0.072 Uiso 1 1 calc R . . 
H1B H 0.5862 0.3390 0.1685 0.072 Uiso 1 1 calc R . . 
H1C H 0.5463 0.2773 0.2382 0.072 Uiso 1 1 calc R . . 
C2 C 0.78338(19) 0.38672(11) 0.27872(16) 0.0503(5) Uani 1 1 d . . . 
H2A H 0.8218 0.4105 0.3363 0.075 Uiso 1 1 calc R . . 
H2B H 0.7568 0.4228 0.2302 0.075 Uiso 1 1 calc R . . 
H2C H 0.8403 0.3543 0.2523 0.075 Uiso 1 1 calc R . . 
C3 C 0.5854(2) 0.39742(12) 0.33966(16) 0.0546(6) Uani 1 1 d . . . 
H3A H 0.5146 0.3715 0.3563 0.082 Uiso 1 1 calc R . . 
H3B H 0.5624 0.4316 0.2878 0.082 Uiso 1 1 calc R . . 
H3C H 0.6212 0.4232 0.3965 0.082 Uiso 1 1 calc R . . 
C4 C 0.67617(16) 0.34405(10) 0.30578(13) 0.0373(4) Uani 1 1 d . . . 
C5 C 0.71075(14) 0.29266(9) 0.38845(12) 0.0294(4) Uani 1 1 d . . . 
C6 C 0.66753(15) 0.29057(9) 0.47556(12) 0.0321(4) Uani 1 1 d . . . 
H6 H 0.6100 0.3222 0.4976 0.038 Uiso 1 1 calc R . . 
C7 C 0.72336(14) 0.23287(9) 0.52818(12) 0.0296(4) Uani 1 1 d . . . 
C8 C 0.70257(16) 0.20922(10) 0.62872(12) 0.0376(4) Uani 1 1 d . . . 
C9 C 0.7390(3) 0.27130(13) 0.69755(15) 0.0676(7) Uani 1 1 d . . . 
H9A H 0.8238 0.2818 0.6952 0.101 Uiso 1 1 calc R . . 
H9B H 0.7246 0.2579 0.7635 0.101 Uiso 1 1 calc R . . 
H9C H 0.6917 0.3138 0.6779 0.101 Uiso 1 1 calc R . . 
C10 C 0.57002(18) 0.19309(14) 0.63154(15) 0.0567(6) Uani 1 1 d . . . 
H10A H 0.5235 0.2365 0.6154 0.085 Uiso 1 1 calc R . . 
H10B H 0.5557 0.1770 0.6964 0.085 Uiso 1 1 calc R . . 
H10C H 0.5459 0.1555 0.5847 0.085 Uiso 1 1 calc R . . 
C11 C 0.77472(17) 0.14287(11) 0.65780(13) 0.0428(5) Uani 1 1 d . . . 
H11A H 0.7498 0.1035 0.6139 0.064 Uiso 1 1 calc R . . 
H11B H 0.7614 0.1294 0.7239 0.064 Uiso 1 1 calc R . . 
H11C H 0.8596 0.1528 0.6544 0.064 Uiso 1 1 calc R . . 
C12 C 0.86592(14) 0.21169(9) 0.32117(12) 0.0300(4) Uani 1 1 d . . . 
C13 C 0.96060(14) 0.15817(9) 0.35007(12) 0.0300(4) Uani 1 1 d . . . 
C14 C 1.03515(15) 0.16321(10) 0.43459(13) 0.0394(4) Uani 1 1 d . . . 
H14 H 1.0204 0.1987 0.4808 0.047 Uiso 1 1 calc R . . 
C15 C 1.13082(17) 0.11736(12) 0.45282(14) 0.0475(5) Uani 1 1 d . . . 
H15 H 1.1807 0.1212 0.5116 0.057 Uiso 1 1 calc R . . 
C16 C 1.15386(17) 0.06659(12) 0.38674(15) 0.0478(5) Uani 1 1 d . . . 
H16 H 1.2185 0.0344 0.4003 0.057 Uiso 1 1 calc R . . 
C17 C 1.08316(16) 0.06194(10) 0.29997(14) 0.0388(4) Uani 1 1 d . . . 
H17 H 1.1010 0.0275 0.2533 0.047 Uiso 1 1 calc R . . 
C18 C 0.98661(14) 0.10719(9) 0.28085(12) 0.0309(4) Uani 1 1 d . . . 
C19 C 0.91972(15) 0.10042(9) 0.18251(12) 0.0332(4) Uani 1 1 d . . . 
C20 C 0.7786(2) 0.18178(12) -0.01330(14) 0.0538(6) Uani 1 1 d . . . 
H20A H 0.7357 0.2201 0.0166 0.081 Uiso 1 1 calc R . . 
H20B H 0.7801 0.1918 -0.0823 0.081 Uiso 1 1 calc R . . 
H20C H 0.8604 0.1791 0.0175 0.081 Uiso 1 1 calc R . . 
C21 C 0.5887(2) 0.11661(15) -0.05191(15) 0.0639(7) Uani 1 1 d . . . 
H21A H 0.5474 0.0707 -0.0482 0.096 Uiso 1 1 calc R . . 
H21B H 0.5933 0.1293 -0.1197 0.096 Uiso 1 1 calc R . . 
H21C H 0.5447 0.1537 -0.0206 0.096 Uiso 1 1 calc R . . 
C22 C 0.7782(2) 0.04872(13) -0.04678(14) 0.0561(6) Uani 1 1 d . . . 
H22A H 0.8597 0.0442 -0.0159 0.084 Uiso 1 1 calc R . . 
H22B H 0.7805 0.0583 -0.1158 0.084 Uiso 1 1 calc R . . 
H22C H 0.7346 0.0041 -0.0384 0.084 Uiso 1 1 calc R . . 
C23 C 0.71546(18) 0.11036(11) -0.00047(13) 0.0455(5) Uani 1 1 d . . . 
C24 C 0.70410(16) 0.09521(10) 0.10572(12) 0.0363(4) Uani 1 1 d . . . 
C25 C 0.60313(16) 0.08439(10) 0.14903(12) 0.0363(4) Uani 1 1 d . . . 
H25 H 0.5242 0.0844 0.1182 0.044 Uiso 1 1 calc R . . 
C26 C 0.63623(15) 0.07305(9) 0.24865(12) 0.0307(4) Uani 1 1 d . . . 
C27 C 0.55770(15) 0.05883(10) 0.32819(12) 0.0333(4) Uani 1 1 d . . . 
C28 C 0.46243(17) 0.00403(11) 0.29339(15) 0.0457(5) Uani 1 1 d . . . 
H28A H 0.4113 0.0239 0.2389 0.069 Uiso 1 1 calc R . . 
H28B H 0.4140 -0.0073 0.3461 0.069 Uiso 1 1 calc R . . 
H28C H 0.5009 -0.0396 0.2728 0.069 Uiso 1 1 calc R . . 
C29 C 0.63268(17) 0.03011(11) 0.41732(13) 0.0434(5) Uani 1 1 d . . . 
H29A H 0.6653 -0.0168 0.4026 0.065 Uiso 1 1 calc R . . 
H29B H 0.5826 0.0254 0.4707 0.065 Uiso 1 1 calc R . . 
H29C H 0.6982 0.0633 0.4357 0.065 Uiso 1 1 calc R . . 
C30 C 0.49793(18) 0.12853(11) 0.35404(15) 0.0460(5) Uani 1 1 d . . . 
H30A H 0.5590 0.1631 0.3784 0.069 Uiso 1 1 calc R . . 
H30B H 0.4441 0.1193 0.4039 0.069 Uiso 1 1 calc R . . 
H30C H 0.4523 0.1480 0.2965 0.069 Uiso 1 1 calc R . . 

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 
O1 0.0468(8) 0.0367(7) 0.0404(7) 0.0098(6) 0.0141(6) 0.0069(6) 
O2 0.0403(8) 0.0625(10) 0.0377(7) -0.0018(6) 0.0138(6) -0.0041(7) 
N1 0.0273(7) 0.0255(8) 0.0326(7) 0.0035(6) 0.0050(6) 0.0023(6) 
N2 0.0290(7) 0.0280(8) 0.0308(7) 0.0020(6) 0.0025(6) 0.0009(6) 
N3 0.0300(8) 0.0342(8) 0.0306(8) 0.0011(6) 0.0044(6) -0.0047(6) 
N4 0.0308(8) 0.0300(8) 0.0294(7) 0.0008(6) 0.0035(6) -0.0033(6) 
C1 0.0435(11) 0.0548(13) 0.0436(11) 0.0108(9) -0.0028(9) 0.0028(10) 
C2 0.0519(12) 0.0328(11) 0.0671(14) 0.0174(10) 0.0111(10) -0.0003(9) 
C3 0.0593(13) 0.0427(12) 0.0627(13) 0.0139(10) 0.0106(11) 0.0230(11) 
C4 0.0368(10) 0.0308(10) 0.0447(10) 0.0095(8) 0.0056(8) 0.0057(8) 
C5 0.0256(8) 0.0223(9) 0.0404(10) -0.0009(7) 0.0030(7) 0.0007(7) 
C6 0.0286(9) 0.0259(9) 0.0422(10) -0.0026(7) 0.0059(7) 0.0052(7) 
C7 0.0265(9) 0.0288(9) 0.0334(9) -0.0023(7) 0.0021(7) -0.0014(7) 
C8 0.0414(10) 0.0410(11) 0.0308(9) 0.0002(8) 0.0048(8) 0.0069(8) 
C9 0.108(2) 0.0568(15) 0.0374(11) -0.0110(10) 0.0019(12) 0.0083(14) 
C10 0.0450(12) 0.0772(17) 0.0506(12) 0.0258(11) 0.0186(10) 0.0144(11) 
C11 0.0428(11) 0.0481(12) 0.0377(10) 0.0083(9) 0.0044(8) 0.0056(9) 
C12 0.0282(9) 0.0250(9) 0.0375(10) 0.0006(7) 0.0063(7) -0.0048(7) 
C13 0.0233(8) 0.0305(10) 0.0367(9) -0.0009(7) 0.0053(7) -0.0004(7) 
C14 0.0314(10) 0.0412(11) 0.0450(11) -0.0088(8) 0.0005(8) 0.0005(8) 
C15 0.0321(10) 0.0616(14) 0.0467(11) -0.0073(10) -0.0069(8) 0.0079(9) 
C16 0.0336(10) 0.0523(13) 0.0566(12) -0.0020(10) -0.0004(9) 0.0145(9) 
C17 0.0321(10) 0.0356(11) 0.0495(11) -0.0062(8) 0.0072(8) 0.0032(8) 
C18 0.0247(8) 0.0309(10) 0.0378(9) 0.0011(7) 0.0061(7) -0.0034(7) 
C19 0.0327(9) 0.0319(10) 0.0360(10) 0.0007(7) 0.0082(8) -0.0019(8) 
C20 0.0640(14) 0.0565(14) 0.0407(11) 0.0145(10) 0.0043(10) -0.0066(11) 
C21 0.0648(15) 0.0877(19) 0.0360(11) 0.0118(11) -0.0110(10) -0.0118(13) 
C22 0.0725(15) 0.0644(15) 0.0320(10) -0.0074(10) 0.0086(10) -0.0087(12) 
C23 0.0510(12) 0.0543(13) 0.0305(10) 0.0045(9) 0.0003(8) -0.0110(10) 
C24 0.0405(10) 0.0358(11) 0.0319(9) 0.0010(7) 0.0002(8) -0.0053(8) 
C25 0.0332(10) 0.0385(11) 0.0359(10) 0.0025(8) -0.0035(8) -0.0051(8) 
C26 0.0306(9) 0.0261(9) 0.0352(9) -0.0009(7) 0.0022(7) -0.0042(7) 
C27 0.0290(9) 0.0332(10) 0.0380(10) -0.0012(8) 0.0055(7) -0.0036(8) 
C28 0.0375(11) 0.0506(13) 0.0506(11) -0.0065(9) 0.0123(9) -0.0137(9) 
C29 0.0452(11) 0.0496(12) 0.0366(10) 0.0074(9) 0.0102(8) -0.0035(9) 
C30 0.0411(11) 0.0430(12) 0.0550(12) -0.0031(9) 0.0097(9) 0.0020(9) 

_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 
O1 C12 1.212(2) . ? 
O2 C19 1.205(2) . ? 
N1 N2 1.3894(18) . ? 
N1 C12 1.400(2) . ? 
N1 C5 1.407(2) . ? 
N2 C7 1.311(2) . ? 
N3 N4 1.3780(19) . ? 
N3 C24 1.393(2) . ? 
N3 C19 1.405(2) . ? 
N4 C26 1.309(2) . ? 
C1 C4 1.534(3) . ? 
C2 C4 1.525(3) . ? 
C3 C4 1.536(3) . ? 
C4 C5 1.521(2) . ? 
C5 C6 1.351(2) . ? 
C6 C7 1.417(2) . ? 
C7 C8 1.508(2) . ? 
C8 C11 1.517(3) . ? 
C8 C10 1.528(3) . ? 
C8 C9 1.535(3) . ? 
C12 C13 1.490(2) . ? 
C13 C14 1.381(2) . ? 
C13 C18 1.406(2) . ? 
C14 C15 1.382(3) . ? 
C15 C16 1.364(3) . ? 
C16 C17 1.384(3) . ? 
C17 C18 1.384(2) . ? 
C18 C19 1.503(2) . ? 
C20 C23 1.532(3) . ? 
C21 C23 1.539(3) . ? 
C22 C23 1.527(3) . ? 
C23 C24 1.523(2) . ? 
C24 C25 1.354(3) . ? 
C25 C26 1.417(2) . ? 
C26 C27 1.507(2) . ? 
C27 C30 1.526(3) . ? 
C27 C28 1.529(3) . ? 
C27 C29 1.530(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 
N2 N1 C12 117.58(13) . . ? 
N2 N1 C5 110.97(12) . . ? 
C12 N1 C5 131.42(14) . . ? 
C7 N2 N1 105.17(13) . . ? 
N4 N3 C24 111.19(13) . . ? 
N4 N3 C19 116.20(13) . . ? 
C24 N3 C19 132.48(14) . . ? 
C26 N4 N3 105.83(13) . . ? 
C5 C4 C2 111.48(15) . . ? 
C5 C4 C1 111.01(15) . . ? 
C2 C4 C1 111.54(16) . . ? 
C5 C4 C3 107.90(14) . . ? 
C2 C4 C3 107.68(16) . . ? 
C1 C4 C3 107.00(16) . . ? 
C6 C5 N1 104.87(14) . . ? 
C6 C5 C4 127.57(15) . . ? 
N1 C5 C4 127.56(14) . . ? 
C5 C6 C7 107.80(15) . . ? 
N2 C7 C6 111.18(14) . . ? 
N2 C7 C8 121.78(15) . . ? 
C6 C7 C8 127.03(15) . . ? 
C7 C8 C11 111.11(15) . . ? 
C7 C8 C10 108.77(15) . . ? 
C11 C8 C10 109.39(17) . . ? 
C7 C8 C9 107.56(16) . . ? 
C11 C8 C9 110.33(17) . . ? 
C10 C8 C9 109.63(18) . . ? 
O1 C12 N1 121.05(15) . . ? 
O1 C12 C13 120.07(15) . . ? 
N1 C12 C13 118.87(14) . . ? 
C14 C13 C18 118.69(16) . . ? 
C14 C13 C12 123.03(16) . . ? 
C18 C13 C12 117.48(15) . . ? 
C13 C14 C15 120.91(17) . . ? 
C16 C15 C14 120.26(18) . . ? 
C15 C16 C17 120.08(18) . . ? 
C18 C17 C16 120.34(17) . . ? 
C17 C18 C13 119.65(16) . . ? 
C17 C18 C19 116.08(15) . . ? 
C13 C18 C19 124.18(15) . . ? 
O2 C19 N3 122.71(16) . . ? 
O2 C19 C18 120.82(16) . . ? 
N3 C19 C18 116.36(14) . . ? 
C24 C23 C22 110.82(17) . . ? 
C24 C23 C20 111.04(16) . . ? 
C22 C23 C20 111.66(17) . . ? 
C24 C23 C21 107.72(16) . . ? 
C22 C23 C21 107.92(18) . . ? 
C20 C23 C21 107.48(18) . . ? 
C25 C24 N3 104.85(15) . . ? 
C25 C24 C23 127.85(17) . . ? 
N3 C24 C23 127.29(16) . . ? 
C24 C25 C26 107.78(16) . . ? 
N4 C26 C25 110.34(15) . . ? 
N4 C26 C27 120.74(15) . . ? 
C25 C26 C27 128.91(15) . . ? 
C26 C27 C30 109.09(15) . . ? 
C26 C27 C28 109.26(14) . . ? 
C30 C27 C28 109.53(15) . . ? 
C26 C27 C29 109.91(14) . . ? 
C30 C27 C29 109.28(15) . . ? 
C28 C27 C29 109.75(16) . . ? 

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 
C12 N1 N2 C7 -178.74(13) . . . . ? 
C5 N1 N2 C7 -0.70(17) . . . . ? 
C24 N3 N4 C26 0.68(18) . . . . ? 
C19 N3 N4 C26 177.08(15) . . . . ? 
N2 N1 C5 C6 1.12(18) . . . . ? 
C12 N1 C5 C6 178.81(16) . . . . ? 
N2 N1 C5 C4 -178.50(15) . . . . ? 
C12 N1 C5 C4 -0.8(3) . . . . ? 
C2 C4 C5 C6 120.73(19) . . . . ? 
C1 C4 C5 C6 -114.3(2) . . . . ? 
C3 C4 C5 C6 2.7(3) . . . . ? 
C2 C4 C5 N1 -59.7(2) . . . . ? 
C1 C4 C5 N1 65.3(2) . . . . ? 
C3 C4 C5 N1 -177.78(17) . . . . ? 
N1 C5 C6 C7 -1.06(18) . . . . ? 
C4 C5 C6 C7 178.56(16) . . . . ? 
N1 N2 C7 C6 0.01(18) . . . . ? 
N1 N2 C7 C8 -179.95(15) . . . . ? 
C5 C6 C7 N2 0.7(2) . . . . ? 
C5 C6 C7 C8 -179.34(16) . . . . ? 
N2 C7 C8 C11 -3.0(2) . . . . ? 
C6 C7 C8 C11 177.02(17) . . . . ? 
N2 C7 C8 C10 -123.51(18) . . . . ? 
C6 C7 C8 C10 56.5(2) . . . . ? 
N2 C7 C8 C9 117.82(19) . . . . ? 
C6 C7 C8 C9 -62.1(2) . . . . ? 
N2 N1 C12 O1 169.02(15) . . . . ? 
C5 N1 C12 O1 -8.6(3) . . . . ? 
N2 N1 C12 C13 -12.2(2) . . . . ? 
C5 N1 C12 C13 170.25(16) . . . . ? 
O1 C12 C13 C14 135.11(18) . . . . ? 
N1 C12 C13 C14 -43.7(2) . . . . ? 
O1 C12 C13 C18 -34.5(2) . . . . ? 
N1 C12 C13 C18 146.67(15) . . . . ? 
C18 C13 C14 C15 -2.5(3) . . . . ? 
C12 C13 C14 C15 -172.02(17) . . . . ? 
C13 C14 C15 C16 0.7(3) . . . . ? 
C14 C15 C16 C17 1.6(3) . . . . ? 
C15 C16 C17 C18 -2.0(3) . . . . ? 
C16 C17 C18 C13 0.1(3) . . . . ? 
C16 C17 C18 C19 176.80(17) . . . . ? 
C14 C13 C18 C17 2.1(2) . . . . ? 
C12 C13 C18 C17 172.21(15) . . . . ? 
C14 C13 C18 C19 -174.31(16) . . . . ? 
C12 C13 C18 C19 -4.2(2) . . . . ? 
N4 N3 C19 O2 166.98(16) . . . . ? 
C24 N3 C19 O2 -17.6(3) . . . . ? 
N4 N3 C19 C18 -9.3(2) . . . . ? 
C24 N3 C19 C18 166.13(18) . . . . ? 
C17 C18 C19 O2 -49.0(2) . . . . ? 
C13 C18 C19 O2 127.55(19) . . . . ? 
C17 C18 C19 N3 127.38(17) . . . . ? 
C13 C18 C19 N3 -56.1(2) . . . . ? 
N4 N3 C24 C25 -0.32(19) . . . . ? 
C19 N3 C24 C25 -175.94(18) . . . . ? 
N4 N3 C24 C23 178.94(17) . . . . ? 
C19 N3 C24 C23 3.3(3) . . . . ? 
C22 C23 C24 C25 -114.1(2) . . . . ? 
C20 C23 C24 C25 121.2(2) . . . . ? 
C21 C23 C24 C25 3.8(3) . . . . ? 
C22 C23 C24 N3 66.8(2) . . . . ? 
C20 C23 C24 N3 -57.9(3) . . . . ? 
C21 C23 C24 N3 -175.32(19) . . . . ? 
N3 C24 C25 C26 -0.1(2) . . . . ? 
C23 C24 C25 C26 -179.40(18) . . . . ? 
N3 N4 C26 C25 -0.76(19) . . . . ? 
N3 N4 C26 C27 179.93(15) . . . . ? 
C24 C25 C26 N4 0.6(2) . . . . ? 
C24 C25 C26 C27 179.83(17) . . . . ? 
N4 C26 C27 C30 103.56(19) . . . . ? 
C25 C26 C27 C30 -75.6(2) . . . . ? 
N4 C26 C27 C28 -136.73(17) . . . . ? 
C25 C26 C27 C28 44.1(2) . . . . ? 
N4 C26 C27 C29 -16.2(2) . . . . ? 
C25 C26 C27 C29 164.58(18) . . . . ? 

_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.228 
_refine_diff_density_min   -0.207 
_refine_diff_density_rms    0.036 

data_darl
_database_code_CSD                  178094

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H42 Cl4 N4 O2 Pd2'
_chemical_formula_weight         845.28

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   11.8754(10)
_cell_length_b                   12.1953(10)
_cell_length_c                   14.4906(13)
_cell_angle_alpha                86.828(2)
_cell_angle_beta                 72.340(2)
_cell_angle_gamma                63.363(2)
_cell_volume                     1779.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             852
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_T_max  0.7750
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      173(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  ?
_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            6754
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         26.38
_reflns_number_total             6754
_reflns_number_gt                5368
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0690P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6754
_refine_ls_number_parameters     391
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.0973
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.34253(3) 0.71960(3) 0.79626(2) 0.02346(11) Uani 1 1 d . . .
Pd2 Pd 0.16358(3) 0.94857(3) 0.69982(2) 0.02309(11) Uani 1 1 d . . .
Cl1 Cl 0.28101(12) 0.63962(11) 0.93672(9) 0.0388(3) Uani 1 1 d . . .
Cl2 Cl -0.05821(10) 1.07121(11) 0.74967(8) 0.0328(3) Uani 1 1 d . . .
Cl3 Cl 0.39476(10) 0.81013(10) 0.65119(7) 0.0274(2) Uani 1 1 d . . .
Cl4 Cl 0.13632(10) 0.78778(10) 0.77686(8) 0.0303(3) Uani 1 1 d . . .
O1 O 0.5751(3) 0.9035(3) 0.8032(3) 0.0428(9) Uani 1 1 d . . .
O2 O 0.0121(3) 1.3086(3) 0.8211(2) 0.0316(7) Uani 1 1 d . . .
N1 N 0.5250(3) 0.6587(3) 0.8113(2) 0.0246(8) Uani 1 1 d . . .
N2 N 0.5528(3) 0.7345(3) 0.8607(2) 0.0242(8) Uani 1 1 d . . .
N3 N 0.1928(3) 1.0895(3) 0.6329(2) 0.0235(8) Uani 1 1 d . . .
N4 N 0.1769(3) 1.1897(3) 0.6854(2) 0.0243(8) Uani 1 1 d . . .
C1 C 0.5431(5) 0.4594(5) 0.6911(4) 0.0465(13) Uani 1 1 d . . .
H1A H 0.4526 0.4892 0.7358 0.070 Uiso 1 1 calc R . .
H1B H 0.5675 0.3839 0.6528 0.070 Uiso 1 1 calc R . .
H1C H 0.5477 0.5225 0.6472 0.070 Uiso 1 1 calc R . .
C2 C 0.6253(5) 0.3426(5) 0.8241(4) 0.0477(13) Uani 1 1 d . . .
H2A H 0.5362 0.3806 0.8715 0.072 Uiso 1 1 calc R . .
H2B H 0.6915 0.3221 0.8576 0.072 Uiso 1 1 calc R . .
H2C H 0.6394 0.2672 0.7912 0.072 Uiso 1 1 calc R . .
C3 C 0.7810(4) 0.3734(4) 0.6760(3) 0.0372(11) Uani 1 1 d . . .
H3A H 0.7963 0.2991 0.6410 0.056 Uiso 1 1 calc R . .
H3B H 0.8455 0.3515 0.7114 0.056 Uiso 1 1 calc R . .
H3C H 0.7913 0.4323 0.6294 0.056 Uiso 1 1 calc R . .
C4 C 0.6387(4) 0.4326(4) 0.7490(3) 0.0314(10) Uani 1 1 d . . .
C5 C 0.6238(4) 0.5461(4) 0.8007(3) 0.0273(9) Uani 1 1 d . . .
C6 C 0.7125(4) 0.5470(4) 0.8460(3) 0.0287(10) Uani 1 1 d . . .
H6 H 0.7889 0.4769 0.8517 0.034 Uiso 1 1 calc R . .
C7 C 0.6711(4) 0.6644(4) 0.8802(3) 0.0243(9) Uani 1 1 d . . .
C8 C 0.7311(4) 0.7144(4) 0.9360(3) 0.0295(10) Uani 1 1 d . . .
C9 C 0.8227(5) 0.6047(4) 0.9793(4) 0.0423(12) Uani 1 1 d . . .
H9A H 0.8581 0.6345 1.0196 0.063 Uiso 1 1 calc R . .
H9B H 0.8962 0.5454 0.9264 0.063 Uiso 1 1 calc R . .
H9C H 0.7721 0.5644 1.0193 0.063 Uiso 1 1 calc R . .
C10 C 0.8161(5) 0.7703(5) 0.8705(4) 0.0399(12) Uani 1 1 d . . .
H10A H 0.7584 0.8490 0.8516 0.060 Uiso 1 1 calc R . .
H10B H 0.8765 0.7136 0.8122 0.060 Uiso 1 1 calc R . .
H10C H 0.8676 0.7842 0.9060 0.060 Uiso 1 1 calc R . .
C11 C 0.6222(5) 0.8081(5) 1.0194(3) 0.0411(12) Uani 1 1 d . . .
H11A H 0.5616 0.8774 0.9933 0.062 Uiso 1 1 calc R . .
H11B H 0.6619 0.8381 1.0557 0.062 Uiso 1 1 calc R . .
H11C H 0.5729 0.7690 1.0629 0.062 Uiso 1 1 calc R . .
C12 C 0.4979(4) 0.8630(4) 0.8435(3) 0.0262(9) Uani 1 1 d . . .
C13 C 0.3545(4) 0.9395(4) 0.8758(3) 0.0229(9) Uani 1 1 d . . .
C14 C 0.3013(4) 1.0325(4) 0.8183(3) 0.0219(9) Uani 1 1 d . . .
H14 H 0.3570 1.0407 0.7584 0.026 Uiso 1 1 calc R . .
C15 C 0.1664(4) 1.1129(4) 0.8491(3) 0.0227(9) Uani 1 1 d . . .
C16 C 0.0860(4) 1.1058(4) 0.9403(3) 0.0249(9) Uani 1 1 d . . .
H16 H -0.0050 1.1641 0.9629 0.030 Uiso 1 1 calc R . .
C17 C 0.1389(4) 1.0136(4) 0.9981(3) 0.0263(9) Uani 1 1 d . . .
H17 H 0.0842 1.0085 1.0597 0.032 Uiso 1 1 calc R . .
C18 C 0.2724(4) 0.9291(4) 0.9648(3) 0.0256(9) Uani 1 1 d . . .
H18 H 0.3081 0.8640 1.0027 0.031 Uiso 1 1 calc R . .
C19 C 0.1070(4) 1.2126(4) 0.7895(3) 0.0242(9) Uani 1 1 d . . .
C20 C 0.2474(6) 1.3812(6) 0.7424(4) 0.0544(15) Uani 1 1 d . . .
H20A H 0.2515 1.4573 0.7547 0.082 Uiso 1 1 calc R . .
H20B H 0.3348 1.3107 0.7325 0.082 Uiso 1 1 calc R . .
H20C H 0.1825 1.3711 0.7984 0.082 Uiso 1 1 calc R . .
C21 C 0.3058(6) 1.4105(5) 0.5657(4) 0.0528(15) Uani 1 1 d . . .
H21A H 0.2790 1.4193 0.5070 0.079 Uiso 1 1 calc R . .
H21B H 0.3940 1.3405 0.5538 0.079 Uiso 1 1 calc R . .
H21C H 0.3084 1.4860 0.5824 0.079 Uiso 1 1 calc R . .
C22 C 0.0673(5) 1.4966(5) 0.6641(4) 0.0534(15) Uani 1 1 d . . .
H22A H 0.0436 1.5001 0.6045 0.080 Uiso 1 1 calc R . .
H22B H 0.0687 1.5737 0.6777 0.080 Uiso 1 1 calc R . .
H22C H 0.0018 1.4852 0.7186 0.080 Uiso 1 1 calc R . .
C23 C 0.2051(5) 1.3882(4) 0.6507(3) 0.0372(11) Uani 1 1 d . . .
C24 C 0.2059(4) 1.2694(4) 0.6219(3) 0.0311(10) Uani 1 1 d . . .
C25 C 0.2393(5) 1.2172(4) 0.5306(3) 0.0357(11) Uani 1 1 d . . .
H25 H 0.2661 1.2496 0.4714 0.043 Uiso 1 1 calc R . .
C26 C 0.2273(4) 1.1073(4) 0.5392(3) 0.0312(10) Uani 1 1 d . . .
C27 C 0.2488(5) 1.0252(5) 0.4544(3) 0.0382(11) Uani 1 1 d . . .
C28 C 0.3997(5) 0.9585(5) 0.4015(4) 0.0500(14) Uani 1 1 d . . .
H28A H 0.4335 1.0195 0.3853 0.075 Uiso 1 1 calc R . .
H28B H 0.4168 0.9119 0.3416 0.075 Uiso 1 1 calc R . .
H28C H 0.4443 0.9019 0.4440 0.075 Uiso 1 1 calc R . .
C29 C 0.1966(6) 0.9301(5) 0.4806(4) 0.0493(14) Uani 1 1 d . . .
H29A H 0.2490 0.8682 0.5166 0.074 Uiso 1 1 calc R . .
H29B H 0.2038 0.8898 0.4209 0.074 Uiso 1 1 calc R . .
H29C H 0.1035 0.9711 0.5211 0.074 Uiso 1 1 calc R . .
C30 C 0.1757(6) 1.1094(5) 0.3861(4) 0.0490(14) Uani 1 1 d . . .
H30A H 0.0809 1.1549 0.4216 0.074 Uiso 1 1 calc R . .
H30B H 0.1883 1.0590 0.3301 0.074 Uiso 1 1 calc R . .
H30C H 0.2118 1.1679 0.3635 0.074 Uiso 1 1 calc R . .

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 0.02021(17) 0.02219(19) 0.02764(19) 0.00411(14) -0.00855(13) -0.00883(14)
Pd2 0.02127(18) 0.02304(19) 0.02354(18) 0.00274(13) -0.00835(13) -0.00806(14)
Cl1 0.0384(6) 0.0380(7) 0.0378(7) 0.0147(5) -0.0102(5) -0.0178(6)
Cl2 0.0227(5) 0.0330(6) 0.0366(6) 0.0063(5) -0.0113(4) -0.0067(5)
Cl3 0.0240(5) 0.0283(6) 0.0254(5) 0.0026(4) -0.0065(4) -0.0088(5)
Cl4 0.0229(5) 0.0282(6) 0.0433(7) 0.0082(5) -0.0133(5) -0.0132(5)
O1 0.0263(17) 0.038(2) 0.061(2) 0.0248(18) -0.0142(16) -0.0132(16)
O2 0.0270(16) 0.0262(17) 0.0310(17) 0.0020(13) -0.0092(13) -0.0029(14)
N1 0.0248(18) 0.0228(19) 0.0267(19) 0.0012(15) -0.0113(15) -0.0090(16)
N2 0.0220(18) 0.0229(19) 0.0268(19) 0.0029(15) -0.0091(14) -0.0084(16)
N3 0.0217(17) 0.0231(19) 0.0232(19) 0.0029(15) -0.0034(14) -0.0105(16)
N4 0.0269(19) 0.0235(19) 0.0229(19) 0.0045(15) -0.0096(15) -0.0107(16)
C1 0.039(3) 0.036(3) 0.068(4) -0.009(3) -0.027(3) -0.012(2)
C2 0.055(3) 0.030(3) 0.058(4) 0.001(2) -0.014(3) -0.022(3)
C3 0.032(3) 0.035(3) 0.042(3) -0.002(2) -0.014(2) -0.011(2)
C4 0.029(2) 0.027(2) 0.038(3) -0.001(2) -0.016(2) -0.009(2)
C5 0.025(2) 0.024(2) 0.030(2) 0.0047(18) -0.0115(18) -0.0070(19)
C6 0.024(2) 0.023(2) 0.035(3) 0.0029(19) -0.0126(19) -0.0054(19)
C7 0.025(2) 0.024(2) 0.025(2) 0.0072(18) -0.0110(17) -0.0100(19)
C8 0.032(2) 0.030(3) 0.032(2) 0.0038(19) -0.0168(19) -0.015(2)
C9 0.053(3) 0.033(3) 0.056(3) 0.011(2) -0.039(3) -0.019(3)
C10 0.041(3) 0.049(3) 0.040(3) 0.005(2) -0.016(2) -0.027(3)
C11 0.044(3) 0.039(3) 0.038(3) -0.006(2) -0.019(2) -0.012(2)
C12 0.031(2) 0.023(2) 0.026(2) 0.0053(18) -0.0135(18) -0.011(2)
C13 0.026(2) 0.019(2) 0.024(2) 0.0000(17) -0.0105(17) -0.0081(18)
C14 0.019(2) 0.022(2) 0.025(2) 0.0014(17) -0.0030(16) -0.0122(18)
C15 0.022(2) 0.020(2) 0.021(2) -0.0001(17) -0.0064(16) -0.0063(18)
C16 0.021(2) 0.021(2) 0.023(2) -0.0036(17) -0.0035(17) -0.0027(18)
C17 0.026(2) 0.030(2) 0.022(2) 0.0045(18) -0.0005(17) -0.017(2)
C18 0.033(2) 0.020(2) 0.026(2) 0.0045(17) -0.0141(18) -0.0110(19)
C19 0.022(2) 0.024(2) 0.026(2) 0.0019(18) -0.0087(17) -0.009(2)
C20 0.071(4) 0.060(4) 0.051(3) 0.004(3) -0.021(3) -0.045(3)
C21 0.063(4) 0.045(3) 0.050(3) 0.006(3) -0.007(3) -0.031(3)
C22 0.048(3) 0.035(3) 0.066(4) 0.004(3) -0.007(3) -0.015(3)
C23 0.046(3) 0.032(3) 0.035(3) 0.006(2) -0.010(2) -0.021(2)
C24 0.028(2) 0.032(3) 0.029(3) 0.010(2) -0.0083(19) -0.012(2)
C25 0.040(3) 0.037(3) 0.025(2) 0.007(2) -0.009(2) -0.014(2)
C26 0.032(2) 0.030(3) 0.024(2) 0.0011(19) -0.0095(19) -0.007(2)
C27 0.049(3) 0.039(3) 0.022(2) 0.002(2) -0.016(2) -0.013(2)
C28 0.047(3) 0.055(4) 0.034(3) -0.003(3) -0.010(2) -0.013(3)
C29 0.074(4) 0.054(4) 0.035(3) 0.006(2) -0.023(3) -0.038(3)
C30 0.063(4) 0.046(3) 0.035(3) 0.008(2) -0.025(3) -0.017(3)

_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 2.029(3) . ?
Pd1 Cl1 2.2683(11) . ?
Pd1 Cl4 2.3094(11) . ?
Pd1 Cl3 2.3640(10) . ?
Pd1 Pd2 3.2117(5) . ?
Pd2 N3 2.040(3) . ?
Pd2 Cl2 2.2647(11) . ?
Pd2 Cl4 2.3031(11) . ?
Pd2 Cl3 2.3844(11) . ?
O1 C12 1.214(5) . ?
O2 C19 1.189(5) . ?
N1 C5 1.325(5) . ?
N1 N2 1.403(5) . ?
N2 C7 1.386(5) . ?
N2 C12 1.443(5) . ?
N3 C26 1.330(5) . ?
N3 N4 1.384(5) . ?
N4 C24 1.385(5) . ?
N4 C19 1.457(5) . ?
C1 C4 1.522(6) . ?
C2 C4 1.527(7) . ?
C3 C4 1.550(6) . ?
C4 C5 1.524(6) . ?
C5 C6 1.404(6) . ?
C6 C7 1.356(6) . ?
C7 C8 1.525(6) . ?
C8 C11 1.523(6) . ?
C8 C10 1.532(6) . ?
C8 C9 1.544(6) . ?
C12 C13 1.459(6) . ?
C13 C14 1.398(6) . ?
C13 C18 1.399(5) . ?
C14 C15 1.390(6) . ?
C15 C16 1.401(5) . ?
C15 C19 1.486(6) . ?
C16 C17 1.393(6) . ?
C17 C18 1.390(6) . ?
C20 C23 1.542(7) . ?
C21 C23 1.544(6) . ?
C22 C23 1.536(7) . ?
C23 C24 1.525(7) . ?
C24 C25 1.364(6) . ?
C25 C26 1.405(7) . ?
C26 C27 1.515(6) . ?
C27 C29 1.525(7) . ?
C27 C28 1.545(7) . ?
C27 C30 1.547(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 Cl1 89.08(10) . . ?
N1 Pd1 Cl4 179.17(10) . . ?
Cl1 Pd1 Cl4 91.49(4) . . ?
N1 Pd1 Cl3 93.69(10) . . ?
Cl1 Pd1 Cl3 176.99(4) . . ?
Cl4 Pd1 Cl3 85.76(4) . . ?
N1 Pd1 Pd2 134.03(10) . . ?
Cl1 Pd1 Pd2 129.29(3) . . ?
Cl4 Pd1 Pd2 45.79(3) . . ?
Cl3 Pd1 Pd2 47.71(3) . . ?
N3 Pd2 Cl2 90.03(10) . . ?
N3 Pd2 Cl4 178.22(10) . . ?
Cl2 Pd2 Cl4 91.36(4) . . ?
N3 Pd2 Cl3 93.19(10) . . ?
Cl2 Pd2 Cl3 176.78(4) . . ?
Cl4 Pd2 Cl3 85.43(4) . . ?
N3 Pd2 Pd1 132.29(10) . . ?
Cl2 Pd2 Pd1 130.14(3) . . ?
Cl4 Pd2 Pd1 45.95(3) . . ?
Cl3 Pd2 Pd1 47.17(3) . . ?
Pd1 Cl3 Pd2 85.12(3) . . ?
Pd2 Cl4 Pd1 88.26(4) . . ?
C5 N1 N2 106.6(3) . . ?
C5 N1 Pd1 131.2(3) . . ?
N2 N1 Pd1 120.5(3) . . ?
C7 N2 N1 109.4(3) . . ?
C7 N2 C12 127.4(3) . . ?
N1 N2 C12 116.3(3) . . ?
C26 N3 N4 107.3(3) . . ?
C26 N3 Pd2 131.0(3) . . ?
N4 N3 Pd2 121.7(2) . . ?
N3 N4 C24 109.5(3) . . ?
N3 N4 C19 119.8(3) . . ?
C24 N4 C19 128.8(4) . . ?
C1 C4 C5 114.7(4) . . ?
C1 C4 C2 110.6(4) . . ?
C5 C4 C2 108.7(4) . . ?
C1 C4 C3 107.3(4) . . ?
C5 C4 C3 106.1(4) . . ?
C2 C4 C3 109.2(4) . . ?
N1 C5 C6 109.2(4) . . ?
N1 C5 C4 125.7(4) . . ?
C6 C5 C4 125.0(4) . . ?
C7 C6 C5 108.7(4) . . ?
C6 C7 N2 106.0(4) . . ?
C6 C7 C8 129.4(4) . . ?
N2 C7 C8 124.5(4) . . ?
C11 C8 C7 110.1(4) . . ?
C11 C8 C10 110.7(4) . . ?
C7 C8 C10 112.7(4) . . ?
C11 C8 C9 108.4(4) . . ?
C7 C8 C9 107.3(4) . . ?
C10 C8 C9 107.5(4) . . ?
O1 C12 N2 117.5(4) . . ?
O1 C12 C13 122.5(4) . . ?
N2 C12 C13 119.9(3) . . ?
C14 C13 C18 119.9(4) . . ?
C14 C13 C12 117.4(4) . . ?
C18 C13 C12 122.4(4) . . ?
C15 C14 C13 119.7(4) . . ?
C14 C15 C16 120.1(4) . . ?
C14 C15 C19 120.9(4) . . ?
C16 C15 C19 118.9(4) . . ?
C17 C16 C15 120.2(4) . . ?
C18 C17 C16 119.5(4) . . ?
C17 C18 C13 120.4(4) . . ?
O2 C19 N4 119.4(4) . . ?
O2 C19 C15 124.9(4) . . ?
N4 C19 C15 115.6(3) . . ?
C24 C23 C22 109.5(4) . . ?
C24 C23 C20 113.0(4) . . ?
C22 C23 C20 111.0(5) . . ?
C24 C23 C21 107.5(4) . . ?
C22 C23 C21 108.0(4) . . ?
C20 C23 C21 107.7(4) . . ?
C25 C24 N4 106.0(4) . . ?
C25 C24 C23 128.2(4) . . ?
N4 C24 C23 125.8(4) . . ?
C24 C25 C26 108.3(4) . . ?
N3 C26 C25 108.8(4) . . ?
N3 C26 C27 126.5(4) . . ?
C25 C26 C27 124.7(4) . . ?
C26 C27 C29 115.7(4) . . ?
C26 C27 C28 107.0(4) . . ?
C29 C27 C28 109.4(4) . . ?
C26 C27 C30 107.5(4) . . ?
C29 C27 C30 107.1(4) . . ?
C28 C27 C30 110.2(4) . . ?

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
N1 Pd1 Pd2 N3 -1.54(19) . . . . ?
Cl1 Pd1 Pd2 N3 138.11(14) . . . . ?
Cl4 Pd1 Pd2 N3 179.59(14) . . . . ?
Cl3 Pd1 Pd2 N3 -42.20(14) . . . . ?
N1 Pd1 Pd2 Cl2 -141.70(14) . . . . ?
Cl1 Pd1 Pd2 Cl2 -2.05(6) . . . . ?
Cl4 Pd1 Pd2 Cl2 39.43(6) . . . . ?
Cl3 Pd1 Pd2 Cl2 177.64(6) . . . . ?
N1 Pd1 Pd2 Cl4 178.87(14) . . . . ?
Cl1 Pd1 Pd2 Cl4 -41.48(6) . . . . ?
Cl3 Pd1 Pd2 Cl4 138.20(6) . . . . ?
N1 Pd1 Pd2 Cl3 40.67(14) . . . . ?
Cl1 Pd1 Pd2 Cl3 -179.69(6) . . . . ?
Cl4 Pd1 Pd2 Cl3 -138.20(6) . . . . ?
N1 Pd1 Cl3 Pd2 -152.00(10) . . . . ?
Cl1 Pd1 Cl3 Pd2 4.6(9) . . . . ?
Cl4 Pd1 Cl3 Pd2 28.62(4) . . . . ?
N3 Pd2 Cl3 Pd1 150.15(10) . . . . ?
Cl2 Pd2 Cl3 Pd1 -34.1(7) . . . . ?
Cl4 Pd2 Cl3 Pd1 -28.72(4) . . . . ?
N3 Pd2 Cl4 Pd1 -10(3) . . . . ?
Cl2 Pd2 Cl4 Pd1 -150.94(4) . . . . ?
Cl3 Pd2 Cl4 Pd1 29.36(4) . . . . ?
N1 Pd1 Cl4 Pd2 -78(7) . . . . ?
Cl1 Pd1 Cl4 Pd2 149.15(5) . . . . ?
Cl3 Pd1 Cl4 Pd2 -29.63(4) . . . . ?
Cl1 Pd1 N1 C5 72.3(4) . . . . ?
Cl4 Pd1 N1 C5 -61(7) . . . . ?
Cl3 Pd1 N1 C5 -108.9(4) . . . . ?
Pd2 Pd1 N1 C5 -137.8(3) . . . . ?
Cl1 Pd1 N1 N2 -91.0(3) . . . . ?
Cl4 Pd1 N1 N2 136(7) . . . . ?
Cl3 Pd1 N1 N2 87.8(3) . . . . ?
Pd2 Pd1 N1 N2 58.9(3) . . . . ?
C5 N1 N2 C7 -0.3(4) . . . . ?
Pd1 N1 N2 C7 166.7(2) . . . . ?
C5 N1 N2 C12 153.1(3) . . . . ?
Pd1 N1 N2 C12 -40.0(4) . . . . ?
Cl2 Pd2 N3 C26 -106.5(4) . . . . ?
Cl4 Pd2 N3 C26 112(3) . . . . ?
Cl3 Pd2 N3 C26 73.3(4) . . . . ?
Pd1 Pd2 N3 C26 102.9(4) . . . . ?
Cl2 Pd2 N3 N4 73.2(3) . . . . ?
Cl4 Pd2 N3 N4 -68(3) . . . . ?
Cl3 Pd2 N3 N4 -107.0(3) . . . . ?
Pd1 Pd2 N3 N4 -77.5(3) . . . . ?
C26 N3 N4 C24 -1.7(5) . . . . ?
Pd2 N3 N4 C24 178.6(3) . . . . ?
C26 N3 N4 C19 164.2(4) . . . . ?
Pd2 N3 N4 C19 -15.5(5) . . . . ?
N2 N1 C5 C6 2.3(4) . . . . ?
Pd1 N1 C5 C6 -162.7(3) . . . . ?
N2 N1 C5 C4 -178.5(4) . . . . ?
Pd1 N1 C5 C4 16.5(6) . . . . ?
C1 C4 C5 N1 11.0(6) . . . . ?
C2 C4 C5 N1 -113.4(5) . . . . ?
C3 C4 C5 N1 129.3(4) . . . . ?
C1 C4 C5 C6 -169.9(4) . . . . ?
C2 C4 C5 C6 65.7(6) . . . . ?
C3 C4 C5 C6 -51.6(6) . . . . ?
N1 C5 C6 C7 -3.6(5) . . . . ?
C4 C5 C6 C7 177.2(4) . . . . ?
C5 C6 C7 N2 3.3(5) . . . . ?
C5 C6 C7 C8 179.0(4) . . . . ?
N1 N2 C7 C6 -1.9(4) . . . . ?
C12 N2 C7 C6 -151.5(4) . . . . ?
N1 N2 C7 C8 -177.9(4) . . . . ?
C12 N2 C7 C8 32.5(6) . . . . ?
C6 C7 C8 C11 -136.8(5) . . . . ?
N2 C7 C8 C11 38.3(6) . . . . ?
C6 C7 C8 C10 99.1(5) . . . . ?
N2 C7 C8 C10 -85.8(5) . . . . ?
C6 C7 C8 C9 -19.0(6) . . . . ?
N2 C7 C8 C9 156.1(4) . . . . ?
C7 N2 C12 O1 32.7(6) . . . . ?
N1 N2 C12 O1 -115.1(4) . . . . ?
C7 N2 C12 C13 -146.2(4) . . . . ?
N1 N2 C12 C13 66.0(5) . . . . ?
O1 C12 C13 C14 35.4(6) . . . . ?
N2 C12 C13 C14 -145.8(4) . . . . ?
O1 C12 C13 C18 -139.3(5) . . . . ?
N2 C12 C13 C18 39.5(6) . . . . ?
C18 C13 C14 C15 -1.1(6) . . . . ?
C12 C13 C14 C15 -175.9(4) . . . . ?
C13 C14 C15 C16 4.2(6) . . . . ?
C13 C14 C15 C19 180.0(4) . . . . ?
C14 C15 C16 C17 -3.9(6) . . . . ?
C19 C15 C16 C17 -179.7(4) . . . . ?
C15 C16 C17 C18 0.4(6) . . . . ?
C16 C17 C18 C13 2.7(6) . . . . ?
C14 C13 C18 C17 -2.3(6) . . . . ?
C12 C13 C18 C17 172.2(4) . . . . ?
N3 N4 C19 O2 -122.5(4) . . . . ?
C24 N4 C19 O2 40.3(6) . . . . ?
N3 N4 C19 C15 60.3(5) . . . . ?
C24 N4 C19 C15 -136.8(4) . . . . ?
C14 C15 C19 O2 -150.7(4) . . . . ?
C16 C15 C19 O2 25.1(6) . . . . ?
C14 C15 C19 N4 26.3(6) . . . . ?
C16 C15 C19 N4 -157.9(4) . . . . ?
N3 N4 C24 C25 0.1(5) . . . . ?
C19 N4 C24 C25 -164.1(4) . . . . ?
N3 N4 C24 C23 -177.6(4) . . . . ?
C19 N4 C24 C23 18.1(7) . . . . ?
C22 C23 C24 C25 91.4(6) . . . . ?
C20 C23 C24 C25 -144.3(5) . . . . ?
C21 C23 C24 C25 -25.7(7) . . . . ?
C22 C23 C24 N4 -91.4(5) . . . . ?
C20 C23 C24 N4 32.9(7) . . . . ?
C21 C23 C24 N4 151.6(5) . . . . ?
N4 C24 C25 C26 1.4(5) . . . . ?
C23 C24 C25 C26 179.1(5) . . . . ?
N4 N3 C26 C25 2.5(5) . . . . ?
Pd2 N3 C26 C25 -177.8(3) . . . . ?
N4 N3 C26 C27 -176.7(4) . . . . ?
Pd2 N3 C26 C27 3.1(7) . . . . ?
C24 C25 C26 N3 -2.5(5) . . . . ?
C24 C25 C26 C27 176.7(4) . . . . ?
N3 C26 C27 C29 14.3(7) . . . . ?
C25 C26 C27 C29 -164.7(5) . . . . ?
N3 C26 C27 C28 -107.8(5) . . . . ?
C25 C26 C27 C28 73.1(6) . . . . ?
N3 C26 C27 C30 133.8(5) . . . . ?
C25 C26 C27 C30 -45.2(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.928
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.928
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.143


data_darp
_database_code_CSD                  178095

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H20 Cl6 N4 O2 Pd2'
_chemical_formula_weight         761.89

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                   11.4285(11)
_cell_length_b                   11.5080(11)
_cell_length_c                   11.9381(12)
_cell_angle_alpha                100.520(2)
_cell_angle_beta                 118.329(2)
_cell_angle_gamma                98.458(2)
_cell_volume                     1308.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    2.012
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_absorpt_correction_T_min  0.6332
_exptl_absorpt_correction_T_max  0.8888
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_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            4790
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4790
_reflns_number_gt                3727
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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^)+(0.0781P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4790
_refine_ls_number_parameters     297
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.968
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.91585(4) 0.54605(3) 0.64287(4) 0.03764(13) Uani 1 1 d . . .
Pd2 Pd 0.76653(4) 0.65501(3) 0.39837(4) 0.03587(13) Uani 1 1 d . . .
Cl1 Cl 0.82737(16) 0.38197(13) 0.68472(16) 0.0624(4) Uani 1 1 d . . .
Cl2 Cl 0.54772(14) 0.59083(12) 0.22018(14) 0.0546(4) Uani 1 1 d . . .
Cl3 Cl 0.99451(12) 0.70777(11) 0.57932(13) 0.0436(3) Uani 1 1 d . . .
Cl4 Cl 0.76399(13) 0.45952(11) 0.41753(13) 0.0461(3) Uani 1 1 d . . .
Cl5 Cl 0.6716(5) 0.8427(6) 0.9761(5) 0.1024(10) Uiso 0.601(7) 1 d PD A -1
Cl6 Cl 0.3848(5) 0.8087(6) 0.9137(7) 0.1290(14) Uiso 0.601(7) 1 d PD A -1
Cl5A Cl 0.6349(8) 0.7889(8) 0.9687(7) 0.1024(10) Uiso 0.399(7) 1 d PD A -2
Cl6A Cl 0.4038(8) 0.8603(10) 0.9629(10) 0.1290(14) Uiso 0.399(7) 1 d PD A -2
O1 O 0.4745(4) 0.8626(4) 0.3888(4) 0.0591(10) Uani 1 1 d . . .
O2 O 1.0391(4) 0.9296(3) 0.8854(4) 0.0633(11) Uani 1 1 d . . .
N3 N 0.7727(4) 0.8298(4) 0.3891(4) 0.0410(10) Uani 1 1 d . . .
N4 N 0.6791(4) 0.8896(4) 0.3947(4) 0.0415(10) Uani 1 1 d . . .
N2 N 1.0520(4) 0.7397(4) 0.9110(4) 0.0444(10) Uani 1 1 d . . .
N1 N 1.0463(4) 0.6273(4) 0.8408(4) 0.0413(10) Uani 1 1 d . . .
C1 C 1.1771(7) 0.4720(6) 0.8926(7) 0.0699(19) Uani 1 1 d . . .
H1A H 1.1143 0.4041 0.8891 0.105 Uiso 1 1 calc R . .
H1B H 1.2700 0.4758 0.9572 0.105 Uiso 1 1 calc R . .
H1C H 1.1679 0.4612 0.8068 0.105 Uiso 1 1 calc R . .
C2 C 1.1446(6) 0.5882(5) 0.9307(6) 0.0496(13) Uani 1 1 d . . .
C3 C 1.2092(6) 0.6734(5) 1.0548(5) 0.0524(14) Uani 1 1 d . . .
H3 H 1.2797 0.6664 1.1333 0.063 Uiso 1 1 calc R . .
C4 C 1.1526(6) 0.7679(5) 1.0420(5) 0.0490(13) Uani 1 1 d . . .
C5 C 1.1793(7) 0.8814(6) 1.1427(6) 0.075(2) Uani 1 1 d . . .
H5A H 1.2337 0.8734 1.2302 0.113 Uiso 1 1 calc R . .
H5B H 1.0931 0.8938 1.1300 0.113 Uiso 1 1 calc R . .
H5C H 1.2283 0.9504 1.1330 0.113 Uiso 1 1 calc R . .
C6 C 0.9774(6) 0.8217(5) 0.8478(5) 0.0440(12) Uani 1 1 d . . .
C7 C 0.8302(5) 0.7709(4) 0.7446(5) 0.0385(11) Uani 1 1 d . . .
C8 C 0.7793(5) 0.8282(4) 0.6446(5) 0.0367(11) Uani 1 1 d . . .
H8 H 0.8380 0.8941 0.6454 0.044 Uiso 1 1 calc R . .
C9 C 0.6439(5) 0.7883(5) 0.5454(5) 0.0382(11) Uani 1 1 d . . .
C10 C 0.5534(5) 0.6934(5) 0.5488(5) 0.0442(12) Uani 1 1 d . . .
H10 H 0.4599 0.6689 0.4844 0.053 Uiso 1 1 calc R . .
C11 C 0.6047(5) 0.6373(5) 0.6483(5) 0.0461(13) Uani 1 1 d . . .
H11 H 0.5458 0.5737 0.6502 0.055 Uiso 1 1 calc R . .
C12 C 0.7436(6) 0.6754(5) 0.7454(5) 0.0451(12) Uani 1 1 d . . .
H12 H 0.7782 0.6362 0.8112 0.054 Uiso 1 1 calc R . .
C13 C 0.5862(6) 0.8460(4) 0.4360(5) 0.0442(12) Uani 1 1 d . . .
C14 C 0.6076(8) 1.0830(6) 0.3551(7) 0.0725(19) Uani 1 1 d . . .
H14A H 0.6507 1.1591 0.3512 0.109 Uiso 1 1 calc R . .
H14B H 0.6056 1.0965 0.4359 0.109 Uiso 1 1 calc R . .
H14C H 0.5150 1.0517 0.2802 0.109 Uiso 1 1 calc R . .
C15 C 0.6872(6) 0.9929(5) 0.3521(5) 0.0501(14) Uani 1 1 d . . .
C16 C 0.7852(6) 0.9945(5) 0.3191(6) 0.0554(15) Uani 1 1 d . . .
H2 H 0.8141 1.0537 0.2873 0.066 Uiso 1 1 calc R . .
C17 C 0.8356(6) 0.8930(5) 0.3406(5) 0.0468(13) Uani 1 1 d . . .
C18 C 0.9444(6) 0.8548(6) 0.3191(6) 0.0581(15) Uani 1 1 d . . .
H18A H 0.9733 0.7935 0.3630 0.087 Uiso 0.50 1 calc PR . .
H18B H 1.0220 0.9247 0.3549 0.087 Uiso 0.50 1 calc PR . .
H18C H 0.9078 0.8216 0.2256 0.087 Uiso 0.50 1 calc PR . .
H18D H 0.9621 0.8997 0.2660 0.087 Uiso 0.50 1 calc PR . .
H18E H 0.9134 0.7685 0.2741 0.087 Uiso 0.50 1 calc PR . .
H18F H 1.0276 0.8716 0.4034 0.087 Uiso 0.50 1 calc PR . .
C19 C 0.5226(9) 0.7490(8) 0.947(2) 0.110(4) Uiso 0.601(7) 1 d PD A -1
H19A H 0.4930 0.6782 0.8718 0.132 Uiso 0.601(7) 1 calc PR A -1
H19B H 0.5449 0.7194 1.0234 0.132 Uiso 0.601(7) 1 calc PR A -1
C19A C 0.4840(17) 0.7454(11) 0.967(3) 0.110(4) Uiso 0.399(7) 1 d PD A -2
H19C H 0.4219 0.6755 0.8897 0.132 Uiso 0.399(7) 1 calc PR A -2
H19D H 0.5034 0.7196 1.0455 0.132 Uiso 0.399(7) 1 calc PR A -2

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 0.0356(2) 0.0352(2) 0.0384(2) 0.01291(16) 0.01529(17) 0.01047(16)
Pd2 0.0359(2) 0.0343(2) 0.0372(2) 0.01264(16) 0.01768(18) 0.01046(15)
Cl1 0.0562(9) 0.0560(8) 0.0701(10) 0.0335(8) 0.0258(8) 0.0071(7)
Cl2 0.0457(8) 0.0501(8) 0.0470(8) 0.0158(6) 0.0084(6) 0.0099(6)
Cl3 0.0363(7) 0.0422(7) 0.0502(7) 0.0169(6) 0.0198(6) 0.0098(5)
Cl4 0.0488(7) 0.0332(6) 0.0433(7) 0.0088(5) 0.0145(6) 0.0122(5)
O1 0.042(2) 0.074(3) 0.065(3) 0.036(2) 0.022(2) 0.028(2)
O2 0.050(2) 0.044(2) 0.063(3) 0.0122(19) 0.007(2) 0.0078(18)
N3 0.042(2) 0.038(2) 0.040(2) 0.0135(18) 0.019(2) 0.0088(18)
N4 0.048(3) 0.036(2) 0.041(2) 0.0173(19) 0.019(2) 0.0146(18)
N2 0.037(2) 0.051(3) 0.039(2) 0.017(2) 0.0113(19) 0.0190(19)
N1 0.035(2) 0.044(2) 0.039(2) 0.0141(19) 0.0123(19) 0.0171(18)
C1 0.064(4) 0.064(4) 0.063(4) 0.016(3) 0.015(3) 0.036(3)
C2 0.046(3) 0.058(3) 0.048(3) 0.021(3) 0.022(3) 0.022(3)
C3 0.042(3) 0.072(4) 0.039(3) 0.023(3) 0.013(2) 0.024(3)
C4 0.041(3) 0.066(4) 0.035(3) 0.015(3) 0.013(2) 0.023(3)
C5 0.067(4) 0.084(5) 0.042(3) -0.003(3) 0.005(3) 0.037(4)
C6 0.049(3) 0.046(3) 0.035(3) 0.013(2) 0.017(2) 0.018(2)
C7 0.031(2) 0.040(3) 0.041(3) 0.008(2) 0.017(2) 0.012(2)
C8 0.034(3) 0.036(2) 0.043(3) 0.012(2) 0.021(2) 0.012(2)
C9 0.043(3) 0.045(3) 0.032(2) 0.016(2) 0.019(2) 0.023(2)
C10 0.031(3) 0.049(3) 0.045(3) 0.015(2) 0.014(2) 0.009(2)
C11 0.038(3) 0.050(3) 0.058(3) 0.026(3) 0.026(3) 0.016(2)
C12 0.056(3) 0.050(3) 0.048(3) 0.026(3) 0.033(3) 0.028(3)
C13 0.046(3) 0.037(3) 0.045(3) 0.010(2) 0.020(3) 0.015(2)
C14 0.095(5) 0.053(4) 0.083(5) 0.036(4) 0.046(4) 0.039(4)
C15 0.062(4) 0.038(3) 0.043(3) 0.013(2) 0.022(3) 0.012(2)
C16 0.072(4) 0.041(3) 0.052(3) 0.018(3) 0.032(3) 0.005(3)
C17 0.054(3) 0.039(3) 0.039(3) 0.010(2) 0.021(3) 0.003(2)
C18 0.061(4) 0.060(4) 0.062(4) 0.022(3) 0.039(3) 0.009(3)

_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 2.029(4) . ?
Pd1 Cl1 2.2583(14) . ?
Pd1 Cl4 2.3072(13) . ?
Pd1 Cl3 2.3490(13) . ?
Pd1 Pd2 3.2004(6) . ?
Pd2 N3 2.027(4) . ?
Pd2 Cl2 2.2712(14) . ?
Pd2 Cl4 2.2998(13) . ?
Pd2 Cl3 2.3532(13) . ?
Cl5 C19 1.714(2) . ?
Cl6 C19 1.713(2) . ?
Cl5A C19A 1.713(2) . ?
Cl6A C19A 1.711(2) . ?
O1 C13 1.189(6) . ?
O2 C6 1.216(6) . ?
N3 C17 1.333(7) . ?
N3 N4 1.374(6) . ?
N4 C15 1.383(6) . ?
N4 C13 1.432(7) . ?
N2 C4 1.368(7) . ?
N2 N1 1.381(6) . ?
N2 C6 1.439(6) . ?
N1 C2 1.340(7) . ?
C1 C2 1.489(8) . ?
C2 C3 1.386(8) . ?
C3 C4 1.341(8) . ?
C4 C5 1.486(8) . ?
C6 C7 1.473(7) . ?
C7 C12 1.370(7) . ?
C7 C8 1.393(7) . ?
C8 C9 1.364(7) . ?
C9 C10 1.410(7) . ?
C9 C13 1.487(7) . ?
C10 C11 1.379(7) . ?
C11 C12 1.386(7) . ?
C14 C15 1.483(9) . ?
C15 C16 1.351(8) . ?
C16 C17 1.388(8) . ?
C17 C18 1.493(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
N1 Pd1 Cl1 90.37(12) . . ?
N1 Pd1 Cl4 177.94(12) . . ?
Cl1 Pd1 Cl4 90.60(5) . . ?
N1 Pd1 Cl3 94.68(12) . . ?
Cl1 Pd1 Cl3 174.95(5) . . ?
Cl4 Pd1 Cl3 84.35(5) . . ?
N1 Pd1 Pd2 132.32(11) . . ?
Cl1 Pd1 Pd2 128.55(4) . . ?
Cl4 Pd1 Pd2 45.90(3) . . ?
Cl3 Pd1 Pd2 47.16(3) . . ?
N3 Pd2 Cl2 89.66(12) . . ?
N3 Pd2 Cl4 177.82(12) . . ?
Cl2 Pd2 Cl4 92.01(5) . . ?
N3 Pd2 Cl3 93.95(12) . . ?
Cl2 Pd2 Cl3 176.08(5) . . ?
Cl4 Pd2 Cl3 84.42(4) . . ?
N3 Pd2 Pd1 131.76(12) . . ?
Cl2 Pd2 Pd1 130.63(4) . . ?
Cl4 Pd2 Pd1 46.09(3) . . ?
Cl3 Pd2 Pd1 47.05(3) . . ?
Pd1 Cl3 Pd2 85.78(4) . . ?
Pd2 Cl4 Pd1 88.00(4) . . ?
C17 N3 N4 106.4(4) . . ?
C17 N3 Pd2 127.4(4) . . ?
N4 N3 Pd2 123.6(3) . . ?
N3 N4 C15 110.1(4) . . ?
N3 N4 C13 123.3(4) . . ?
C15 N4 C13 126.7(5) . . ?
C4 N2 N1 110.4(4) . . ?
C4 N2 C6 125.9(5) . . ?
N1 N2 C6 123.0(4) . . ?
C2 N1 N2 105.1(4) . . ?
C2 N1 Pd1 129.4(4) . . ?
N2 N1 Pd1 125.5(3) . . ?
N1 C2 C3 109.8(5) . . ?
N1 C2 C1 121.9(5) . . ?
C3 C2 C1 128.3(5) . . ?
C4 C3 C2 108.2(5) . . ?
C3 C4 N2 106.5(5) . . ?
C3 C4 C5 130.9(5) . . ?
N2 C4 C5 122.5(5) . . ?
O2 C6 N2 117.8(5) . . ?
O2 C6 C7 123.9(5) . . ?
N2 C6 C7 118.3(4) . . ?
C12 C7 C8 120.1(5) . . ?
C12 C7 C6 123.7(5) . . ?
C8 C7 C6 116.1(4) . . ?
C9 C8 C7 120.3(4) . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 C13 121.9(5) . . ?
C10 C9 C13 118.3(5) . . ?
C11 C10 C9 119.4(5) . . ?
C10 C11 C12 120.2(5) . . ?
C7 C12 C11 120.1(5) . . ?
O1 C13 N4 120.5(5) . . ?
O1 C13 C9 124.2(5) . . ?
N4 C13 C9 115.2(5) . . ?
C16 C15 N4 105.6(5) . . ?
C16 C15 C14 130.3(5) . . ?
N4 C15 C14 123.9(6) . . ?
C15 C16 C17 108.6(5) . . ?
N3 C17 C16 109.2(5) . . ?
N3 C17 C18 122.0(5) . . ?
C16 C17 C18 128.8(5) . . ?
Cl6 C19 Cl5 118.2(4) . . ?
Cl6A C19A Cl5A 112.9(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Pd1 Pd2 N3 0.9(2) . . . . ?
Cl1 Pd1 Pd2 N3 138.37(18) . . . . ?
Cl4 Pd1 Pd2 N3 179.47(17) . . . . ?
Cl3 Pd1 Pd2 N3 -45.16(17) . . . . ?
N1 Pd1 Pd2 Cl2 -138.17(17) . . . . ?
Cl1 Pd1 Pd2 Cl2 -0.71(9) . . . . ?
Cl4 Pd1 Pd2 Cl2 40.39(8) . . . . ?
Cl3 Pd1 Pd2 Cl2 175.76(7) . . . . ?
N1 Pd1 Pd2 Cl4 -178.57(17) . . . . ?
Cl1 Pd1 Pd2 Cl4 -41.11(8) . . . . ?
Cl3 Pd1 Pd2 Cl4 135.36(7) . . . . ?
N1 Pd1 Pd2 Cl3 46.07(17) . . . . ?
Cl1 Pd1 Pd2 Cl3 -176.47(8) . . . . ?
Cl4 Pd1 Pd2 Cl3 -135.36(7) . . . . ?
N1 Pd1 Cl3 Pd2 -147.71(12) . . . . ?
Cl1 Pd1 Cl3 Pd2 33.2(6) . . . . ?
Cl4 Pd1 Cl3 Pd2 30.47(5) . . . . ?
N3 Pd2 Cl3 Pd1 147.98(13) . . . . ?
Cl2 Pd2 Cl3 Pd1 -55.2(8) . . . . ?
Cl4 Pd2 Cl3 Pd1 -30.57(5) . . . . ?
N3 Pd2 Cl4 Pd1 -10(3) . . . . ?
Cl2 Pd2 Cl4 Pd1 -150.52(6) . . . . ?
Cl3 Pd2 Cl4 Pd1 31.11(5) . . . . ?
N1 Pd1 Cl4 Pd2 31(3) . . . . ?
Cl1 Pd1 Cl4 Pd2 149.06(6) . . . . ?
Cl3 Pd1 Cl4 Pd2 -31.18(5) . . . . ?
Cl2 Pd2 N3 C17 -102.6(4) . . . . ?
Cl4 Pd2 N3 C17 117(3) . . . . ?
Cl3 Pd2 N3 C17 75.8(4) . . . . ?
Pd1 Pd2 N3 C17 107.2(4) . . . . ?
Cl2 Pd2 N3 N4 56.7(4) . . . . ?
Cl4 Pd2 N3 N4 -83(3) . . . . ?
Cl3 Pd2 N3 N4 -124.8(4) . . . . ?
Pd1 Pd2 N3 N4 -93.5(4) . . . . ?
C17 N3 N4 C15 -1.5(5) . . . . ?
Pd2 N3 N4 C15 -164.5(3) . . . . ?
C17 N3 N4 C13 176.9(5) . . . . ?
Pd2 N3 N4 C13 13.9(6) . . . . ?
C4 N2 N1 C2 -0.2(6) . . . . ?
C6 N2 N1 C2 170.3(5) . . . . ?
C4 N2 N1 Pd1 -179.2(4) . . . . ?
C6 N2 N1 Pd1 -8.7(7) . . . . ?
Cl1 Pd1 N1 C2 60.1(5) . . . . ?
Cl4 Pd1 N1 C2 178(57) . . . . ?
Cl3 Pd1 N1 C2 -119.8(5) . . . . ?
Pd2 Pd1 N1 C2 -151.8(4) . . . . ?
Cl1 Pd1 N1 N2 -121.1(4) . . . . ?
Cl4 Pd1 N1 N2 -3(4) . . . . ?
Cl3 Pd1 N1 N2 59.0(4) . . . . ?
Pd2 Pd1 N1 N2 27.0(5) . . . . ?
N2 N1 C2 C3 0.8(6) . . . . ?
Pd1 N1 C2 C3 179.8(4) . . . . ?
N2 N1 C2 C1 -176.5(5) . . . . ?
Pd1 N1 C2 C1 2.5(8) . . . . ?
N1 C2 C3 C4 -1.2(7) . . . . ?
C1 C2 C3 C4 175.9(6) . . . . ?
C2 C3 C4 N2 1.0(7) . . . . ?
C2 C3 C4 C5 177.9(6) . . . . ?
N1 N2 C4 C3 -0.5(6) . . . . ?
C6 N2 C4 C3 -170.7(5) . . . . ?
N1 N2 C4 C5 -177.7(5) . . . . ?
C6 N2 C4 C5 12.1(9) . . . . ?
C4 N2 C6 O2 34.9(8) . . . . ?
N1 N2 C6 O2 -134.1(5) . . . . ?
C4 N2 C6 C7 -143.1(5) . . . . ?
N1 N2 C6 C7 47.9(7) . . . . ?
O2 C6 C7 C12 -145.7(6) . . . . ?
N2 C6 C7 C12 32.2(7) . . . . ?
O2 C6 C7 C8 32.4(8) . . . . ?
N2 C6 C7 C8 -149.7(5) . . . . ?
C12 C7 C8 C9 -1.3(7) . . . . ?
C6 C7 C8 C9 -179.4(5) . . . . ?
C7 C8 C9 C10 3.8(7) . . . . ?
C7 C8 C9 C13 -179.2(5) . . . . ?
C8 C9 C10 C11 -3.7(8) . . . . ?
C13 C9 C10 C11 179.1(5) . . . . ?
C9 C10 C11 C12 1.1(8) . . . . ?
C8 C7 C12 C11 -1.4(8) . . . . ?
C6 C7 C12 C11 176.6(5) . . . . ?
C10 C11 C12 C7 1.4(8) . . . . ?
N3 N4 C13 O1 -147.0(5) . . . . ?
C15 N4 C13 O1 31.2(8) . . . . ?
N3 N4 C13 C9 37.0(6) . . . . ?
C15 N4 C13 C9 -144.8(5) . . . . ?
C8 C9 C13 O1 -141.7(6) . . . . ?
C10 C9 C13 O1 35.3(8) . . . . ?
C8 C9 C13 N4 34.2(7) . . . . ?
C10 C9 C13 N4 -148.8(5) . . . . ?
N3 N4 C15 C16 0.7(6) . . . . ?
C13 N4 C15 C16 -177.7(5) . . . . ?
N3 N4 C15 C14 -175.3(5) . . . . ?
C13 N4 C15 C14 6.3(9) . . . . ?
N4 C15 C16 C17 0.4(6) . . . . ?
C14 C15 C16 C17 176.0(6) . . . . ?
N4 N3 C17 C16 1.7(6) . . . . ?
Pd2 N3 C17 C16 163.9(4) . . . . ?
N4 N3 C17 C18 -179.5(5) . . . . ?
Pd2 N3 C17 C18 -17.3(7) . . . . ?
C15 C16 C17 N3 -1.3(7) . . . . ?
C15 C16 C17 C18 -180.0(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.931
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.931
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.123

data_darv
_database_code_CSD                  178097

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H62 Cl6 N6 O3 Pd2'
_chemical_formula_weight         1136.49

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.6994(6)
_cell_length_b                   14.6275(7)
_cell_length_c                   17.7885(10)
_cell_angle_alpha                72.2120(10)
_cell_angle_beta                 86.3650(10)
_cell_angle_gamma                81.4770(10)
_cell_volume                     2621.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_type   'Empirical with SADABS'
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_T_max  0.8201
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10840
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         24.00
_reflns_number_total             7779
_reflns_number_gt                6583
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0650P)^2^+9.4683P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7779
_refine_ls_number_parameters     564
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1306
_refine_ls_wR_factor_gt          0.1256
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      0.995
_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 0.19595(3) 0.04197(3) 0.22903(2) 0.03463(13) Uani 1 1 d . . .
Pd2 Pd 0.08224(4) 0.17663(3) 0.33989(2) 0.04173(14) Uani 1 1 d . . .
Cl1 Cl 0.11960(12) 0.02208(11) 0.12052(8) 0.0470(3) Uani 1 1 d . . .
Cl2 Cl -0.09442(14) 0.28832(13) 0.32448(10) 0.0615(4) Uani 1 1 d . . .
Cl3 Cl -0.00390(12) 0.09521(11) 0.26775(8) 0.0467(3) Uani 1 1 d . . .
Cl4 Cl 0.26009(13) 0.05974(10) 0.34815(7) 0.0443(3) Uani 1 1 d . . .
C43 C 0.6794(6) 0.1250(5) 0.3637(2) 0.077(2) Uani 1 1 d D A 1
H43A H 0.6637 0.1964 0.3413 0.092 Uiso 1 1 calc R A 1
H43B H 0.7707 0.1055 0.3742 0.092 Uiso 1 1 calc R A 1
Cl5 Cl 0.6328(2) 0.07043(17) 0.29791(15) 0.1003(7) Uani 1 1 d D A 1
Cl6 Cl 0.5913(8) 0.0875(7) 0.4507(3) 0.096(2) Uiso 0.34 1 d PD A 1
Cl6A Cl 0.6511(10) 0.1173(8) 0.4625(3) 0.120(3) Uiso 0.33 1 d PD B 2
Cl6B Cl 0.6270(12) 0.0488(8) 0.4522(5) 0.141(4) Uiso 0.33 1 d PD C 3
C44 C 0.8532(10) 0.4974(10) 0.3314(11) 0.062(5) Uani 0.324(5) 1 d PD D 1
H44A H 0.8805 0.5033 0.2761 0.075 Uiso 0.324(5) 1 calc PR D 1
H44B H 0.8161 0.4363 0.3527 0.075 Uiso 0.324(5) 1 calc PR D 1
Cl7 Cl 0.7376(5) 0.5942(4) 0.3324(3) 0.0583(16) Uani 0.324(5) 1 d PD D 1
Cl8 Cl 0.9848(5) 0.4913(4) 0.3863(3) 0.0731(19) Uani 0.324(5) 1 d PD D 1
O1 O 0.3464(3) 0.1733(3) 0.0140(2) 0.0442(9) Uani 1 1 d . . .
O2 O 0.4405(4) 0.2875(3) 0.3132(3) 0.0581(11) Uani 1 1 d . . .
O3 O -0.0866(3) 0.3488(3) 0.0772(2) 0.0497(10) Uani 1 1 d . . .
N1 N 0.3748(4) 0.0074(3) 0.1915(2) 0.0334(9) Uani 1 1 d . . .
N2 N 0.4308(4) 0.0751(3) 0.1319(2) 0.0332(9) Uani 1 1 d . . .
N3 N 0.1627(4) 0.2456(3) 0.4037(3) 0.0456(11) Uani 1 1 d . . .
N4 N 0.2463(4) 0.3124(3) 0.3689(3) 0.0452(11) Uani 1 1 d . . .
N5 N -0.0687(4) 0.4804(3) 0.1178(2) 0.0335(9) Uani 1 1 d . . .
N6 N 0.0213(4) 0.5345(3) 0.1274(2) 0.0366(10) Uani 1 1 d . . .
C1 C 0.3015(5) -0.1733(6) 0.2915(6) 0.078(2) Uani 0.50 1 d PD E 1
H1A H 0.2625 -0.1197 0.3110 0.117 Uiso 0.50 1 calc PR E 1
H1B H 0.2913 -0.2351 0.3315 0.117 Uiso 0.50 1 calc PR E 1
H1C H 0.2605 -0.1698 0.2428 0.117 Uiso 0.50 1 calc PR E 1
C2 C 0.5077(10) -0.1733(6) 0.3515(3) 0.078(2) Uani 0.50 1 d PD E 1
H2A H 0.4692 -0.1201 0.3717 0.117 Uiso 0.50 1 calc PR E 1
H2B H 0.5980 -0.1690 0.3409 0.117 Uiso 0.50 1 calc PR E 1
H2C H 0.4972 -0.2354 0.3909 0.117 Uiso 0.50 1 calc PR E 1
C3 C 0.5034(10) -0.2505(3) 0.2437(5) 0.078(2) Uani 0.50 1 d PD E 1
H3A H 0.4786 -0.2376 0.1890 0.117 Uiso 0.50 1 calc PR E 1
H3B H 0.4744 -0.3109 0.2765 0.117 Uiso 0.50 1 calc PR E 1
H3C H 0.5957 -0.2567 0.2460 0.117 Uiso 0.50 1 calc PR E 1
C1A C 0.3125(6) -0.1939(6) 0.2664(6) 0.078(2) Uani 0.50 1 d PD E 2
H1AA H 0.2465 -0.1496 0.2829 0.117 Uiso 0.50 1 calc PR E 2
H1AB H 0.3077 -0.2605 0.2998 0.117 Uiso 0.50 1 calc PR E 2
H1AC H 0.3003 -0.1894 0.2112 0.117 Uiso 0.50 1 calc PR E 2
C2A C 0.4523(11) -0.1563(6) 0.3580(2) 0.078(2) Uani 0.50 1 d PD E 2
H2AA H 0.4025 -0.0955 0.3607 0.117 Uiso 0.50 1 calc PR E 2
H2AB H 0.5409 -0.1562 0.3690 0.117 Uiso 0.50 1 calc PR E 2
H2AC H 0.4194 -0.2109 0.3972 0.117 Uiso 0.50 1 calc PR E 2
C3A C 0.5467(8) -0.2460(4) 0.2636(6) 0.078(2) Uani 0.50 1 d PD E 2
H3AA H 0.6224 -0.2459 0.2918 0.117 Uiso 0.50 1 calc PR E 2
H3AB H 0.5674 -0.2340 0.2073 0.117 Uiso 0.50 1 calc PR E 2
H3AC H 0.5164 -0.3092 0.2847 0.117 Uiso 0.50 1 calc PR E 2
C4 C 0.4431(4) -0.1661(4) 0.2747(3) 0.0543(15) Uani 1 1 d D . .
C5 C 0.4599(4) -0.0709(4) 0.2134(3) 0.0410(12) Uani 1 1 d D E .
C6 C 0.5735(5) -0.0509(4) 0.1699(4) 0.0446(13) Uani 1 1 d . . .
H6B H 0.6507 -0.0937 0.1758 0.054 Uiso 1 1 calc R E .
C7 C 0.5528(4) 0.0402(4) 0.1178(3) 0.0370(12) Uani 1 1 d . E .
C8 C 0.6458(5) 0.0977(4) 0.0622(4) 0.0447(13) Uani 1 1 d . . .
C9 C 0.7796(5) 0.0460(5) 0.0860(5) 0.073(2) Uani 1 1 d . E .
H9A H 0.7947 0.0439 0.1403 0.109 Uiso 1 1 calc R . .
H9B H 0.8418 0.0813 0.0503 0.109 Uiso 1 1 calc R . .
H9C H 0.7877 -0.0202 0.0826 0.109 Uiso 1 1 calc R . .
C10 C 0.6255(6) 0.0994(5) -0.0230(4) 0.0570(16) Uani 1 1 d . E .
H10A H 0.5405 0.1321 -0.0395 0.085 Uiso 1 1 calc R . .
H10B H 0.6346 0.0329 -0.0258 0.085 Uiso 1 1 calc R . .
H10C H 0.6884 0.1345 -0.0582 0.085 Uiso 1 1 calc R . .
C11 C 0.6349(5) 0.2002(4) 0.0686(4) 0.0518(15) Uani 1 1 d . E .
H11A H 0.5501 0.2342 0.0532 0.078 Uiso 1 1 calc R . .
H11B H 0.6981 0.2351 0.0335 0.078 Uiso 1 1 calc R . .
H11C H 0.6496 0.1972 0.1232 0.078 Uiso 1 1 calc R . .
C12 C 0.3509(4) 0.1597(4) 0.0836(3) 0.0328(11) Uani 1 1 d . . .
C13 C 0.2844(4) 0.2251(4) 0.1267(3) 0.0323(11) Uani 1 1 d . . .
C14 C 0.3364(4) 0.2343(3) 0.1924(3) 0.0326(11) Uani 1 1 d . . .
H14A H 0.4169 0.1998 0.2099 0.039 Uiso 1 1 calc R . .
C15 C 0.2701(4) 0.2945(4) 0.2332(3) 0.0331(11) Uani 1 1 d . . .
C16 C 0.1549(4) 0.3484(3) 0.2061(3) 0.0310(10) Uani 1 1 d . . .
H16A H 0.1101 0.3892 0.2342 0.037 Uiso 1 1 calc R . .
C17 C 0.1054(4) 0.3424(3) 0.1376(3) 0.0319(11) Uani 1 1 d . . .
C18 C 0.1691(4) 0.2800(3) 0.0983(3) 0.0319(11) Uani 1 1 d . . .
H18A H 0.1344 0.2747 0.0522 0.038 Uiso 1 1 calc R . .
C19 C 0.3282(5) 0.2975(4) 0.3052(3) 0.0400(12) Uani 1 1 d . . .
C20 C 0.3634(10) 0.4890(6) 0.3133(3) 0.079(2) Uani 0.50 1 d PD F 1
H20A H 0.2805 0.5215 0.2923 0.119 Uiso 0.50 1 calc PR F 1
H20B H 0.3944 0.4387 0.2883 0.119 Uiso 0.50 1 calc PR F 1
H20C H 0.4230 0.5365 0.3023 0.119 Uiso 0.50 1 calc PR F 1
C21 C 0.4837(5) 0.4048(6) 0.4378(6) 0.079(2) Uani 0.50 1 d PD F 1
H21A H 0.4824 0.4057 0.4927 0.119 Uiso 0.50 1 calc PR F 1
H21B H 0.5442 0.4465 0.4068 0.119 Uiso 0.50 1 calc PR F 1
H21C H 0.5090 0.3384 0.4359 0.119 Uiso 0.50 1 calc PR F 1
C22 C 0.2856(8) 0.5196(5) 0.4407(6) 0.079(2) Uani 0.50 1 d PD F 1
H22A H 0.1966 0.5359 0.4257 0.119 Uiso 0.50 1 calc PR F 1
H22B H 0.3274 0.5779 0.4218 0.119 Uiso 0.50 1 calc PR F 1
H22C H 0.2910 0.4941 0.4983 0.119 Uiso 0.50 1 calc PR F 1
C20A C 0.3296(10) 0.5085(5) 0.3182(3) 0.079(2) Uani 0.50 1 d PD F 2
H20D H 0.2400 0.5349 0.3116 0.119 Uiso 0.50 1 calc PR F 2
H20E H 0.3548 0.4710 0.2812 0.119 Uiso 0.50 1 calc PR F 2
H20F H 0.3804 0.5618 0.3075 0.119 Uiso 0.50 1 calc PR F 2
C21A C 0.4927(4) 0.4017(6) 0.4133(7) 0.079(2) Uani 0.50 1 d PD F 2
H21D H 0.5144 0.3543 0.3842 0.119 Uiso 0.50 1 calc PR F 2
H21E H 0.5099 0.3703 0.4695 0.119 Uiso 0.50 1 calc PR F 2
H21F H 0.5436 0.4548 0.3927 0.119 Uiso 0.50 1 calc PR F 2
C22A C 0.3125(9) 0.5017(6) 0.4611(5) 0.079(2) Uani 0.50 1 d PD F 2
H22D H 0.2230 0.5288 0.4544 0.119 Uiso 0.50 1 calc PR F 2
H22E H 0.3641 0.5545 0.4504 0.119 Uiso 0.50 1 calc PR F 2
H22F H 0.3257 0.4596 0.5154 0.119 Uiso 0.50 1 calc PR F 2
C23 C 0.3512(5) 0.4424(4) 0.4033(2) 0.070(2) Uani 1 1 d D . .
C24 C 0.2735(6) 0.3596(4) 0.4204(3) 0.0579(17) Uani 1 1 d D F .
C25 C 0.2043(7) 0.3232(6) 0.4880(4) 0.072(2) Uani 1 1 d . . .
H25A H 0.1999 0.3430 0.5343 0.086 Uiso 1 1 calc R F .
C26 C 0.1395(6) 0.2493(4) 0.4757(3) 0.0595(17) Uani 1 1 d D F .
C27 C 0.0534(5) 0.1946(3) 0.5382(3) 0.071(2) Uani 1 1 d D . .
C28 C -0.0631(7) 0.2642(5) 0.5511(6) 0.083(2) Uani 0.50 1 d PD F 1
H28A H -0.1088 0.2930 0.5016 0.124 Uiso 0.50 1 calc PR F 1
H28B H -0.0357 0.3156 0.5683 0.124 Uiso 0.50 1 calc PR F 1
H28C H -0.1188 0.2283 0.5918 0.124 Uiso 0.50 1 calc PR F 1
C29 C 0.1244(8) 0.1499(8) 0.6166(3) 0.083(2) Uani 0.50 1 d PD F 1
H29A H 0.1978 0.1045 0.6092 0.124 Uiso 0.50 1 calc PR F 1
H29B H 0.0677 0.1153 0.6573 0.124 Uiso 0.50 1 calc PR F 1
H29C H 0.1528 0.2015 0.6330 0.124 Uiso 0.50 1 calc PR F 1
C30 C 0.0097(10) 0.1132(6) 0.5128(5) 0.083(2) Uani 0.50 1 d PD F 1
H30A H -0.0364 0.1413 0.4634 0.124 Uiso 0.50 1 calc PR F 1
H30B H -0.0459 0.0780 0.5540 0.124 Uiso 0.50 1 calc PR F 1
H30C H 0.0835 0.0685 0.5050 0.124 Uiso 0.50 1 calc PR F 1
C28A C -0.0787(5) 0.2544(6) 0.5339(6) 0.083(2) Uani 0.50 1 d PD F 2
H28D H -0.1073 0.2764 0.4792 0.124 Uiso 0.50 1 calc PR F 2
H28E H -0.0745 0.3107 0.5521 0.124 Uiso 0.50 1 calc PR F 2
H28F H -0.1382 0.2141 0.5676 0.124 Uiso 0.50 1 calc PR F 2
C29A C 0.1074(9) 0.1756(8) 0.6205(2) 0.083(2) Uani 0.50 1 d PD F 2
H29D H 0.0776 0.2308 0.6403 0.124 Uiso 0.50 1 calc PR F 2
H29E H 0.2000 0.1671 0.6170 0.124 Uiso 0.50 1 calc PR F 2
H29F H 0.0791 0.1168 0.6568 0.124 Uiso 0.50 1 calc PR F 2
C30A C 0.0412(11) 0.0970(5) 0.5252(5) 0.083(2) Uani 0.50 1 d PD F 2
H30D H -0.0036 0.1087 0.4761 0.124 Uiso 0.50 1 calc PR F 2
H30E H -0.0062 0.0584 0.5696 0.124 Uiso 0.50 1 calc PR F 2
H30F H 0.1256 0.0617 0.5216 0.124 Uiso 0.50 1 calc PR F 2
C31 C -0.0245(4) 0.3887(4) 0.1075(3) 0.0350(11) Uani 1 1 d . . .
C32 C -0.4225(5) 0.5738(5) 0.1144(4) 0.0594(17) Uani 1 1 d . . .
H32A H -0.4188 0.5799 0.1675 0.089 Uiso 1 1 calc R . .
H32B H -0.5033 0.5532 0.1082 0.089 Uiso 1 1 calc R . .
H32C H -0.4148 0.6365 0.0751 0.089 Uiso 1 1 calc R . .
C33 C -0.3221(5) 0.4913(5) 0.0181(4) 0.0529(15) Uani 1 1 d . . .
H33A H -0.2528 0.4439 0.0087 0.079 Uiso 1 1 calc R . .
H33B H -0.3158 0.5548 -0.0203 0.079 Uiso 1 1 calc R . .
H33C H -0.4031 0.4707 0.0124 0.079 Uiso 1 1 calc R . .
C34 C -0.3299(6) 0.4018(4) 0.1650(4) 0.0566(16) Uani 1 1 d . . .
H34A H -0.3232 0.4085 0.2177 0.085 Uiso 1 1 calc R . .
H34B H -0.2639 0.3511 0.1574 0.085 Uiso 1 1 calc R . .
H34C H -0.4131 0.3842 0.1598 0.085 Uiso 1 1 calc R . .
C35 C -0.3135(5) 0.4981(4) 0.1024(3) 0.0447(13) Uani 1 1 d . . .
C36 C -0.1904(4) 0.5327(4) 0.1120(3) 0.0349(11) Uani 1 1 d . . .
C37 C -0.1729(5) 0.6206(4) 0.1182(3) 0.0386(12) Uani 1 1 d . . .
H37A H -0.2371 0.6735 0.1167 0.046 Uiso 1 1 calc R . .
C38 C -0.0411(4) 0.6189(4) 0.1275(2) 0.0383(12) Uani 1 1 d D G .
C39 C 0.0240(4) 0.6998(3) 0.13554(19) 0.0515(15) Uani 1 1 d D . .
C40 C -0.0282(9) 0.7962(3) 0.0756(5) 0.0671(17) Uani 0.50 1 d PD G 1
H40A H -0.1020 0.8269 0.0987 0.101 Uiso 0.50 1 calc PR G 1
H40B H -0.0530 0.7840 0.0278 0.101 Uiso 0.50 1 calc PR G 1
H40C H 0.0372 0.8393 0.0620 0.101 Uiso 0.50 1 calc PR G 1
C41 C 0.0014(10) 0.7089(7) 0.2196(3) 0.0671(17) Uani 0.50 1 d PD G 1
H41A H 0.0206 0.6450 0.2584 0.101 Uiso 0.50 1 calc PR G 1
H41B H -0.0872 0.7348 0.2260 0.101 Uiso 0.50 1 calc PR G 1
H41C H 0.0564 0.7529 0.2278 0.101 Uiso 0.50 1 calc PR G 1
C42 C 0.1672(4) 0.6786(6) 0.1209(7) 0.0671(17) Uani 0.50 1 d PD G 1
H42A H 0.2030 0.6219 0.1631 0.101 Uiso 0.50 1 calc PR G 1
H42B H 0.2074 0.7349 0.1203 0.101 Uiso 0.50 1 calc PR G 1
H42C H 0.1824 0.6656 0.0700 0.101 Uiso 0.50 1 calc PR G 1
C40A C -0.0002(10) 0.7889(4) 0.0619(4) 0.0671(17) Uani 0.50 1 d PD G 2
H40D H 0.0195 0.7689 0.0142 0.101 Uiso 0.50 1 calc PR G 2
H40E H 0.0536 0.8371 0.0631 0.101 Uiso 0.50 1 calc PR G 2
H40F H -0.0892 0.8171 0.0616 0.101 Uiso 0.50 1 calc PR G 2
C41A C -0.0267(9) 0.7286(7) 0.2090(4) 0.0671(17) Uani 0.50 1 d PD G 2
H41D H -0.0127 0.6722 0.2560 0.101 Uiso 0.50 1 calc PR G 2
H41E H -0.1174 0.7517 0.2036 0.101 Uiso 0.50 1 calc PR G 2
H41F H 0.0177 0.7803 0.2142 0.101 Uiso 0.50 1 calc PR G 2
C42A C 0.1675(4) 0.6675(6) 0.1429(7) 0.0671(17) Uani 0.50 1 d PD G 2
H42D H 0.1842 0.6111 0.1896 0.101 Uiso 0.50 1 calc PR G 2
H42E H 0.2090 0.7206 0.1480 0.101 Uiso 0.50 1 calc PR G 2
H42F H 0.2005 0.6502 0.0956 0.101 Uiso 0.50 1 calc PR G 2

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 0.0309(2) 0.0419(3) 0.0329(2) -0.00972(18) 0.00285(15) -0.01525(17)
Pd2 0.0472(3) 0.0500(3) 0.0331(2) -0.01287(19) 0.00713(17) -0.0248(2)
Cl1 0.0329(6) 0.0712(10) 0.0472(7) -0.0319(7) 0.0010(5) -0.0099(6)
Cl2 0.0492(8) 0.0751(11) 0.0617(9) -0.0219(8) 0.0126(7) -0.0159(8)
Cl3 0.0349(7) 0.0717(10) 0.0461(7) -0.0306(7) 0.0110(5) -0.0238(6)
Cl4 0.0547(8) 0.0447(8) 0.0339(7) -0.0055(6) -0.0045(6) -0.0200(6)
C43 0.050(4) 0.104(6) 0.077(5) -0.027(5) -0.008(3) -0.010(4)
Cl5 0.0989(16) 0.0845(15) 0.1207(18) -0.0299(13) -0.0515(14) -0.0035(12)
C44 0.082(15) 0.047(12) 0.059(12) -0.013(10) -0.006(10) -0.017(10)
Cl7 0.059(3) 0.057(3) 0.054(3) -0.014(2) -0.002(2) 0.002(2)
Cl8 0.067(3) 0.071(4) 0.072(4) -0.008(3) -0.017(3) -0.002(3)
O1 0.044(2) 0.046(2) 0.037(2) -0.0113(17) 0.0038(16) 0.0053(17)
O2 0.048(3) 0.067(3) 0.063(3) -0.019(2) -0.013(2) -0.016(2)
O3 0.036(2) 0.051(2) 0.071(3) -0.033(2) -0.0105(18) 0.0036(17)
N1 0.031(2) 0.029(2) 0.038(2) -0.0034(18) -0.0014(17) -0.0131(18)
N2 0.027(2) 0.028(2) 0.042(2) -0.0057(18) 0.0003(17) -0.0040(17)
N3 0.059(3) 0.050(3) 0.033(2) -0.012(2) 0.005(2) -0.025(2)
N4 0.059(3) 0.048(3) 0.034(2) -0.011(2) -0.002(2) -0.026(2)
N5 0.028(2) 0.032(2) 0.039(2) -0.0109(19) 0.0051(17) -0.0043(17)
N6 0.038(2) 0.034(3) 0.036(2) -0.0077(19) -0.0007(18) -0.0065(19)
C1 0.083(5) 0.041(3) 0.098(5) 0.003(3) -0.007(3) -0.019(3)
C2 0.083(5) 0.041(3) 0.098(5) 0.003(3) -0.007(3) -0.019(3)
C3 0.083(5) 0.041(3) 0.098(5) 0.003(3) -0.007(3) -0.019(3)
C1A 0.083(5) 0.041(3) 0.098(5) 0.003(3) -0.007(3) -0.019(3)
C2A 0.083(5) 0.041(3) 0.098(5) 0.003(3) -0.007(3) -0.019(3)
C3A 0.083(5) 0.041(3) 0.098(5) 0.003(3) -0.007(3) -0.019(3)
C4 0.068(4) 0.034(3) 0.057(4) -0.001(3) -0.013(3) -0.015(3)
C5 0.041(3) 0.030(3) 0.050(3) -0.006(2) -0.013(2) -0.007(2)
C6 0.029(3) 0.036(3) 0.068(4) -0.015(3) -0.008(2) -0.001(2)
C7 0.024(2) 0.032(3) 0.056(3) -0.014(2) 0.000(2) -0.005(2)
C8 0.028(3) 0.036(3) 0.073(4) -0.021(3) 0.013(2) -0.011(2)
C9 0.027(3) 0.068(5) 0.122(6) -0.028(4) 0.007(3) -0.008(3)
C10 0.049(3) 0.060(4) 0.072(4) -0.035(3) 0.024(3) -0.018(3)
C11 0.046(3) 0.047(4) 0.069(4) -0.022(3) 0.017(3) -0.024(3)
C12 0.026(2) 0.033(3) 0.037(3) -0.007(2) 0.004(2) -0.007(2)
C13 0.025(2) 0.035(3) 0.031(2) -0.001(2) 0.0060(19) -0.006(2)
C14 0.028(2) 0.025(3) 0.039(3) 0.000(2) 0.001(2) -0.0076(19)
C15 0.034(3) 0.035(3) 0.029(2) -0.003(2) 0.003(2) -0.013(2)
C16 0.036(3) 0.022(3) 0.034(3) -0.005(2) 0.008(2) -0.012(2)
C17 0.031(2) 0.028(3) 0.032(3) -0.002(2) 0.003(2) -0.006(2)
C18 0.032(2) 0.031(3) 0.032(3) -0.008(2) 0.002(2) -0.005(2)
C19 0.046(3) 0.034(3) 0.039(3) -0.004(2) -0.002(2) -0.018(2)
C20 0.117(5) 0.080(4) 0.056(4) -0.023(3) -0.012(3) -0.055(3)
C21 0.117(5) 0.080(4) 0.056(4) -0.023(3) -0.012(3) -0.055(3)
C22 0.117(5) 0.080(4) 0.056(4) -0.023(3) -0.012(3) -0.055(3)
C20A 0.117(5) 0.080(4) 0.056(4) -0.023(3) -0.012(3) -0.055(3)
C21A 0.117(5) 0.080(4) 0.056(4) -0.023(3) -0.012(3) -0.055(3)
C22A 0.117(5) 0.080(4) 0.056(4) -0.023(3) -0.012(3) -0.055(3)
C23 0.102(6) 0.071(5) 0.054(4) -0.024(4) -0.004(4) -0.053(4)
C24 0.084(5) 0.060(4) 0.038(3) -0.015(3) -0.003(3) -0.039(3)
C25 0.108(6) 0.088(6) 0.040(3) -0.029(4) 0.010(3) -0.057(5)
C26 0.082(5) 0.063(4) 0.040(3) -0.015(3) 0.005(3) -0.036(4)
C27 0.094(5) 0.088(5) 0.043(4) -0.028(4) 0.022(3) -0.043(4)
C28 0.126(5) 0.093(4) 0.044(3) -0.023(3) 0.018(3) -0.064(4)
C29 0.126(5) 0.093(4) 0.044(3) -0.023(3) 0.018(3) -0.064(4)
C30 0.126(5) 0.093(4) 0.044(3) -0.023(3) 0.018(3) -0.064(4)
C28A 0.126(5) 0.093(4) 0.044(3) -0.023(3) 0.018(3) -0.064(4)
C29A 0.126(5) 0.093(4) 0.044(3) -0.023(3) 0.018(3) -0.064(4)
C30A 0.126(5) 0.093(4) 0.044(3) -0.023(3) 0.018(3) -0.064(4)
C31 0.031(3) 0.034(3) 0.039(3) -0.011(2) 0.002(2) -0.001(2)
C32 0.038(3) 0.051(4) 0.083(5) -0.018(3) 0.004(3) 0.003(3)
C33 0.033(3) 0.063(4) 0.065(4) -0.024(3) -0.005(3) -0.001(3)
C34 0.041(3) 0.047(4) 0.073(4) -0.006(3) 0.008(3) -0.011(3)
C35 0.031(3) 0.045(3) 0.055(3) -0.013(3) 0.004(2) -0.004(2)
C36 0.032(3) 0.032(3) 0.036(3) -0.006(2) 0.005(2) 0.001(2)
C37 0.042(3) 0.033(3) 0.038(3) -0.010(2) -0.001(2) 0.003(2)
C38 0.048(3) 0.032(3) 0.031(3) -0.004(2) -0.003(2) -0.004(2)
C39 0.065(4) 0.042(3) 0.049(3) -0.014(3) -0.016(3) -0.005(3)
C40 0.071(3) 0.062(3) 0.072(4) -0.019(3) -0.017(2) -0.016(3)
C41 0.071(3) 0.062(3) 0.072(4) -0.019(3) -0.017(2) -0.016(3)
C42 0.071(3) 0.062(3) 0.072(4) -0.019(3) -0.017(2) -0.016(3)
C40A 0.071(3) 0.062(3) 0.072(4) -0.019(3) -0.017(2) -0.016(3)
C41A 0.071(3) 0.062(3) 0.072(4) -0.019(3) -0.017(2) -0.016(3)
C42A 0.071(3) 0.062(3) 0.072(4) -0.019(3) -0.017(2) -0.016(3)

_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 2.030(4) . ?
Pd1 Cl1 2.2564(13) . ?
Pd1 Cl3 2.3023(13) . ?
Pd1 Cl4 2.3669(13) . ?
Pd1 Pd2 3.2569(6) . ?
Pd2 N3 2.033(4) . ?
Pd2 Cl2 2.2789(17) . ?
Pd2 Cl3 2.3074(13) . ?
Pd2 Cl4 2.3418(15) . ?
C43 Cl5 1.737(2) . ?
C43 Cl6 1.742(2) . ?
C44 Cl7 1.740(2) . ?
C44 Cl8 1.740(2) . ?
O1 C12 1.194(6) . ?
O2 C19 1.201(6) . ?
O3 C31 1.193(6) . ?
N1 C5 1.325(6) . ?
N1 N2 1.384(6) . ?
N2 C7 1.367(6) . ?
N2 C12 1.459(6) . ?
N3 C26 1.304(7) . ?
N3 N4 1.399(6) . ?
N4 C24 1.372(7) . ?
N4 C19 1.437(7) . ?
N5 N6 1.383(6) . ?
N5 C36 1.402(6) . ?
N5 C31 1.417(6) . ?
N6 C38 1.314(6) . ?
C1 C4 1.5383(19) . ?
C2 C4 1.5380(19) . ?
C3 C4 1.5427(19) . ?
C1A C4 1.5395(19) . ?
C2A C4 1.5423(19) . ?
C3A C4 1.5376(19) . ?
C4 C5 1.511(8) . ?
C5 C6 1.418(7) . ?
C6 C7 1.366(8) . ?
C7 C8 1.514(7) . ?
C8 C11 1.524(8) . ?
C8 C9 1.537(8) . ?
C8 C10 1.537(9) . ?
C12 C13 1.479(7) . ?
C13 C14 1.377(7) . ?
C13 C18 1.400(7) . ?
C14 C15 1.395(7) . ?
C15 C16 1.389(7) . ?
C15 C19 1.473(7) . ?
C16 C17 1.391(7) . ?
C17 C18 1.389(7) . ?
C17 C31 1.507(7) . ?
C20 C23 1.5407(19) . ?
C21 C23 1.5370(19) . ?
C22 C23 1.5421(19) . ?
C20A C23 1.5372(19) . ?
C21A C23 1.5426(19) . ?
C22A C23 1.5401(19) . ?
C23 C24 1.513(8) . ?
C24 C25 1.374(8) . ?
C25 C26 1.443(8) . ?
C26 C27 1.507(8) . ?
C27 C30 1.5369(19) . ?
C27 C29A 1.5379(19) . ?
C27 C28 1.5401(19) . ?
C27 C28A 1.5404(19) . ?
C27 C30A 1.5405(19) . ?
C27 C29 1.5418(19) . ?
C32 C35 1.536(8) . ?
C33 C35 1.543(8) . ?
C34 C35 1.531(8) . ?
C35 C36 1.515(7) . ?
C36 C37 1.365(7) . ?
C37 C38 1.426(7) . ?
C38 C39 1.505(7) . ?
C39 C41A 1.5357(19) . ?
C39 C40 1.5371(19) . ?
C39 C42 1.5389(19) . ?
C39 C42A 1.5390(19) . ?
C39 C41 1.5422(19) . ?
C39 C40A 1.5436(19) . ?

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 89.89(12) . . ?
N1 Pd1 Cl3 174.96(12) . . ?
Cl1 Pd1 Cl3 91.17(5) . . ?
N1 Pd1 Cl4 94.32(12) . . ?
Cl1 Pd1 Cl4 175.30(5) . . ?
Cl3 Pd1 Cl4 84.82(5) . . ?
N1 Pd1 Pd2 131.79(11) . . ?
Cl1 Pd1 Pd2 131.42(4) . . ?
Cl3 Pd1 Pd2 45.11(3) . . ?
Cl4 Pd1 Pd2 45.92(4) . . ?
N3 Pd2 Cl2 90.42(15) . . ?
N3 Pd2 Cl3 178.36(15) . . ?
Cl2 Pd2 Cl3 91.22(6) . . ?
N3 Pd2 Cl4 93.08(15) . . ?
Cl2 Pd2 Cl4 176.18(5) . . ?
Cl3 Pd2 Cl4 85.28(5) . . ?
N3 Pd2 Pd1 133.54(14) . . ?
Cl2 Pd2 Pd1 129.63(5) . . ?
Cl3 Pd2 Pd1 44.98(3) . . ?
Cl4 Pd2 Pd1 46.56(3) . . ?
Pd1 Cl3 Pd2 89.91(4) . . ?
Pd2 Cl4 Pd1 87.53(5) . . ?
Cl5 C43 Cl6 107.5(4) . . ?
Cl7 C44 Cl8 113.2(4) . . ?
C5 N1 N2 106.7(4) . . ?
C5 N1 Pd1 133.4(4) . . ?
N2 N1 Pd1 119.8(3) . . ?
C7 N2 N1 111.0(4) . . ?
C7 N2 C12 128.7(4) . . ?
N1 N2 C12 118.8(4) . . ?
C26 N3 N4 107.2(4) . . ?
C26 N3 Pd2 130.7(4) . . ?
N4 N3 Pd2 121.6(3) . . ?
C24 N4 N3 110.8(4) . . ?
C24 N4 C19 124.7(5) . . ?
N3 N4 C19 119.0(4) . . ?
N6 N5 C36 111.6(4) . . ?
N6 N5 C31 117.2(4) . . ?
C36 N5 C31 130.8(4) . . ?
C38 N6 N5 105.7(4) . . ?
C5 C4 C3A 109.9(3) . . ?
C5 C4 C2 109.8(3) . . ?
C3A C4 C2 87.8(5) . . ?
C5 C4 C1 109.9(3) . . ?
C3A C4 C1 127.2(6) . . ?
C2 C4 C1 109.4(3) . . ?
C5 C4 C1A 109.8(3) . . ?
C3A C4 C1A 109.3(3) . . ?
C2 C4 C1A 127.4(6) . . ?
C1 C4 C1A 22.8(6) . . ?
C5 C4 C2A 109.6(3) . . ?
C3A C4 C2A 109.2(3) . . ?
C2 C4 C2A 23.5(6) . . ?
C1 C4 C2A 88.3(5) . . ?
C1A C4 C2A 109.0(3) . . ?
C5 C4 C3 109.5(3) . . ?
C3A C4 C3 23.3(5) . . ?
C2 C4 C3 109.2(3) . . ?
C1 C4 C3 109.1(3) . . ?
C1A C4 C3 88.4(5) . . ?
C2A C4 C3 127.9(6) . . ?
N1 C5 C6 108.5(5) . . ?
N1 C5 C4 127.2(4) . . ?
C6 C5 C4 124.3(4) . . ?
C7 C6 C5 108.3(5) . . ?
C6 C7 N2 105.3(4) . . ?
C6 C7 C8 129.0(5) . . ?
N2 C7 C8 125.3(4) . . ?
C7 C8 C11 111.1(4) . . ?
C7 C8 C9 107.7(5) . . ?
C11 C8 C9 108.6(5) . . ?
C7 C8 C10 110.2(4) . . ?
C11 C8 C10 111.1(5) . . ?
C9 C8 C10 108.0(5) . . ?
O1 C12 N2 119.9(4) . . ?
O1 C12 C13 125.0(4) . . ?
N2 C12 C13 115.1(4) . . ?
C14 C13 C18 120.1(5) . . ?
C14 C13 C12 120.8(4) . . ?
C18 C13 C12 119.1(4) . . ?
C13 C14 C15 119.6(4) . . ?
C16 C15 C14 120.5(4) . . ?
C16 C15 C19 122.6(5) . . ?
C14 C15 C19 116.9(4) . . ?
C15 C16 C17 119.7(4) . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 C31 115.2(4) . . ?
C16 C17 C31 124.3(4) . . ?
C17 C18 C13 120.0(5) . . ?
O2 C19 N4 118.7(5) . . ?
O2 C19 C15 123.0(5) . . ?
N4 C19 C15 118.3(4) . . ?
C24 C23 C21 110.0(3) . . ?
C24 C23 C20A 110.0(3) . . ?
C21 C23 C20A 122.7(7) . . ?
C24 C23 C22A 109.7(3) . . ?
C21 C23 C22A 93.6(6) . . ?
C20A C23 C22A 109.3(3) . . ?
C24 C23 C20 109.8(3) . . ?
C21 C23 C20 109.3(3) . . ?
C20A C23 C20 16.7(7) . . ?
C22A C23 C20 123.0(7) . . ?
C24 C23 C22 109.6(3) . . ?
C21 C23 C22 109.2(3) . . ?
C20A C23 C22 93.8(6) . . ?
C22A C23 C22 17.4(7) . . ?
C20 C23 C22 108.9(3) . . ?
C24 C23 C21A 109.6(3) . . ?
C21 C23 C21A 16.9(7) . . ?
C20A C23 C21A 109.2(3) . . ?
C22A C23 C21A 109.0(3) . . ?
C20 C23 C21A 94.3(6) . . ?
C22 C23 C21A 123.2(6) . . ?
N4 C24 C25 105.5(5) . . ?
N4 C24 C23 127.1(4) . . ?
C25 C24 C23 127.1(4) . . ?
C24 C25 C26 107.5(5) . . ?
N3 C26 C25 108.9(5) . . ?
N3 C26 C27 129.3(4) . . ?
C25 C26 C27 121.6(4) . . ?
C26 C27 C30 110.1(3) . . ?
C26 C27 C29A 110.0(3) . . ?
C30 C27 C29A 121.6(7) . . ?
C26 C27 C28 109.8(3) . . ?
C30 C27 C28 109.2(3) . . ?
C29A C27 C28 94.9(7) . . ?
C26 C27 C28A 109.8(3) . . ?
C30 C27 C28A 95.0(7) . . ?
C29A C27 C28A 109.1(3) . . ?
C28 C27 C28A 16.0(7) . . ?
C26 C27 C30A 109.9(3) . . ?
C30 C27 C30A 15.5(8) . . ?
C29A C27 C30A 109.1(3) . . ?
C28 C27 C30A 122.0(7) . . ?
C28A C27 C30A 108.9(3) . . ?
C26 C27 C29 109.7(3) . . ?
C30 C27 C29 109.1(3) . . ?
C29A C27 C29 15.5(8) . . ?
C28 C27 C29 108.9(3) . . ?
C28A C27 C29 122.0(7) . . ?
C30A C27 C29 95.3(7) . . ?
O3 C31 N5 122.3(4) . . ?
O3 C31 C17 120.9(5) . . ?
N5 C31 C17 116.8(4) . . ?
C36 C35 C34 111.6(5) . . ?
C36 C35 C32 107.9(5) . . ?
C34 C35 C32 107.4(5) . . ?
C36 C35 C33 110.5(4) . . ?
C34 C35 C33 111.5(5) . . ?
C32 C35 C33 107.8(5) . . ?
C37 C36 N5 104.4(4) . . ?
C37 C36 C35 128.1(5) . . ?
N5 C36 C35 127.5(5) . . ?
C36 C37 C38 107.8(4) . . ?
N6 C38 C37 110.5(5) . . ?
N6 C38 C39 122.2(4) . . ?
C37 C38 C39 127.3(4) . . ?
C38 C39 C41A 110.3(3) . . ?
C38 C39 C40 110.2(3) . . ?
C41A C39 C40 95.5(7) . . ?
C38 C39 C42 110.1(3) . . ?
C41A C39 C42 120.6(7) . . ?
C40 C39 C42 109.1(3) . . ?
C38 C39 C42A 110.1(3) . . ?
C41A C39 C42A 109.2(3) . . ?
C40 C39 C42A 120.5(7) . . ?
C42 C39 C42A 14.0(7) . . ?
C38 C39 C41 109.8(3) . . ?
C41A C39 C41 14.8(7) . . ?
C40 C39 C41 108.9(3) . . ?
C42 C39 C41 108.7(3) . . ?
C42A C39 C41 96.3(7) . . ?
C38 C39 C40A 109.7(3) . . ?
C41A C39 C40A 108.9(3) . . ?
C40 C39 C40A 14.8(7) . . ?
C42 C39 C40A 96.1(7) . . ?
C42A C39 C40A 108.6(3) . . ?
C41 C39 C40A 121.3(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
N1 Pd1 Pd2 N3 -6.5(2) . . . . ?
Cl1 Pd1 Pd2 N3 -148.20(19) . . . . ?
Cl3 Pd1 Pd2 N3 179.00(19) . . . . ?
Cl4 Pd1 Pd2 N3 37.08(19) . . . . ?
N1 Pd1 Pd2 Cl2 136.67(16) . . . . ?
Cl1 Pd1 Pd2 Cl2 -5.05(8) . . . . ?
Cl3 Pd1 Pd2 Cl2 -37.85(8) . . . . ?
Cl4 Pd1 Pd2 Cl2 -179.78(7) . . . . ?
N1 Pd1 Pd2 Cl3 174.53(16) . . . . ?
Cl1 Pd1 Pd2 Cl3 32.80(8) . . . . ?
Cl4 Pd1 Pd2 Cl3 -141.93(7) . . . . ?
N1 Pd1 Pd2 Cl4 -43.55(16) . . . . ?
Cl1 Pd1 Pd2 Cl4 174.72(7) . . . . ?
Cl3 Pd1 Pd2 Cl4 141.93(7) . . . . ?
N1 Pd1 Cl3 Pd2 -54.0(13) . . . . ?
Cl1 Pd1 Cl3 Pd2 -156.03(6) . . . . ?
Cl4 Pd1 Cl3 Pd2 26.41(5) . . . . ?
N3 Pd2 Cl3 Pd1 -26(5) . . . . ?
Cl2 Pd2 Cl3 Pd1 151.79(6) . . . . ?
Cl4 Pd2 Cl3 Pd1 -26.70(5) . . . . ?
N3 Pd2 Cl4 Pd1 -154.04(13) . . . . ?
Cl2 Pd2 Cl4 Pd1 2.6(9) . . . . ?
Cl3 Pd2 Cl4 Pd1 25.94(5) . . . . ?
N1 Pd1 Cl4 Pd2 148.99(12) . . . . ?
Cl1 Pd1 Cl4 Pd2 -57.3(7) . . . . ?
Cl3 Pd1 Cl4 Pd2 -26.02(5) . . . . ?
Cl1 Pd1 N1 C5 -104.9(4) . . . . ?
Cl3 Pd1 N1 C5 153.0(11) . . . . ?
Cl4 Pd1 N1 C5 73.0(4) . . . . ?
Pd2 Pd1 N1 C5 102.8(4) . . . . ?
Cl1 Pd1 N1 N2 77.0(3) . . . . ?
Cl3 Pd1 N1 N2 -25.1(16) . . . . ?
Cl4 Pd1 N1 N2 -105.1(3) . . . . ?
Pd2 Pd1 N1 N2 -75.4(4) . . . . ?
C5 N1 N2 C7 -1.7(5) . . . . ?
Pd1 N1 N2 C7 176.9(3) . . . . ?
C5 N1 N2 C12 165.6(4) . . . . ?
Pd1 N1 N2 C12 -15.8(5) . . . . ?
Cl2 Pd2 N3 C26 73.7(5) . . . . ?
Cl3 Pd2 N3 C26 -108(4) . . . . ?
Cl4 Pd2 N3 C26 -107.8(5) . . . . ?
Pd1 Pd2 N3 C26 -133.8(5) . . . . ?
Cl2 Pd2 N3 N4 -96.4(4) . . . . ?
Cl3 Pd2 N3 N4 82(5) . . . . ?
Cl4 Pd2 N3 N4 82.1(4) . . . . ?
Pd1 Pd2 N3 N4 56.1(5) . . . . ?
C26 N3 N4 C24 -1.0(6) . . . . ?
Pd2 N3 N4 C24 171.1(4) . . . . ?
C26 N3 N4 C19 154.3(5) . . . . ?
Pd2 N3 N4 C19 -33.6(6) . . . . ?
C36 N5 N6 C38 -0.2(5) . . . . ?
C31 N5 N6 C38 173.7(4) . . . . ?
N2 N1 C5 C6 2.8(5) . . . . ?
Pd1 N1 C5 C6 -175.5(4) . . . . ?
N2 N1 C5 C4 -177.8(4) . . . . ?
Pd1 N1 C5 C4 3.9(7) . . . . ?
C3A C4 C5 N1 162.1(6) . . . . ?
C2 C4 C5 N1 -102.8(6) . . . . ?
C1 C4 C5 N1 17.6(6) . . . . ?
C1A C4 C5 N1 41.8(6) . . . . ?
C2A C4 C5 N1 -77.9(6) . . . . ?
C3 C4 C5 N1 137.3(6) . . . . ?
C3A C4 C5 C6 -18.6(6) . . . . ?
C2 C4 C5 C6 76.5(6) . . . . ?
C1 C4 C5 C6 -163.1(6) . . . . ?
C1A C4 C5 C6 -138.9(6) . . . . ?
C2A C4 C5 C6 101.4(6) . . . . ?
C3 C4 C5 C6 -43.4(6) . . . . ?
N1 C5 C6 C7 -3.1(6) . . . . ?
C4 C5 C6 C7 177.5(4) . . . . ?
C5 C6 C7 N2 2.0(6) . . . . ?
C5 C6 C7 C8 175.4(5) . . . . ?
N1 N2 C7 C6 -0.2(6) . . . . ?
C12 N2 C7 C6 -166.0(5) . . . . ?
N1 N2 C7 C8 -174.0(5) . . . . ?
C12 N2 C7 C8 20.3(8) . . . . ?
C6 C7 C8 C11 -131.6(6) . . . . ?
N2 C7 C8 C11 40.7(7) . . . . ?
C6 C7 C8 C9 -12.7(8) . . . . ?
N2 C7 C8 C9 159.5(5) . . . . ?
C6 C7 C8 C10 104.9(7) . . . . ?
N2 C7 C8 C10 -82.8(6) . . . . ?
C7 N2 C12 O1 45.7(7) . . . . ?
N1 N2 C12 O1 -119.1(5) . . . . ?
C7 N2 C12 C13 -131.9(5) . . . . ?
N1 N2 C12 C13 63.3(6) . . . . ?
O1 C12 C13 C14 -147.4(5) . . . . ?
N2 C12 C13 C14 30.0(6) . . . . ?
O1 C12 C13 C18 30.6(7) . . . . ?
N2 C12 C13 C18 -151.9(4) . . . . ?
C18 C13 C14 C15 3.6(7) . . . . ?
C12 C13 C14 C15 -178.3(5) . . . . ?
C13 C14 C15 C16 -2.8(7) . . . . ?
C13 C14 C15 C19 177.2(4) . . . . ?
C14 C15 C16 C17 -0.2(7) . . . . ?
C19 C15 C16 C17 179.8(4) . . . . ?
C15 C16 C17 C18 2.3(7) . . . . ?
C15 C16 C17 C31 173.0(4) . . . . ?
C16 C17 C18 C13 -1.5(7) . . . . ?
C31 C17 C18 C13 -173.0(4) . . . . ?
C14 C13 C18 C17 -1.5(7) . . . . ?
C12 C13 C18 C17 -179.6(4) . . . . ?
C24 N4 C19 O2 32.0(8) . . . . ?
N3 N4 C19 O2 -119.6(6) . . . . ?
C24 N4 C19 C15 -148.5(5) . . . . ?
N3 N4 C19 C15 59.9(6) . . . . ?
C16 C15 C19 O2 -148.2(5) . . . . ?
C14 C15 C19 O2 31.8(7) . . . . ?
C16 C15 C19 N4 32.4(7) . . . . ?
C14 C15 C19 N4 -147.6(5) . . . . ?
N3 N4 C24 C25 -1.1(7) . . . . ?
C19 N4 C24 C25 -154.7(6) . . . . ?
N3 N4 C24 C23 -174.7(4) . . . . ?
C19 N4 C24 C23 31.7(8) . . . . ?
C21 C23 C24 N4 -102.9(7) . . . . ?
C20A C23 C24 N4 35.2(7) . . . . ?
C22A C23 C24 N4 155.5(6) . . . . ?
C20 C23 C24 N4 17.4(7) . . . . ?
C22 C23 C24 N4 137.0(6) . . . . ?
C21A C23 C24 N4 -84.9(6) . . . . ?
C21 C23 C24 C25 84.8(8) . . . . ?
C20A C23 C24 C25 -137.1(8) . . . . ?
C22A C23 C24 C25 -16.8(8) . . . . ?
C20 C23 C24 C25 -154.9(8) . . . . ?
C22 C23 C24 C25 -35.3(8) . . . . ?
C21A C23 C24 C25 102.8(8) . . . . ?
N4 C24 C25 C26 2.6(8) . . . . ?
C23 C24 C25 C26 176.2(4) . . . . ?
N4 N3 C26 C25 2.6(7) . . . . ?
Pd2 N3 C26 C25 -168.5(5) . . . . ?
N4 N3 C26 C27 178.2(4) . . . . ?
Pd2 N3 C26 C27 7.1(8) . . . . ?
C24 C25 C26 N3 -3.4(8) . . . . ?
C24 C25 C26 C27 -179.4(5) . . . . ?
N3 C26 C27 C30 11.3(7) . . . . ?
C25 C26 C27 C30 -173.6(7) . . . . ?
N3 C26 C27 C29A 147.9(7) . . . . ?
C25 C26 C27 C29A -37.0(7) . . . . ?
N3 C26 C27 C28 -109.0(7) . . . . ?
C25 C26 C27 C28 66.1(7) . . . . ?
N3 C26 C27 C28A -92.0(7) . . . . ?
C25 C26 C27 C28A 83.1(7) . . . . ?
N3 C26 C27 C30A 27.8(7) . . . . ?
C25 C26 C27 C30A -157.1(7) . . . . ?
N3 C26 C27 C29 131.3(7) . . . . ?
C25 C26 C27 C29 -53.6(7) . . . . ?
N6 N5 C31 O3 -158.3(5) . . . . ?
C36 N5 C31 O3 14.2(8) . . . . ?
N6 N5 C31 C17 22.4(6) . . . . ?
C36 N5 C31 C17 -165.2(5) . . . . ?
C18 C17 C31 O3 28.5(7) . . . . ?
C16 C17 C31 O3 -142.6(5) . . . . ?
C18 C17 C31 N5 -152.1(4) . . . . ?
C16 C17 C31 N5 36.8(7) . . . . ?
N6 N5 C36 C37 0.1(5) . . . . ?
C31 N5 C36 C37 -172.7(5) . . . . ?
N6 N5 C36 C35 -179.0(5) . . . . ?
C31 N5 C36 C35 8.2(8) . . . . ?
C34 C35 C36 C37 -126.9(6) . . . . ?
C32 C35 C36 C37 -9.2(8) . . . . ?
C33 C35 C36 C37 108.4(6) . . . . ?
C34 C35 C36 N5 51.9(7) . . . . ?
C32 C35 C36 N5 169.6(5) . . . . ?
C33 C35 C36 N5 -72.8(7) . . . . ?
N5 C36 C37 C38 0.1(5) . . . . ?
C35 C36 C37 C38 179.1(5) . . . . ?
N5 N6 C38 C37 0.2(5) . . . . ?
N5 N6 C38 C39 -179.1(3) . . . . ?
C36 C37 C38 N6 -0.2(6) . . . . ?
C36 C37 C38 C39 179.1(4) . . . . ?
N6 C38 C39 C41A -120.3(6) . . . . ?
C37 C38 C39 C41A 60.4(6) . . . . ?
N6 C38 C39 C40 135.5(6) . . . . ?
C37 C38 C39 C40 -43.8(6) . . . . ?
N6 C38 C39 C42 15.1(6) . . . . ?
C37 C38 C39 C42 -164.2(6) . . . . ?
N6 C38 C39 C42A 0.2(6) . . . . ?
C37 C38 C39 C42A -179.1(6) . . . . ?
N6 C38 C39 C41 -104.6(6) . . . . ?
C37 C38 C39 C41 76.1(6) . . . . ?
N6 C38 C39 C40A 119.7(6) . . . . ?
C37 C38 C39 C40A -59.6(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         1.022
_refine_diff_density_min         -1.090
_refine_diff_density_rms         0.096