Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 #========================================================= data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 loop_ _publ_author_name 'Andreas Danopoulos' 'Graham R. Eastham' 'Michael B. Hursthouse' 'Arran A. D. Tulloch' ; S.Winston ; _publ_contact_author_name 'Dr Andreas Danopoulos' _publ_contact_author_address ; Chemistry University of Southampton Highfield Southampton Hampshire SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email AD1@SOTON.AC.UK _publ_section_title ; Chelating and 'pincer' dicarbene complexes of palladium; synthesis and structural studies ; _publ_section_references ; ENTER OTHER REFERENCES WinGX - L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838 ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565. PLATON/PLUTON - (a) A. L. Spek, Acta Crystallogr., Sect A 1990, 46, C34. (b) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, A. L. Spek, 1998. ; data_Compound4d _database_code_CSD 194842 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01sot044 _chemical_melting_point ? _chemical_formula_moiety 'C31 H33 Cl2 N5 Pd' _chemical_formula_sum 'C31 H33 Cl2 N5 Pd' _chemical_formula_weight 652.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.823(2) _cell_length_b 20.571(4) _cell_length_c 19.286(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.86(3) _cell_angle_gamma 90.00 _cell_volume 4293.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37158 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8934 _exptl_absorpt_correction_T_max 0.9553 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and omega scans to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30684 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9674 _reflns_number_gt 5800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1588P)^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 9674 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2511 _refine_ls_wR_factor_gt 0.2334 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.013 _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 C1 C 0.2067(5) 0.2037(3) 0.7866(3) 0.0339(14) Uani 1 1 d . . . C2 C 0.1836(6) 0.2667(3) 0.7647(4) 0.0433(16) Uani 1 1 d . . . H2 H 0.1405 0.2962 0.7934 0.052 Uiso 1 1 calc R . . C3 C 0.2245(7) 0.2859(3) 0.7000(4) 0.0507(19) Uani 1 1 d . . . H3 H 0.2118 0.3294 0.6849 0.061 Uiso 1 1 calc R . . C4 C 0.2849(6) 0.2413(3) 0.6566(4) 0.0466(17) Uani 1 1 d . . . H4 H 0.3128 0.2531 0.6118 0.056 Uiso 1 1 calc R . . C5 C 0.3013(6) 0.1783(3) 0.6835(4) 0.0396(15) Uani 1 1 d . . . C6 C 0.3687(6) 0.1289(3) 0.6388(4) 0.0418(15) Uani 1 1 d . . . H6A H 0.3123 0.0927 0.6263 0.050 Uiso 1 1 calc R . . H6B H 0.3961 0.1498 0.5954 0.050 Uiso 1 1 calc R . . C7 C 0.4597(6) 0.0719(3) 0.7381(3) 0.0304(13) Uani 1 1 d . . . C8 C 0.5984(6) 0.1104(4) 0.6615(4) 0.0519(19) Uani 1 1 d . . . H8 H 0.6315 0.1304 0.6215 0.062 Uiso 1 1 calc R . . C9 C 0.6620(6) 0.0834(4) 0.7131(4) 0.0480(17) Uani 1 1 d . . . H9 H 0.7495 0.0814 0.7173 0.058 Uiso 1 1 calc R . . C10 C 0.6118(5) 0.0298(3) 0.8255(3) 0.0277(12) Uani 1 1 d . . . C11 C 0.6037(6) 0.0660(3) 0.8863(4) 0.0374(14) Uani 1 1 d . . . C12 C 0.5661(8) 0.1347(3) 0.8855(4) 0.057(2) Uani 1 1 d . . . H12A H 0.5193 0.1444 0.9274 0.085 Uiso 1 1 calc R . . H12B H 0.5141 0.1431 0.8444 0.085 Uiso 1 1 calc R . . H12C H 0.6397 0.1624 0.8842 0.085 Uiso 1 1 calc R . . C13 C 0.6362(6) 0.0326(3) 0.9491(3) 0.0357(14) Uani 1 1 d . . . H13 H 0.6281 0.0545 0.9922 0.043 Uiso 1 1 calc R . . C14 C 0.6796(6) -0.0314(4) 0.9484(4) 0.0436(16) Uani 1 1 d . . . C15 C 0.7169(8) -0.0639(4) 1.0143(5) 0.063(2) Uani 1 1 d . . . H15A H 0.7803 -0.0378 1.0381 0.094 Uiso 1 1 calc R . . H15B H 0.7502 -0.1071 1.0041 0.094 Uiso 1 1 calc R . . H15C H 0.6448 -0.0683 1.0441 0.094 Uiso 1 1 calc R . . C16 C 0.6884(6) -0.0632(3) 0.8869(4) 0.0425(16) Uani 1 1 d . . . H16 H 0.7188 -0.1065 0.8864 0.051 Uiso 1 1 calc R . . C17 C 0.6544(5) -0.0343(3) 0.8258(4) 0.0394(15) Uani 1 1 d . . . C18 C 0.6528(7) -0.0733(3) 0.7568(4) 0.0526(19) Uani 1 1 d . . . H18A H 0.5678 -0.0862 0.7452 0.079 Uiso 1 1 calc R . . H18B H 0.7044 -0.1122 0.7620 0.079 Uiso 1 1 calc R . . H18C H 0.6850 -0.0460 0.7195 0.079 Uiso 1 1 calc R . . C19 C 0.1715(6) 0.1816(3) 0.8577(3) 0.0353(14) Uani 1 1 d . . . H19A H 0.2473 0.1701 0.8843 0.042 Uiso 1 1 calc R . . H19B H 0.1309 0.2180 0.8821 0.042 Uiso 1 1 calc R . . C20 C 0.1248(5) 0.0700(2) 0.8250(3) 0.0316(13) Uani 1 1 d . . . C21 C -0.0266(6) 0.1214(3) 0.8843(4) 0.0429(16) Uani 1 1 d . . . H21 H -0.0706 0.1539 0.9087 0.051 Uiso 1 1 calc R . . C22 C -0.0647(6) 0.0610(3) 0.8696(4) 0.0426(16) Uani 1 1 d . . . H22 H -0.1414 0.0424 0.8823 0.051 Uiso 1 1 calc R . . C23 C 0.0140(5) -0.0331(3) 0.8048(4) 0.0386(16) Uani 1 1 d . . . C24 C 0.0007(6) -0.0430(3) 0.7337(4) 0.0427(16) Uani 1 1 d . . . C25 C 0.0101(7) 0.0123(4) 0.6828(4) 0.0547(19) Uani 1 1 d . . . H25A H -0.0315 0.0507 0.7014 0.082 Uiso 1 1 calc R . . H25B H -0.0295 -0.0002 0.6387 0.082 Uiso 1 1 calc R . . H25C H 0.0973 0.0224 0.6750 0.082 Uiso 1 1 calc R . . C26 C -0.0195(6) -0.1049(3) 0.7078(4) 0.0506(18) Uani 1 1 d . . . H26 H -0.0289 -0.1111 0.6592 0.061 Uiso 1 1 calc R . . C27 C -0.0260(6) -0.1571(3) 0.7510(5) 0.052(2) Uani 1 1 d . . . C28 C -0.0448(7) -0.2244(4) 0.7255(5) 0.066(2) Uani 1 1 d . . . H28A H 0.0349 -0.2429 0.7122 0.099 Uiso 1 1 calc R . . H28B H -0.1008 -0.2238 0.6851 0.099 Uiso 1 1 calc R . . H28C H -0.0808 -0.2509 0.7622 0.099 Uiso 1 1 calc R . . C29 C -0.0119(6) -0.1476(3) 0.8255(4) 0.0486(19) Uani 1 1 d . . . H29 H -0.0185 -0.1840 0.8556 0.058 Uiso 1 1 calc R . . C30 C 0.0103(6) -0.0876(3) 0.8532(4) 0.0395(15) Uani 1 1 d . . . C31 C 0.0319(7) -0.0785(3) 0.9281(4) 0.0455(17) Uani 1 1 d . . . H31A H -0.0094 -0.1132 0.9536 0.068 Uiso 1 1 calc R . . H31B H -0.0014 -0.0363 0.9423 0.068 Uiso 1 1 calc R . . H31C H 0.1208 -0.0798 0.9382 0.068 Uiso 1 1 calc R . . N1 N 0.2629(4) 0.1602(2) 0.7462(3) 0.0259(10) Uani 1 1 d . . . N2 N 0.4744(5) 0.1041(3) 0.6771(3) 0.0410(13) Uani 1 1 d . . . N3 N 0.5783(4) 0.0586(2) 0.7598(3) 0.0355(12) Uani 1 1 d . . . N4 N 0.0903(5) 0.1269(2) 0.8565(3) 0.0392(13) Uani 1 1 d . . . N5 N 0.0266(4) 0.0309(2) 0.8333(3) 0.0336(12) Uani 1 1 d . . . Cl1 Cl 0.32693(13) -0.03745(7) 0.82005(9) 0.0400(4) Uani 1 1 d . . . Pd1 Pd 0.29317(4) 0.06622(2) 0.78117(2) 0.02926(19) Uani 1 1 d . . . Cl2A Cl 0.5966(13) 0.2240(6) 0.5215(8) 0.007(3) Uiso 0.20 1 d P . . Cl2B Cl 0.5805(8) 0.2334(4) 0.5251(4) 0.0080(16) Uani 0.30 1 d P . . Cl2C Cl 0.1800(3) 0.42896(11) 0.85572(14) 0.0131(5) Uani 0.40 1 d P . . Cl2D Cl 0.212(2) 0.3970(11) 0.9282(12) 0.016(4) Uiso 0.05 1 d P . . Cl2E Cl 0.165(3) 0.4235(12) 0.9412(14) 0.025(5) Uiso 0.05 1 d P . . 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 C1 0.027(3) 0.025(3) 0.050(4) -0.003(3) -0.004(3) -0.005(2) C2 0.037(4) 0.035(3) 0.058(5) 0.003(3) -0.003(3) 0.002(3) C3 0.064(5) 0.024(3) 0.064(5) 0.024(3) -0.008(4) -0.003(3) C4 0.045(4) 0.040(4) 0.054(5) 0.015(3) -0.012(3) -0.007(3) C5 0.029(3) 0.047(4) 0.042(4) 0.004(3) -0.011(3) 0.007(3) C6 0.041(4) 0.050(4) 0.035(4) 0.010(3) 0.004(3) 0.002(3) C7 0.037(3) 0.032(3) 0.023(3) -0.001(2) 0.008(2) -0.002(2) C8 0.031(4) 0.092(6) 0.033(4) 0.001(4) 0.009(3) -0.009(3) C9 0.023(3) 0.075(5) 0.047(4) 0.006(4) 0.006(3) 0.004(3) C10 0.017(3) 0.037(3) 0.029(3) -0.001(2) -0.002(2) 0.004(2) C11 0.031(3) 0.036(3) 0.045(4) 0.003(3) 0.009(3) -0.005(2) C12 0.091(6) 0.038(4) 0.042(4) 0.001(3) 0.011(4) 0.017(4) C13 0.040(3) 0.038(3) 0.029(3) 0.001(3) 0.005(3) -0.005(3) C14 0.026(3) 0.061(4) 0.043(4) 0.009(3) 0.004(3) 0.001(3) C15 0.045(4) 0.086(6) 0.057(5) 0.033(4) 0.002(4) 0.016(4) C16 0.032(3) 0.026(3) 0.069(5) 0.000(3) 0.004(3) 0.004(2) C17 0.023(3) 0.036(3) 0.059(5) -0.002(3) -0.007(3) 0.000(2) C18 0.048(4) 0.054(4) 0.056(5) -0.019(3) -0.007(4) 0.022(3) C19 0.031(3) 0.032(3) 0.043(4) -0.001(3) 0.005(3) 0.004(2) C20 0.026(3) 0.025(3) 0.044(4) 0.010(2) 0.004(3) -0.001(2) C21 0.040(4) 0.029(3) 0.060(5) 0.006(3) 0.019(3) 0.008(3) C22 0.027(3) 0.043(4) 0.058(5) 0.001(3) 0.017(3) -0.007(3) C23 0.028(3) 0.019(3) 0.069(5) 0.003(3) 0.015(3) 0.002(2) C24 0.022(3) 0.043(4) 0.062(5) 0.002(3) -0.013(3) 0.001(3) C25 0.051(5) 0.059(5) 0.054(5) 0.003(4) -0.011(4) -0.010(3) C26 0.031(4) 0.050(4) 0.071(5) -0.005(4) -0.019(3) 0.009(3) C27 0.033(4) 0.042(4) 0.081(6) -0.011(4) -0.015(4) 0.001(3) C28 0.041(4) 0.046(4) 0.112(8) -0.015(4) -0.015(4) -0.004(3) C29 0.023(3) 0.040(4) 0.083(6) 0.005(3) 0.002(3) 0.003(3) C30 0.035(3) 0.030(3) 0.053(4) 0.006(3) 0.004(3) 0.002(2) C31 0.047(4) 0.035(3) 0.054(5) 0.016(3) 0.012(3) 0.001(3) N1 0.017(2) 0.025(2) 0.036(3) 0.0039(19) 0.001(2) -0.0035(17) N2 0.028(3) 0.059(3) 0.036(3) 0.001(3) -0.002(2) -0.007(2) N3 0.024(3) 0.046(3) 0.037(3) 0.002(2) 0.008(2) 0.002(2) N4 0.027(3) 0.038(3) 0.053(4) -0.004(2) 0.004(2) 0.008(2) N5 0.021(2) 0.023(2) 0.057(4) 0.002(2) 0.005(2) 0.0032(18) Cl1 0.0296(8) 0.0270(7) 0.0637(11) 0.0041(7) 0.0077(7) 0.0032(6) Pd1 0.0222(3) 0.0248(3) 0.0409(3) 0.00059(18) 0.00504(19) 0.00031(16) Cl2B 0.009(3) 0.011(3) 0.003(3) 0.000(2) -0.0002(19) 0.007(2) Cl2C 0.0224(14) 0.0058(11) 0.0109(13) 0.0031(9) -0.0035(11) -0.0079(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 C1 N1 1.339(8) . ? C1 C2 1.385(9) . ? C1 C19 1.500(9) . ? C2 C3 1.387(11) . ? C3 C4 1.410(11) . ? C4 C5 1.407(9) . ? C5 N1 1.338(8) . ? C5 C6 1.526(9) . ? C6 N2 1.446(8) . ? C7 N2 1.363(8) . ? C7 N3 1.371(8) . ? C7 Pd1 1.999(6) . ? C8 C9 1.322(10) . ? C8 N2 1.386(8) . ? C9 N3 1.385(9) . ? C10 C11 1.393(9) . ? C10 C17 1.397(8) . ? C10 N3 1.441(8) . ? C11 C13 1.432(9) . ? C11 C12 1.471(9) . ? C13 C14 1.399(9) . ? C14 C16 1.360(10) . ? C14 C15 1.487(10) . ? C16 C17 1.365(10) . ? C17 C18 1.554(10) . ? C19 N4 1.427(8) . ? C20 N5 1.345(7) . ? C20 N4 1.374(8) . ? C20 Pd1 2.021(6) . ? C21 C22 1.338(9) . ? C21 N4 1.385(8) . ? C22 N5 1.369(8) . ? C23 C24 1.392(10) . ? C23 N5 1.432(8) . ? C23 C30 1.461(9) . ? C24 C26 1.385(10) . ? C24 C25 1.507(10) . ? C26 C27 1.360(11) . ? C27 C29 1.456(12) . ? C27 C28 1.482(10) . ? C29 C30 1.365(10) . ? C30 C31 1.471(10) . ? N1 Pd1 2.071(4) . ? Cl1 Pd1 2.2880(15) . ? Cl2C Cl2D 1.58(2) . ? Cl2C Cl2E 1.66(3) . ? Cl2D Cl2E 0.79(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 N1 C1 C2 122.0(6) . . ? N1 C1 C19 116.9(5) . . ? C2 C1 C19 121.1(6) . . ? C1 C2 C3 118.9(6) . . ? C2 C3 C4 120.4(6) . . ? C5 C4 C3 116.0(7) . . ? N1 C5 C4 123.4(6) . . ? N1 C5 C6 118.9(5) . . ? C4 C5 C6 117.6(6) . . ? N2 C6 C5 109.1(5) . . ? N2 C7 N3 103.8(5) . . ? N2 C7 Pd1 120.3(4) . . ? N3 C7 Pd1 135.1(4) . . ? C9 C8 N2 107.0(6) . . ? C8 C9 N3 107.8(6) . . ? C11 C10 C17 121.7(6) . . ? C11 C10 N3 120.2(5) . . ? C17 C10 N3 118.1(5) . . ? C10 C11 C13 116.0(5) . . ? C10 C11 C12 121.7(6) . . ? C13 C11 C12 122.2(6) . . ? C14 C13 C11 121.4(6) . . ? C16 C14 C13 119.3(6) . . ? C16 C14 C15 120.6(7) . . ? C13 C14 C15 120.2(7) . . ? C14 C16 C17 121.5(6) . . ? C16 C17 C10 120.0(6) . . ? C16 C17 C18 121.0(6) . . ? C10 C17 C18 118.9(6) . . ? N4 C19 C1 112.8(5) . . ? N5 C20 N4 103.7(5) . . ? N5 C20 Pd1 138.2(4) . . ? N4 C20 Pd1 118.1(4) . . ? C22 C21 N4 105.9(5) . . ? C21 C22 N5 107.8(5) . . ? C24 C23 N5 121.3(6) . . ? C24 C23 C30 121.0(6) . . ? N5 C23 C30 117.7(6) . . ? C26 C24 C23 120.1(7) . . ? C26 C24 C25 118.2(7) . . ? C23 C24 C25 121.6(6) . . ? C27 C26 C24 121.0(8) . . ? C26 C27 C29 119.5(6) . . ? C26 C27 C28 122.8(8) . . ? C29 C27 C28 117.7(7) . . ? C30 C29 C27 121.5(7) . . ? C29 C30 C23 116.8(7) . . ? C29 C30 C31 121.6(6) . . ? C23 C30 C31 121.6(6) . . ? C5 N1 C1 119.4(5) . . ? C5 N1 Pd1 120.3(4) . . ? C1 N1 Pd1 120.4(4) . . ? C7 N2 C8 111.0(6) . . ? C7 N2 C6 120.8(5) . . ? C8 N2 C6 128.2(6) . . ? C7 N3 C9 110.3(5) . . ? C7 N3 C10 124.9(5) . . ? C9 N3 C10 124.5(5) . . ? C20 N4 C21 111.0(5) . . ? C20 N4 C19 120.5(5) . . ? C21 N4 C19 128.5(5) . . ? C20 N5 C22 111.6(5) . . ? C20 N5 C23 125.1(5) . . ? C22 N5 C23 123.2(5) . . ? C7 Pd1 C20 174.5(2) . . ? C7 Pd1 N1 87.1(2) . . ? C20 Pd1 N1 87.76(19) . . ? C7 Pd1 Cl1 92.85(16) . . ? C20 Pd1 Cl1 92.27(15) . . ? N1 Pd1 Cl1 179.82(15) . . ? Cl2D Cl2C Cl2E 28.0(10) . . ? Cl2E Cl2D Cl2C 82(3) . . ? Cl2D Cl2E Cl2C 70(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.897 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.180 #==END data_Compound5a _database_code_CSD 194843 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01SW048 _chemical_melting_point ? _chemical_formula_moiety 'C42 H49 Br N4 O Pd' _chemical_formula_sum 'C42 H49 Br N4 O Pd' _chemical_formula_weight 812.16 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0839(2) _cell_length_b 15.3863(3) _cell_length_c 20.9393(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.3890(10) _cell_angle_gamma 90.00 _cell_volume 3893.08(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13704 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.540 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8613 _exptl_absorpt_correction_T_max 0.9410 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24463 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8755 _reflns_number_gt 6974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0526P)^2^+5.0616P] 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 8755 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.8510(3) 0.2234(2) 0.15606(15) 0.0218(7) Uani 1 1 d . . . C2 C 0.8652(3) 0.3106(2) 0.13751(16) 0.0230(7) Uani 1 1 d . . . C3 C 0.8613(3) 0.3355(2) 0.07271(17) 0.0286(8) Uani 1 1 d . . . C4 C 0.8432(3) 0.2712(3) 0.02712(17) 0.0329(8) Uani 1 1 d . . . H4 H 0.8409 0.2872 -0.0167 0.040 Uiso 1 1 calc R . . C5 C 0.8283(3) 0.1850(3) 0.04326(17) 0.0305(8) Uani 1 1 d . . . C6 C 0.8875(3) 0.3780(2) 0.18886(16) 0.0256(7) Uani 1 1 d . . . H6A H 0.8975 0.4358 0.1690 0.031 Uiso 1 1 calc R . . H6B H 0.8237 0.3812 0.2181 0.031 Uiso 1 1 calc R . . C7 C 1.0014(3) 0.2739(2) 0.25071(15) 0.0207(7) Uani 1 1 d . . . C8 C 1.0815(3) 0.4046(2) 0.23107(16) 0.0247(7) Uani 1 1 d . . . H8 H 1.0907 0.4628 0.2169 0.030 Uiso 1 1 calc R . . C9 C 1.1574(3) 0.3549(2) 0.26123(16) 0.0245(7) Uani 1 1 d . . . H9 H 1.2310 0.3712 0.2721 0.029 Uiso 1 1 calc R . . C10 C 1.1707(3) 0.2035(2) 0.29940(17) 0.0235(7) Uani 1 1 d . . . C11 C 1.2024(3) 0.2065(2) 0.36348(17) 0.0267(7) Uani 1 1 d . . . C12 C 1.2738(3) 0.1414(3) 0.38583(19) 0.0325(8) Uani 1 1 d . . . H12 H 1.2985 0.1424 0.4290 0.039 Uiso 1 1 calc R . . C13 C 1.3089(3) 0.0756(3) 0.3457(2) 0.0386(10) Uani 1 1 d . . . H13 H 1.3580 0.0321 0.3613 0.046 Uiso 1 1 calc R . . C14 C 1.2726(3) 0.0729(2) 0.2831(2) 0.0371(9) Uani 1 1 d . . . H14 H 1.2957 0.0264 0.2565 0.044 Uiso 1 1 calc R . . C15 C 1.2028(3) 0.1370(2) 0.25788(18) 0.0292(8) Uani 1 1 d . . . C16 C 1.1619(3) 0.2763(3) 0.40909(18) 0.0364(9) Uani 1 1 d . . . H16 H 1.1017 0.3100 0.3874 0.044 Uiso 1 1 calc R . . C17 C 1.2538(5) 0.3385(3) 0.4270(3) 0.0633(15) Uani 1 1 d . . . H17A H 1.3127 0.3068 0.4494 0.095 Uiso 1 1 calc R . . H17B H 1.2246 0.3840 0.4550 0.095 Uiso 1 1 calc R . . H17C H 1.2837 0.3652 0.3883 0.095 Uiso 1 1 calc R . . C18 C 1.1152(4) 0.2371(3) 0.4707(2) 0.0516(12) Uani 1 1 d . . . H18A H 1.1753 0.2101 0.4953 0.077 Uiso 1 1 calc R . . H18B H 1.0596 0.1931 0.4598 0.077 Uiso 1 1 calc R . . H18C H 1.0810 0.2831 0.4962 0.077 Uiso 1 1 calc R . . C19 C 1.1685(4) 0.1348(3) 0.18783(19) 0.0383(9) Uani 1 1 d . . . H19 H 1.1067 0.1773 0.1818 0.046 Uiso 1 1 calc R . . C20 C 1.2629(7) 0.1632(7) 0.1460(3) 0.144(5) Uani 1 1 d . . . H20A H 1.3244 0.1221 0.1506 0.217 Uiso 1 1 calc R . . H20B H 1.2875 0.2213 0.1589 0.217 Uiso 1 1 calc R . . H20C H 1.2381 0.1646 0.1014 0.217 Uiso 1 1 calc R . . C21 C 1.1275(6) 0.0473(4) 0.1667(3) 0.0723(17) Uani 1 1 d . . . H21A H 1.0989 0.0512 0.1229 0.108 Uiso 1 1 calc R . . H21B H 1.0683 0.0280 0.1952 0.108 Uiso 1 1 calc R . . H21C H 1.1886 0.0054 0.1683 0.108 Uiso 1 1 calc R . . C22 C 0.8301(3) 0.1613(2) 0.10828(16) 0.0250(7) Uani 1 1 d . . . C23 C 0.8082(3) 0.0679(2) 0.12696(16) 0.0285(8) Uani 1 1 d . . . H23A H 0.7777 0.0361 0.0897 0.034 Uiso 1 1 calc R . . H23B H 0.8788 0.0398 0.1395 0.034 Uiso 1 1 calc R . . C24 C 0.7473(3) 0.1047(2) 0.23570(15) 0.0202(6) Uani 1 1 d . . . C25 C 0.6308(3) 0.0167(2) 0.18014(17) 0.0291(8) Uani 1 1 d . . . H25 H 0.6015 -0.0178 0.1464 0.035 Uiso 1 1 calc R . . C26 C 0.5847(3) 0.0313(2) 0.23713(16) 0.0253(7) Uani 1 1 d . . . H26 H 0.5158 0.0093 0.2515 0.030 Uiso 1 1 calc R . . C27 C 0.6337(3) 0.1133(2) 0.33548(15) 0.0218(7) Uani 1 1 d . . . C28 C 0.6389(3) 0.0515(2) 0.38500(16) 0.0252(7) Uani 1 1 d . . . C29 C 0.6145(3) 0.0804(2) 0.44651(17) 0.0318(8) Uani 1 1 d . . . H29 H 0.6155 0.0403 0.4810 0.038 Uiso 1 1 calc R . . C30 C 0.5888(3) 0.1669(3) 0.45810(18) 0.0351(9) Uani 1 1 d . . . H30 H 0.5746 0.1856 0.5005 0.042 Uiso 1 1 calc R . . C31 C 0.5836(3) 0.2260(2) 0.40835(18) 0.0337(8) Uani 1 1 d . . . H31 H 0.5654 0.2850 0.4168 0.040 Uiso 1 1 calc R . . C32 C 0.6049(3) 0.1997(2) 0.34593(17) 0.0260(7) Uani 1 1 d . . . C33 C 0.5898(3) 0.2642(2) 0.29143(18) 0.0313(8) Uani 1 1 d . . . H33 H 0.6270 0.2400 0.2528 0.038 Uiso 1 1 calc R . . C34 C 0.4666(4) 0.2744(4) 0.2761(3) 0.0625(15) Uani 1 1 d . . . H34A H 0.4273 0.2930 0.3145 0.094 Uiso 1 1 calc R . . H34B H 0.4366 0.2187 0.2613 0.094 Uiso 1 1 calc R . . H34C H 0.4569 0.3182 0.2425 0.094 Uiso 1 1 calc R . . C35 C 0.6399(4) 0.3520(3) 0.3057(2) 0.0483(11) Uani 1 1 d . . . H35A H 0.6019 0.3783 0.3421 0.072 Uiso 1 1 calc R . . H35B H 0.6316 0.3898 0.2683 0.072 Uiso 1 1 calc R . . H35C H 0.7186 0.3451 0.3159 0.072 Uiso 1 1 calc R . . C36 C 0.6678(3) -0.0431(2) 0.37480(17) 0.0299(8) Uani 1 1 d . . . H36 H 0.6890 -0.0506 0.3290 0.036 Uiso 1 1 calc R . . C37 C 0.5665(4) -0.1011(3) 0.3874(2) 0.0467(11) Uani 1 1 d . . . H37A H 0.5423 -0.0932 0.4316 0.070 Uiso 1 1 calc R . . H37B H 0.5865 -0.1621 0.3805 0.070 Uiso 1 1 calc R . . H37C H 0.5063 -0.0849 0.3582 0.070 Uiso 1 1 calc R . . C38 C 0.7658(4) -0.0714(3) 0.41601(19) 0.0408(10) Uani 1 1 d . . . H38A H 0.8280 -0.0317 0.4091 0.061 Uiso 1 1 calc R . . H38B H 0.7877 -0.1306 0.4043 0.061 Uiso 1 1 calc R . . H38C H 0.7447 -0.0700 0.4611 0.061 Uiso 1 1 calc R . . C39 C 0.8141(4) 0.1187(3) -0.01016(18) 0.0444(11) Uani 1 1 d . . . H39A H 0.8224 0.1476 -0.0515 0.067 Uiso 1 1 calc R . . H39B H 0.7402 0.0926 -0.0076 0.067 Uiso 1 1 calc R . . H39C H 0.8703 0.0732 -0.0057 0.067 Uiso 1 1 calc R . . C40 C 0.8802(4) 0.4281(3) 0.05123(19) 0.0379(9) Uani 1 1 d . . . H40A H 0.8758 0.4311 0.0045 0.057 Uiso 1 1 calc R . . H40B H 0.9535 0.4475 0.0655 0.057 Uiso 1 1 calc R . . H40C H 0.8234 0.4658 0.0697 0.057 Uiso 1 1 calc R . . N1 N 1.1078(2) 0.27520(17) 0.27341(13) 0.0202(6) Uani 1 1 d . . . N2 N 0.9881(2) 0.35403(18) 0.22499(12) 0.0208(6) Uani 1 1 d . . . N3 N 0.7300(2) 0.06209(18) 0.18021(13) 0.0234(6) Uani 1 1 d . . . N4 N 0.6561(2) 0.08451(17) 0.27120(13) 0.0205(6) Uani 1 1 d . . . Pd1 Pd 0.877911(19) 0.184579(15) 0.247693(11) 0.01814(8) Uani 1 1 d . . . Br1 Br 0.92203(3) 0.12544(2) 0.356416(15) 0.02743(10) Uani 1 1 d . . . C101 C 0.5081(5) 0.1305(4) 0.0494(3) 0.0660(14) Uiso 1 1 d . . . C99 C 0.4368(16) 0.0543(14) 0.0507(9) 0.254(8) Uiso 1 1 d . . . O1 O 0.5101(16) -0.0194(13) 0.0313(8) 0.341(8) Uiso 1 1 d . . . 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 C1 0.0178(16) 0.0306(18) 0.0172(15) 0.0030(13) 0.0026(12) 0.0003(13) C2 0.0178(16) 0.0288(18) 0.0224(17) 0.0064(13) 0.0015(13) 0.0016(14) C3 0.0254(18) 0.037(2) 0.0236(18) 0.0101(15) 0.0014(14) 0.0037(15) C4 0.0293(19) 0.049(2) 0.0202(17) 0.0085(16) -0.0008(14) -0.0012(17) C5 0.0260(18) 0.044(2) 0.0212(17) 0.0009(15) 0.0003(14) -0.0048(16) C6 0.0231(17) 0.0287(18) 0.0249(17) 0.0082(14) -0.0008(13) 0.0047(14) C7 0.0226(16) 0.0209(16) 0.0187(15) 0.0011(12) 0.0031(12) 0.0021(13) C8 0.0269(18) 0.0204(16) 0.0269(18) 0.0036(13) 0.0013(14) -0.0023(14) C9 0.0237(17) 0.0227(17) 0.0272(18) 0.0021(13) -0.0010(14) -0.0054(14) C10 0.0160(16) 0.0215(16) 0.0329(18) 0.0067(14) 0.0017(13) -0.0017(13) C11 0.0204(17) 0.0265(18) 0.0333(19) 0.0069(14) 0.0009(14) 0.0000(14) C12 0.0242(18) 0.036(2) 0.038(2) 0.0158(17) -0.0020(15) 0.0008(16) C13 0.0230(19) 0.029(2) 0.064(3) 0.0166(18) 0.0022(18) 0.0029(16) C14 0.029(2) 0.0243(19) 0.058(3) 0.0012(17) 0.0079(18) 0.0034(16) C15 0.0257(18) 0.0230(18) 0.039(2) 0.0012(15) 0.0018(15) 0.0003(15) C16 0.042(2) 0.040(2) 0.0273(19) 0.0049(16) -0.0033(16) 0.0091(18) C17 0.089(4) 0.043(3) 0.059(3) -0.006(2) 0.022(3) -0.021(3) C18 0.051(3) 0.070(3) 0.034(2) -0.005(2) 0.0051(19) -0.011(2) C19 0.040(2) 0.035(2) 0.040(2) -0.0074(17) 0.0042(18) 0.0081(18) C20 0.156(8) 0.237(11) 0.041(3) 0.023(5) -0.002(4) -0.141(8) C21 0.107(5) 0.056(3) 0.054(3) -0.006(2) -0.009(3) -0.038(3) C22 0.0232(17) 0.0315(18) 0.0204(17) 0.0003(14) 0.0017(13) -0.0036(14) C23 0.0306(19) 0.033(2) 0.0214(17) -0.0054(14) 0.0080(14) -0.0032(15) C24 0.0234(16) 0.0209(16) 0.0162(15) 0.0015(12) 0.0020(12) 0.0008(13) C25 0.0280(18) 0.0301(19) 0.0290(19) -0.0001(14) -0.0024(14) -0.0050(15) C26 0.0204(16) 0.0273(18) 0.0281(18) 0.0024(14) 0.0002(13) -0.0065(14) C27 0.0192(16) 0.0254(17) 0.0208(16) 0.0003(13) 0.0049(12) -0.0039(13) C28 0.0257(17) 0.0253(17) 0.0248(17) 0.0033(13) 0.0061(14) -0.0015(14) C29 0.038(2) 0.034(2) 0.0241(18) 0.0035(15) 0.0121(15) 0.0016(16) C30 0.042(2) 0.038(2) 0.0263(19) -0.0034(15) 0.0128(16) -0.0001(18) C31 0.040(2) 0.0266(19) 0.035(2) -0.0032(15) 0.0134(17) 0.0011(16) C32 0.0234(17) 0.0254(18) 0.0293(18) 0.0009(14) 0.0078(14) -0.0016(14) C33 0.033(2) 0.0241(18) 0.037(2) 0.0037(15) 0.0081(16) 0.0019(15) C34 0.046(3) 0.064(3) 0.077(4) 0.040(3) -0.014(2) -0.015(2) C35 0.056(3) 0.032(2) 0.057(3) 0.009(2) 0.008(2) -0.009(2) C36 0.037(2) 0.0259(18) 0.0269(18) 0.0038(14) 0.0112(15) 0.0011(16) C37 0.052(3) 0.031(2) 0.057(3) 0.0015(19) 0.019(2) -0.004(2) C38 0.058(3) 0.032(2) 0.033(2) 0.0064(16) 0.0025(19) 0.0102(19) C39 0.059(3) 0.056(3) 0.0188(19) -0.0040(17) 0.0036(18) -0.007(2) C40 0.045(2) 0.039(2) 0.029(2) 0.0120(16) 0.0007(17) 0.0041(18) N1 0.0227(14) 0.0178(13) 0.0201(13) 0.0026(10) 0.0014(11) -0.0014(11) N2 0.0222(14) 0.0209(14) 0.0193(13) 0.0030(11) 0.0013(11) 0.0004(11) N3 0.0238(14) 0.0252(15) 0.0213(14) -0.0028(11) 0.0035(11) -0.0037(12) N4 0.0212(14) 0.0211(14) 0.0192(13) -0.0001(10) 0.0032(11) -0.0021(11) Pd1 0.01878(14) 0.01928(14) 0.01638(13) 0.00123(9) 0.00230(9) -0.00138(9) Br1 0.0307(2) 0.0318(2) 0.01977(17) 0.00445(13) -0.00038(13) -0.00548(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 C1 C22 1.405(5) . ? C1 C2 1.408(5) . ? C1 Pd1 2.033(3) . ? C2 C3 1.410(5) . ? C2 C6 1.516(5) . ? C3 C4 1.391(5) . ? C3 C40 1.512(5) . ? C4 C5 1.381(5) . ? C5 C22 1.409(5) . ? C5 C39 1.523(5) . ? C6 N2 1.474(4) . ? C7 N2 1.354(4) . ? C7 N1 1.368(4) . ? C7 Pd1 2.030(3) . ? C8 C9 1.348(5) . ? C8 N2 1.376(4) . ? C9 N1 1.389(4) . ? C10 C11 1.394(5) . ? C10 C15 1.399(5) . ? C10 N1 1.444(4) . ? C11 C12 1.401(5) . ? C11 C16 1.520(5) . ? C12 C13 1.384(6) . ? C13 C14 1.379(6) . ? C14 C15 1.399(5) . ? C15 C19 1.522(5) . ? C16 C17 1.511(6) . ? C16 C18 1.534(6) . ? C19 C21 1.501(6) . ? C19 C20 1.507(8) . ? C22 C23 1.513(5) . ? C23 N3 1.469(4) . ? C24 N3 1.349(4) . ? C24 N4 1.369(4) . ? C24 Pd1 2.015(3) . ? C25 C26 1.339(5) . ? C25 N3 1.387(4) . ? C26 N4 1.384(4) . ? C27 C32 1.393(5) . ? C27 C28 1.408(5) . ? C27 N4 1.444(4) . ? C28 C29 1.396(5) . ? C28 C36 1.513(5) . ? C29 C30 1.388(6) . ? C30 C31 1.384(5) . ? C31 C32 1.394(5) . ? C32 C33 1.522(5) . ? C33 C35 1.510(6) . ? C33 C34 1.529(6) . ? C36 C38 1.524(5) . ? C36 C37 1.539(5) . ? Pd1 Br1 2.5057(4) . ? C101 C99 1.454(19) . ? C99 O1 1.50(2) . ? C99 O1 1.91(3) 3_655 ? O1 O1 1.46(3) 3_655 ? O1 C99 1.91(3) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 C1 C2 118.3(3) . . ? C22 C1 Pd1 119.9(3) . . ? C2 C1 Pd1 121.4(2) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 C6 118.5(3) . . ? C3 C2 C6 120.1(3) . . ? C4 C3 C2 118.1(3) . . ? C4 C3 C40 119.3(3) . . ? C2 C3 C40 122.6(3) . . ? C5 C4 C3 122.4(3) . . ? C4 C5 C22 118.9(3) . . ? C4 C5 C39 118.6(3) . . ? C22 C5 C39 122.5(3) . . ? N2 C6 C2 109.6(3) . . ? N2 C7 N1 103.5(3) . . ? N2 C7 Pd1 121.2(2) . . ? N1 C7 Pd1 135.2(2) . . ? C9 C8 N2 106.1(3) . . ? C8 C9 N1 107.1(3) . . ? C11 C10 C15 123.2(3) . . ? C11 C10 N1 118.5(3) . . ? C15 C10 N1 118.2(3) . . ? C10 C11 C12 117.5(3) . . ? C10 C11 C16 122.8(3) . . ? C12 C11 C16 119.7(3) . . ? C13 C12 C11 120.7(4) . . ? C14 C13 C12 120.1(3) . . ? C13 C14 C15 121.7(4) . . ? C10 C15 C14 116.7(3) . . ? C10 C15 C19 122.7(3) . . ? C14 C15 C19 120.5(3) . . ? C17 C16 C11 111.4(4) . . ? C17 C16 C18 108.3(4) . . ? C11 C16 C18 111.8(3) . . ? C21 C19 C20 109.8(5) . . ? C21 C19 C15 113.0(4) . . ? C20 C19 C15 110.6(4) . . ? C1 C22 C5 120.9(3) . . ? C1 C22 C23 119.5(3) . . ? C5 C22 C23 119.6(3) . . ? N3 C23 C22 111.6(3) . . ? N3 C24 N4 103.7(3) . . ? N3 C24 Pd1 121.3(2) . . ? N4 C24 Pd1 134.7(2) . . ? C26 C25 N3 106.2(3) . . ? C25 C26 N4 107.3(3) . . ? C32 C27 C28 122.6(3) . . ? C32 C27 N4 119.2(3) . . ? C28 C27 N4 118.2(3) . . ? C29 C28 C27 117.1(3) . . ? C29 C28 C36 119.2(3) . . ? C27 C28 C36 123.7(3) . . ? C30 C29 C28 121.0(3) . . ? C31 C30 C29 120.5(3) . . ? C30 C31 C32 120.4(4) . . ? C27 C32 C31 118.2(3) . . ? C27 C32 C33 122.2(3) . . ? C31 C32 C33 119.4(3) . . ? C35 C33 C32 112.9(3) . . ? C35 C33 C34 109.7(4) . . ? C32 C33 C34 109.7(3) . . ? C28 C36 C38 111.9(3) . . ? C28 C36 C37 110.5(3) . . ? C38 C36 C37 110.7(3) . . ? C7 N1 C9 110.8(3) . . ? C7 N1 C10 127.6(3) . . ? C9 N1 C10 121.2(3) . . ? C7 N2 C8 112.5(3) . . ? C7 N2 C6 121.8(3) . . ? C8 N2 C6 125.4(3) . . ? C24 N3 C25 111.9(3) . . ? C24 N3 C23 121.9(3) . . ? C25 N3 C23 126.2(3) . . ? C24 N4 C26 110.8(3) . . ? C24 N4 C27 126.4(3) . . ? C26 N4 C27 122.8(3) . . ? C24 Pd1 C7 172.86(12) . . ? C24 Pd1 C1 86.64(13) . . ? C7 Pd1 C1 86.75(13) . . ? C24 Pd1 Br1 93.06(9) . . ? C7 Pd1 Br1 93.77(9) . . ? C1 Pd1 Br1 174.59(9) . . ? C101 C99 O1 104.7(15) . . ? C101 C99 O1 90.4(11) . 3_655 ? O1 C99 O1 48.8(12) . 3_655 ? O1 O1 C99 80.8(16) 3_655 . ? O1 O1 C99 50.5(12) 3_655 3_655 ? C99 O1 C99 131.2(12) . 3_655 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.711 _refine_diff_density_min -1.365 _refine_diff_density_rms 0.106 #==END data_compound5c _database_code_CSD 194844 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 01sw049 _chemical_melting_point ? _chemical_formula_moiety 'C118 H145 Br3 N12 O Pd3' _chemical_formula_sum 'C118 H145 Br3 N12 O Pd3' _chemical_formula_weight 2306.39 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' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 '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 16.0118(6) _cell_length_b 16.4652(6) _cell_length_c 23.5036(10) _cell_angle_alpha 110.001(2) _cell_angle_beta 96.4400(10) _cell_angle_gamma 93.111(2) _cell_volume 5757.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 194744 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 30.51 _exptl_crystal_description Plate _exptl_crystal_colour Clear _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9548 _exptl_absorpt_correction_T_max 0.9846 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius KappaCCD Area Detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald Sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75784 _diffrn_reflns_av_R_equivalents 0.2463 _diffrn_reflns_av_sigmaI/netI 0.3523 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.43 _reflns_number_total 25601 _reflns_number_gt 9219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^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 25601 _refine_ls_number_parameters 1234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2882 _refine_ls_R_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.2074 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 C1 C 0.4877(6) 0.1167(6) 0.6719(4) 0.034(2) Uani 1 1 d . . . C2 C 0.6154(6) 0.1777(6) 0.6694(4) 0.036(3) Uani 1 1 d . . . H2 H 0.6743 0.1849 0.6679 0.043 Uiso 1 1 calc R . . C3 C 0.5616(6) 0.2367(6) 0.6717(4) 0.037(3) Uani 1 1 d . . . H3 H 0.5745 0.2941 0.6725 0.045 Uiso 1 1 calc R . . C4 C 0.4063(6) 0.2422(6) 0.6781(5) 0.041(3) Uani 1 1 d . . . H4A H 0.3649 0.2138 0.6409 0.049 Uiso 1 1 calc R . . H4B H 0.4191 0.3036 0.6823 0.049 Uiso 1 1 calc R . . C5 C 0.3693(6) 0.2377(6) 0.7337(4) 0.032(2) Uani 1 1 d . . . C6 C 0.3613(5) 0.1585(6) 0.7440(4) 0.028(2) Uani 1 1 d . . . C7 C 0.3351(5) 0.1593(6) 0.7987(5) 0.036(3) Uani 1 1 d . . . C8 C 0.3114(6) 0.2347(6) 0.8409(4) 0.040(3) Uani 1 1 d . . . H8 H 0.2923 0.2332 0.8775 0.048 Uiso 1 1 calc R . . C9 C 0.3160(6) 0.3116(7) 0.8289(5) 0.043(3) Uani 1 1 d . . . H9 H 0.2984 0.3629 0.8564 0.052 Uiso 1 1 calc R . . C10 C 0.3465(6) 0.3127(6) 0.7764(5) 0.040(3) Uani 1 1 d . . . H10 H 0.3520 0.3659 0.7691 0.048 Uiso 1 1 calc R . . C11 C 0.3273(6) 0.0748(6) 0.8104(4) 0.042(3) Uani 1 1 d . . . H11A H 0.3827 0.0509 0.8105 0.050 Uiso 1 1 calc R . . H11B H 0.3086 0.0846 0.8508 0.050 Uiso 1 1 calc R . . C12 C 0.1868(6) -0.0149(6) 0.7675(4) 0.036(2) Uani 1 1 d . . . H12 H 0.1645 -0.0086 0.8044 0.043 Uiso 1 1 calc R . . C13 C 0.1463(6) -0.0543(6) 0.7092(4) 0.034(2) Uani 1 1 d . . . H13 H 0.0894 -0.0796 0.6977 0.041 Uiso 1 1 calc R . . C14 C 0.2774(6) -0.0049(6) 0.7023(4) 0.034(2) Uani 1 1 d . . . C15 C 0.1767(5) -0.0797(6) 0.6049(4) 0.032(2) Uani 1 1 d . . . C16 C 0.1740(6) -0.1678(6) 0.5709(4) 0.031(2) Uani 1 1 d . . . C17 C 0.1392(6) -0.1938(7) 0.5103(5) 0.048(3) Uani 1 1 d . . . H17 H 0.1373 -0.2533 0.4856 0.057 Uiso 1 1 calc R . . C18 C 0.1072(6) -0.1369(7) 0.4845(5) 0.046(3) Uani 1 1 d . . . H18 H 0.0825 -0.1571 0.4428 0.055 Uiso 1 1 calc R . . C19 C 0.1111(6) -0.0503(7) 0.5195(5) 0.040(3) Uani 1 1 d . . . H19 H 0.0892 -0.0112 0.5012 0.048 Uiso 1 1 calc R . . C20 C 0.1458(6) -0.0182(6) 0.5804(5) 0.034(2) Uani 1 1 d . . . C21 C 0.1482(6) 0.0768(6) 0.6179(5) 0.040(3) Uani 1 1 d . . . H21 H 0.1901 0.0888 0.6555 0.048 Uiso 1 1 calc R . . C22 C 0.0612(7) 0.0972(7) 0.6389(6) 0.074(4) Uani 1 1 d . . . H22A H 0.0432 0.0566 0.6585 0.110 Uiso 1 1 calc R . . H22B H 0.0197 0.0910 0.6033 0.110 Uiso 1 1 calc R . . H22C H 0.0654 0.1568 0.6681 0.110 Uiso 1 1 calc R . . C23 C 0.1746(8) 0.1356(7) 0.5864(5) 0.067(4) Uani 1 1 d . . . H23A H 0.2321 0.1262 0.5768 0.101 Uiso 1 1 calc R . . H23B H 0.1733 0.1960 0.6130 0.101 Uiso 1 1 calc R . . H23C H 0.1359 0.1237 0.5485 0.101 Uiso 1 1 calc R . . C24 C 0.2038(6) -0.2342(6) 0.5984(4) 0.039(3) Uani 1 1 d . . . H24 H 0.2403 -0.2016 0.6381 0.047 Uiso 1 1 calc R . . C25 C 0.1303(7) -0.2832(7) 0.6125(5) 0.057(3) Uani 1 1 d . . . H25A H 0.1520 -0.3232 0.6320 0.086 Uiso 1 1 calc R . . H25B H 0.0932 -0.3162 0.5745 0.086 Uiso 1 1 calc R . . H25C H 0.0983 -0.2418 0.6402 0.086 Uiso 1 1 calc R . . C26 C 0.2575(6) -0.2973(7) 0.5581(5) 0.050(3) Uani 1 1 d . . . H26A H 0.2216 -0.3364 0.5213 0.076 Uiso 1 1 calc R . . H26B H 0.2842 -0.3314 0.5807 0.076 Uiso 1 1 calc R . . H26C H 0.3013 -0.2647 0.5463 0.076 Uiso 1 1 calc R . . C27 C 0.6025(5) 0.0212(6) 0.6625(4) 0.027(2) Uani 1 1 d . . . C28 C 0.6094(6) -0.0075(6) 0.7121(5) 0.038(3) Uani 1 1 d . . . C29 C 0.6377(6) -0.0898(7) 0.7027(5) 0.043(3) Uani 1 1 d . . . H29 H 0.6429 -0.1116 0.7354 0.052 Uiso 1 1 calc R . . C30 C 0.6582(6) -0.1393(7) 0.6464(5) 0.043(3) Uani 1 1 d . . . H30 H 0.6731 -0.1966 0.6396 0.052 Uiso 1 1 calc R . . C31 C 0.6568(6) -0.1054(6) 0.6001(5) 0.040(3) Uani 1 1 d . . . H31 H 0.6763 -0.1380 0.5631 0.048 Uiso 1 1 calc R . . C32 C 0.6278(6) -0.0249(6) 0.6059(4) 0.031(2) Uani 1 1 d . . . C33 C 0.6242(6) 0.0083(6) 0.5533(4) 0.031(2) Uani 1 1 d . . . H33 H 0.5885 0.0580 0.5624 0.037 Uiso 1 1 calc R . . C34 C 0.5849(6) -0.0599(6) 0.4927(4) 0.042(3) Uani 1 1 d . . . H34A H 0.6228 -0.1056 0.4799 0.063 Uiso 1 1 calc R . . H34B H 0.5759 -0.0328 0.4617 0.063 Uiso 1 1 calc R . . H34C H 0.5306 -0.0854 0.4976 0.063 Uiso 1 1 calc R . . C35 C 0.7133(6) 0.0426(7) 0.5474(5) 0.052(3) Uani 1 1 d . . . H35A H 0.7368 0.0897 0.5855 0.078 Uiso 1 1 calc R . . H35B H 0.7097 0.0646 0.5134 0.078 Uiso 1 1 calc R . . H35C H 0.7500 -0.0046 0.5395 0.078 Uiso 1 1 calc R . . C36 C 0.5913(6) 0.0473(7) 0.7749(4) 0.040(3) Uani 1 1 d . . . H36 H 0.5460 0.0842 0.7688 0.048 Uiso 1 1 calc R . . C37 C 0.5604(8) -0.0023(8) 0.8133(5) 0.073(4) Uani 1 1 d . . . H37A H 0.5371 0.0375 0.8479 0.110 Uiso 1 1 calc R . . H37B H 0.6077 -0.0280 0.8286 0.110 Uiso 1 1 calc R . . H37C H 0.5165 -0.0484 0.7883 0.110 Uiso 1 1 calc R . . C38 C 0.6699(7) 0.1092(8) 0.8111(5) 0.072(4) Uani 1 1 d . . . H38A H 0.6836 0.1496 0.7903 0.108 Uiso 1 1 calc R . . H38B H 0.7178 0.0754 0.8138 0.108 Uiso 1 1 calc R . . H38C H 0.6584 0.1421 0.8524 0.108 Uiso 1 1 calc R . . C39 C 0.4616(6) 0.5996(5) 0.6789(4) 0.032(2) Uani 1 1 d . . . C40 C 0.4811(6) 0.6024(6) 0.5862(4) 0.035(2) Uani 1 1 d . . . H40 H 0.4883 0.5828 0.5443 0.042 Uiso 1 1 calc R . . C41 C 0.4755(6) 0.6848(6) 0.6217(4) 0.035(2) Uani 1 1 d . . . H41 H 0.4793 0.7350 0.6104 0.042 Uiso 1 1 calc R . . C42 C 0.4459(6) 0.7565(6) 0.7292(4) 0.038(3) Uani 1 1 d . . . H42A H 0.4429 0.8080 0.7167 0.046 Uiso 1 1 calc R . . H42B H 0.4919 0.7699 0.7639 0.046 Uiso 1 1 calc R . . C43 C 0.4791(6) 0.4579(6) 0.5957(4) 0.030(2) Uani 1 1 d . . . C44 C 0.5582(7) 0.4302(6) 0.5891(5) 0.038(3) Uani 1 1 d . . . C45 C 0.5615(8) 0.3420(8) 0.5556(5) 0.052(3) Uani 1 1 d . . . H45 H 0.6152 0.3206 0.5507 0.062 Uiso 1 1 calc R . . C46 C 0.4900(9) 0.2852(7) 0.5297(5) 0.056(3) Uani 1 1 d . . . H46 H 0.4940 0.2265 0.5053 0.067 Uiso 1 1 calc R . . C47 C 0.4113(8) 0.3159(7) 0.5400(5) 0.057(3) Uani 1 1 d . . . H47 H 0.3618 0.2762 0.5251 0.069 Uiso 1 1 calc R . . C48 C 0.4035(7) 0.4026(7) 0.5715(5) 0.045(3) Uani 1 1 d . . . C49 C 0.3144(7) 0.4321(7) 0.5811(5) 0.056(3) Uani 1 1 d . . . H49 H 0.3165 0.4954 0.5871 0.067 Uiso 1 1 calc R . . C50 C 0.2449(8) 0.3828(10) 0.5272(6) 0.103(6) Uani 1 1 d . . . H50A H 0.2652 0.3787 0.4886 0.154 Uiso 1 1 calc R . . H50B H 0.1943 0.4142 0.5312 0.154 Uiso 1 1 calc R . . H50C H 0.2310 0.3243 0.5275 0.154 Uiso 1 1 calc R . . C51 C 0.2904(7) 0.4203(8) 0.6368(5) 0.068(4) Uani 1 1 d . . . H51A H 0.2351 0.4415 0.6439 0.103 Uiso 1 1 calc R . . H51B H 0.3327 0.4531 0.6719 0.103 Uiso 1 1 calc R . . H51C H 0.2875 0.3585 0.6316 0.103 Uiso 1 1 calc R . . C52 C 0.6384(6) 0.4879(7) 0.6173(5) 0.042(3) Uani 1 1 d . . . H52 H 0.6241 0.5406 0.6499 0.051 Uiso 1 1 calc R . . C53 C 0.7050(6) 0.4480(8) 0.6465(5) 0.056(3) Uani 1 1 d . . . H53A H 0.7529 0.4917 0.6674 0.084 Uiso 1 1 calc R . . H53B H 0.7243 0.3993 0.6149 0.084 Uiso 1 1 calc R . . H53C H 0.6813 0.4270 0.6761 0.084 Uiso 1 1 calc R . . C54 C 0.6754(7) 0.5183(7) 0.5693(5) 0.056(3) Uani 1 1 d . . . H54A H 0.6336 0.5482 0.5523 0.084 Uiso 1 1 calc R . . H54B H 0.6897 0.4679 0.5365 0.084 Uiso 1 1 calc R . . H54C H 0.7265 0.5582 0.5888 0.084 Uiso 1 1 calc R . . C55 C 0.2668(7) 0.6400(6) 0.7764(4) 0.036(2) Uani 1 1 d . . . C56 C 0.3467(6) 0.6584(6) 0.7595(4) 0.038(3) Uani 1 1 d . . . C57 C 0.3620(7) 0.7347(6) 0.7483(4) 0.040(3) Uani 1 1 d . . . C58 C 0.3010(7) 0.7925(7) 0.7540(4) 0.044(3) Uani 1 1 d . . . H58 H 0.3136 0.8453 0.7474 0.053 Uiso 1 1 calc R . . C59 C 0.2250(7) 0.7763(6) 0.7686(5) 0.044(3) Uani 1 1 d . . . H59 H 0.1841 0.8168 0.7717 0.053 Uiso 1 1 calc R . . C60 C 0.2060(7) 0.6979(7) 0.7795(4) 0.043(3) Uani 1 1 d . . . H60 H 0.1518 0.6851 0.7889 0.051 Uiso 1 1 calc R . . C61 C 0.2501(6) 0.5589(6) 0.7894(4) 0.036(2) Uani 1 1 d . . . H61A H 0.1943 0.5583 0.8037 0.043 Uiso 1 1 calc R . . H61B H 0.2482 0.5082 0.7513 0.043 Uiso 1 1 calc R . . C62 C 0.3010(6) 0.5411(6) 0.8891(4) 0.035(2) Uani 1 1 d . . . H62 H 0.2477 0.5342 0.9020 0.042 Uiso 1 1 calc R . . C63 C 0.3768(6) 0.5421(6) 0.9197(4) 0.034(2) Uani 1 1 d . . . H63 H 0.3879 0.5368 0.9587 0.041 Uiso 1 1 calc R . . C64 C 0.3980(6) 0.5591(6) 0.8308(4) 0.032(2) Uani 1 1 d . . . C65 C 0.5268(5) 0.5653(6) 0.9073(4) 0.026(2) Uani 1 1 d . . . C66 C 0.5683(6) 0.4927(6) 0.9079(4) 0.030(2) Uani 1 1 d . . . C67 C 0.6514(6) 0.5090(6) 0.9381(4) 0.031(2) Uani 1 1 d . . . H67 H 0.6826 0.4618 0.9389 0.037 Uiso 1 1 calc R . . C68 C 0.6878(6) 0.5924(7) 0.9666(4) 0.037(3) Uani 1 1 d . . . H68 H 0.7437 0.6021 0.9876 0.045 Uiso 1 1 calc R . . C69 C 0.6459(6) 0.6625(7) 0.9656(4) 0.037(3) Uani 1 1 d . . . H69 H 0.6735 0.7196 0.9851 0.045 Uiso 1 1 calc R . . C70 C 0.5639(7) 0.6507(6) 0.9363(4) 0.038(3) Uani 1 1 d . . . C71 C 0.5183(6) 0.7299(6) 0.9334(4) 0.041(3) Uani 1 1 d . . . H71 H 0.4568 0.7104 0.9198 0.050 Uiso 1 1 calc R . . C72 C 0.5510(7) 0.7624(7) 0.8873(5) 0.056(3) Uani 1 1 d . . . H72A H 0.6119 0.7793 0.8988 0.083 Uiso 1 1 calc R . . H72B H 0.5222 0.8128 0.8860 0.083 Uiso 1 1 calc R . . H72C H 0.5404 0.7164 0.8470 0.083 Uiso 1 1 calc R . . C73 C 0.5277(7) 0.8026(7) 0.9964(5) 0.058(3) Uani 1 1 d . . . H73A H 0.5024 0.7809 1.0252 0.087 Uiso 1 1 calc R . . H73B H 0.4989 0.8520 0.9928 0.087 Uiso 1 1 calc R . . H73C H 0.5878 0.8212 1.0114 0.087 Uiso 1 1 calc R . . C74 C 0.5256(6) 0.4008(6) 0.8803(4) 0.030(2) Uani 1 1 d . . . H74 H 0.4737 0.4015 0.8526 0.037 Uiso 1 1 calc R . . C75 C 0.5798(6) 0.3359(6) 0.8424(5) 0.044(3) Uani 1 1 d . . . H75A H 0.5468 0.2791 0.8232 0.067 Uiso 1 1 calc R . . H75B H 0.6294 0.3306 0.8689 0.067 Uiso 1 1 calc R . . H75C H 0.5982 0.3560 0.8107 0.067 Uiso 1 1 calc R . . C76 C 0.4980(6) 0.3683(7) 0.9296(5) 0.047(3) Uani 1 1 d . . . H76A H 0.4649 0.3117 0.9102 0.070 Uiso 1 1 calc R . . H76B H 0.4633 0.4099 0.9546 0.070 Uiso 1 1 calc R . . H76C H 0.5479 0.3627 0.9556 0.070 Uiso 1 1 calc R . . C77 C 0.8530(6) 0.6755(6) 0.7837(4) 0.032(2) Uani 1 1 d . . . C78 C 0.7724(6) 0.6538(5) 0.7949(4) 0.029(2) Uani 1 1 d . . . C79 C 0.7020(6) 0.6701(6) 0.7613(5) 0.045(3) Uani 1 1 d . . . H79 H 0.6470 0.6549 0.7684 0.054 Uiso 1 1 calc R . . C80 C 0.7108(6) 0.7078(6) 0.7181(5) 0.046(3) Uani 1 1 d . . . H80 H 0.6624 0.7177 0.6950 0.056 Uiso 1 1 calc R . . C81 C 0.8607(6) 0.7170(6) 0.7430(4) 0.036(3) Uani 1 1 d . . . C82 C 0.7916(6) 0.7313(7) 0.7087(5) 0.042(3) Uani 1 1 d . . . H82 H 0.7988 0.7570 0.6788 0.051 Uiso 1 1 calc R . . C83 C 0.9500(6) 0.7486(6) 0.7358(4) 0.039(3) Uani 1 1 d . . . H83A H 0.9810 0.6980 0.7170 0.047 Uiso 1 1 calc R . . H83B H 0.9458 0.7830 0.7085 0.047 Uiso 1 1 calc R . . C84 C 1.0528(6) 0.9140(6) 0.8716(5) 0.038(3) Uani 1 1 d . . . H84 H 1.0754 0.9711 0.8968 0.045 Uiso 1 1 calc R . . C85 C 1.0068(5) 0.7722(6) 0.8426(4) 0.030(2) Uani 1 1 d . . . C86 C 1.0231(6) 0.8879(6) 0.8126(5) 0.036(3) Uani 1 1 d . . . H86 H 1.0217 0.9225 0.7875 0.043 Uiso 1 1 calc R . . C87 C 1.0700(6) 0.8489(6) 0.9525(4) 0.031(2) Uani 1 1 d . . . C88 C 1.1569(6) 0.8605(6) 0.9733(5) 0.037(3) Uani 1 1 d . . . C89 C 1.0079(6) 0.8487(6) 0.9892(5) 0.040(3) Uani 1 1 d . . . C90 C 1.1809(7) 0.8786(7) 1.0363(6) 0.055(3) Uani 1 1 d . . . H90 H 1.2390 0.8897 1.0529 0.066 Uiso 1 1 calc R . . C91 C 1.1199(8) 0.8803(7) 1.0738(5) 0.055(3) Uani 1 1 d . . . H91 H 1.1366 0.8918 1.1161 0.066 Uiso 1 1 calc R . . C92 C 1.0366(7) 0.8657(7) 1.0511(5) 0.047(3) Uani 1 1 d . . . H92 H 0.9963 0.8671 1.0781 0.056 Uiso 1 1 calc R . . C93 C 1.2247(6) 0.8570(6) 0.9330(5) 0.043(3) Uani 1 1 d . . . H93 H 1.1960 0.8368 0.8898 0.052 Uiso 1 1 calc R . . C94 C 1.2861(7) 0.7913(7) 0.9373(5) 0.061(3) Uani 1 1 d . . . H94A H 1.3214 0.8134 0.9773 0.092 Uiso 1 1 calc R . . H94B H 1.3220 0.7821 0.9050 0.092 Uiso 1 1 calc R . . H94C H 1.2544 0.7362 0.9324 0.092 Uiso 1 1 calc R . . C95 C 1.2747(7) 0.9448(7) 0.9456(6) 0.063(3) Uani 1 1 d . . . H95A H 1.3164 0.9376 0.9172 0.095 Uiso 1 1 calc R . . H95B H 1.3038 0.9665 0.9877 0.095 Uiso 1 1 calc R . . H95C H 1.2359 0.9863 0.9399 0.095 Uiso 1 1 calc R . . C96 C 0.8788(6) 0.9041(7) 0.9469(5) 0.047(3) Uani 1 1 d . . . H96A H 0.9109 0.9154 0.9168 0.070 Uiso 1 1 calc R . . H96B H 0.8840 0.9564 0.9835 0.070 Uiso 1 1 calc R . . H96C H 0.8192 0.8882 0.9293 0.070 Uiso 1 1 calc R . . C97 C 0.9137(6) 0.8292(6) 0.9641(4) 0.038(3) Uani 1 1 d . . . H97 H 0.9073 0.7769 0.9259 0.046 Uiso 1 1 calc R . . C98 C 0.8593(7) 0.8086(7) 1.0071(5) 0.058(3) Uani 1 1 d . . . H98A H 0.8023 0.7859 0.9854 0.086 Uiso 1 1 calc R . . H98B H 0.8563 0.8615 1.0420 0.086 Uiso 1 1 calc R . . H98C H 0.8840 0.7649 1.0217 0.086 Uiso 1 1 calc R . . C99 C 0.7593(6) 0.6081(6) 0.8382(5) 0.042(3) Uani 1 1 d . . . H99A H 0.7777 0.6483 0.8806 0.050 Uiso 1 1 calc R . . H99B H 0.6985 0.5895 0.8343 0.050 Uiso 1 1 calc R . . C100 C 0.8903(6) 0.5366(6) 0.8218(4) 0.035(2) Uani 1 1 d . . . C101 C 0.7701(7) 0.4487(7) 0.8108(5) 0.042(3) Uani 1 1 d . . . H101 H 0.7125 0.4300 0.8093 0.051 Uiso 1 1 calc R . . C102 C 0.8331(7) 0.4006(8) 0.7991(5) 0.058(3) Uani 1 1 d . . . H102 H 0.8294 0.3393 0.7884 0.069 Uiso 1 1 calc R . . C103 C 0.9857(7) 0.4196(6) 0.7908(6) 0.044(3) Uani 1 1 d . . . C104 C 1.0092(7) 0.4115(6) 0.7354(6) 0.045(3) Uani 1 1 d . . . C105 C 1.0820(8) 0.3697(8) 0.7178(7) 0.071(4) Uani 1 1 d . . . H105 H 1.1005 0.3645 0.6798 0.085 Uiso 1 1 calc R . . C106 C 1.1253(8) 0.3368(8) 0.7580(6) 0.060(3) Uani 1 1 d . . . H106 H 1.1739 0.3078 0.7471 0.072 Uiso 1 1 calc R . . C107 C 1.1000(8) 0.3450(8) 0.8120(7) 0.068(4) Uani 1 1 d . . . H107 H 1.1324 0.3223 0.8384 0.082 Uiso 1 1 calc R . . C108 C 1.0297(7) 0.3843(7) 0.8310(6) 0.059(3) Uani 1 1 d . . . C109 C 0.9629(7) 0.4474(7) 0.6898(5) 0.055(3) Uani 1 1 d . . . H109 H 0.9147 0.4761 0.7092 0.066 Uiso 1 1 calc R . . C110 C 0.9240(7) 0.3748(8) 0.6303(6) 0.075(4) Uani 1 1 d . . . H11C H 0.8775 0.3411 0.6386 0.113 Uiso 1 1 calc R . . H11D H 0.9672 0.3366 0.6142 0.113 Uiso 1 1 calc R . . H11E H 0.9024 0.4004 0.6003 0.113 Uiso 1 1 calc R . . C111 C 1.0152(8) 0.5162(8) 0.6758(6) 0.081(4) Uani 1 1 d . . . H11F H 0.9792 0.5408 0.6506 0.122 Uiso 1 1 calc R . . H11G H 1.0610 0.4899 0.6537 0.122 Uiso 1 1 calc R . . H11H H 1.0392 0.5624 0.7142 0.122 Uiso 1 1 calc R . . C112 C 1.0801(8) 0.4255(9) 0.9453(6) 0.079(4) Uani 1 1 d . . . H11I H 1.1225 0.3840 0.9353 0.119 Uiso 1 1 calc R . . H11J H 1.0609 0.4277 0.9839 0.119 Uiso 1 1 calc R . . H11K H 1.1049 0.4832 0.9493 0.119 Uiso 1 1 calc R . . C113 C 0.9608(9) 0.3093(10) 0.8931(7) 0.107(5) Uani 1 1 d . . . H11L H 0.9398 0.3179 0.9321 0.161 Uiso 1 1 calc R . . H11M H 1.0014 0.2656 0.8865 0.161 Uiso 1 1 calc R . . H11N H 0.9134 0.2893 0.8598 0.161 Uiso 1 1 calc R . . C114 C 1.0051(7) 0.3967(8) 0.8944(6) 0.063(3) Uani 1 1 d . . . H114 H 0.9641 0.4416 0.9038 0.075 Uiso 1 1 calc R . . N1 N 0.4831(4) 0.1987(4) 0.6727(3) 0.0293(18) Uani 1 1 d . . . N2 N 0.5694(5) 0.1022(4) 0.6697(3) 0.0310(19) Uani 1 1 d . . . N3 N 0.2652(5) 0.0132(5) 0.7618(3) 0.0330(19) Uani 1 1 d . . . N4 N 0.2036(4) -0.0506(5) 0.6700(3) 0.0314(19) Uani 1 1 d . . . N5 N 0.4629(4) 0.6813(5) 0.6780(3) 0.0309(19) Uani 1 1 d . . . N6 N 0.4743(5) 0.5507(5) 0.6219(3) 0.0319(19) Uani 1 1 d . . . N7 N 0.3147(5) 0.5519(5) 0.8355(3) 0.0284(18) Uani 1 1 d . . . N8 N 0.4365(4) 0.5525(5) 0.8831(3) 0.0288(19) Uani 1 1 d . . . N9 N 0.9948(4) 0.8010(5) 0.7944(3) 0.0304(19) Uani 1 1 d . . . N10 N 1.0447(4) 0.8422(5) 0.8899(4) 0.0294(19) Uani 1 1 d . . . N11 N 0.8068(5) 0.5329(5) 0.8258(3) 0.035(2) Uani 1 1 d . . . N12 N 0.9067(5) 0.4541(5) 0.8047(4) 0.042(2) Uani 1 1 d . . . Pd1 Pd 0.38374(4) 0.04565(4) 0.68107(3) 0.0292(2) Uani 1 1 d . . . Pd2 Pd 0.43711(5) 0.57566(5) 0.75525(3) 0.0300(2) Uani 1 1 d . . . Pd3 Pd 0.95612(4) 0.65181(5) 0.83436(3) 0.0317(2) Uani 1 1 d . . . Br1 Br 0.40780(6) -0.09810(6) 0.60457(5) 0.0393(3) Uani 1 1 d . . . Br2 Br 0.54501(6) 0.47018(6) 0.74880(5) 0.0412(3) Uani 1 1 d . . . Br3 Br 1.07985(6) 0.62401(7) 0.89842(5) 0.0452(3) Uani 1 1 d . . . O1 O 0.9217(7) 0.9311(8) 0.6681(6) 0.095(3) Uani 1 1 d . . . C201 C 0.9335(15) 0.8172(17) 0.5782(10) 0.169(12) Uani 1 1 d . . . H20A H 0.9170 0.7987 0.5339 0.254 Uiso 1 1 calc R . . H20B H 0.9154 0.7707 0.5926 0.254 Uiso 1 1 calc R . . H20C H 0.9950 0.8299 0.5878 0.254 Uiso 1 1 calc R . . C200 C 0.8975(12) 0.8871(16) 0.6053(12) 0.133(8) Uani 1 1 d . . . H20D H 0.8358 0.8707 0.5986 0.160 Uiso 1 1 calc R . . H20E H 0.9076 0.9287 0.5842 0.160 Uiso 1 1 calc R . . C203 C 0.9070(15) 1.0505(18) 0.7555(8) 0.214(15) Uani 1 1 d . . . H20F H 0.8761 1.1018 0.7702 0.321 Uiso 1 1 calc R . . H20G H 0.9673 1.0689 0.7598 0.321 Uiso 1 1 calc R . . H20H H 0.8987 1.0133 0.7796 0.321 Uiso 1 1 calc R . . C202 C 0.8758(12) 1.0027(17) 0.6918(11) 0.147(8) Uani 1 1 d . . . H20I H 0.8154 0.9821 0.6877 0.177 Uiso 1 1 calc R . . H20J H 0.8804 1.0416 0.6679 0.177 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 C1 0.030(6) 0.032(5) 0.035(6) 0.005(5) 0.006(5) 0.008(5) C2 0.032(6) 0.028(5) 0.042(7) 0.003(5) 0.015(5) -0.011(5) C3 0.032(6) 0.031(6) 0.047(7) 0.010(5) 0.010(5) 0.001(5) C4 0.048(7) 0.016(5) 0.061(7) 0.021(5) -0.004(6) -0.002(5) C5 0.025(6) 0.034(6) 0.035(6) 0.011(5) -0.001(5) 0.001(5) C6 0.024(5) 0.037(6) 0.025(6) 0.013(5) 0.006(4) 0.011(4) C7 0.018(5) 0.034(6) 0.045(7) 0.005(5) -0.004(5) -0.008(4) C8 0.034(6) 0.043(7) 0.028(6) -0.005(5) 0.001(5) 0.010(5) C9 0.037(7) 0.036(6) 0.046(7) 0.000(6) 0.008(5) 0.000(5) C10 0.025(6) 0.026(6) 0.061(8) 0.006(6) -0.001(5) 0.006(5) C11 0.048(7) 0.040(6) 0.031(6) 0.005(5) 0.008(5) 0.008(5) C12 0.027(6) 0.052(7) 0.021(6) 0.002(5) 0.010(5) -0.003(5) C13 0.029(6) 0.035(6) 0.044(7) 0.017(5) 0.014(5) 0.009(5) C14 0.029(6) 0.026(5) 0.039(6) 0.006(5) -0.004(5) 0.005(4) C15 0.028(6) 0.032(6) 0.030(6) 0.008(5) -0.002(4) -0.009(5) C16 0.034(6) 0.033(6) 0.020(6) 0.005(5) 0.000(5) -0.001(5) C17 0.036(7) 0.046(7) 0.053(8) 0.015(6) -0.013(6) -0.008(5) C18 0.038(7) 0.061(8) 0.035(7) 0.018(6) -0.010(5) -0.006(6) C19 0.042(7) 0.042(7) 0.031(7) 0.005(5) 0.003(5) 0.003(5) C20 0.026(6) 0.028(5) 0.051(7) 0.019(5) 0.003(5) -0.001(5) C21 0.039(6) 0.029(6) 0.059(7) 0.028(6) -0.007(5) -0.003(5) C22 0.061(9) 0.044(7) 0.104(11) 0.006(7) 0.019(8) 0.017(6) C23 0.088(10) 0.050(7) 0.066(9) 0.022(7) 0.017(7) -0.005(7) C24 0.039(6) 0.044(6) 0.031(6) 0.011(5) 0.002(5) 0.002(5) C25 0.069(8) 0.036(6) 0.078(9) 0.027(6) 0.031(7) 0.007(6) C26 0.044(7) 0.045(7) 0.056(8) 0.011(6) -0.001(6) 0.014(6) C27 0.008(5) 0.037(6) 0.041(7) 0.020(5) 0.004(4) -0.001(4) C28 0.026(6) 0.040(6) 0.047(7) 0.017(6) -0.002(5) 0.004(5) C29 0.046(7) 0.057(7) 0.035(7) 0.027(6) 0.001(5) 0.017(6) C30 0.025(6) 0.048(7) 0.074(9) 0.042(7) 0.008(6) 0.010(5) C31 0.029(6) 0.044(7) 0.055(7) 0.027(6) 0.009(5) -0.005(5) C32 0.025(6) 0.033(6) 0.035(6) 0.012(5) 0.003(5) 0.001(5) C33 0.032(6) 0.025(5) 0.037(6) 0.008(5) 0.011(5) 0.013(4) C34 0.050(7) 0.034(6) 0.045(7) 0.019(6) -0.003(5) 0.010(5) C35 0.051(7) 0.049(7) 0.069(8) 0.034(6) 0.021(6) -0.001(6) C36 0.045(7) 0.046(6) 0.036(7) 0.018(6) 0.008(5) 0.020(5) C37 0.121(11) 0.062(8) 0.061(9) 0.039(7) 0.053(8) 0.016(8) C38 0.070(9) 0.080(9) 0.049(8) 0.010(7) -0.008(7) -0.012(7) C39 0.032(6) 0.015(5) 0.050(7) 0.015(5) 0.005(5) 0.007(4) C40 0.043(6) 0.033(6) 0.034(6) 0.017(5) 0.004(5) 0.004(5) C41 0.038(6) 0.029(6) 0.050(7) 0.027(5) 0.012(5) 0.008(5) C42 0.045(7) 0.031(6) 0.043(7) 0.016(5) 0.007(5) 0.016(5) C43 0.050(7) 0.026(5) 0.017(5) 0.009(4) 0.006(5) 0.007(5) C44 0.052(8) 0.033(6) 0.040(7) 0.023(5) 0.012(6) 0.018(6) C45 0.073(9) 0.060(8) 0.045(7) 0.038(7) 0.029(7) 0.020(7) C46 0.106(11) 0.025(6) 0.039(7) 0.009(5) 0.029(7) 0.002(7) C47 0.076(10) 0.036(7) 0.057(8) 0.015(6) 0.014(7) -0.016(7) C48 0.050(8) 0.042(7) 0.044(7) 0.020(6) 0.003(6) 0.000(6) C49 0.054(8) 0.052(7) 0.069(9) 0.038(7) -0.006(7) -0.015(6) C50 0.071(10) 0.159(15) 0.089(11) 0.076(11) -0.019(8) -0.055(10) C51 0.046(8) 0.087(10) 0.056(9) 0.004(7) 0.004(6) 0.016(7) C52 0.044(7) 0.051(7) 0.036(7) 0.016(6) 0.013(5) 0.027(6) C53 0.038(7) 0.083(9) 0.065(8) 0.044(7) 0.019(6) 0.018(6) C54 0.062(8) 0.050(7) 0.057(8) 0.019(6) 0.010(6) 0.014(6) C55 0.054(7) 0.029(6) 0.029(6) 0.016(5) 0.011(5) 0.009(5) C56 0.053(7) 0.024(5) 0.033(6) 0.012(5) -0.011(5) -0.014(5) C57 0.055(7) 0.033(6) 0.031(6) 0.003(5) 0.012(5) 0.025(6) C58 0.060(8) 0.046(7) 0.027(6) 0.011(5) 0.017(6) 0.004(6) C59 0.062(8) 0.031(6) 0.047(7) 0.018(5) 0.011(6) 0.030(6) C60 0.043(7) 0.049(7) 0.033(6) 0.010(5) 0.002(5) 0.010(6) C61 0.036(6) 0.027(5) 0.036(6) 0.001(5) 0.003(5) -0.007(5) C62 0.036(7) 0.033(6) 0.040(7) 0.015(5) 0.013(5) 0.001(5) C63 0.033(6) 0.036(6) 0.035(6) 0.018(5) 0.006(5) -0.011(5) C64 0.027(6) 0.028(5) 0.033(6) 0.005(5) -0.006(5) 0.001(4) C65 0.028(6) 0.033(6) 0.024(6) 0.017(5) 0.005(4) -0.003(5) C66 0.033(6) 0.038(6) 0.022(6) 0.013(5) 0.006(5) -0.002(5) C67 0.026(6) 0.040(6) 0.038(6) 0.027(5) 0.010(5) 0.006(5) C68 0.018(5) 0.053(7) 0.045(7) 0.024(6) 0.000(5) 0.002(5) C69 0.043(7) 0.045(7) 0.022(6) 0.015(5) -0.004(5) -0.012(6) C70 0.051(7) 0.032(6) 0.032(6) 0.012(5) 0.014(5) -0.009(5) C71 0.044(7) 0.035(6) 0.038(7) 0.008(5) -0.003(5) -0.011(5) C72 0.073(9) 0.056(7) 0.041(7) 0.021(6) 0.011(6) 0.001(6) C73 0.079(9) 0.048(7) 0.047(8) 0.016(6) 0.020(7) 0.002(6) C74 0.028(6) 0.040(6) 0.022(6) 0.009(5) 0.002(4) 0.007(5) C75 0.038(6) 0.041(6) 0.056(7) 0.022(6) 0.001(6) -0.004(5) C76 0.045(7) 0.054(7) 0.045(7) 0.029(6) -0.008(5) -0.007(6) C77 0.027(6) 0.030(5) 0.039(6) 0.010(5) 0.012(5) 0.001(4) C78 0.044(7) 0.020(5) 0.024(6) 0.008(4) 0.007(5) -0.006(5) C79 0.027(6) 0.045(7) 0.075(9) 0.038(7) 0.005(6) 0.000(5) C80 0.027(6) 0.038(6) 0.075(9) 0.026(6) -0.008(6) -0.005(5) C81 0.029(6) 0.043(6) 0.040(7) 0.019(5) 0.008(5) -0.003(5) C82 0.033(7) 0.059(7) 0.041(7) 0.031(6) -0.010(5) -0.004(5) C83 0.047(7) 0.041(6) 0.037(7) 0.022(5) 0.004(5) 0.009(5) C84 0.040(7) 0.027(6) 0.047(8) 0.013(5) 0.011(6) -0.001(5) C85 0.021(5) 0.043(6) 0.029(6) 0.014(5) 0.008(4) 0.010(5) C86 0.032(6) 0.033(6) 0.053(8) 0.022(6) 0.021(5) 0.006(5) C87 0.031(6) 0.026(5) 0.036(6) 0.013(5) 0.004(5) -0.007(4) C88 0.027(6) 0.040(6) 0.045(7) 0.015(5) 0.001(5) 0.006(5) C89 0.046(7) 0.033(6) 0.041(7) 0.010(5) 0.012(6) -0.002(5) C90 0.039(7) 0.062(8) 0.064(9) 0.025(7) -0.008(7) 0.000(6) C91 0.068(9) 0.054(7) 0.041(7) 0.021(6) -0.007(7) -0.007(7) C92 0.046(8) 0.050(7) 0.051(8) 0.030(6) 0.006(6) -0.003(6) C93 0.023(6) 0.046(7) 0.053(7) 0.010(6) 0.002(5) 0.000(5) C94 0.040(7) 0.057(8) 0.074(9) 0.009(7) 0.001(6) 0.005(6) C95 0.043(7) 0.063(8) 0.083(10) 0.023(7) 0.019(7) -0.002(6) C96 0.039(7) 0.056(7) 0.039(7) 0.010(6) 0.003(5) 0.007(6) C97 0.034(6) 0.041(6) 0.032(6) 0.007(5) 0.002(5) -0.005(5) C98 0.049(7) 0.058(7) 0.061(8) 0.018(7) 0.007(6) -0.016(6) C99 0.018(5) 0.047(7) 0.051(7) 0.005(6) 0.000(5) 0.000(5) C100 0.035(7) 0.035(6) 0.036(6) 0.012(5) 0.006(5) 0.007(5) C101 0.024(6) 0.042(7) 0.061(8) 0.019(6) 0.002(5) -0.001(5) C102 0.034(7) 0.049(7) 0.086(10) 0.024(7) -0.002(6) -0.012(6) C103 0.033(7) 0.033(6) 0.060(8) 0.011(6) -0.006(6) -0.004(5) C104 0.029(7) 0.031(6) 0.069(9) 0.013(6) -0.005(6) 0.007(5) C105 0.049(8) 0.056(8) 0.081(10) -0.004(8) -0.007(8) 0.001(7) C106 0.045(8) 0.063(9) 0.060(9) 0.005(7) 0.001(7) 0.019(6) C107 0.044(8) 0.052(8) 0.101(12) 0.024(8) -0.012(8) 0.008(7) C108 0.032(7) 0.048(7) 0.094(11) 0.021(8) -0.001(7) 0.014(6) C109 0.058(8) 0.043(7) 0.042(7) -0.014(6) 0.001(6) 0.012(6) C110 0.056(8) 0.076(9) 0.073(10) 0.002(8) 0.004(7) 0.007(7) C111 0.081(10) 0.071(9) 0.080(10) 0.014(8) 0.001(8) 0.008(8) C112 0.062(9) 0.093(10) 0.099(11) 0.062(9) -0.009(8) -0.007(8) C113 0.098(12) 0.104(12) 0.145(15) 0.085(12) -0.004(11) -0.006(10) C114 0.052(8) 0.055(8) 0.090(11) 0.041(8) 0.002(8) 0.010(6) N1 0.027(4) 0.032(4) 0.027(5) 0.009(4) 0.001(4) 0.003(4) N2 0.039(5) 0.027(4) 0.035(5) 0.019(4) 0.009(4) 0.005(4) N3 0.039(5) 0.029(4) 0.026(5) 0.006(4) -0.001(4) 0.002(4) N4 0.024(4) 0.032(4) 0.038(5) 0.011(4) 0.009(4) -0.001(4) N5 0.027(5) 0.035(4) 0.031(5) 0.013(4) 0.002(4) 0.006(4) N6 0.038(5) 0.029(4) 0.032(5) 0.011(4) 0.010(4) 0.007(4) N7 0.025(5) 0.033(5) 0.031(5) 0.018(4) -0.001(4) 0.001(4) N8 0.020(4) 0.038(5) 0.028(5) 0.014(4) -0.004(4) -0.005(4) N9 0.020(4) 0.045(5) 0.031(5) 0.020(4) 0.006(4) -0.003(4) N10 0.025(5) 0.029(5) 0.038(5) 0.014(4) 0.010(4) 0.002(4) N11 0.035(5) 0.028(5) 0.044(5) 0.017(4) 0.004(4) -0.005(4) N12 0.030(5) 0.030(5) 0.069(7) 0.025(5) 0.004(5) 0.005(4) Pd1 0.0264(4) 0.0267(4) 0.0349(5) 0.0117(4) 0.0034(3) 0.0015(3) Pd2 0.0319(5) 0.0283(4) 0.0314(5) 0.0127(4) 0.0033(4) 0.0034(3) Pd3 0.0271(4) 0.0317(4) 0.0372(5) 0.0147(4) 0.0013(4) 0.0003(3) Br1 0.0376(6) 0.0320(6) 0.0469(7) 0.0114(5) 0.0095(5) 0.0015(5) Br2 0.0415(7) 0.0411(6) 0.0462(7) 0.0207(6) 0.0084(5) 0.0073(5) Br3 0.0344(6) 0.0451(6) 0.0568(8) 0.0228(6) -0.0055(5) 0.0009(5) O1 0.076(8) 0.123(9) 0.102(10) 0.054(8) 0.028(7) 0.012(7) C201 0.21(3) 0.25(3) 0.114(18) 0.109(19) 0.088(17) 0.12(2) C200 0.095(16) 0.19(2) 0.14(2) 0.10(2) -0.011(15) -0.033(15) C203 0.22(2) 0.40(4) 0.049(12) 0.068(18) 0.069(14) 0.20(3) C202 0.083(14) 0.22(3) 0.17(2) 0.11(2) 0.029(15) 0.038(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.346(9) . ? C1 N1 1.349(9) . ? C1 Pd1 2.057(9) . ? C2 C3 1.325(12) . ? C2 N2 1.412(8) . ? C3 N1 1.379(9) . ? C4 N1 1.453(9) . ? C4 C5 1.516(13) . ? C5 C10 1.395(13) . ? C5 C6 1.406(12) . ? C6 C7 1.392(12) . ? C6 Pd1 2.021(9) . ? C7 C8 1.401(12) . ? C7 C11 1.511(13) . ? C8 C9 1.390(13) . ? C9 C10 1.383(14) . ? C11 N3 1.472(9) . ? C12 N3 1.350(9) . ? C12 C13 1.367(12) . ? C13 N4 1.385(9) . ? C14 N4 1.361(9) . ? C14 N3 1.368(10) . ? C14 Pd1 2.039(9) . ? C15 C16 1.393(12) . ? C15 C20 1.410(12) . ? C15 N4 1.444(9) . ? C16 C17 1.378(13) . ? C16 C24 1.520(13) . ? C17 C18 1.372(13) . ? C18 C19 1.374(13) . ? C19 C20 1.383(13) . ? C20 C21 1.506(13) . ? C21 C23 1.478(13) . ? C21 C22 1.545(14) . ? C24 C25 1.522(13) . ? C24 C26 1.524(13) . ? C27 C28 1.397(12) . ? C27 C32 1.404(12) . ? C27 N2 1.425(9) . ? C28 C29 1.404(13) . ? C28 C36 1.513(13) . ? C29 C30 1.382(13) . ? C30 C31 1.380(13) . ? C31 C32 1.397(13) . ? C32 C33 1.510(12) . ? C33 C34 1.521(12) . ? C33 C35 1.545(12) . ? C36 C37 1.512(13) . ? C36 C38 1.542(14) . ? C39 N5 1.351(8) . ? C39 N6 1.353(9) . ? C39 Pd2 2.037(9) . ? C40 C41 1.342(12) . ? C40 N6 1.391(9) . ? C41 N5 1.382(9) . ? C42 N5 1.465(9) . ? C42 C57 1.527(13) . ? C43 C44 1.376(13) . ? C43 C48 1.411(13) . ? C43 N6 1.449(9) . ? C44 C45 1.403(14) . ? C44 C52 1.496(14) . ? C45 C46 1.377(15) . ? C46 C47 1.399(15) . ? C47 C48 1.384(14) . ? C48 C49 1.548(14) . ? C49 C51 1.476(15) . ? C49 C50 1.545(16) . ? C52 C53 1.503(13) . ? C52 C54 1.541(13) . ? C55 C60 1.389(12) . ? C55 C56 1.429(13) . ? C55 C61 1.484(9) . ? C56 C57 1.382(13) . ? C56 Pd2 2.029(10) . ? C57 C58 1.386(13) . ? C58 C59 1.338(13) . ? C59 C60 1.423(13) . ? C61 N7 1.451(11) . ? C62 C63 1.336(12) . ? C62 N7 1.370(11) . ? C63 N8 1.395(11) . ? C64 N7 1.352(11) . ? C64 N8 1.355(11) . ? C64 Pd2 2.044(10) . ? C65 C70 1.399(12) . ? C65 C66 1.401(12) . ? C65 N8 1.469(11) . ? C66 C67 1.403(12) . ? C66 C74 1.515(12) . ? C67 C68 1.368(13) . ? C68 C69 1.372(13) . ? C69 C70 1.384(13) . ? C70 C71 1.545(13) . ? C71 C72 1.493(13) . ? C71 C73 1.539(13) . ? C74 C75 1.520(12) . ? C74 C76 1.529(12) . ? C77 C81 1.364(12) . ? C77 C78 1.399(12) . ? C77 Pd3 2.059(9) . ? C78 C79 1.395(12) . ? C78 C99 1.482(13) . ? C79 C80 1.374(13) . ? C80 C82 1.392(13) . ? C81 C82 1.373(12) . ? C81 C83 1.542(13) . ? C83 N9 1.433(11) . ? C84 C86 1.325(13) . ? C84 N10 1.393(11) . ? C85 N10 1.354(11) . ? C85 N9 1.369(11) . ? C85 Pd3 2.037(10) . ? C86 N9 1.379(11) . ? C87 C89 1.389(13) . ? C87 C88 1.402(12) . ? C87 N10 1.445(11) . ? C88 C90 1.409(14) . ? C88 C93 1.509(13) . ? C89 C92 1.401(14) . ? C89 C97 1.532(13) . ? C90 C91 1.383(15) . ? C91 C92 1.356(14) . ? C93 C94 1.521(14) . ? C93 C95 1.532(14) . ? C96 C97 1.537(13) . ? C97 C98 1.514(13) . ? C99 N11 1.450(11) . ? C100 N12 1.329(11) . ? C100 N11 1.350(11) . ? C100 Pd3 2.031(10) . ? C101 C102 1.311(13) . ? C101 N11 1.387(11) . ? C102 N12 1.397(12) . ? C103 C104 1.362(14) . ? C103 C108 1.414(15) . ? C103 N12 1.439(12) . ? C104 C105 1.415(15) . ? C104 C109 1.533(15) . ? C105 C106 1.382(16) . ? C106 C107 1.340(16) . ? C107 C108 1.371(15) . ? C108 C114 1.532(17) . ? C109 C111 1.519(16) . ? C109 C110 1.532(14) . ? C112 C114 1.524(15) . ? C113 C114 1.559(16) . ? Pd1 Br1 2.5153(12) . ? Pd2 Br2 2.4957(12) . ? Pd3 Br3 2.5105(13) . ? O1 C200 1.40(2) . ? O1 C202 1.41(2) . ? C201 C200 1.31(2) . ? C203 C202 1.45(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 C1 N1 105.8(6) . . ? N2 C1 Pd1 133.1(6) . . ? N1 C1 Pd1 120.8(5) . . ? C3 C2 N2 107.6(8) . . ? C2 C3 N1 106.7(8) . . ? N1 C4 C5 109.4(7) . . ? C10 C5 C6 119.6(9) . . ? C10 C5 C4 120.3(9) . . ? C6 C5 C4 120.1(8) . . ? C7 C6 C5 118.0(8) . . ? C7 C6 Pd1 120.2(7) . . ? C5 C6 Pd1 121.8(7) . . ? C6 C7 C8 122.0(9) . . ? C6 C7 C11 118.4(9) . . ? C8 C7 C11 119.5(9) . . ? C9 C8 C7 119.3(10) . . ? C10 C9 C8 119.2(10) . . ? C9 C10 C5 121.8(10) . . ? N3 C11 C7 108.5(7) . . ? N3 C12 C13 105.7(7) . . ? C12 C13 N4 107.2(7) . . ? N4 C14 N3 103.5(6) . . ? N4 C14 Pd1 135.3(6) . . ? N3 C14 Pd1 120.8(5) . . ? C16 C15 C20 123.4(9) . . ? C16 C15 N4 118.7(8) . . ? C20 C15 N4 117.6(8) . . ? C17 C16 C15 116.5(9) . . ? C17 C16 C24 120.4(9) . . ? C15 C16 C24 123.0(8) . . ? C18 C17 C16 122.4(10) . . ? C17 C18 C19 119.4(10) . . ? C18 C19 C20 122.2(10) . . ? C19 C20 C15 116.1(9) . . ? C19 C20 C21 121.1(9) . . ? C15 C20 C21 122.8(9) . . ? C23 C21 C20 114.0(9) . . ? C23 C21 C22 110.0(9) . . ? C20 C21 C22 110.0(8) . . ? C16 C24 C25 111.7(8) . . ? C16 C24 C26 112.2(8) . . ? C25 C24 C26 110.7(8) . . ? C28 C27 C32 123.4(9) . . ? C28 C27 N2 118.6(8) . . ? C32 C27 N2 118.0(7) . . ? C27 C28 C29 117.3(9) . . ? C27 C28 C36 122.8(9) . . ? C29 C28 C36 119.8(9) . . ? C30 C29 C28 120.6(9) . . ? C31 C30 C29 120.0(9) . . ? C30 C31 C32 122.2(10) . . ? C31 C32 C27 116.0(9) . . ? C31 C32 C33 120.6(9) . . ? C27 C32 C33 123.4(8) . . ? C32 C33 C34 112.8(7) . . ? C32 C33 C35 110.6(8) . . ? C34 C33 C35 109.6(8) . . ? C37 C36 C28 115.8(9) . . ? C37 C36 C38 109.0(9) . . ? C28 C36 C38 110.2(8) . . ? N5 C39 N6 104.2(6) . . ? N5 C39 Pd2 120.1(6) . . ? N6 C39 Pd2 135.5(5) . . ? C41 C40 N6 107.8(8) . . ? C40 C41 N5 105.3(7) . . ? N5 C42 C57 108.1(7) . . ? C44 C43 C48 123.6(9) . . ? C44 C43 N6 117.1(8) . . ? C48 C43 N6 118.8(8) . . ? C43 C44 C45 116.7(10) . . ? C43 C44 C52 123.6(9) . . ? C45 C44 C52 119.7(10) . . ? C46 C45 C44 122.5(11) . . ? C45 C46 C47 118.5(10) . . ? C48 C47 C46 121.8(11) . . ? C47 C48 C43 116.8(10) . . ? C47 C48 C49 119.1(10) . . ? C43 C48 C49 124.0(9) . . ? C51 C49 C50 108.3(9) . . ? C51 C49 C48 109.4(9) . . ? C50 C49 C48 114.0(11) . . ? C44 C52 C53 114.7(9) . . ? C44 C52 C54 110.2(8) . . ? C53 C52 C54 109.1(8) . . ? C60 C55 C56 119.1(9) . . ? C60 C55 C61 121.5(8) . . ? C56 C55 C61 119.4(8) . . ? C57 C56 C55 118.9(9) . . ? C57 C56 Pd2 121.0(8) . . ? C55 C56 Pd2 120.0(7) . . ? C56 C57 C58 120.4(10) . . ? C56 C57 C42 120.7(9) . . ? C58 C57 C42 118.8(9) . . ? C59 C58 C57 122.1(10) . . ? C58 C59 C60 119.3(10) . . ? C55 C60 C59 120.1(10) . . ? N7 C61 C55 111.4(6) . . ? C63 C62 N7 106.8(8) . . ? C62 C63 N8 106.7(8) . . ? N7 C64 N8 104.1(8) . . ? N7 C64 Pd2 120.3(7) . . ? N8 C64 Pd2 135.6(7) . . ? C70 C65 C66 123.0(9) . . ? C70 C65 N8 117.7(8) . . ? C66 C65 N8 118.7(8) . . ? C65 C66 C67 116.8(8) . . ? C65 C66 C74 122.8(8) . . ? C67 C66 C74 120.4(8) . . ? C68 C67 C66 120.4(9) . . ? C67 C68 C69 121.9(9) . . ? C68 C69 C70 120.5(9) . . ? C69 C70 C65 117.5(9) . . ? C69 C70 C71 120.1(9) . . ? C65 C70 C71 122.3(9) . . ? C72 C71 C73 110.9(8) . . ? C72 C71 C70 109.9(9) . . ? C73 C71 C70 111.6(8) . . ? C66 C74 C75 113.9(7) . . ? C66 C74 C76 111.3(8) . . ? C75 C74 C76 108.6(8) . . ? C81 C77 C78 119.0(9) . . ? C81 C77 Pd3 122.5(7) . . ? C78 C77 Pd3 118.4(7) . . ? C79 C78 C77 119.0(8) . . ? C79 C78 C99 119.0(8) . . ? C77 C78 C99 121.9(9) . . ? C80 C79 C78 121.1(9) . . ? C79 C80 C82 119.2(10) . . ? C77 C81 C82 122.0(9) . . ? C77 C81 C83 118.4(9) . . ? C82 C81 C83 119.6(8) . . ? C81 C82 C80 119.5(9) . . ? N9 C83 C81 109.9(8) . . ? C86 C84 N10 107.5(9) . . ? N10 C85 N9 104.6(8) . . ? N10 C85 Pd3 134.5(7) . . ? N9 C85 Pd3 120.4(7) . . ? C84 C86 N9 107.2(9) . . ? C89 C87 C88 123.9(9) . . ? C89 C87 N10 118.8(9) . . ? C88 C87 N10 117.2(8) . . ? C87 C88 C90 116.9(9) . . ? C87 C88 C93 124.2(9) . . ? C90 C88 C93 119.0(9) . . ? C87 C89 C92 115.9(10) . . ? C87 C89 C97 122.7(9) . . ? C92 C89 C97 121.4(9) . . ? C91 C90 C88 119.9(10) . . ? C92 C91 C90 121.1(11) . . ? C91 C92 C89 122.2(10) . . ? C88 C93 C94 111.6(9) . . ? C88 C93 C95 114.2(9) . . ? C94 C93 C95 109.0(8) . . ? C98 C97 C89 113.9(8) . . ? C98 C97 C96 108.6(8) . . ? C89 C97 C96 111.8(8) . . ? N11 C99 C78 110.6(8) . . ? N12 C100 N11 103.9(9) . . ? N12 C100 Pd3 135.8(8) . . ? N11 C100 Pd3 120.1(7) . . ? C102 C101 N11 104.3(9) . . ? C101 C102 N12 109.0(10) . . ? C104 C103 C108 122.1(11) . . ? C104 C103 N12 118.4(10) . . ? C108 C103 N12 118.9(11) . . ? C103 C104 C105 119.7(11) . . ? C103 C104 C109 124.1(10) . . ? C105 C104 C109 116.2(12) . . ? C106 C105 C104 117.5(13) . . ? C107 C106 C105 121.4(12) . . ? C106 C107 C108 123.4(13) . . ? C107 C108 C103 115.8(13) . . ? C107 C108 C114 122.1(12) . . ? C103 C108 C114 121.9(11) . . ? C111 C109 C110 110.4(10) . . ? C111 C109 C104 114.7(10) . . ? C110 C109 C104 112.0(9) . . ? C112 C114 C108 113.4(10) . . ? C112 C114 C113 108.8(10) . . ? C108 C114 C113 108.8(11) . . ? C1 N1 C3 111.0(6) . . ? C1 N1 C4 123.9(5) . . ? C3 N1 C4 125.0(5) . . ? C1 N2 C2 108.8(6) . . ? C1 N2 C27 125.5(5) . . ? C2 N2 C27 125.4(5) . . ? C12 N3 C14 112.9(6) . . ? C12 N3 C11 126.8(6) . . ? C14 N3 C11 118.7(5) . . ? C14 N4 C13 110.4(6) . . ? C14 N4 C15 128.5(5) . . ? C13 N4 C15 120.2(5) . . ? C39 N5 C41 112.4(6) . . ? C39 N5 C42 123.9(5) . . ? C41 N5 C42 123.6(5) . . ? C39 N6 C40 110.2(5) . . ? C39 N6 C43 129.5(5) . . ? C40 N6 C43 120.2(5) . . ? C64 N7 C62 111.8(8) . . ? C64 N7 C61 122.4(8) . . ? C62 N7 C61 125.8(8) . . ? C64 N8 C63 110.5(8) . . ? C64 N8 C65 129.4(8) . . ? C63 N8 C65 119.6(7) . . ? C85 N9 C86 110.5(8) . . ? C85 N9 C83 123.0(8) . . ? C86 N9 C83 126.2(8) . . ? C85 N10 C84 110.1(8) . . ? C85 N10 C87 128.1(8) . . ? C84 N10 C87 121.7(8) . . ? C100 N11 C101 112.8(8) . . ? C100 N11 C99 123.3(8) . . ? C101 N11 C99 123.6(8) . . ? C100 N12 C102 110.0(9) . . ? C100 N12 C103 127.7(8) . . ? C102 N12 C103 122.2(8) . . ? C6 Pd1 C14 84.9(4) . . ? C6 Pd1 C1 84.8(3) . . ? C14 Pd1 C1 169.8(4) . . ? C6 Pd1 Br1 177.7(3) . . ? C14 Pd1 Br1 92.9(2) . . ? C1 Pd1 Br1 97.3(2) . . ? C56 Pd2 C39 85.5(4) . . ? C56 Pd2 C64 87.0(3) . . ? C39 Pd2 C64 172.4(3) . . ? C56 Pd2 Br2 178.3(3) . . ? C39 Pd2 Br2 94.8(2) . . ? C64 Pd2 Br2 92.5(3) . . ? C100 Pd3 C85 172.1(4) . . ? C100 Pd3 C77 86.2(4) . . ? C85 Pd3 C77 86.0(4) . . ? C100 Pd3 Br3 93.5(3) . . ? C85 Pd3 Br3 94.2(3) . . ? C77 Pd3 Br3 178.6(3) . . ? C200 O1 C202 112.7(17) . . ? C201 C200 O1 119(2) . . ? O1 C202 C203 111.1(17) . . ? _diffrn_measured_fraction_theta_max 0.733 _diffrn_reflns_theta_full 30.43 _diffrn_measured_fraction_theta_full 0.733 _refine_diff_density_max 0.917 _refine_diff_density_min -1.113 _refine_diff_density_rms 0.154 #==END data_compound8 _database_code_CSD 194845 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 00sw003 _chemical_melting_point ? _chemical_formula_moiety 'C76 H92 Cl4 N8 Pd2' _chemical_formula_sum 'C76 H92 Cl4 N8 Pd2' _chemical_formula_weight 1472.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.948(3) _cell_length_b 33.444(7) _cell_length_c 16.958(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.70(3) _cell_angle_gamma 90.00 _cell_volume 9501(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28621 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Octahedron _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9492 _exptl_absorpt_correction_T_max 0.9792 _exptl_absorpt_process_details Sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33683 _diffrn_reflns_av_R_equivalents 0.2468 _diffrn_reflns_av_sigmaI/netI 0.4396 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.04 _reflns_number_total 12810 _reflns_number_gt 3479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo a. Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1091P)^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 12810 _refine_ls_number_parameters 827 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.3377 _refine_ls_R_factor_gt 0.0982 _refine_ls_wR_factor_ref 0.2694 _refine_ls_wR_factor_gt 0.2110 _refine_ls_goodness_of_fit_ref 0.840 _refine_ls_restrained_S_all 0.839 _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 C1 C 0.5232(16) 0.1067(8) 0.480(2) 0.132(11) Uani 1 1 d . . . H1 H 0.4857 0.1244 0.4506 0.158 Uiso 1 1 calc R . . C2 C 0.5417(17) 0.1087(7) 0.5660(16) 0.106(9) Uani 1 1 d . . . H2 H 0.5145 0.1273 0.5947 0.127 Uiso 1 1 calc R . . C3 C 0.5974(12) 0.0843(7) 0.6057(14) 0.075(7) Uani 1 1 d . . . C4 C 0.6351(10) 0.0566(5) 0.5650(12) 0.050(5) Uani 1 1 d . . . C5 C 0.6220(13) 0.0535(7) 0.4808(12) 0.075(7) Uani 1 1 d . . . C6 C 0.5617(16) 0.0785(7) 0.4428(11) 0.103(8) Uani 1 1 d . . . H6 H 0.5466 0.0754 0.3869 0.124 Uiso 1 1 calc R . . C7 C 0.6651(14) 0.0236(6) 0.4380(12) 0.085(8) Uani 1 1 d . . . H7 H 0.7080 0.0116 0.4780 0.102 Uiso 1 1 calc R . . C8 C 0.6041(14) -0.0109(5) 0.4082(12) 0.118(9) Uani 1 1 d . . . H8A H 0.5885 -0.0248 0.4543 0.177 Uiso 1 1 calc R . . H8B H 0.6294 -0.0299 0.3758 0.177 Uiso 1 1 calc R . . H8C H 0.5567 0.0006 0.3760 0.177 Uiso 1 1 calc R . . C9 C 0.7064(12) 0.0430(6) 0.3717(11) 0.115(9) Uani 1 1 d . . . H9A H 0.6670 0.0470 0.3238 0.172 Uiso 1 1 calc R . . H9B H 0.7490 0.0254 0.3592 0.172 Uiso 1 1 calc R . . H9C H 0.7292 0.0688 0.3904 0.172 Uiso 1 1 calc R . . C10 C 0.6065(11) 0.0889(7) 0.6960(12) 0.071(6) Uani 1 1 d . . . H10 H 0.6633 0.0824 0.7175 0.085 Uiso 1 1 calc R . . C11 C 0.5555(14) 0.0580(6) 0.7294(10) 0.111(9) Uani 1 1 d . . . H11A H 0.5008 0.0680 0.7260 0.167 Uiso 1 1 calc R . . H11B H 0.5773 0.0527 0.7853 0.167 Uiso 1 1 calc R . . H11C H 0.5554 0.0332 0.6986 0.167 Uiso 1 1 calc R . . C12 C 0.5874(14) 0.1291(8) 0.7331(15) 0.156(11) Uani 1 1 d . . . H12A H 0.6253 0.1495 0.7206 0.233 Uiso 1 1 calc R . . H12B H 0.5918 0.1262 0.7911 0.233 Uiso 1 1 calc R . . H12C H 0.5330 0.1374 0.7111 0.233 Uiso 1 1 calc R . . C13 C 0.7608(12) 0.0412(5) 0.6488(9) 0.044(5) Uani 1 1 d . . . C14 C 0.6706(11) -0.0080(6) 0.6226(11) 0.059(6) Uani 1 1 d . . . H14 H 0.6230 -0.0212 0.5995 0.071 Uiso 1 1 calc R . . C15 C 0.7321(13) -0.0254(5) 0.6700(10) 0.057(6) Uani 1 1 d . . . H15 H 0.7355 -0.0519 0.6900 0.068 Uiso 1 1 calc R . . C16 C 0.8721(10) 0.0002(4) 0.7321(9) 0.042(5) Uani 1 1 d . . . H16A H 0.8785 0.0216 0.7729 0.050 Uiso 1 1 calc R . . H16B H 0.8748 -0.0257 0.7607 0.050 Uiso 1 1 calc R . . C17 C 0.9400(11) 0.0024(5) 0.6878(10) 0.038(5) Uani 1 1 d U . . C18 C 0.9387(12) -0.0281(5) 0.6328(11) 0.065(6) Uani 1 1 d . . . H18 H 0.8947 -0.0460 0.6241 0.078 Uiso 1 1 calc R . . C19 C 1.0053(14) -0.0327(6) 0.5880(10) 0.063(6) Uani 1 1 d . . . H19 H 1.0078 -0.0549 0.5534 0.076 Uiso 1 1 calc R . . C20 C 1.0640(13) -0.0043(6) 0.5972(12) 0.063(6) Uani 1 1 d . . . H20 H 1.1081 -0.0062 0.5689 0.076 Uiso 1 1 calc R . . C21 C 1.0577(11) 0.0280(5) 0.6495(11) 0.055(6) Uani 1 1 d . . . H21 H 1.0964 0.0487 0.6540 0.066 Uiso 1 1 calc R . . C22 C 0.9968(11) 0.0300(5) 0.6938(9) 0.035(5) Uani 1 1 d . . . C23 C 1.0036(10) 0.0622(5) 0.7533(9) 0.042(5) Uani 1 1 d . . . H23A H 1.0529 0.0580 0.7918 0.050 Uiso 1 1 calc R . . H23B H 0.9579 0.0604 0.7831 0.050 Uiso 1 1 calc R . . C24 C 0.9384(11) 0.1201(5) 0.6746(9) 0.040(5) Uani 1 1 d . . . C25 C 1.0733(12) 0.1281(6) 0.7252(11) 0.071(7) Uani 1 1 d . . . H25 H 1.1257 0.1233 0.7522 0.085 Uiso 1 1 calc R . . C26 C 1.0439(11) 0.1614(6) 0.6820(10) 0.057(6) Uani 1 1 d . . . H26 H 1.0747 0.1841 0.6724 0.068 Uiso 1 1 calc R . . C27 C 0.9146(10) 0.1855(5) 0.6024(10) 0.038(4) Uani 1 1 d U . . C28 C 0.9286(11) 0.1917(6) 0.5254(11) 0.050(5) Uani 1 1 d U . . C29 C 0.8843(14) 0.2175(5) 0.4805(12) 0.077(7) Uani 1 1 d . . . H29 H 0.8882 0.2187 0.4253 0.092 Uiso 1 1 calc R . . C30 C 0.8313(15) 0.2434(6) 0.5110(14) 0.100(9) Uani 1 1 d . . . H30 H 0.8068 0.2652 0.4807 0.120 Uiso 1 1 calc R . . C31 C 0.8166(14) 0.2354(6) 0.5880(15) 0.094(8) Uani 1 1 d . . . H31 H 0.7765 0.2504 0.6084 0.113 Uiso 1 1 calc R . . C32 C 0.8602(10) 0.2050(6) 0.6384(11) 0.051(5) Uani 1 1 d . . . C33 C 0.9845(14) 0.1683(5) 0.4873(11) 0.077(7) Uani 1 1 d . . . H33 H 1.0038 0.1459 0.5242 0.092 Uiso 1 1 calc R . . C34 C 1.0576(11) 0.1948(6) 0.4782(10) 0.082(7) Uani 1 1 d . . . H34A H 1.0447 0.2120 0.4313 0.123 Uiso 1 1 calc R . . H34B H 1.1031 0.1777 0.4717 0.123 Uiso 1 1 calc R . . H34C H 1.0712 0.2114 0.5260 0.123 Uiso 1 1 calc R . . C35 C 0.9459(13) 0.1492(5) 0.4058(10) 0.106(8) Uani 1 1 d . . . H35A H 0.8994 0.1332 0.4140 0.158 Uiso 1 1 calc R . . H35B H 0.9851 0.1321 0.3854 0.158 Uiso 1 1 calc R . . H35C H 0.9290 0.1705 0.3671 0.158 Uiso 1 1 calc R . . C36 C 0.8405(14) 0.1988(5) 0.7216(12) 0.080(7) Uani 1 1 d . . . H36 H 0.8512 0.1699 0.7340 0.096 Uiso 1 1 calc R . . C37 C 0.8967(15) 0.2218(6) 0.7828(11) 0.135(11) Uani 1 1 d . . . H37A H 0.9519 0.2148 0.7779 0.202 Uiso 1 1 calc R . . H37B H 0.8861 0.2149 0.8364 0.202 Uiso 1 1 calc R . . H37C H 0.8886 0.2505 0.7737 0.202 Uiso 1 1 calc R . . C38 C 0.7501(14) 0.2061(7) 0.7323(14) 0.159(12) Uani 1 1 d . . . H38A H 0.7353 0.2338 0.7182 0.238 Uiso 1 1 calc R . . H38B H 0.7437 0.2011 0.7879 0.238 Uiso 1 1 calc R . . H38C H 0.7156 0.1878 0.6974 0.238 Uiso 1 1 calc R . . C39 C 0.2862(14) 0.2235(6) 0.0438(14) 0.086(7) Uani 1 1 d . . . H39 H 0.3282 0.2304 0.0150 0.103 Uiso 1 1 calc R . . C40 C 0.2876(15) 0.2366(6) 0.1221(16) 0.103(9) Uani 1 1 d . . . H40 H 0.3292 0.2535 0.1466 0.124 Uiso 1 1 calc R . . C41 C 0.2252(15) 0.2241(6) 0.1650(11) 0.070(7) Uani 1 1 d . . . H41 H 0.2269 0.2326 0.2187 0.083 Uiso 1 1 calc R . . C42 C 0.1635(12) 0.2004(5) 0.1320(12) 0.047(5) Uani 1 1 d . . . C43 C 0.1652(12) 0.1902(5) 0.0537(11) 0.045(5) Uani 1 1 d . . . C44 C 0.2232(12) 0.2006(6) 0.0089(12) 0.054(6) Uani 1 1 d . . . C45 C 0.2226(11) 0.1874(5) -0.0784(10) 0.055(5) Uani 1 1 d . . . H45 H 0.1826 0.1655 -0.0913 0.066 Uiso 1 1 calc R . . C46 C 0.1975(14) 0.2232(5) -0.1324(11) 0.123(10) Uani 1 1 d . . . H46A H 0.2288 0.2467 -0.1123 0.184 Uiso 1 1 calc R . . H46B H 0.1406 0.2287 -0.1327 0.184 Uiso 1 1 calc R . . H46C H 0.2069 0.2172 -0.1867 0.184 Uiso 1 1 calc R . . C47 C 0.3033(12) 0.1723(6) -0.0911(11) 0.111(9) Uani 1 1 d . . . H47A H 0.3409 0.1947 -0.0881 0.166 Uiso 1 1 calc R . . H47B H 0.2992 0.1597 -0.1438 0.166 Uiso 1 1 calc R . . H47C H 0.3225 0.1526 -0.0498 0.166 Uiso 1 1 calc R . . C48 C 0.1003(12) 0.1873(5) 0.1817(12) 0.069(6) Uani 1 1 d . . . H48 H 0.0728 0.1637 0.1537 0.083 Uiso 1 1 calc R . . C49 C 0.0363(12) 0.2196(5) 0.1827(11) 0.101(8) Uani 1 1 d . . . H49A H 0.0611 0.2442 0.2062 0.151 Uiso 1 1 calc R . . H49B H -0.0038 0.2103 0.2146 0.151 Uiso 1 1 calc R . . H49C H 0.0105 0.2249 0.1281 0.151 Uiso 1 1 calc R . . C50 C 0.1375(12) 0.1725(5) 0.2666(10) 0.088(7) Uani 1 1 d . . . H50A H 0.1718 0.1494 0.2616 0.133 Uiso 1 1 calc R . . H50B H 0.0947 0.1648 0.2965 0.133 Uiso 1 1 calc R . . H50C H 0.1692 0.1941 0.2949 0.133 Uiso 1 1 calc R . . C51 C 0.0923(9) 0.1253(5) 0.0062(9) 0.029(4) Uani 1 1 d U . . C52 C 0.0206(11) 0.1852(6) -0.0152(10) 0.052(5) Uani 1 1 d U . . H52 H 0.0082 0.2130 -0.0171 0.063 Uiso 1 1 calc R . . C53 C -0.0279(11) 0.1560(5) -0.0383(10) 0.062(6) Uani 1 1 d . . . H53 H -0.0831 0.1583 -0.0583 0.074 Uiso 1 1 calc R . . C54 C -0.0186(9) 0.0795(5) -0.0385(8) 0.043(5) Uani 1 1 d . . . H54A H -0.0610 0.0794 -0.0856 0.052 Uiso 1 1 calc R . . H54B H 0.0235 0.0606 -0.0492 0.052 Uiso 1 1 calc R . . C55 C -0.0522(9) 0.0656(5) 0.0310(10) 0.032(4) Uani 1 1 d . . . C56 C -0.0305(10) 0.0800(5) 0.1106(11) 0.049(5) Uani 1 1 d . . . H56 H 0.0073 0.1012 0.1185 0.058 Uiso 1 1 calc R . . C57 C -0.0590(13) 0.0663(6) 0.1757(10) 0.065(7) Uani 1 1 d . . . H57 H -0.0410 0.0775 0.2267 0.078 Uiso 1 1 calc R . . C58 C -0.1150(11) 0.0355(5) 0.1669(10) 0.049(5) Uani 1 1 d . . . H58 H -0.1370 0.0257 0.2115 0.059 Uiso 1 1 calc R . . C59 C -0.1374(10) 0.0199(4) 0.0928(10) 0.045(5) Uani 1 1 d . . . H59 H -0.1737 -0.0019 0.0875 0.054 Uiso 1 1 calc R . . C60 C -0.1105(10) 0.0338(5) 0.0239(9) 0.038(5) Uani 1 1 d . . . C61 C -0.1402(11) 0.0128(5) -0.0550(9) 0.049(5) Uani 1 1 d . . . H61A H -0.1336 0.0309 -0.0997 0.059 Uiso 1 1 calc R . . H61B H -0.1070 -0.0112 -0.0596 0.059 Uiso 1 1 calc R . . C77 C 0.4906(12) 0.1143(5) -0.0140(13) 0.071(6) Uani 1 1 d . . . H77 H 0.5303 0.1321 -0.0271 0.086 Uiso 1 1 calc R . . C78 C 0.4566(11) 0.0854(6) -0.0705(10) 0.067(6) Uani 1 1 d . . . H78 H 0.4713 0.0856 -0.1223 0.080 Uiso 1 1 calc R . . C79 C 0.4029(11) 0.0570(5) -0.0524(10) 0.049(5) Uani 1 1 d . . . C80 C 0.3816(10) 0.0593(5) 0.0274(12) 0.057(6) Uani 1 1 d . . . C81 C 0.4144(10) 0.0902(5) 0.0828(10) 0.041(5) Uani 1 1 d . . . C82 C 0.4668(11) 0.1165(6) 0.0584(11) 0.069(7) Uani 1 1 d . . . H82 H 0.4875 0.1373 0.0937 0.083 Uiso 1 1 calc R . . C83 C 0.3883(10) 0.0911(5) 0.1663(8) 0.049(5) Uani 1 1 d . . . H83 H 0.3385 0.0749 0.1650 0.059 Uiso 1 1 calc R . . C84 C 0.4506(10) 0.0749(5) 0.2280(9) 0.080(7) Uani 1 1 d . . . H84A H 0.4503 0.0456 0.2250 0.120 Uiso 1 1 calc R . . H84B H 0.4401 0.0833 0.2808 0.120 Uiso 1 1 calc R . . H84C H 0.5029 0.0849 0.2193 0.120 Uiso 1 1 calc R . . C85 C 0.3699(11) 0.1349(5) 0.1830(11) 0.086(7) Uani 1 1 d . . . H85A H 0.3123 0.1381 0.1822 0.129 Uiso 1 1 calc R . . H85B H 0.3875 0.1520 0.1421 0.129 Uiso 1 1 calc R . . H85C H 0.3982 0.1425 0.2356 0.129 Uiso 1 1 calc R . . C86 C 0.3590(11) 0.0272(6) -0.1102(11) 0.064(6) Uani 1 1 d . . . H86 H 0.3101 0.0175 -0.0896 0.077 Uiso 1 1 calc R . . C87 C 0.3361(11) 0.0441(6) -0.1946(10) 0.097(8) Uani 1 1 d . . . H87A H 0.3142 0.0711 -0.1915 0.145 Uiso 1 1 calc R . . H87B H 0.2959 0.0268 -0.2251 0.145 Uiso 1 1 calc R . . H87C H 0.3836 0.0452 -0.2211 0.145 Uiso 1 1 calc R . . C88 C 0.4162(12) -0.0072(7) -0.1141(13) 0.126(9) Uani 1 1 d . . . H88A H 0.4345 -0.0173 -0.0602 0.189 Uiso 1 1 calc R . . H88B H 0.4622 0.0020 -0.1379 0.189 Uiso 1 1 calc R . . H88C H 0.3890 -0.0287 -0.1469 0.189 Uiso 1 1 calc R . . C89 C 0.2453(9) 0.0356(4) 0.0450(8) 0.026(4) Uani 1 1 d U . . C90 C 0.3496(11) -0.0085(5) 0.0667(9) 0.051(5) Uani 1 1 d . . . H90 H 0.4022 -0.0189 0.0711 0.061 Uiso 1 1 calc R . . C91 C -0.2813(11) 0.0289(5) -0.0759(9) 0.045(5) Uani 1 1 d U . . H91 H -0.2765 0.0563 -0.0891 0.053 Uiso 1 1 calc R . . N1 N 0.6865(9) 0.0302(5) 0.6131(8) 0.044(4) Uani 1 1 d . . . N2 N 0.7885(9) 0.0042(4) 0.6828(7) 0.042(4) Uani 1 1 d . . . N3 N 1.0056(9) 0.1033(5) 0.7189(8) 0.046(4) Uani 1 1 d . . . N4 N 0.9597(8) 0.1567(4) 0.6534(6) 0.033(4) Uani 1 1 d . . . N5 N 0.0952(9) 0.1678(4) 0.0132(8) 0.054(4) Uani 1 1 d . . . N6 N 0.0161(8) 0.1202(4) -0.0285(6) 0.039(4) Uani 1 1 d . . . N7 N 0.3258(9) 0.0301(4) 0.0498(8) 0.046(4) Uani 1 1 d U . . N8 N -0.2217(9) 0.0011(4) -0.0620(7) 0.046(4) Uani 1 1 d . . . Cl1 Cl 0.8515(3) 0.07830(11) 0.5268(2) 0.0466(12) Uani 1 1 d . . . Cl2 Cl 0.8173(2) 0.09759(11) 0.7902(2) 0.0435(13) Uani 1 1 d . . . Cl3 Cl 0.1730(2) 0.08731(11) 0.1624(2) 0.0416(11) Uani 1 1 d . . . Cl4 Cl 0.1813(2) 0.08224(12) -0.1084(2) 0.0437(12) Uani 1 1 d . . . Pd1 Pd 0.17520(7) 0.08372(4) 0.02667(7) 0.0368(4) Uani 1 1 d . . . Pd2 Pd 0.83688(8) 0.08630(4) 0.65766(7) 0.0409(4) Uani 1 1 d . . . 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 C1 0.12(3) 0.10(2) 0.18(3) -0.01(2) 0.07(3) 0.050(18) C2 0.12(3) 0.13(2) 0.071(19) -0.044(18) 0.043(19) -0.03(2) C3 0.042(14) 0.092(18) 0.079(18) 0.010(16) -0.025(12) 0.042(14) C4 0.032(13) 0.032(12) 0.086(17) -0.005(12) 0.005(12) 0.022(10) C5 0.090(19) 0.089(18) 0.030(13) 0.001(13) -0.036(13) 0.004(14) C6 0.15(3) 0.11(2) 0.033(13) 0.022(14) -0.030(15) 0.006(18) C7 0.11(2) 0.076(17) 0.052(15) -0.029(14) -0.037(14) 0.024(16) C8 0.16(3) 0.066(16) 0.11(2) -0.026(14) -0.019(18) 0.001(16) C9 0.09(2) 0.19(3) 0.053(15) 0.052(16) -0.001(14) 0.012(17) C10 0.055(15) 0.098(18) 0.062(15) -0.003(15) 0.012(12) 0.025(14) C11 0.14(2) 0.17(2) 0.031(13) 0.013(14) 0.021(14) 0.01(2) C12 0.10(2) 0.20(3) 0.16(3) -0.07(2) 0.02(2) -0.01(2) C13 0.077(16) 0.028(12) 0.030(11) 0.010(9) 0.019(11) 0.009(11) C14 0.057(16) 0.040(15) 0.075(16) -0.001(11) -0.002(13) -0.025(12) C15 0.089(18) 0.019(12) 0.060(14) 0.004(10) 0.006(13) -0.035(13) C16 0.056(14) 0.044(11) 0.023(10) 0.010(8) -0.003(10) 0.001(10) C17 0.038(5) 0.038(5) 0.037(5) -0.0001(10) 0.0058(12) 0.0002(10) C18 0.050(15) 0.078(15) 0.057(14) 0.014(12) -0.024(12) -0.015(12) C19 0.075(18) 0.078(18) 0.036(12) -0.004(12) 0.006(12) 0.036(14) C20 0.083(19) 0.045(15) 0.065(16) 0.028(12) 0.022(14) 0.022(13) C21 0.061(16) 0.050(14) 0.053(14) -0.012(11) 0.004(12) 0.002(12) C22 0.055(14) 0.021(11) 0.032(10) 0.010(8) 0.017(10) 0.009(10) C23 0.057(13) 0.027(11) 0.037(11) 0.002(9) -0.003(10) 0.004(10) C24 0.070(15) 0.018(11) 0.032(11) -0.012(8) 0.013(10) -0.007(11) C25 0.061(16) 0.066(15) 0.078(16) 0.039(12) -0.015(13) -0.033(13) C26 0.045(15) 0.079(17) 0.048(13) -0.016(11) 0.014(11) -0.041(13) C27 0.038(5) 0.037(5) 0.038(5) 0.0000(10) 0.0055(12) 0.0002(10) C28 0.050(5) 0.050(5) 0.050(5) 0.0001(10) 0.0075(13) 0.0004(10) C29 0.12(2) 0.041(14) 0.064(15) 0.017(12) 0.004(14) 0.028(13) C30 0.15(3) 0.073(18) 0.068(18) 0.029(15) -0.030(17) 0.043(16) C31 0.13(2) 0.053(16) 0.11(2) -0.026(15) 0.061(19) 0.023(15) C32 0.037(13) 0.068(14) 0.043(13) 0.017(11) -0.008(10) 0.017(11) C33 0.12(2) 0.060(15) 0.054(14) 0.029(11) 0.024(15) 0.004(15) C34 0.081(18) 0.101(17) 0.071(15) 0.010(13) 0.035(13) 0.038(15) C35 0.18(2) 0.096(17) 0.034(13) -0.003(12) -0.019(15) -0.030(16) C36 0.14(2) 0.056(14) 0.053(15) 0.004(12) 0.032(16) 0.009(14) C37 0.23(3) 0.14(2) 0.034(14) -0.011(14) 0.018(18) -0.06(2) C38 0.11(2) 0.25(3) 0.14(3) 0.03(2) 0.11(2) 0.05(2) C39 0.08(2) 0.101(19) 0.085(19) -0.013(15) 0.046(16) 0.008(16) C40 0.14(3) 0.053(16) 0.13(2) -0.016(16) 0.07(2) -0.025(15) C41 0.10(2) 0.070(16) 0.028(12) -0.027(11) -0.016(13) 0.026(15) C42 0.059(16) 0.032(12) 0.050(14) -0.008(10) 0.007(12) 0.008(11) C43 0.056(16) 0.044(13) 0.034(12) 0.014(10) 0.009(12) 0.011(11) C44 0.033(14) 0.075(15) 0.048(14) 0.013(12) -0.010(12) -0.008(12) C45 0.065(16) 0.066(14) 0.034(12) 0.009(10) 0.005(11) -0.015(12) C46 0.25(3) 0.062(15) 0.064(16) 0.031(13) 0.036(18) 0.034(17) C47 0.09(2) 0.15(2) 0.11(2) -0.053(16) 0.082(16) -0.035(17) C48 0.081(17) 0.050(14) 0.083(17) -0.042(12) 0.036(15) 0.009(13) C49 0.12(2) 0.066(15) 0.13(2) -0.028(13) 0.043(16) 0.037(14) C50 0.16(2) 0.065(14) 0.047(14) -0.008(11) 0.023(15) 0.014(14) C51 0.029(4) 0.029(4) 0.029(4) -0.0002(10) 0.0045(12) 0.0001(10) C52 0.052(5) 0.052(5) 0.052(5) 0.0000(10) 0.0077(13) 0.0002(10) C53 0.057(15) 0.044(13) 0.084(15) 0.020(11) 0.011(12) 0.024(12) C54 0.052(12) 0.058(13) 0.023(9) 0.004(9) 0.018(9) -0.014(11) C55 0.029(11) 0.031(11) 0.041(12) -0.003(9) 0.023(9) 0.006(9) C56 0.048(12) 0.027(11) 0.069(13) -0.015(11) 0.005(11) -0.005(10) C57 0.11(2) 0.068(16) 0.020(11) 0.023(10) 0.018(12) 0.043(14) C58 0.066(15) 0.031(12) 0.048(13) 0.017(10) -0.004(11) -0.022(11) C59 0.057(14) 0.028(11) 0.046(12) -0.007(10) -0.006(11) -0.017(9) C60 0.060(14) 0.042(12) 0.012(10) 0.010(9) 0.004(9) 0.011(10) C61 0.074(16) 0.050(13) 0.026(11) -0.001(9) 0.015(11) -0.025(12) C77 0.061(16) 0.065(15) 0.090(18) -0.026(14) 0.021(14) -0.035(12) C78 0.045(13) 0.115(18) 0.046(13) 0.021(14) 0.025(10) -0.028(14) C79 0.043(14) 0.075(15) 0.025(11) 0.003(11) -0.004(10) 0.007(11) C80 0.035(13) 0.051(13) 0.078(16) -0.007(12) -0.012(12) 0.024(11) C81 0.035(12) 0.037(12) 0.051(12) -0.027(10) 0.006(10) -0.001(10) C82 0.054(15) 0.108(18) 0.043(13) -0.023(13) 0.000(11) -0.063(13) C83 0.044(12) 0.080(15) 0.023(10) -0.010(11) 0.005(9) 0.007(11) C84 0.069(15) 0.114(17) 0.047(13) -0.001(12) -0.024(11) -0.012(13) C85 0.103(19) 0.068(15) 0.098(18) -0.007(13) 0.051(15) 0.022(14) C86 0.031(13) 0.108(17) 0.048(14) -0.030(12) -0.012(11) 0.008(12) C87 0.068(16) 0.18(2) 0.040(13) -0.023(14) 0.017(12) 0.012(15) C88 0.040(16) 0.23(3) 0.11(2) -0.041(19) 0.002(14) 0.001(18) C89 0.026(4) 0.026(4) 0.026(4) -0.0005(10) 0.0038(12) -0.0002(10) C90 0.052(14) 0.043(13) 0.055(13) 0.008(10) -0.001(10) 0.028(11) C91 0.044(5) 0.044(5) 0.045(5) 0.0000(10) 0.0067(13) 0.0001(10) N1 0.042(11) 0.037(11) 0.045(10) -0.001(8) -0.020(8) -0.003(9) N2 0.067(12) 0.040(10) 0.023(8) -0.001(7) 0.013(8) -0.008(9) N3 0.038(11) 0.064(12) 0.031(9) 0.001(8) -0.005(8) 0.021(9) N4 0.047(10) 0.026(9) 0.023(8) 0.003(7) -0.001(8) -0.004(8) N5 0.051(12) 0.068(12) 0.044(10) 0.006(8) 0.012(9) -0.005(10) N6 0.057(11) 0.045(10) 0.012(7) 0.002(7) -0.004(7) -0.008(9) N7 0.046(4) 0.046(4) 0.046(4) -0.0001(10) 0.0067(12) 0.0001(10) N8 0.050(12) 0.044(10) 0.041(9) -0.007(7) 0.001(8) 0.013(9) Cl1 0.065(3) 0.049(3) 0.028(2) -0.001(2) 0.013(2) -0.002(3) Cl2 0.040(3) 0.062(3) 0.028(2) 0.002(2) 0.002(2) 0.006(2) Cl3 0.055(3) 0.043(3) 0.027(2) 0.000(2) 0.008(2) 0.005(3) Cl4 0.046(3) 0.054(3) 0.032(2) -0.003(2) 0.007(2) -0.004(3) Pd1 0.0416(10) 0.0335(8) 0.0342(8) 0.0005(7) 0.0024(7) -0.0008(8) Pd2 0.0466(10) 0.0442(9) 0.0305(8) 0.0003(7) 0.0013(7) 0.0016(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 C1 C6 1.35(3) . ? C1 C2 1.45(3) . ? C2 C3 1.35(3) . ? C3 C4 1.37(2) . ? C3 C10 1.52(2) . ? C4 N1 1.410(19) . ? C4 C5 1.42(2) . ? C5 C6 1.40(3) . ? C5 C7 1.49(2) . ? C7 C9 1.55(2) . ? C7 C8 1.58(2) . ? C10 C11 1.51(2) . ? C10 C12 1.54(2) . ? C13 N1 1.362(19) . ? C13 N2 1.414(17) . ? C13 Pd2 1.976(17) . ? C14 N1 1.320(17) . ? C14 C15 1.35(2) . ? C15 N2 1.368(17) . ? C16 C17 1.467(19) . ? C16 N2 1.540(18) . ? C17 C22 1.328(19) . ? C17 C18 1.38(2) . ? C18 C19 1.46(2) . ? C19 C20 1.37(2) . ? C20 C21 1.41(2) . ? C21 C22 1.37(2) . ? C22 C23 1.468(18) . ? C23 N3 1.495(17) . ? C24 N4 1.343(16) . ? C24 N3 1.384(18) . ? C24 Pd2 2.043(17) . ? C25 C26 1.38(2) . ? C25 N3 1.408(19) . ? C26 N4 1.443(18) . ? C27 C32 1.35(2) . ? C27 C28 1.38(2) . ? C27 N4 1.435(17) . ? C28 C29 1.31(2) . ? C28 C33 1.45(2) . ? C29 C30 1.40(2) . ? C30 C31 1.39(2) . ? C31 C32 1.46(2) . ? C32 C36 1.51(2) . ? C33 C34 1.55(2) . ? C33 C35 1.57(2) . ? C36 C37 1.51(2) . ? C36 C38 1.59(2) . ? C39 C44 1.37(2) . ? C39 C40 1.40(3) . ? C40 C41 1.44(2) . ? C41 C42 1.36(2) . ? C42 C43 1.38(2) . ? C42 C48 1.52(2) . ? C43 C44 1.37(2) . ? C43 N5 1.48(2) . ? C44 C45 1.54(2) . ? C45 C47 1.50(2) . ? C45 C46 1.528(19) . ? C48 C49 1.53(2) . ? C48 C50 1.56(2) . ? C51 N6 1.346(17) . ? C51 N5 1.427(16) . ? C51 Pd1 1.969(15) . ? C52 C53 1.300(19) . ? C52 N5 1.408(19) . ? C53 N6 1.406(17) . ? C54 C55 1.461(17) . ? C54 N6 1.483(16) . ? C55 C56 1.429(19) . ? C55 C60 1.444(19) . ? C56 C57 1.349(19) . ? C57 C58 1.39(2) . ? C58 C59 1.362(19) . ? C59 C60 1.396(18) . ? C60 C61 1.529(19) . ? C61 N8 1.423(18) . ? C77 C82 1.35(2) . ? C77 C78 1.42(2) . ? C78 C79 1.38(2) . ? C79 C80 1.45(2) . ? C79 C86 1.51(2) . ? C80 C81 1.45(2) . ? C80 N7 1.447(19) . ? C81 C82 1.36(2) . ? C81 C83 1.547(19) . ? C83 C84 1.475(19) . ? C83 C85 1.532(18) . ? C86 C88 1.51(2) . ? C86 C87 1.53(2) . ? C89 N8 1.336(16) 3 ? C89 N7 1.366(17) . ? C89 Pd1 1.996(15) . ? C90 N7 1.370(16) . ? C90 C91 1.372(19) 3 ? C91 N8 1.367(17) . ? C91 C90 1.372(19) 3 ? N8 C89 1.336(16) 3 ? Cl1 Pd2 2.286(4) . ? Cl2 Pd2 2.352(4) . ? Cl3 Pd1 2.310(4) . ? Cl4 Pd1 2.309(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 C6 C1 C2 117(3) . . ? C3 C2 C1 120(2) . . ? C2 C3 C4 120(2) . . ? C2 C3 C10 113(2) . . ? C4 C3 C10 126.2(19) . . ? C3 C4 N1 115.3(19) . . ? C3 C4 C5 122.9(19) . . ? N1 C4 C5 121.8(17) . . ? C6 C5 C4 114(2) . . ? C6 C5 C7 123.6(19) . . ? C4 C5 C7 121.7(19) . . ? C1 C6 C5 125(2) . . ? C5 C7 C9 112.3(18) . . ? C5 C7 C8 107.5(19) . . ? C9 C7 C8 114.7(17) . . ? C11 C10 C3 109.3(18) . . ? C11 C10 C12 106.1(18) . . ? C3 C10 C12 120.3(19) . . ? N1 C13 N2 99.9(14) . . ? N1 C13 Pd2 142.0(14) . . ? N2 C13 Pd2 117.7(14) . . ? N1 C14 C15 109.6(16) . . ? C14 C15 N2 104.0(15) . . ? C17 C16 N2 116.5(13) . . ? C22 C17 C18 120.2(18) . . ? C22 C17 C16 127.6(18) . . ? C18 C17 C16 112.1(18) . . ? C17 C18 C19 119.6(18) . . ? C20 C19 C18 118.3(19) . . ? C19 C20 C21 119(2) . . ? C22 C21 C20 121.2(18) . . ? C17 C22 C21 121.5(17) . . ? C17 C22 C23 123.0(17) . . ? C21 C22 C23 115.2(17) . . ? C22 C23 N3 114.3(12) . . ? N4 C24 N3 106.5(15) . . ? N4 C24 Pd2 136.3(14) . . ? N3 C24 Pd2 117.3(12) . . ? C26 C25 N3 102.1(17) . . ? C25 C26 N4 110.5(16) . . ? C32 C27 C28 125.7(18) . . ? C32 C27 N4 113.0(16) . . ? C28 C27 N4 121.3(17) . . ? C29 C28 C27 119(2) . . ? C29 C28 C33 117(2) . . ? C27 C28 C33 123.9(19) . . ? C28 C29 C30 122(2) . . ? C29 C30 C31 116.4(19) . . ? C30 C31 C32 122.5(19) . . ? C27 C32 C31 113.2(17) . . ? C27 C32 C36 128.2(17) . . ? C31 C32 C36 118.7(18) . . ? C28 C33 C34 108.8(16) . . ? C28 C33 C35 113.4(19) . . ? C34 C33 C35 112.2(16) . . ? C37 C36 C32 111.4(18) . . ? C37 C36 C38 111.3(18) . . ? C32 C36 C38 116.0(18) . . ? C44 C39 C40 119(2) . . ? C39 C40 C41 119(2) . . ? C42 C41 C40 122.7(19) . . ? C41 C42 C43 114.5(19) . . ? C41 C42 C48 120(2) . . ? C43 C42 C48 125.5(19) . . ? C44 C43 C42 126(2) . . ? C44 C43 N5 117.5(17) . . ? C42 C43 N5 116.2(18) . . ? C43 C44 C39 119(2) . . ? C43 C44 C45 123.7(18) . . ? C39 C44 C45 118(2) . . ? C47 C45 C46 110.7(16) . . ? C47 C45 C44 111.1(15) . . ? C46 C45 C44 108.1(15) . . ? C42 C48 C49 111.2(16) . . ? C42 C48 C50 112.5(17) . . ? C49 C48 C50 113.6(15) . . ? N6 C51 N5 100.3(13) . . ? N6 C51 Pd1 126.8(12) . . ? N5 C51 Pd1 132.5(12) . . ? C53 C52 N5 106.6(16) . . ? C52 C53 N6 107.7(17) . . ? C55 C54 N6 113.3(13) . . ? C56 C55 C60 113.7(14) . . ? C56 C55 C54 125.4(16) . . ? C60 C55 C54 120.9(15) . . ? C57 C56 C55 125.8(17) . . ? C56 C57 C58 119.1(18) . . ? C59 C58 C57 118.2(17) . . ? C58 C59 C60 124.3(16) . . ? C59 C60 C55 118.9(14) . . ? C59 C60 C61 118.2(16) . . ? C55 C60 C61 122.8(14) . . ? N8 C61 C60 112.7(14) . . ? C82 C77 C78 120.2(18) . . ? C79 C78 C77 122.2(17) . . ? C78 C79 C80 115.8(16) . . ? C78 C79 C86 125.9(17) . . ? C80 C79 C86 118.0(18) . . ? C81 C80 C79 121.0(17) . . ? C81 C80 N7 120.8(17) . . ? C79 C80 N7 118.2(16) . . ? C82 C81 C80 118.0(16) . . ? C82 C81 C83 123.9(16) . . ? C80 C81 C83 118.1(16) . . ? C77 C82 C81 122.7(17) . . ? C84 C83 C85 111.4(14) . . ? C84 C83 C81 111.7(14) . . ? C85 C83 C81 106.4(13) . . ? C79 C86 C88 106.0(15) . . ? C79 C86 C87 113.1(16) . . ? C88 C86 C87 108.2(16) . . ? N8 C89 N7 101.1(14) 3 . ? N8 C89 Pd1 125.6(12) 3 . ? N7 C89 Pd1 133.1(13) . . ? N7 C90 C91 105.4(16) . 3 ? N8 C91 C90 104.9(16) . 3 ? C14 N1 C13 113.5(15) . . ? C14 N1 C4 123.8(17) . . ? C13 N1 C4 122.5(16) . . ? C15 N2 C13 112.7(15) . . ? C15 N2 C16 126.0(16) . . ? C13 N2 C16 121.2(15) . . ? C24 N3 C25 113.3(15) . . ? C24 N3 C23 121.3(15) . . ? C25 N3 C23 125.4(15) . . ? C24 N4 C27 129.3(15) . . ? C24 N4 C26 107.5(13) . . ? C27 N4 C26 122.7(15) . . ? C52 N5 C51 111.5(15) . . ? C52 N5 C43 124.4(15) . . ? C51 N5 C43 123.8(14) . . ? C51 N6 C53 113.7(14) . . ? C51 N6 C54 120.2(14) . . ? C53 N6 C54 125.0(15) . . ? C90 N7 C89 113.5(15) . . ? C90 N7 C80 120.4(15) . . ? C89 N7 C80 125.4(15) . . ? C89 N8 C91 115.1(15) 3 . ? C89 N8 C61 123.6(14) 3 . ? C91 N8 C61 120.7(15) . . ? C51 Pd1 C89 171.2(7) . . ? C51 Pd1 Cl4 88.8(4) . . ? C89 Pd1 Cl4 91.3(4) . . ? C51 Pd1 Cl3 91.2(4) . . ? C89 Pd1 Cl3 89.2(4) . . ? Cl4 Pd1 Cl3 177.61(16) . . ? C13 Pd2 C24 163.6(7) . . ? C13 Pd2 Cl1 90.1(4) . . ? C24 Pd2 Cl1 89.3(4) . . ? C13 Pd2 Cl2 90.6(4) . . ? C24 Pd2 Cl2 90.8(4) . . ? Cl1 Pd2 Cl2 176.85(16) . . ? _diffrn_measured_fraction_theta_max 0.762 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.762 _refine_diff_density_max 1.161 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.139 #==END