Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' #================================================================== _journal_coden_Cambridge 0222 _audit_creation_date 27-07-01 _publ_section_title ;Structural variation, dynamics, and catalytic application of palladium(II) complexes of di-N-heterocyclic carbene-amine ligands ; _publ_contact_author_name 'Richard E. Douthwaite' _publ_contact_author_address ; Department of Chemistry University of York Heslington York YO10 5DD ; _publ_contact_author_phone ' 01904 434183 ' _publ_contact_author_fax ' 01904 432516 ' _publ_contact_author_email red4@york.ac.uk _publ_requested_category CM _publ_section_references ; PLATON- (a) Spek, A. L. (1990) Acta Cryst. A46, C34. (b) Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. SHELXTL, program suite for structure solution and refinement, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SMART, program for instrument control and data aquisition, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SAINTPLUS, program suite for data processing, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SHELXS86 - Program for Crystal Structure solution. G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, Tammanstrasse 4, D-3400 Gottingen, Germany, 1986. SHELX97. Programs for Crystal Structure Analysis (Release 97-2). University of Gottingen, Germany. Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; loop_ _publ_author_name 'Richard Douthwaite' 'Gavin Dyson' 'Jennifer Houghton' 'Benson Kariuki' 'Adrian C. Whitwood' #============= Material Relevant to Compound(2)===================== data_compound2 _database_code_depnum_ccdc_archive 'CCDC 639054' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H39 Cl2 N5 O2' _chemical_formula_weight 516.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.3231(3) _cell_length_b 9.7685(3) _cell_length_c 9.9897(3) _cell_angle_alpha 68.850(2) _cell_angle_beta 78.751(2) _cell_angle_gamma 83.055(2) _cell_volume 741.81(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 278 _exptl_absorpt_coefficient_mu 2.188 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5598 _exptl_absorpt_correction_T_max 0.8444 _exptl_absorpt_process_details 'Sadabs in SaintPlus' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 6000 CCD' _diffrn_measurement_method 'CCD slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4382 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 70.51 _reflns_number_total 3069 _reflns_number_gt 2781 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four hydrogen atoms for water molecules containing O1 and O2 were not located or included in the solution/refinement. ; _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^)+(0.1369P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.073(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 3069 _refine_ls_number_parameters 314 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.1796 _refine_ls_wR_factor_gt 0.1751 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.323(2) 1.3241(11) 0.2091(11) 0.143(5) Uani 1 1 d . . . H1A H 0.2353 1.3761 0.1577 0.172 Uiso 1 1 calc R . . H1B H 0.4234 1.3311 0.1414 0.172 Uiso 1 1 calc R . . H1C H 0.3342 1.3665 0.2795 0.172 Uiso 1 1 calc R . . C2 C 0.4020(14) 1.0825(14) 0.3917(11) 0.122(3) Uani 1 1 d . . . H2A H 0.5134 1.0944 0.3426 0.147 Uiso 1 1 calc R . . H2B H 0.3800 0.9801 0.4295 0.147 Uiso 1 1 calc R . . H2C H 0.3856 1.1199 0.4703 0.147 Uiso 1 1 calc R . . C3 C 0.1156(11) 1.1506(10) 0.3726(10) 0.105(2) Uani 1 1 d . . . H3A H 0.0960 1.0481 0.4204 0.126 Uiso 1 1 calc R . . H3B H 0.0361 1.1965 0.3096 0.126 Uiso 1 1 calc R . . H3C H 0.1063 1.1967 0.4442 0.126 Uiso 1 1 calc R . . C4 C 0.2855(8) 1.1673(7) 0.2842(7) 0.0783(15) Uani 1 1 d . . . C5 C 0.3403(7) 1.1567(6) 0.0303(6) 0.0649(11) Uani 1 1 d . . . H5 H 0.3700 1.2532 -0.0183 0.078 Uiso 1 1 calc R . . C6 C 0.2633(8) 0.9546(7) 0.2015(6) 0.0776(15) Uani 1 1 d . . . H6 H 0.2321 0.8858 0.2934 0.093 Uiso 1 1 calc R . . C7 C 0.2812(8) 0.9322(6) 0.0748(7) 0.0785(15) Uani 1 1 d . . . H7 H 0.2620 0.8464 0.0617 0.094 Uiso 1 1 calc R . . C8 C 0.3699(6) 1.0874(6) -0.1894(6) 0.0655(12) Uani 1 1 d . . . H8A H 0.3043 1.1730 -0.2392 0.079 Uiso 1 1 calc R . . H8B H 0.3387 1.0038 -0.2072 0.079 Uiso 1 1 calc R . . C9 C 0.5501(6) 1.1121(5) -0.2525(5) 0.0603(11) Uani 1 1 d . . . H9A H 0.5635 1.1391 -0.3573 0.072 Uiso 1 1 calc R . . H9B H 0.5812 1.1944 -0.2324 0.072 Uiso 1 1 calc R . . C10 C 0.8292(7) 1.0329(6) -0.2286(6) 0.0686(12) Uani 1 1 d . . . H10A H 0.8552 1.0881 -0.3318 0.082 Uiso 1 1 calc R . . H10B H 0.9047 0.9469 -0.2067 0.082 Uiso 1 1 calc R . . C11 C 0.8550(6) 1.1260(6) -0.1450(6) 0.0655(12) Uani 1 1 d . . . C12 C 0.7913(9) 1.0895(9) 0.0042(7) 0.0880(17) Uani 1 1 d . . . H12 H 0.7296 1.0073 0.0521 0.106 Uiso 1 1 calc R . . C13 C 0.8197(11) 1.1733(11) 0.0779(9) 0.102(2) Uani 1 1 d . . . H13 H 0.7769 1.1472 0.1765 0.122 Uiso 1 1 calc R . . C14 C 0.9110(11) 1.2979(10) 0.0113(11) 0.101(2) Uani 1 1 d . . . H14 H 0.9306 1.3537 0.0642 0.121 Uiso 1 1 calc R . . C15 C 0.9711(9) 1.3357(7) -0.1343(11) 0.093(2) Uani 1 1 d . . . H15 H 1.0292 1.4203 -0.1820 0.111 Uiso 1 1 calc R . . C16 C 0.9462(7) 1.2493(6) -0.2114(7) 0.0765(14) Uani 1 1 d . . . H16 H 0.9916 1.2746 -0.3093 0.092 Uiso 1 1 calc R . . C17 C 0.6510(7) 0.8726(6) -0.2582(6) 0.0677(12) Uani 1 1 d . . . H17A H 0.6961 0.9093 -0.3610 0.081 Uiso 1 1 calc R . . H17B H 0.5361 0.8567 -0.2496 0.081 Uiso 1 1 calc R . . C18 C 0.7392(8) 0.7257(6) -0.1874(6) 0.0708(13) Uani 1 1 d . . . H18A H 0.7062 0.6521 -0.2192 0.085 Uiso 1 1 calc R . . H18B H 0.8566 0.7343 -0.2186 0.085 Uiso 1 1 calc R . . C19 C 0.7993(7) 0.6786(6) 0.0592(6) 0.0687(12) Uani 1 1 d . . . H19 H 0.9077 0.7050 0.0300 0.082 Uiso 1 1 calc R . . C20 C 0.5531(7) 0.6328(7) 0.0546(7) 0.0786(15) Uani 1 1 d . . . H20 H 0.4610 0.6216 0.0204 0.094 Uiso 1 1 calc R . . C21 C 0.5646(7) 0.6072(7) 0.1944(7) 0.0790(15) Uani 1 1 d . . . H21 H 0.4822 0.5761 0.2746 0.095 Uiso 1 1 calc R . . C22 C 0.7892(9) 0.6208(9) 0.3280(8) 0.0885(18) Uani 1 1 d . . . C23 C 0.7772(16) 0.4652(12) 0.4256(11) 0.131(4) Uani 1 1 d . . . H23A H 0.8195 0.4019 0.3708 0.157 Uiso 1 1 calc R . . H23B H 0.6645 0.4463 0.4670 0.157 Uiso 1 1 calc R . . H23C H 0.8400 0.4468 0.5020 0.157 Uiso 1 1 calc R . . C24 C 0.6745(17) 0.7177(12) 0.4016(10) 0.127(3) Uani 1 1 d . . . H24A H 0.5660 0.6822 0.4289 0.153 Uiso 1 1 calc R . . H24B H 0.6716 0.8173 0.3351 0.153 Uiso 1 1 calc R . . H24C H 0.7142 0.7143 0.4868 0.153 Uiso 1 1 calc R . . C25 C 0.9667(14) 0.662(2) 0.2803(13) 0.163(6) Uani 1 1 d . . . H25A H 0.9713 0.7665 0.2471 0.195 Uiso 1 1 calc R . . H25B H 1.0161 0.6265 0.2026 0.195 Uiso 1 1 calc R . . H25C H 1.0250 0.6175 0.3609 0.195 Uiso 1 1 calc R . . N1 N 0.2989(6) 1.0957(5) 0.1723(5) 0.0669(10) Uani 1 1 d . . . N2 N 0.3333(5) 1.0606(4) -0.0322(5) 0.0623(10) Uani 1 1 d . . . N3 N 0.6625(5) 0.9850(4) -0.1964(4) 0.0590(9) Uani 1 1 d . . . N4 N 0.7024(6) 0.6783(5) -0.0283(5) 0.0649(11) Uani 1 1 d . . . N5 N 0.7225(6) 0.6362(5) 0.1954(5) 0.0678(10) Uani 1 1 d . . . Cl1 Cl 0.29479(13) 0.44740(11) 0.52673(11) 0.0678(4) Uani 1 1 d . . . Cl2 Cl 0.19343(13) 0.72173(13) 0.87033(13) 0.0722(4) Uani 1 1 d . . . O1 O 0.1311(10) 0.7538(8) 0.5494(7) 0.129(2) Uani 1 1 d . . . O2 O 0.4414(8) 0.4719(6) 0.7972(6) 0.1050(16) 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 0.260(14) 0.091(5) 0.088(6) -0.052(5) 0.017(7) -0.052(7) C2 0.140(7) 0.163(8) 0.086(5) -0.061(6) -0.029(5) -0.015(6) C3 0.114(6) 0.112(5) 0.087(5) -0.053(4) 0.014(4) 0.011(4) C4 0.102(4) 0.087(4) 0.058(3) -0.041(3) -0.009(3) -0.004(3) C5 0.080(3) 0.063(2) 0.050(3) -0.021(2) -0.006(2) -0.006(2) C6 0.109(4) 0.071(3) 0.050(3) -0.021(2) 0.006(3) -0.027(3) C7 0.109(4) 0.065(3) 0.062(3) -0.025(3) 0.005(3) -0.024(3) C8 0.069(3) 0.079(3) 0.052(3) -0.028(2) -0.014(2) 0.005(2) C9 0.075(3) 0.061(2) 0.039(2) -0.0127(18) -0.008(2) -0.0008(19) C10 0.070(3) 0.071(3) 0.058(3) -0.020(2) 0.001(2) -0.006(2) C11 0.061(3) 0.070(3) 0.062(3) -0.018(2) -0.012(2) -0.002(2) C12 0.109(4) 0.098(4) 0.061(3) -0.029(3) -0.004(3) -0.030(3) C13 0.114(5) 0.127(6) 0.077(5) -0.050(4) -0.007(4) -0.021(4) C14 0.106(5) 0.105(5) 0.114(7) -0.057(5) -0.031(5) -0.009(4) C15 0.090(4) 0.075(3) 0.117(6) -0.028(4) -0.031(4) -0.013(3) C16 0.071(3) 0.073(3) 0.078(4) -0.016(3) -0.011(3) -0.011(2) C17 0.091(3) 0.070(3) 0.044(2) -0.021(2) -0.014(2) -0.001(2) C18 0.093(4) 0.068(3) 0.056(3) -0.028(2) -0.010(3) -0.002(2) C19 0.071(3) 0.073(3) 0.058(3) -0.018(2) -0.013(2) 0.000(2) C20 0.071(3) 0.091(4) 0.068(3) -0.015(3) -0.008(3) -0.024(3) C21 0.078(3) 0.088(4) 0.060(3) -0.007(3) -0.012(3) -0.022(3) C22 0.102(4) 0.101(4) 0.063(4) -0.023(3) -0.028(3) -0.004(3) C23 0.162(9) 0.130(7) 0.076(5) -0.003(5) -0.047(6) 0.032(6) C24 0.194(10) 0.120(7) 0.079(5) -0.052(5) -0.021(6) 0.001(6) C25 0.125(8) 0.272(17) 0.089(6) -0.034(8) -0.037(5) -0.066(9) N1 0.086(3) 0.069(2) 0.047(2) -0.0256(19) -0.0003(19) -0.007(2) N2 0.069(2) 0.063(2) 0.056(2) -0.0252(19) -0.0049(19) -0.0035(17) N3 0.068(2) 0.061(2) 0.0438(19) -0.0142(16) -0.0054(16) -0.0052(16) N4 0.080(3) 0.058(2) 0.058(3) -0.0186(19) -0.015(2) -0.0048(18) N5 0.081(3) 0.065(2) 0.050(2) -0.0105(18) -0.0104(19) -0.0048(18) Cl1 0.0911(8) 0.0725(7) 0.0379(5) -0.0195(5) 0.0013(5) -0.0150(5) Cl2 0.0583(6) 0.0992(9) 0.0777(9) -0.0547(7) -0.0092(5) -0.0008(5) O1 0.183(6) 0.113(4) 0.075(3) -0.011(3) -0.029(4) 0.005(4) O2 0.137(4) 0.093(3) 0.084(3) -0.030(3) -0.030(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.483(11) . ? C2 C4 1.533(12) . ? C3 C4 1.507(11) . ? C4 N1 1.499(7) . ? C5 N2 1.313(7) . ? C5 N1 1.317(7) . ? C6 C7 1.338(9) . ? C6 N1 1.359(7) . ? C7 N2 1.374(8) . ? C8 N2 1.470(7) . ? C8 C9 1.522(8) . ? C9 N3 1.467(6) . ? C10 N3 1.457(7) . ? C10 C11 1.496(8) . ? C11 C16 1.383(8) . ? C11 C12 1.409(9) . ? C12 C13 1.348(11) . ? C13 C14 1.394(13) . ? C14 C15 1.370(13) . ? C15 C16 1.386(10) . ? C17 N3 1.460(7) . ? C17 C18 1.521(7) . ? C18 N4 1.466(7) . ? C19 N4 1.301(7) . ? C19 N5 1.322(8) . ? C20 C21 1.348(9) . ? C20 N4 1.376(8) . ? C21 N5 1.381(8) . ? C22 C23 1.483(13) . ? C22 N5 1.486(8) . ? C22 C25 1.516(13) . ? C22 C24 1.536(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C4 N1 108.8(6) . . ? C1 C4 C3 111.8(8) . . ? N1 C4 C3 109.2(6) . . ? C1 C4 C2 112.9(9) . . ? N1 C4 C2 108.5(6) . . ? C3 C4 C2 105.6(7) . . ? N2 C5 N1 109.8(5) . . ? C7 C6 N1 107.9(5) . . ? C6 C7 N2 106.7(5) . . ? N2 C8 C9 113.0(4) . . ? N3 C9 C8 114.7(4) . . ? N3 C10 C11 113.5(4) . . ? C16 C11 C12 117.8(6) . . ? C16 C11 C10 120.9(5) . . ? C12 C11 C10 121.4(5) . . ? C13 C12 C11 120.2(7) . . ? C12 C13 C14 122.2(8) . . ? C15 C14 C13 118.0(7) . . ? C14 C15 C16 120.7(6) . . ? C11 C16 C15 121.1(7) . . ? N3 C17 C18 114.6(4) . . ? N4 C18 C17 111.6(4) . . ? N4 C19 N5 110.7(5) . . ? C21 C20 N4 107.6(5) . . ? C20 C21 N5 106.6(5) . . ? C23 C22 N5 107.6(7) . . ? C23 C22 C25 110.9(9) . . ? N5 C22 C25 107.4(6) . . ? C23 C22 C24 108.7(9) . . ? N5 C22 C24 106.0(6) . . ? C25 C22 C24 115.9(10) . . ? C5 N1 C6 107.7(4) . . ? C5 N1 C4 127.4(5) . . ? C6 N1 C4 124.9(5) . . ? C5 N2 C7 107.9(5) . . ? C5 N2 C8 126.0(4) . . ? C7 N2 C8 126.1(5) . . ? C10 N3 C17 111.4(4) . . ? C10 N3 C9 109.5(4) . . ? C17 N3 C9 110.5(4) . . ? C19 N4 C20 107.7(5) . . ? C19 N4 C18 127.0(5) . . ? C20 N4 C18 125.2(5) . . ? C19 N5 C21 107.4(5) . . ? C19 N5 C22 127.8(5) . . ? C21 N5 C22 124.8(5) . . ? _diffrn_measured_fraction_theta_max 0.866 _diffrn_reflns_theta_full 70.51 _diffrn_measured_fraction_theta_full 0.866 _refine_diff_density_max 0.642 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.114 #============= Material Relevant to Compound(4)===================== data_compound4 _database_code_depnum_ccdc_archive 'CCDC 639055' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H33 N5, 2(C24 H20 B), C2 H3 N' _chemical_formula_sum 'C68 H76 B2 N6' _chemical_formula_weight 998.97 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6678(7) _cell_length_b 13.3876(8) _cell_length_c 18.3438(11) _cell_angle_alpha 86.420(2) _cell_angle_beta 80.4290(10) _cell_angle_gamma 89.4830(10) _cell_volume 2820.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5193 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.46 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19815 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12926 _reflns_number_gt 9840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+0.5416P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12926 _refine_ls_number_parameters 692 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 B1 B 0.75549(14) 0.24481(12) 0.43359(8) 0.0201(3) Uani 1 1 d . . . B2 B 0.23720(13) 0.76376(11) 0.05078(8) 0.0181(3) Uani 1 1 d . . . C1 C 0.23341(17) 0.27677(12) 0.38118(10) 0.0377(4) Uani 1 1 d . . . H1A H 0.1514 0.2676 0.3971 0.057 Uiso 1 1 calc R . . H1B H 0.2747 0.2461 0.4178 0.057 Uiso 1 1 calc R . . H1C H 0.2567 0.2463 0.3350 0.057 Uiso 1 1 calc R . . C2 C 0.26106(13) 0.38739(12) 0.37106(8) 0.0263(3) Uani 1 1 d . . . C3 C 0.39114(15) 0.40351(17) 0.34666(10) 0.0463(5) Uani 1 1 d . . . H3C H 0.4157 0.3736 0.3004 0.069 Uiso 1 1 calc R . . H3D H 0.4322 0.3731 0.3835 0.069 Uiso 1 1 calc R . . H3E H 0.4076 0.4740 0.3407 0.069 Uiso 1 1 calc R . . C4 C 0.21674(15) 0.43911(13) 0.44180(8) 0.0325(4) Uani 1 1 d . . . H4A H 0.2299 0.5099 0.4333 0.049 Uiso 1 1 calc R . . H4B H 0.2573 0.4136 0.4804 0.049 Uiso 1 1 calc R . . H4C H 0.1350 0.4265 0.4563 0.049 Uiso 1 1 calc R . . C5 C 0.20937(15) 0.53045(12) 0.28370(9) 0.0332(4) Uani 1 1 d . . . H5 H 0.2580 0.5785 0.2967 0.040 Uiso 1 1 calc R . . C6 C 0.13639(15) 0.54424(12) 0.23433(9) 0.0314(4) Uani 1 1 d . . . H6 H 0.1252 0.6033 0.2070 0.038 Uiso 1 1 calc R . . C7 C 0.12104(12) 0.38866(11) 0.27912(7) 0.0213(3) Uani 1 1 d . . . H7 H 0.0974 0.3222 0.2880 0.026 Uiso 1 1 calc R . . C8 C -0.00749(12) 0.43669(11) 0.18669(8) 0.0227(3) Uani 1 1 d . . . H8A H -0.0285 0.4997 0.1634 0.027 Uiso 1 1 calc R . . H8B H -0.0765 0.4096 0.2184 0.027 Uiso 1 1 calc R . . C9 C 0.03367(13) 0.36480(10) 0.12768(8) 0.0235(3) Uani 1 1 d . . . H9A H -0.0199 0.3660 0.0925 0.028 Uiso 1 1 calc R . . H9B H 0.1095 0.3857 0.1012 0.028 Uiso 1 1 calc R . . C10 C 0.09780(12) 0.19529(10) 0.10650(8) 0.0218(3) Uani 1 1 d . . . H10A H 0.1793 0.2131 0.0930 0.026 Uiso 1 1 calc R . . H10B H 0.0627 0.2026 0.0621 0.026 Uiso 1 1 calc R . . C11 C 0.08762(12) 0.08748(10) 0.13674(8) 0.0224(3) Uani 1 1 d . . . H11A H 0.0062 0.0710 0.1528 0.027 Uiso 1 1 calc R . . H11B H 0.1181 0.0444 0.0975 0.027 Uiso 1 1 calc R . . C12 C 0.10458(14) 0.05666(12) 0.27332(8) 0.0284(3) Uani 1 1 d . . . H12 H 0.0269 0.0639 0.2942 0.034 Uiso 1 1 calc R . . C13 C 0.19331(14) 0.03328(12) 0.30991(8) 0.0304(3) Uani 1 1 d . . . H13 H 0.1880 0.0214 0.3609 0.036 Uiso 1 1 calc R . . C14 C 0.26427(12) 0.05158(10) 0.19203(8) 0.0222(3) Uani 1 1 d . . . H14 H 0.3156 0.0548 0.1473 0.027 Uiso 1 1 calc R . . C15 C 0.41464(14) 0.00776(12) 0.27323(9) 0.0304(3) Uani 1 1 d . . . C16 C 0.45884(16) 0.09987(15) 0.30469(12) 0.0488(5) Uani 1 1 d . . . H16A H 0.4563 0.1568 0.2704 0.073 Uiso 1 1 calc R . . H16B H 0.5374 0.0888 0.3125 0.073 Uiso 1 1 calc R . . H16C H 0.4106 0.1122 0.3510 0.073 Uiso 1 1 calc R . . C17 C 0.40682(19) -0.08350(16) 0.32755(11) 0.0528(5) Uani 1 1 d . . . H17A H 0.3617 -0.0673 0.3740 0.079 Uiso 1 1 calc R . . H17B H 0.4835 -0.1033 0.3349 0.079 Uiso 1 1 calc R . . H17C H 0.3702 -0.1375 0.3080 0.079 Uiso 1 1 calc R . . C18 C 0.49073(14) -0.01479(14) 0.20074(9) 0.0366(4) Uani 1 1 d . . . H18A H 0.4564 -0.0678 0.1788 0.055 Uiso 1 1 calc R . . H18B H 0.5665 -0.0349 0.2100 0.055 Uiso 1 1 calc R . . H18C H 0.4975 0.0441 0.1676 0.055 Uiso 1 1 calc R . . C19 C 0.61960(12) 0.24941(11) 0.47676(7) 0.0217(3) Uani 1 1 d . . . C20 C 0.54053(13) 0.16990(11) 0.48283(8) 0.0246(3) Uani 1 1 d . . . H20 H 0.5642 0.1116 0.4596 0.030 Uiso 1 1 calc R . . C21 C 0.42816(13) 0.17464(12) 0.52222(8) 0.0300(3) Uani 1 1 d . . . H21 H 0.3786 0.1200 0.5247 0.036 Uiso 1 1 calc R . . C22 C 0.38936(14) 0.25978(13) 0.55770(9) 0.0321(4) Uani 1 1 d . . . H22 H 0.3145 0.2627 0.5844 0.039 Uiso 1 1 calc R . . C23 C 0.46412(14) 0.34044(12) 0.55263(8) 0.0308(3) Uani 1 1 d . . . H23 H 0.4396 0.3985 0.5759 0.037 Uiso 1 1 calc R . . C24 C 0.57591(13) 0.33474(12) 0.51276(8) 0.0269(3) Uani 1 1 d . . . H24 H 0.6243 0.3902 0.5097 0.032 Uiso 1 1 calc R . . C25 C 0.79164(12) 0.35868(10) 0.39792(7) 0.0218(3) Uani 1 1 d . . . C26 C 0.72152(13) 0.41291(11) 0.35405(8) 0.0261(3) Uani 1 1 d . . . H26 H 0.6557 0.3821 0.3434 0.031 Uiso 1 1 calc R . . C27 C 0.74631(15) 0.51019(12) 0.32608(8) 0.0330(4) Uani 1 1 d . . . H27 H 0.6979 0.5429 0.2969 0.040 Uiso 1 1 calc R . . C28 C 0.84305(16) 0.55901(12) 0.34150(9) 0.0348(4) Uani 1 1 d . . . H28 H 0.8597 0.6246 0.3232 0.042 Uiso 1 1 calc R . . C29 C 0.91411(15) 0.50875(12) 0.38435(8) 0.0314(4) Uani 1 1 d . . . H29 H 0.9792 0.5405 0.3953 0.038 Uiso 1 1 calc R . . C30 C 0.88885(13) 0.41064(11) 0.41137(8) 0.0245(3) Uani 1 1 d . . . H30 H 0.9388 0.3781 0.4396 0.029 Uiso 1 1 calc R . . C31 C 0.84177(12) 0.21256(10) 0.49372(8) 0.0212(3) Uani 1 1 d . . . C32 C 0.94329(14) 0.15769(13) 0.47462(8) 0.0312(4) Uani 1 1 d . . . H32 H 0.9584 0.1326 0.4278 0.037 Uiso 1 1 calc R . . C33 C 1.02304(14) 0.13875(14) 0.52229(9) 0.0365(4) Uani 1 1 d . . . H33 H 1.0892 0.1012 0.5072 0.044 Uiso 1 1 calc R . . C34 C 1.00432(15) 0.17536(13) 0.59151(9) 0.0349(4) Uani 1 1 d . . . H34 H 1.0584 0.1645 0.6231 0.042 Uiso 1 1 calc R . . C35 C 0.90375(15) 0.22856(14) 0.61343(9) 0.0367(4) Uani 1 1 d . . . H35 H 0.8892 0.2529 0.6604 0.044 Uiso 1 1 calc R . . C36 C 0.82437(14) 0.24568(12) 0.56538(8) 0.0279(3) Uani 1 1 d . . . H36 H 0.7567 0.2807 0.5817 0.034 Uiso 1 1 calc R . . C37 C 0.76778(12) 0.16375(10) 0.36912(8) 0.0203(3) Uani 1 1 d . . . C38 C 0.76143(12) 0.06019(11) 0.38766(8) 0.0240(3) Uani 1 1 d . . . H38 H 0.7540 0.0383 0.4373 0.029 Uiso 1 1 calc R . . C39 C 0.76573(12) -0.01085(11) 0.33530(8) 0.0250(3) Uani 1 1 d . . . H39 H 0.7604 -0.0785 0.3503 0.030 Uiso 1 1 calc R . . C40 C 0.77798(12) 0.01897(11) 0.26058(8) 0.0238(3) Uani 1 1 d . . . H40 H 0.7807 -0.0281 0.2251 0.029 Uiso 1 1 calc R . . C41 C 0.78604(12) 0.12006(11) 0.23988(8) 0.0231(3) Uani 1 1 d . . . H41 H 0.7946 0.1414 0.1900 0.028 Uiso 1 1 calc R . . C42 C 0.78142(12) 0.19008(11) 0.29321(8) 0.0213(3) Uani 1 1 d . . . H42 H 0.7877 0.2576 0.2776 0.026 Uiso 1 1 calc R . . C43 C 0.34794(12) 0.73714(9) 0.09393(8) 0.0204(3) Uani 1 1 d . . . C44 C 0.34424(13) 0.72342(10) 0.17056(8) 0.0226(3) Uani 1 1 d . . . H44 H 0.2732 0.7295 0.2015 0.027 Uiso 1 1 calc R . . C45 C 0.44294(14) 0.70091(11) 0.20248(9) 0.0283(3) Uani 1 1 d . . . H45 H 0.4364 0.6922 0.2537 0.034 Uiso 1 1 calc R . . C46 C 0.54956(14) 0.69164(11) 0.15861(10) 0.0314(4) Uani 1 1 d . . . H46 H 0.6154 0.6770 0.1797 0.038 Uiso 1 1 calc R . . C47 C 0.55737(13) 0.70446(11) 0.08241(9) 0.0287(3) Uani 1 1 d . . . H47 H 0.6289 0.6983 0.0520 0.034 Uiso 1 1 calc R . . C48 C 0.45881(12) 0.72647(10) 0.05135(8) 0.0239(3) Uani 1 1 d . . . H48 H 0.4664 0.7345 0.0001 0.029 Uiso 1 1 calc R . . C49 C 0.24733(12) 0.87921(10) 0.01359(7) 0.0182(3) Uani 1 1 d . . . C50 C 0.33635(12) 0.94618(10) 0.01900(8) 0.0212(3) Uani 1 1 d . . . H50 H 0.3958 0.9245 0.0441 0.025 Uiso 1 1 calc R . . C51 C 0.33941(12) 1.04423(10) -0.01187(8) 0.0242(3) Uani 1 1 d . . . H51 H 0.4001 1.0865 -0.0069 0.029 Uiso 1 1 calc R . . C52 C 0.25252(13) 1.07885(11) -0.04980(8) 0.0236(3) Uani 1 1 d . . . H52 H 0.2549 1.1439 -0.0710 0.028 Uiso 1 1 calc R . . C53 C 0.16164(13) 1.01507(11) -0.05579(8) 0.0230(3) Uani 1 1 d . . . H53 H 0.1021 1.0374 -0.0806 0.028 Uiso 1 1 calc R . . C54 C 0.16026(12) 0.91800(10) -0.02451(8) 0.0220(3) Uani 1 1 d . . . H54 H 0.0986 0.8765 -0.0290 0.026 Uiso 1 1 calc R . . C55 C 0.24422(12) 0.68327(10) -0.01372(8) 0.0196(3) Uani 1 1 d . . . C56 C 0.28573(12) 0.70711(11) -0.08884(8) 0.0227(3) Uani 1 1 d . . . H56 H 0.3077 0.7728 -0.1037 0.027 Uiso 1 1 calc R . . C57 C 0.29546(13) 0.63666(11) -0.14216(8) 0.0262(3) Uani 1 1 d . . . H57 H 0.3236 0.6558 -0.1914 0.031 Uiso 1 1 calc R . . C58 C 0.26348(13) 0.53819(11) -0.12217(8) 0.0259(3) Uani 1 1 d . . . H58 H 0.2687 0.4910 -0.1577 0.031 Uiso 1 1 calc R . . C59 C 0.22344(13) 0.51104(11) -0.04799(8) 0.0247(3) Uani 1 1 d . . . H59 H 0.2021 0.4451 -0.0335 0.030 Uiso 1 1 calc R . . C60 C 0.21527(12) 0.58201(10) 0.00431(8) 0.0213(3) Uani 1 1 d . . . H60 H 0.1894 0.5618 0.0537 0.026 Uiso 1 1 calc R . . C61 C 0.11035(12) 0.75995(9) 0.10500(7) 0.0178(3) Uani 1 1 d . . . C62 C 0.01262(12) 0.70778(10) 0.09186(8) 0.0199(3) Uani 1 1 d . . . H62 H 0.0207 0.6674 0.0518 0.024 Uiso 1 1 calc R . . C63 C -0.09574(12) 0.71403(10) 0.13629(8) 0.0232(3) Uani 1 1 d . . . H63 H -0.1580 0.6780 0.1256 0.028 Uiso 1 1 calc R . . C64 C -0.11182(13) 0.77316(11) 0.19616(8) 0.0243(3) Uani 1 1 d . . . H64 H -0.1841 0.7769 0.2262 0.029 Uiso 1 1 calc R . . C65 C -0.01774(13) 0.82695(10) 0.21060(8) 0.0233(3) Uani 1 1 d . . . H65 H -0.0269 0.8678 0.2504 0.028 Uiso 1 1 calc R . . C66 C 0.08954(12) 0.81998(10) 0.16599(7) 0.0202(3) Uani 1 1 d . . . H66 H 0.1510 0.8569 0.1769 0.024 Uiso 1 1 calc R . . C67 C 0.38690(14) 0.36028(13) 0.13526(9) 0.0331(4) Uani 1 1 d . . . C68 C 0.43470(16) 0.45327(13) 0.09849(10) 0.0392(4) Uani 1 1 d . . . H68A H 0.5156 0.4444 0.0794 0.059 Uiso 1 1 calc R . . H68B H 0.4262 0.5046 0.1332 0.059 Uiso 1 1 calc R . . H68C H 0.3940 0.4725 0.0584 0.059 Uiso 1 1 calc R . . N1 N 0.19907(10) 0.43258(9) 0.31139(6) 0.0227(3) Uani 1 1 d . . . N2 N 0.08204(10) 0.45488(9) 0.23204(6) 0.0209(2) Uani 1 1 d . . . N3 N 0.04113(10) 0.26301(8) 0.16037(6) 0.0211(2) Uani 1 1 d . . . H3 H -0.0310 0.2403 0.1786 0.025 Uiso 1 1 d R . . N4 N 0.15071(10) 0.06773(8) 0.19948(6) 0.0202(2) Uani 1 1 d . . . N5 N 0.29344(11) 0.03010(9) 0.25818(7) 0.0238(3) Uani 1 1 d . . . N6 N 0.34950(15) 0.28715(13) 0.16393(9) 0.0523(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 B1 0.0207(8) 0.0217(8) 0.0186(7) -0.0016(6) -0.0048(6) 0.0009(6) B2 0.0204(7) 0.0139(7) 0.0208(7) -0.0008(6) -0.0061(6) -0.0007(6) C1 0.0515(11) 0.0298(9) 0.0373(9) -0.0018(7) -0.0237(8) 0.0090(8) C2 0.0246(8) 0.0328(8) 0.0239(7) -0.0022(6) -0.0110(6) 0.0029(6) C3 0.0270(9) 0.0746(14) 0.0394(10) -0.0023(9) -0.0124(8) 0.0014(9) C4 0.0373(9) 0.0364(9) 0.0274(8) -0.0068(7) -0.0145(7) 0.0054(7) C5 0.0412(9) 0.0285(8) 0.0325(8) 0.0046(7) -0.0153(7) -0.0148(7) C6 0.0420(9) 0.0234(8) 0.0304(8) 0.0063(6) -0.0128(7) -0.0105(7) C7 0.0232(7) 0.0197(7) 0.0217(7) -0.0034(5) -0.0054(6) 0.0014(5) C8 0.0236(7) 0.0212(7) 0.0251(7) -0.0023(6) -0.0091(6) 0.0018(6) C9 0.0273(8) 0.0225(7) 0.0225(7) -0.0024(6) -0.0090(6) 0.0017(6) C10 0.0218(7) 0.0226(7) 0.0224(7) -0.0049(6) -0.0068(6) 0.0015(5) C11 0.0211(7) 0.0227(7) 0.0261(7) -0.0069(6) -0.0098(6) 0.0007(5) C12 0.0253(8) 0.0352(9) 0.0249(7) -0.0066(6) -0.0033(6) -0.0011(6) C13 0.0304(8) 0.0386(9) 0.0226(7) -0.0041(7) -0.0049(6) -0.0005(7) C14 0.0227(7) 0.0195(7) 0.0251(7) -0.0037(6) -0.0055(6) 0.0005(5) C15 0.0263(8) 0.0355(9) 0.0336(8) -0.0095(7) -0.0148(7) 0.0092(6) C16 0.0298(9) 0.0603(12) 0.0654(13) -0.0371(11) -0.0226(9) 0.0126(8) C17 0.0536(12) 0.0614(13) 0.0449(11) 0.0056(10) -0.0169(10) 0.0234(10) C18 0.0268(8) 0.0465(10) 0.0404(9) -0.0133(8) -0.0133(7) 0.0081(7) C19 0.0220(7) 0.0272(7) 0.0166(6) -0.0002(6) -0.0062(5) 0.0024(6) C20 0.0258(8) 0.0269(8) 0.0212(7) 0.0007(6) -0.0051(6) 0.0008(6) C21 0.0258(8) 0.0359(9) 0.0274(8) 0.0052(7) -0.0045(6) -0.0041(7) C22 0.0216(8) 0.0456(10) 0.0266(8) 0.0042(7) 0.0008(6) 0.0044(7) C23 0.0292(8) 0.0360(9) 0.0267(8) -0.0044(7) -0.0022(6) 0.0085(7) C24 0.0242(8) 0.0307(8) 0.0260(7) -0.0052(6) -0.0038(6) 0.0006(6) C25 0.0248(7) 0.0217(7) 0.0178(6) -0.0032(5) 0.0002(6) 0.0037(6) C26 0.0280(8) 0.0289(8) 0.0207(7) -0.0030(6) -0.0018(6) 0.0073(6) C27 0.0436(10) 0.0316(9) 0.0214(7) -0.0002(6) 0.0000(7) 0.0168(7) C28 0.0498(10) 0.0212(8) 0.0277(8) 0.0000(6) 0.0096(7) 0.0048(7) C29 0.0366(9) 0.0267(8) 0.0279(8) -0.0047(6) 0.0044(7) -0.0044(7) C30 0.0262(8) 0.0246(7) 0.0220(7) -0.0021(6) -0.0011(6) 0.0011(6) C31 0.0227(7) 0.0196(7) 0.0214(7) 0.0014(5) -0.0049(6) -0.0021(5) C32 0.0284(8) 0.0426(9) 0.0238(7) -0.0061(7) -0.0063(6) 0.0082(7) C33 0.0267(8) 0.0507(11) 0.0326(9) -0.0028(8) -0.0073(7) 0.0123(7) C34 0.0322(9) 0.0462(10) 0.0286(8) 0.0038(7) -0.0144(7) 0.0054(7) C35 0.0425(10) 0.0484(10) 0.0218(8) -0.0058(7) -0.0122(7) 0.0086(8) C36 0.0298(8) 0.0303(8) 0.0244(7) -0.0030(6) -0.0063(6) 0.0064(6) C37 0.0153(6) 0.0228(7) 0.0231(7) -0.0015(6) -0.0043(5) 0.0014(5) C38 0.0244(7) 0.0261(7) 0.0211(7) 0.0012(6) -0.0034(6) 0.0029(6) C39 0.0230(7) 0.0202(7) 0.0315(8) -0.0006(6) -0.0043(6) 0.0031(6) C40 0.0192(7) 0.0261(7) 0.0273(7) -0.0082(6) -0.0049(6) 0.0027(6) C41 0.0208(7) 0.0290(8) 0.0203(7) -0.0013(6) -0.0058(6) 0.0009(6) C42 0.0205(7) 0.0203(7) 0.0236(7) -0.0004(6) -0.0051(6) -0.0003(5) C43 0.0234(7) 0.0103(6) 0.0289(7) -0.0013(5) -0.0082(6) -0.0013(5) C44 0.0225(7) 0.0182(7) 0.0282(7) 0.0011(6) -0.0082(6) -0.0026(5) C45 0.0331(8) 0.0212(7) 0.0338(8) 0.0041(6) -0.0172(7) -0.0033(6) C46 0.0268(8) 0.0203(7) 0.0514(10) 0.0001(7) -0.0205(7) 0.0005(6) C47 0.0196(7) 0.0180(7) 0.0490(10) -0.0046(7) -0.0062(7) 0.0007(5) C48 0.0247(7) 0.0169(7) 0.0309(8) -0.0023(6) -0.0061(6) 0.0003(5) C49 0.0200(7) 0.0165(6) 0.0180(6) -0.0037(5) -0.0015(5) 0.0013(5) C50 0.0181(7) 0.0202(7) 0.0258(7) -0.0020(6) -0.0049(6) 0.0018(5) C51 0.0201(7) 0.0193(7) 0.0326(8) -0.0012(6) -0.0028(6) -0.0034(5) C52 0.0269(8) 0.0172(7) 0.0258(7) 0.0022(6) -0.0025(6) 0.0009(6) C53 0.0256(7) 0.0229(7) 0.0219(7) -0.0014(6) -0.0082(6) 0.0029(6) C54 0.0236(7) 0.0198(7) 0.0242(7) -0.0030(6) -0.0081(6) -0.0024(5) C55 0.0173(7) 0.0188(7) 0.0241(7) -0.0024(5) -0.0073(5) 0.0027(5) C56 0.0246(7) 0.0198(7) 0.0243(7) 0.0001(6) -0.0065(6) 0.0023(6) C57 0.0279(8) 0.0309(8) 0.0206(7) -0.0022(6) -0.0065(6) 0.0067(6) C58 0.0274(8) 0.0262(8) 0.0272(7) -0.0106(6) -0.0107(6) 0.0076(6) C59 0.0269(8) 0.0170(7) 0.0316(8) -0.0044(6) -0.0085(6) 0.0020(6) C60 0.0228(7) 0.0203(7) 0.0213(7) -0.0009(5) -0.0052(6) 0.0016(5) C61 0.0209(7) 0.0137(6) 0.0196(6) 0.0017(5) -0.0073(5) 0.0021(5) C62 0.0232(7) 0.0168(6) 0.0212(7) -0.0019(5) -0.0077(6) 0.0011(5) C63 0.0215(7) 0.0188(7) 0.0300(7) 0.0006(6) -0.0070(6) -0.0012(5) C64 0.0226(7) 0.0222(7) 0.0259(7) 0.0037(6) 0.0006(6) 0.0035(6) C65 0.0314(8) 0.0193(7) 0.0194(7) -0.0023(5) -0.0046(6) 0.0044(6) C66 0.0244(7) 0.0153(6) 0.0226(7) -0.0004(5) -0.0091(6) -0.0002(5) C67 0.0277(8) 0.0390(10) 0.0342(9) -0.0072(7) -0.0081(7) -0.0032(7) C68 0.0356(9) 0.0322(9) 0.0507(10) 0.0027(8) -0.0120(8) -0.0002(7) N1 0.0233(6) 0.0245(6) 0.0212(6) -0.0013(5) -0.0062(5) -0.0017(5) N2 0.0232(6) 0.0201(6) 0.0202(6) -0.0016(5) -0.0060(5) -0.0005(5) N3 0.0209(6) 0.0182(6) 0.0239(6) -0.0031(5) -0.0022(5) -0.0005(5) N4 0.0208(6) 0.0179(6) 0.0235(6) -0.0046(5) -0.0071(5) -0.0005(4) N5 0.0248(6) 0.0227(6) 0.0260(6) -0.0039(5) -0.0091(5) 0.0015(5) N6 0.0528(10) 0.0487(10) 0.0558(10) 0.0034(8) -0.0112(8) -0.0189(8) _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 B1 C37 1.643(2) . ? B1 C31 1.649(2) . ? B1 C25 1.651(2) . ? B1 C19 1.653(2) . ? B2 C61 1.639(2) . ? B2 C55 1.641(2) . ? B2 C49 1.6473(19) . ? B2 C43 1.649(2) . ? C1 C2 1.512(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.5033(18) . ? C2 C4 1.521(2) . ? C2 C3 1.523(2) . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C3 H3E 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.346(2) . ? C5 N1 1.3742(19) . ? C5 H5 0.9300 . ? C6 N2 1.3652(18) . ? C6 H6 0.9300 . ? C7 N1 1.3256(17) . ? C7 N2 1.3292(18) . ? C7 H7 0.9300 . ? C8 N2 1.4702(17) . ? C8 C9 1.509(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N3 1.4620(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N3 1.4559(18) . ? C10 C11 1.5120(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.4752(17) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.349(2) . ? C12 N4 1.3713(18) . ? C12 H12 0.9300 . ? C13 N5 1.379(2) . ? C13 H13 0.9300 . ? C14 N4 1.3264(18) . ? C14 N5 1.3278(18) . ? C14 H14 0.9300 . ? C15 N5 1.5091(19) . ? C15 C18 1.517(2) . ? C15 C17 1.521(2) . ? C15 C16 1.523(2) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.402(2) . ? C19 C24 1.404(2) . ? C20 C21 1.391(2) . ? C20 H20 0.9300 . ? C21 C22 1.383(2) . ? C21 H21 0.9300 . ? C22 C23 1.383(2) . ? C22 H22 0.9300 . ? C23 C24 1.389(2) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.400(2) . ? C25 C26 1.407(2) . ? C26 C27 1.385(2) . ? C26 H26 0.9300 . ? C27 C28 1.387(2) . ? C27 H27 0.9300 . ? C28 C29 1.378(2) . ? C28 H28 0.9300 . ? C29 C30 1.391(2) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.394(2) . ? C31 C36 1.396(2) . ? C32 C33 1.391(2) . ? C32 H32 0.9300 . ? C33 C34 1.373(2) . ? C33 H33 0.9300 . ? C34 C35 1.382(2) . ? C34 H34 0.9300 . ? C35 C36 1.389(2) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.3980(19) . ? C37 C38 1.406(2) . ? C38 C39 1.388(2) . ? C38 H38 0.9300 . ? C39 C40 1.388(2) . ? C39 H39 0.9300 . ? C40 C41 1.382(2) . ? C40 H40 0.9300 . ? C41 C42 1.3910(19) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.400(2) . ? C43 C48 1.407(2) . ? C44 C45 1.398(2) . ? C44 H44 0.9300 . ? C45 C46 1.374(2) . ? C45 H45 0.9300 . ? C46 C47 1.385(2) . ? C46 H46 0.9300 . ? C47 C48 1.387(2) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.3980(18) . ? C49 C54 1.4041(19) . ? C50 C51 1.3951(19) . ? C50 H50 0.9300 . ? C51 C52 1.383(2) . ? C51 H51 0.9300 . ? C52 C53 1.3901(19) . ? C52 H52 0.9300 . ? C53 C54 1.3865(19) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.4005(19) . ? C55 C60 1.4058(19) . ? C56 C57 1.391(2) . ? C56 H56 0.9300 . ? C57 C58 1.384(2) . ? C57 H57 0.9300 . ? C58 C59 1.390(2) . ? C58 H58 0.9300 . ? C59 C60 1.3835(19) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.4046(18) . ? C61 C66 1.4055(19) . ? C62 C63 1.391(2) . ? C62 H62 0.9300 . ? C63 C64 1.380(2) . ? C63 H63 0.9300 . ? C64 C65 1.389(2) . ? C64 H64 0.9300 . ? C65 C66 1.383(2) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 N6 1.137(2) . ? C67 C68 1.449(2) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? N3 H3 0.9000 . ? 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 C37 B1 C31 109.78(11) . . ? C37 B1 C25 111.38(11) . . ? C31 B1 C25 108.25(11) . . ? C37 B1 C19 110.32(11) . . ? C31 B1 C19 109.68(11) . . ? C25 B1 C19 107.35(11) . . ? C61 B2 C55 111.52(11) . . ? C61 B2 C49 104.31(11) . . ? C55 B2 C49 110.56(11) . . ? C61 B2 C43 114.21(11) . . ? C55 B2 C43 105.65(11) . . ? C49 B2 C43 110.69(10) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 108.29(11) . . ? N1 C2 C4 107.69(12) . . ? C1 C2 C4 110.64(13) . . ? N1 C2 C3 108.45(13) . . ? C1 C2 C3 110.30(15) . . ? C4 C2 C3 111.36(13) . . ? C2 C3 H3C 109.5 . . ? C2 C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? C2 C3 H3E 109.5 . . ? H3C C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N1 107.74(13) . . ? C6 C5 H5 126.1 . . ? N1 C5 H5 126.1 . . ? C5 C6 N2 106.89(13) . . ? C5 C6 H6 126.6 . . ? N2 C6 H6 126.6 . . ? N1 C7 N2 109.01(12) . . ? N1 C7 H7 125.5 . . ? N2 C7 H7 125.5 . . ? N2 C8 C9 111.95(12) . . ? N2 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N3 C9 C8 110.87(11) . . ? N3 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N3 C10 C11 111.66(11) . . ? N3 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N3 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? N4 C11 C10 112.56(11) . . ? N4 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N4 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C13 C12 N4 106.94(13) . . ? C13 C12 H12 126.5 . . ? N4 C12 H12 126.5 . . ? C12 C13 N5 107.70(13) . . ? C12 C13 H13 126.1 . . ? N5 C13 H13 126.1 . . ? N4 C14 N5 109.53(13) . . ? N4 C14 H14 125.2 . . ? N5 C14 H14 125.2 . . ? N5 C15 C18 108.35(12) . . ? N5 C15 C17 107.40(14) . . ? C18 C15 C17 110.21(14) . . ? N5 C15 C16 107.84(13) . . ? C18 C15 C16 110.67(15) . . ? C17 C15 C16 112.22(15) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 114.72(13) . . ? C20 C19 B1 124.04(13) . . ? C24 C19 B1 121.21(12) . . ? C21 C20 C19 122.65(14) . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C22 C21 C20 120.63(14) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 118.70(15) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C24 119.99(15) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 123.30(14) . . ? C23 C24 H24 118.4 . . ? C19 C24 H24 118.4 . . ? C30 C25 C26 114.87(13) . . ? C30 C25 B1 123.77(12) . . ? C26 C25 B1 121.28(12) . . ? C27 C26 C25 122.84(15) . . ? C27 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C26 C27 C28 120.23(15) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 118.89(15) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 120.24(15) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 122.92(14) . . ? C29 C30 H30 118.5 . . ? C25 C30 H30 118.5 . . ? C32 C31 C36 114.92(13) . . ? C32 C31 B1 122.33(12) . . ? C36 C31 B1 122.51(13) . . ? C33 C32 C31 123.03(14) . . ? C33 C32 H32 118.5 . . ? C31 C32 H32 118.5 . . ? C34 C33 C32 120.16(16) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 118.87(15) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C34 C35 C36 120.14(15) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 122.84(15) . . ? C35 C36 H36 118.6 . . ? C31 C36 H36 118.6 . . ? C42 C37 C38 114.72(13) . . ? C42 C37 B1 124.17(12) . . ? C38 C37 B1 121.08(12) . . ? C39 C38 C37 123.09(13) . . ? C39 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C40 C39 C38 120.10(13) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 118.68(13) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C40 C41 C42 120.34(13) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 123.06(13) . . ? C41 C42 H42 118.5 . . ? C37 C42 H42 118.5 . . ? C44 C43 C48 114.78(13) . . ? C44 C43 B2 126.60(13) . . ? C48 C43 B2 118.62(12) . . ? C45 C44 C43 122.74(14) . . ? C45 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? C46 C45 C44 120.39(14) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 118.89(14) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? C46 C47 C48 120.22(15) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 122.98(14) . . ? C47 C48 H48 118.5 . . ? C43 C48 H48 118.5 . . ? C50 C49 C54 115.20(12) . . ? C50 C49 B2 124.72(12) . . ? C54 C49 B2 120.04(11) . . ? C51 C50 C49 122.56(13) . . ? C51 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? C52 C51 C50 120.25(13) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 119.07(13) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C54 C53 C52 119.67(13) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C49 123.24(12) . . ? C53 C54 H54 118.4 . . ? C49 C54 H54 118.4 . . ? C56 C55 C60 114.99(13) . . ? C56 C55 B2 123.75(12) . . ? C60 C55 B2 121.13(12) . . ? C57 C56 C55 122.78(13) . . ? C57 C56 H56 118.6 . . ? C55 C56 H56 118.6 . . ? C58 C57 C56 120.28(14) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 118.78(13) . . ? C57 C58 H58 120.6 . . ? C59 C58 H58 120.6 . . ? C60 C59 C58 120.09(13) . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 123.05(13) . . ? C59 C60 H60 118.5 . . ? C55 C60 H60 118.5 . . ? C62 C61 C66 114.67(12) . . ? C62 C61 B2 125.03(12) . . ? C66 C61 B2 119.98(11) . . ? C63 C62 C61 122.64(13) . . ? C63 C62 H62 118.7 . . ? C61 C62 H62 118.7 . . ? C64 C63 C62 120.67(13) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 118.56(13) . . ? C63 C64 H64 120.7 . . ? C65 C64 H64 120.7 . . ? C66 C65 C64 120.16(13) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C65 C66 C61 123.30(12) . . ? C65 C66 H66 118.4 . . ? C61 C66 H66 118.4 . . ? N6 C67 C68 179.8(2) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C7 N1 C5 107.74(12) . . ? C7 N1 C2 127.18(12) . . ? C5 N1 C2 124.98(12) . . ? C7 N2 C6 108.62(12) . . ? C7 N2 C8 126.07(12) . . ? C6 N2 C8 125.28(12) . . ? C10 N3 C9 111.89(11) . . ? C10 N3 H3 109.2 . . ? C9 N3 H3 109.2 . . ? C14 N4 C12 108.37(12) . . ? C14 N4 C11 124.00(12) . . ? C12 N4 C11 127.51(12) . . ? C14 N5 C13 107.45(12) . . ? C14 N5 C15 125.75(13) . . ? C13 N5 C15 126.79(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C5 C6 N2 -0.05(19) . . . . ? N2 C8 C9 N3 71.67(15) . . . . ? N3 C10 C11 N4 -65.45(15) . . . . ? N4 C12 C13 N5 -0.04(17) . . . . ? C37 B1 C19 C20 26.49(18) . . . . ? C31 B1 C19 C20 -94.57(15) . . . . ? C25 B1 C19 C20 148.03(13) . . . . ? C37 B1 C19 C24 -155.61(12) . . . . ? C31 B1 C19 C24 83.34(15) . . . . ? C25 B1 C19 C24 -34.07(16) . . . . ? C24 C19 C20 C21 -0.8(2) . . . . ? B1 C19 C20 C21 177.22(13) . . . . ? C19 C20 C21 C22 -0.1(2) . . . . ? C20 C21 C22 C23 0.6(2) . . . . ? C21 C22 C23 C24 -0.3(2) . . . . ? C22 C23 C24 C19 -0.6(2) . . . . ? C20 C19 C24 C23 1.2(2) . . . . ? B1 C19 C24 C23 -176.92(13) . . . . ? C37 B1 C25 C30 -113.63(14) . . . . ? C31 B1 C25 C30 7.16(19) . . . . ? C19 B1 C25 C30 125.50(14) . . . . ? C37 B1 C25 C26 69.78(16) . . . . ? C31 B1 C25 C26 -169.43(12) . . . . ? C19 B1 C25 C26 -51.09(16) . . . . ? C30 C25 C26 C27 0.1(2) . . . . ? B1 C25 C26 C27 176.95(14) . . . . ? C25 C26 C27 C28 -0.7(2) . . . . ? C26 C27 C28 C29 0.6(2) . . . . ? C27 C28 C29 C30 0.1(2) . . . . ? C28 C29 C30 C25 -0.8(2) . . . . ? C26 C25 C30 C29 0.7(2) . . . . ? B1 C25 C30 C29 -176.09(14) . . . . ? C37 B1 C31 C32 27.16(18) . . . . ? C25 B1 C31 C32 -94.62(16) . . . . ? C19 B1 C31 C32 148.54(14) . . . . ? C37 B1 C31 C36 -158.78(13) . . . . ? C25 B1 C31 C36 79.44(16) . . . . ? C19 B1 C31 C36 -37.40(18) . . . . ? C36 C31 C32 C33 -1.3(2) . . . . ? B1 C31 C32 C33 173.15(15) . . . . ? C31 C32 C33 C34 -0.6(3) . . . . ? C32 C33 C34 C35 1.8(3) . . . . ? C33 C34 C35 C36 -1.0(3) . . . . ? C34 C35 C36 C31 -1.0(3) . . . . ? C32 C31 C36 C35 2.2(2) . . . . ? B1 C31 C36 C35 -172.32(14) . . . . ? C31 B1 C37 C42 -133.23(13) . . . . ? C25 B1 C37 C42 -13.34(18) . . . . ? C19 B1 C37 C42 105.78(15) . . . . ? C31 B1 C37 C38 48.81(17) . . . . ? C25 B1 C37 C38 168.70(12) . . . . ? C19 B1 C37 C38 -72.18(16) . . . . ? C42 C37 C38 C39 -1.3(2) . . . . ? B1 C37 C38 C39 176.80(13) . . . . ? C37 C38 C39 C40 0.7(2) . . . . ? C38 C39 C40 C41 0.2(2) . . . . ? C39 C40 C41 C42 -0.3(2) . . . . ? C40 C41 C42 C37 -0.5(2) . . . . ? C38 C37 C42 C41 1.3(2) . . . . ? B1 C37 C42 C41 -176.81(13) . . . . ? C61 B2 C43 C44 -7.53(18) . . . . ? C55 B2 C43 C44 -130.47(13) . . . . ? C49 B2 C43 C44 109.82(15) . . . . ? C61 B2 C43 C48 172.42(11) . . . . ? C55 B2 C43 C48 49.48(15) . . . . ? C49 B2 C43 C48 -70.23(15) . . . . ? C48 C43 C44 C45 0.04(19) . . . . ? B2 C43 C44 C45 179.99(12) . . . . ? C43 C44 C45 C46 0.2(2) . . . . ? C44 C45 C46 C47 -0.3(2) . . . . ? C45 C46 C47 C48 0.1(2) . . . . ? C46 C47 C48 C43 0.2(2) . . . . ? C44 C43 C48 C47 -0.25(19) . . . . ? B2 C43 C48 C47 179.80(12) . . . . ? C61 B2 C49 C50 122.15(14) . . . . ? C55 B2 C49 C50 -117.84(14) . . . . ? C43 B2 C49 C50 -1.13(19) . . . . ? C61 B2 C49 C54 -55.31(15) . . . . ? C55 B2 C49 C54 64.69(16) . . . . ? C43 B2 C49 C54 -178.59(12) . . . . ? C54 C49 C50 C51 -0.7(2) . . . . ? B2 C49 C50 C51 -178.24(13) . . . . ? C49 C50 C51 C52 -0.2(2) . . . . ? C50 C51 C52 C53 0.9(2) . . . . ? C51 C52 C53 C54 -0.7(2) . . . . ? C52 C53 C54 C49 -0.2(2) . . . . ? C50 C49 C54 C53 0.8(2) . . . . ? B2 C49 C54 C53 178.54(13) . . . . ? C61 B2 C55 C56 132.36(13) . . . . ? C49 B2 C55 C56 16.79(18) . . . . ? C43 B2 C55 C56 -103.01(14) . . . . ? C61 B2 C55 C60 -51.95(17) . . . . ? C49 B2 C55 C60 -167.53(12) . . . . ? C43 B2 C55 C60 72.67(15) . . . . ? C60 C55 C56 C57 1.3(2) . . . . ? B2 C55 C56 C57 177.24(13) . . . . ? C55 C56 C57 C58 0.1(2) . . . . ? C56 C57 C58 C59 -1.0(2) . . . . ? C57 C58 C59 C60 0.5(2) . . . . ? C58 C59 C60 C55 1.0(2) . . . . ? C56 C55 C60 C59 -1.9(2) . . . . ? B2 C55 C60 C59 -177.91(13) . . . . ? C55 B2 C61 C62 -10.04(18) . . . . ? C49 B2 C61 C62 109.31(14) . . . . ? C43 B2 C61 C62 -129.73(13) . . . . ? C55 B2 C61 C66 176.81(11) . . . . ? C49 B2 C61 C66 -63.83(14) . . . . ? C43 B2 C61 C66 57.13(16) . . . . ? C66 C61 C62 C63 -0.82(19) . . . . ? B2 C61 C62 C63 -174.28(12) . . . . ? C61 C62 C63 C64 0.2(2) . . . . ? C62 C63 C64 C65 0.6(2) . . . . ? C63 C64 C65 C66 -0.6(2) . . . . ? C64 C65 C66 C61 -0.1(2) . . . . ? C62 C61 C66 C65 0.78(19) . . . . ? B2 C61 C66 C65 174.61(12) . . . . ? N2 C7 N1 C5 0.19(17) . . . . ? N2 C7 N1 C2 176.70(13) . . . . ? C6 C5 N1 C7 -0.08(19) . . . . ? C6 C5 N1 C2 -176.69(14) . . . . ? C1 C2 N1 C7 8.4(2) . . . . ? C4 C2 N1 C7 -111.30(16) . . . . ? C3 C2 N1 C7 128.07(16) . . . . ? C1 C2 N1 C5 -175.68(15) . . . . ? C4 C2 N1 C5 64.65(18) . . . . ? C3 C2 N1 C5 -56.0(2) . . . . ? N1 C7 N2 C6 -0.22(17) . . . . ? N1 C7 N2 C8 -178.32(13) . . . . ? C5 C6 N2 C7 0.17(18) . . . . ? C5 C6 N2 C8 178.29(14) . . . . ? C9 C8 N2 C7 -67.90(18) . . . . ? C9 C8 N2 C6 114.30(16) . . . . ? C11 C10 N3 C9 -170.51(11) . . . . ? C8 C9 N3 C10 -170.93(11) . . . . ? N5 C14 N4 C12 0.23(16) . . . . ? N5 C14 N4 C11 -176.15(11) . . . . ? C13 C12 N4 C14 -0.11(16) . . . . ? C13 C12 N4 C11 176.10(13) . . . . ? C10 C11 N4 C14 -81.06(16) . . . . ? C10 C11 N4 C12 103.27(16) . . . . ? N4 C14 N5 C13 -0.25(16) . . . . ? N4 C14 N5 C15 -179.54(12) . . . . ? C12 C13 N5 C14 0.18(17) . . . . ? C12 C13 N5 C15 179.46(13) . . . . ? C18 C15 N5 C14 -15.7(2) . . . . ? C17 C15 N5 C14 -134.72(15) . . . . ? C16 C15 N5 C14 104.14(17) . . . . ? C18 C15 N5 C13 165.16(14) . . . . ? C17 C15 N5 C13 46.1(2) . . . . ? C16 C15 N5 C13 -75.01(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.321 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.043 #============= Material Relevant to Compound(12)===================== data_compound12 _database_code_depnum_ccdc_archive 'CCDC 639056' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H37 Cl2 N5 Pd' _chemical_formula_sum 'C25 H37 Cl2 N5 Pd' _chemical_formula_weight 584.90 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9590(11) _cell_length_b 13.4961(11) _cell_length_c 16.3190(14) _cell_angle_alpha 105.876(2) _cell_angle_beta 102.093(2) _cell_angle_gamma 92.241(2) _cell_volume 2670.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2903 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.10 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19413 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.1028 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.32 _reflns_number_total 13121 _reflns_number_gt 8171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the t-butyl gropus shows considerable disorder [C(11)-C(14)] and each of the methyl groups are modelled in two positions of equal weighting differing by a rotation of 60 degrees about the N(1)-C(11) bond. ; _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^)+(0.0484P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13121 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.965 _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 0.3276(4) 0.3076(3) 0.1340(3) 0.0216(10) Uani 1 1 d . . . C2 C 0.4776(3) 0.3574(3) 0.0991(3) 0.0224(10) Uani 1 1 d . . . H2 H 0.5253 0.3947 0.0806 0.027 Uiso 1 1 calc R . . C3 C 0.4949(4) 0.2720(4) 0.1254(3) 0.0249(10) Uani 1 1 d . . . H3 H 0.5567 0.2390 0.1285 0.030 Uiso 1 1 calc R . . C4 C 0.3908(4) 0.1569(3) 0.1840(3) 0.0235(10) Uani 1 1 d . . . H4A H 0.3523 0.1781 0.2299 0.028 Uiso 1 1 calc R . . H4B H 0.4604 0.1418 0.2105 0.028 Uiso 1 1 calc R . . C5 C 0.3316(4) 0.0580(3) 0.1160(3) 0.0204(10) Uani 1 1 d . . . H5A H 0.2786 0.0763 0.0725 0.024 Uiso 1 1 calc R . . H5B H 0.3813 0.0191 0.0863 0.024 Uiso 1 1 calc R . . C6 C 0.1836(3) 0.0354(3) 0.1821(3) 0.0201(9) Uani 1 1 d . . . H6A H 0.2014 0.1076 0.2158 0.024 Uiso 1 1 calc R . . H6B H 0.1609 -0.0013 0.2198 0.024 Uiso 1 1 calc R . . C7 C 0.0902(3) 0.0281(3) 0.1050(3) 0.0190(9) Uani 1 1 d . . . H7A H 0.1170 0.0404 0.0570 0.023 Uiso 1 1 calc R . . H7B H 0.0538 -0.0413 0.0851 0.023 Uiso 1 1 calc R . . C8 C -0.0841(3) 0.0756(3) 0.1396(3) 0.0212(10) Uani 1 1 d . . . H8 H -0.1130 0.0092 0.1338 0.025 Uiso 1 1 calc R . . C9 C -0.1301(4) 0.1634(3) 0.1607(3) 0.0226(10) Uani 1 1 d . . . H9 H -0.1971 0.1693 0.1725 0.027 Uiso 1 1 calc R . . C10 C 0.0322(3) 0.2071(3) 0.1422(3) 0.0169(9) Uani 1 1 d . . . C11 C 0.3298(4) 0.4763(3) 0.0920(3) 0.0218(10) Uani 1 1 d . . . C12A C 0.2146(7) 0.4538(7) 0.0336(6) 0.022(2) Uani 0.50 1 d P A 1 H12A H 0.1710 0.4153 0.0575 0.034 Uiso 0.50 1 calc PR A 1 H12B H 0.2160 0.4143 -0.0247 0.034 Uiso 0.50 1 calc PR A 1 H12C H 0.1861 0.5181 0.0323 0.034 Uiso 0.50 1 calc PR A 1 C13A C 0.3962(7) 0.5332(7) 0.0502(7) 0.025(2) Uani 0.50 1 d P A 1 H13A H 0.3630 0.5928 0.0411 0.038 Uiso 0.50 1 calc PR A 1 H13B H 0.4023 0.4881 -0.0050 0.038 Uiso 0.50 1 calc PR A 1 H13C H 0.4656 0.5548 0.0880 0.038 Uiso 0.50 1 calc PR A 1 C14A C 0.3295(8) 0.5426(7) 0.1839(6) 0.027(2) Uani 0.50 1 d P A 1 H14A H 0.3114 0.6104 0.1819 0.040 Uiso 0.50 1 calc PR A 1 H14B H 0.3987 0.5483 0.2213 0.040 Uiso 0.50 1 calc PR A 1 H14C H 0.2783 0.5110 0.2063 0.040 Uiso 0.50 1 calc PR A 1 C12B C 0.3078(10) 0.4571(9) -0.0072(7) 0.046(3) Uani 0.50 1 d P A 2 H12D H 0.2509 0.4029 -0.0352 0.070 Uiso 0.50 1 calc PR A 2 H12E H 0.3705 0.4369 -0.0274 0.070 Uiso 0.50 1 calc PR A 2 H12F H 0.2884 0.5194 -0.0213 0.070 Uiso 0.50 1 calc PR A 2 C13B C 0.4106(10) 0.5654(9) 0.1333(9) 0.050(3) Uani 0.50 1 d P A 2 H13D H 0.3802 0.6276 0.1277 0.075 Uiso 0.50 1 calc PR A 2 H13E H 0.4690 0.5562 0.1050 0.075 Uiso 0.50 1 calc PR A 2 H13F H 0.4356 0.5705 0.1941 0.075 Uiso 0.50 1 calc PR A 2 C14B C 0.2327(10) 0.4947(9) 0.1209(10) 0.055(4) Uani 0.50 1 d P A 2 H14D H 0.1786 0.4396 0.0869 0.083 Uiso 0.50 1 calc PR A 2 H14E H 0.2104 0.5593 0.1134 0.083 Uiso 0.50 1 calc PR A 2 H14F H 0.2443 0.4975 0.1816 0.083 Uiso 0.50 1 calc PR A 2 C15 C -0.0845(4) 0.3549(3) 0.1847(3) 0.0216(10) Uani 1 1 d . . . C16 C -0.0106(4) 0.4217(3) 0.1551(3) 0.0269(11) Uani 1 1 d . . . H16A H 0.0604 0.4263 0.1890 0.040 Uiso 1 1 calc R . . H16B H -0.0335 0.4898 0.1633 0.040 Uiso 1 1 calc R . . H16C H -0.0124 0.3911 0.0943 0.040 Uiso 1 1 calc R . . C17 C -0.0720(4) 0.3927(4) 0.2838(3) 0.0295(11) Uani 1 1 d . . . H17A H -0.1184 0.3491 0.3011 0.044 Uiso 1 1 calc R . . H17B H -0.0898 0.4627 0.3002 0.044 Uiso 1 1 calc R . . H17C H 0.0001 0.3901 0.3125 0.044 Uiso 1 1 calc R . . C18 C -0.1993(4) 0.3572(4) 0.1370(3) 0.0288(11) Uani 1 1 d . . . H18A H -0.2077 0.3252 0.0755 0.043 Uiso 1 1 calc R . . H18B H -0.2155 0.4277 0.1467 0.043 Uiso 1 1 calc R . . H18C H -0.2466 0.3202 0.1591 0.043 Uiso 1 1 calc R . . C19 C 0.2595(4) -0.1148(3) 0.1063(3) 0.0210(10) Uani 1 1 d . . . H19A H 0.3258 -0.1404 0.0957 0.025 Uiso 1 1 calc R . . H19B H 0.2129 -0.1200 0.0501 0.025 Uiso 1 1 calc R . . C20 C 0.2095(4) -0.1812(3) 0.1508(3) 0.0209(10) Uani 1 1 d . . . C21 C 0.2516(4) -0.1750(4) 0.2379(3) 0.0276(11) Uani 1 1 d . . . H21 H 0.3136 -0.1320 0.2678 0.033 Uiso 1 1 calc R . . C22 C 0.2031(4) -0.2313(4) 0.2809(3) 0.0299(12) Uani 1 1 d . . . H22 H 0.2323 -0.2259 0.3393 0.036 Uiso 1 1 calc R . . C23 C 0.1111(4) -0.2958(4) 0.2370(3) 0.0288(11) Uani 1 1 d . . . H23 H 0.0787 -0.3347 0.2655 0.035 Uiso 1 1 calc R . . C24 C 0.0679(4) -0.3022(4) 0.1509(3) 0.0304(11) Uani 1 1 d . . . H24 H 0.0055 -0.3447 0.1211 0.037 Uiso 1 1 calc R . . C25 C 0.1181(4) -0.2448(3) 0.1087(3) 0.0232(10) Uani 1 1 d . . . H25 H 0.0887 -0.2498 0.0504 0.028 Uiso 1 1 calc R . . C26 C 0.6979(4) 0.2464(3) 0.4856(3) 0.0190(9) Uani 1 1 d . . . C27 C 0.6385(4) 0.3717(4) 0.5809(3) 0.0252(10) Uani 1 1 d . . . H27 H 0.5937 0.4074 0.6137 0.030 Uiso 1 1 calc R . . C28 C 0.7373(4) 0.4052(3) 0.5832(3) 0.0234(10) Uani 1 1 d . . . H28 H 0.7744 0.4683 0.6178 0.028 Uiso 1 1 calc R . . C29 C 0.8744(4) 0.3398(3) 0.4982(3) 0.0218(10) Uani 1 1 d . . . H29A H 0.9011 0.4126 0.5182 0.026 Uiso 1 1 calc R . . H29B H 0.8610 0.3180 0.4348 0.026 Uiso 1 1 calc R . . C30 C 0.9599(3) 0.2779(3) 0.5344(3) 0.0212(10) Uani 1 1 d . . . H30A H 0.9977 0.3178 0.5928 0.025 Uiso 1 1 calc R . . H30B H 0.9267 0.2142 0.5385 0.025 Uiso 1 1 calc R . . C31 C 0.9915(4) 0.1704(3) 0.3960(3) 0.0207(10) Uani 1 1 d . . . H31A H 1.0395 0.1670 0.3572 0.025 Uiso 1 1 calc R . . H31B H 0.9242 0.1879 0.3674 0.025 Uiso 1 1 calc R . . C32 C 0.9743(3) 0.0628(3) 0.4089(3) 0.0201(10) Uani 1 1 d . . . H32A H 1.0413 0.0329 0.4153 0.024 Uiso 1 1 calc R . . H32B H 0.9500 0.0701 0.4624 0.024 Uiso 1 1 calc R . . C33 C 0.9237(4) -0.0922(3) 0.2773(3) 0.0228(10) Uani 1 1 d . . . H33 H 0.9911 -0.1137 0.2780 0.027 Uiso 1 1 calc R . . C34 C 0.8330(4) -0.1377(3) 0.2193(3) 0.0235(10) Uani 1 1 d . . . H34 H 0.8260 -0.1965 0.1720 0.028 Uiso 1 1 calc R . . C35 C 0.7915(4) 0.0004(3) 0.3159(3) 0.0187(9) Uani 1 1 d . . . C36 C 0.5051(4) 0.2172(4) 0.4986(3) 0.0261(11) Uani 1 1 d . . . C37 C 0.4295(5) 0.2832(5) 0.4554(5) 0.0591(19) Uani 1 1 d . . . H37A H 0.4340 0.3511 0.4953 0.089 Uiso 1 1 calc R . . H37B H 0.3581 0.2509 0.4406 0.089 Uiso 1 1 calc R . . H37C H 0.4494 0.2886 0.4032 0.089 Uiso 1 1 calc R . . C38 C 0.4784(5) 0.2072(6) 0.5820(4) 0.066(2) Uani 1 1 d . . . H38A H 0.5284 0.1677 0.6082 0.098 Uiso 1 1 calc R . . H38B H 0.4081 0.1726 0.5688 0.098 Uiso 1 1 calc R . . H38C H 0.4815 0.2748 0.6220 0.098 Uiso 1 1 calc R . . C39 C 0.4973(4) 0.1114(4) 0.4326(4) 0.0416(14) Uani 1 1 d . . . H39A H 0.5172 0.1192 0.3811 0.062 Uiso 1 1 calc R . . H39B H 0.4257 0.0795 0.4172 0.062 Uiso 1 1 calc R . . H39C H 0.5440 0.0686 0.4578 0.062 Uiso 1 1 calc R . . C40 C 0.6401(4) -0.1023(4) 0.1891(3) 0.0243(10) Uani 1 1 d . . . C41 C 0.6319(4) -0.0483(4) 0.1184(3) 0.0335(12) Uani 1 1 d . . . H41A H 0.6462 0.0252 0.1449 0.050 Uiso 1 1 calc R . . H41B H 0.5617 -0.0639 0.0814 0.050 Uiso 1 1 calc R . . H41C H 0.6826 -0.0718 0.0840 0.050 Uiso 1 1 calc R . . C42 C 0.5635(4) -0.0653(4) 0.2461(3) 0.0337(12) Uani 1 1 d . . . H42A H 0.5774 -0.0927 0.2954 0.051 Uiso 1 1 calc R . . H42B H 0.4921 -0.0886 0.2129 0.051 Uiso 1 1 calc R . . H42C H 0.5721 0.0090 0.2665 0.051 Uiso 1 1 calc R . . C43 C 0.6156(5) -0.2191(4) 0.1457(4) 0.0528(18) Uani 1 1 d . . . H43A H 0.6638 -0.2423 0.1087 0.079 Uiso 1 1 calc R . . H43B H 0.5441 -0.2338 0.1111 0.079 Uiso 1 1 calc R . . H43C H 0.6236 -0.2545 0.1900 0.079 Uiso 1 1 calc R . . C44 C 1.1376(3) 0.2320(3) 0.5239(3) 0.0252(10) Uani 1 1 d . . . H44A H 1.1763 0.1966 0.4815 0.030 Uiso 1 1 calc R . . H44B H 1.1254 0.1861 0.5582 0.030 Uiso 1 1 calc R . . C45 C 1.2047(3) 0.3299(3) 0.5841(3) 0.0211(10) Uani 1 1 d . . . C46 C 1.2473(4) 0.3387(4) 0.6708(3) 0.0299(12) Uani 1 1 d . . . H46 H 1.2310 0.2858 0.6939 0.036 Uiso 1 1 calc R . . C47 C 1.3145(4) 0.4258(4) 0.7245(3) 0.0346(13) Uani 1 1 d . . . H47 H 1.3422 0.4310 0.7831 0.042 Uiso 1 1 calc R . . C48 C 1.3396(4) 0.5040(4) 0.6908(3) 0.0310(12) Uani 1 1 d . . . H48 H 1.3852 0.5617 0.7263 0.037 Uiso 1 1 calc R . . C49 C 1.2970(4) 0.4967(4) 0.6042(3) 0.0292(11) Uani 1 1 d . . . H49 H 1.3138 0.5496 0.5813 0.035 Uiso 1 1 calc R . . C50 C 1.2290(4) 0.4103(3) 0.5512(3) 0.0261(11) Uani 1 1 d . . . H50 H 1.1994 0.4064 0.4932 0.031 Uiso 1 1 calc R . . Cl3 Cl 0.68604(9) 0.20989(8) 0.29305(7) 0.0199(2) Uani 1 1 d . . . Cl4 Cl 0.76130(9) 0.03249(8) 0.50341(7) 0.0223(2) Uani 1 1 d . . . Cl1 Cl 0.21826(10) 0.33106(9) 0.29138(7) 0.0272(3) Uani 1 1 d . . . Cl2 Cl 0.13759(9) 0.20314(9) -0.01130(7) 0.0251(3) Uani 1 1 d . . . N1 N 0.3748(3) 0.3791(3) 0.1048(2) 0.0216(8) Uani 1 1 d . A . N2 N 0.4035(3) 0.2431(3) 0.1468(3) 0.0218(8) Uani 1 1 d . . . N3 N 0.2801(3) -0.0062(3) 0.1583(2) 0.0190(8) Uani 1 1 d . . . N4 N 0.0146(3) 0.1029(3) 0.1282(2) 0.0188(8) Uani 1 1 d . . . N5 N -0.0591(3) 0.2443(3) 0.1615(2) 0.0176(8) Uani 1 1 d . . . N6 N 0.6140(3) 0.2737(3) 0.5209(2) 0.0211(8) Uani 1 1 d . . . N7 N 0.7742(3) 0.3279(3) 0.5240(2) 0.0193(8) Uani 1 1 d . . . N8 N 1.0349(3) 0.2533(3) 0.4773(2) 0.0212(8) Uani 1 1 d . . . N9 N 0.8969(3) -0.0072(3) 0.3358(2) 0.0180(8) Uani 1 1 d . . . N10 N 0.7519(3) -0.0801(3) 0.2434(2) 0.0188(8) Uani 1 1 d . . . Pd2 Pd 0.73076(3) 0.11950(3) 0.39681(2) 0.01594(9) Uani 1 1 d . . . Pd1 Pd 0.17656(3) 0.26958(3) 0.13986(2) 0.01671(9) 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 0.021(2) 0.013(2) 0.028(2) 0.0006(19) 0.006(2) -0.0022(18) C2 0.017(2) 0.020(2) 0.029(3) 0.005(2) 0.006(2) 0.0013(18) C3 0.019(2) 0.022(2) 0.030(3) 0.003(2) 0.004(2) 0.0006(19) C4 0.021(2) 0.019(2) 0.032(3) 0.013(2) 0.003(2) 0.0017(19) C5 0.021(2) 0.017(2) 0.026(2) 0.009(2) 0.0058(19) 0.0038(18) C6 0.023(2) 0.014(2) 0.024(2) 0.0046(19) 0.0066(19) 0.0011(18) C7 0.021(2) 0.012(2) 0.026(2) 0.0050(19) 0.0092(19) 0.0047(17) C8 0.023(2) 0.015(2) 0.027(2) 0.007(2) 0.008(2) -0.0022(18) C9 0.022(2) 0.019(2) 0.031(3) 0.008(2) 0.012(2) 0.0005(19) C10 0.019(2) 0.013(2) 0.018(2) 0.0042(18) 0.0054(18) 0.0023(17) C11 0.028(3) 0.010(2) 0.030(3) 0.008(2) 0.006(2) 0.0021(18) C12A 0.023(5) 0.020(5) 0.028(5) 0.017(4) 0.001(4) 0.004(4) C13A 0.024(5) 0.015(5) 0.041(6) 0.011(5) 0.010(4) 0.006(4) C14A 0.040(6) 0.012(4) 0.031(5) 0.004(4) 0.013(5) 0.008(4) C12B 0.056(8) 0.038(7) 0.052(7) 0.018(6) 0.016(6) 0.019(6) C13B 0.063(9) 0.027(6) 0.072(9) 0.022(7) 0.031(7) 0.008(6) C14B 0.047(8) 0.036(7) 0.102(12) 0.036(8) 0.037(8) 0.012(6) C15 0.025(2) 0.012(2) 0.026(2) 0.0018(19) 0.009(2) 0.0028(18) C16 0.034(3) 0.014(2) 0.038(3) 0.007(2) 0.018(2) 0.004(2) C17 0.040(3) 0.022(3) 0.027(3) 0.004(2) 0.011(2) 0.006(2) C18 0.033(3) 0.017(2) 0.036(3) 0.004(2) 0.011(2) 0.005(2) C19 0.028(3) 0.013(2) 0.022(2) 0.0039(18) 0.0061(19) 0.0020(18) C20 0.025(2) 0.010(2) 0.029(3) 0.0057(19) 0.007(2) 0.0073(18) C21 0.031(3) 0.021(2) 0.027(3) 0.006(2) 0.002(2) -0.001(2) C22 0.047(3) 0.021(3) 0.023(2) 0.006(2) 0.008(2) 0.010(2) C23 0.036(3) 0.017(2) 0.037(3) 0.009(2) 0.015(2) 0.004(2) C24 0.032(3) 0.022(3) 0.036(3) 0.008(2) 0.006(2) -0.001(2) C25 0.033(3) 0.015(2) 0.020(2) 0.0031(19) 0.003(2) 0.0041(19) C26 0.023(2) 0.018(2) 0.017(2) 0.0070(19) 0.0041(18) 0.0048(18) C27 0.031(3) 0.027(3) 0.019(2) 0.006(2) 0.009(2) 0.013(2) C28 0.033(3) 0.016(2) 0.018(2) 0.0000(19) 0.006(2) 0.006(2) C29 0.027(2) 0.014(2) 0.026(2) 0.0056(19) 0.008(2) 0.0022(18) C30 0.022(2) 0.020(2) 0.021(2) 0.004(2) 0.0074(19) -0.0010(19) C31 0.019(2) 0.019(2) 0.023(2) 0.003(2) 0.0071(19) 0.0020(18) C32 0.017(2) 0.018(2) 0.024(2) 0.0035(19) 0.0037(19) 0.0046(18) C33 0.033(3) 0.012(2) 0.027(2) 0.004(2) 0.016(2) 0.0082(19) C34 0.036(3) 0.016(2) 0.020(2) 0.004(2) 0.011(2) 0.004(2) C35 0.029(3) 0.012(2) 0.015(2) 0.0035(18) 0.0066(19) 0.0042(18) C36 0.021(2) 0.031(3) 0.028(3) 0.007(2) 0.009(2) 0.005(2) C37 0.037(4) 0.053(4) 0.077(5) 0.014(4) -0.006(3) 0.017(3) C38 0.047(4) 0.112(6) 0.033(3) 0.017(4) 0.010(3) -0.034(4) C39 0.024(3) 0.030(3) 0.068(4) 0.002(3) 0.017(3) 0.002(2) C40 0.028(3) 0.020(2) 0.021(2) 0.005(2) 0.000(2) -0.002(2) C41 0.031(3) 0.048(3) 0.025(3) 0.018(3) 0.005(2) 0.004(2) C42 0.023(3) 0.050(3) 0.026(3) 0.010(3) 0.004(2) -0.005(2) C43 0.058(4) 0.019(3) 0.058(4) 0.001(3) -0.020(3) -0.007(3) C44 0.018(2) 0.019(2) 0.036(3) 0.005(2) 0.004(2) 0.0011(19) C45 0.016(2) 0.018(2) 0.027(2) 0.003(2) 0.0039(19) 0.0023(18) C46 0.035(3) 0.027(3) 0.032(3) 0.015(2) 0.008(2) 0.003(2) C47 0.046(3) 0.028(3) 0.021(3) 0.004(2) -0.006(2) 0.003(2) C48 0.032(3) 0.019(2) 0.031(3) -0.006(2) 0.000(2) 0.002(2) C49 0.036(3) 0.016(2) 0.033(3) 0.005(2) 0.005(2) 0.002(2) C50 0.034(3) 0.019(2) 0.022(2) 0.006(2) 0.001(2) 0.002(2) Cl3 0.0229(6) 0.0178(5) 0.0210(5) 0.0075(5) 0.0065(4) 0.0044(4) Cl4 0.0269(6) 0.0191(5) 0.0235(6) 0.0094(5) 0.0062(5) 0.0060(5) Cl1 0.0337(7) 0.0204(6) 0.0208(6) -0.0022(5) 0.0024(5) 0.0034(5) Cl2 0.0264(6) 0.0304(6) 0.0196(6) 0.0077(5) 0.0069(5) 0.0037(5) N1 0.022(2) 0.0132(18) 0.030(2) 0.0047(17) 0.0079(17) -0.0010(15) N2 0.021(2) 0.0132(19) 0.033(2) 0.0100(17) 0.0054(17) 0.0004(15) N3 0.0208(19) 0.0120(18) 0.024(2) 0.0037(16) 0.0069(16) 0.0027(15) N4 0.022(2) 0.0139(18) 0.0210(19) 0.0051(16) 0.0069(16) 0.0016(15) N5 0.023(2) 0.0129(18) 0.0186(19) 0.0020(15) 0.0112(16) 0.0010(15) N6 0.023(2) 0.019(2) 0.025(2) 0.0074(17) 0.0109(17) 0.0084(16) N7 0.024(2) 0.0130(18) 0.021(2) 0.0047(16) 0.0060(16) 0.0035(15) N8 0.0170(19) 0.019(2) 0.025(2) 0.0039(17) 0.0030(16) -0.0002(15) N9 0.0197(19) 0.0135(18) 0.0205(19) 0.0038(16) 0.0046(16) 0.0037(15) N10 0.025(2) 0.0114(18) 0.0177(19) 0.0020(15) 0.0040(16) 0.0009(15) Pd2 0.01774(18) 0.01174(16) 0.01824(17) 0.00320(14) 0.00503(14) 0.00360(13) Pd1 0.01852(18) 0.01131(17) 0.02011(18) 0.00390(14) 0.00507(14) 0.00013(13) _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 1.360(6) . ? C1 N1 1.364(5) . ? C1 Pd1 2.032(4) . ? C2 C3 1.346(6) . ? C2 N1 1.391(6) . ? C2 H2 0.9300 . ? C3 N2 1.374(6) . ? C3 H3 0.9300 . ? C4 N2 1.471(5) . ? C4 C5 1.535(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.466(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.474(5) . ? C6 C7 1.530(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.464(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.341(6) . ? C8 N4 1.381(5) . ? C8 H8 0.9300 . ? C9 N5 1.395(5) . ? C9 H9 0.9300 . ? C10 N4 1.364(5) . ? C10 N5 1.366(5) . ? C10 Pd1 2.034(4) . ? C11 C14B 1.442(12) . ? C11 C13B 1.470(12) . ? C11 N1 1.504(5) . ? C11 C13A 1.508(10) . ? C11 C14A 1.523(10) . ? C11 C12B 1.529(12) . ? C11 C12A 1.561(9) . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15 N5 1.504(5) . ? C15 C16 1.526(6) . ? C15 C17 1.528(6) . ? C15 C18 1.533(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.460(5) . ? C19 C20 1.503(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C25 1.367(6) . ? C20 C21 1.390(6) . ? C21 C22 1.379(7) . ? C21 H21 0.9300 . ? C22 C23 1.383(7) . ? C22 H22 0.9300 . ? C23 C24 1.377(7) . ? C23 H23 0.9300 . ? C24 C25 1.392(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 N6 1.352(6) . ? C26 N7 1.364(5) . ? C26 Pd2 2.042(4) . ? C27 C28 1.331(7) . ? C27 N6 1.391(6) . ? C27 H27 0.9300 . ? C28 N7 1.391(6) . ? C28 H28 0.9300 . ? C29 N7 1.463(6) . ? C29 C30 1.531(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N8 1.470(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N8 1.468(5) . ? C31 C32 1.537(6) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N9 1.459(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.346(6) . ? C33 N9 1.385(5) . ? C33 H33 0.9300 . ? C34 N10 1.390(6) . ? C34 H34 0.9300 . ? C35 N9 1.350(6) . ? C35 N10 1.356(5) . ? C35 Pd2 2.079(4) . ? C36 N6 1.501(6) . ? C36 C38 1.511(7) . ? C36 C39 1.521(7) . ? C36 C37 1.541(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 N10 1.503(6) . ? C40 C42 1.508(7) . ? C40 C41 1.514(6) . ? C40 C43 1.531(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 N8 1.469(5) . ? C44 C45 1.520(6) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.378(6) . ? C45 C50 1.387(6) . ? C46 C47 1.394(7) . ? C46 H46 0.9300 . ? C47 C48 1.374(7) . ? C47 H47 0.9300 . ? C48 C49 1.380(7) . ? C48 H48 0.9300 . ? C49 C50 1.390(6) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? Cl3 Pd2 2.3378(11) . ? Cl4 Pd2 2.3298(11) . ? Cl1 Pd1 2.3189(12) . ? Cl2 Pd1 2.3187(12) . ? 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 104.1(4) . . ? N2 C1 Pd1 120.1(3) . . ? N1 C1 Pd1 134.8(3) . . ? C3 C2 N1 107.1(4) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 106.6(4) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 C5 113.2(4) . . ? N2 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N2 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.8 . . ? N3 C5 C4 110.4(4) . . ? N3 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? N3 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N3 C6 C7 115.3(4) . . ? N3 C6 H6A 108.5 . . ? C7 C6 H6A 108.5 . . ? N3 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N4 C7 C6 112.2(4) . . ? N4 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? N4 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 N4 106.7(4) . . ? C9 C8 H8 126.6 . . ? N4 C8 H8 126.6 . . ? C8 C9 N5 107.4(4) . . ? C8 C9 H9 126.3 . . ? N5 C9 H9 126.3 . . ? N4 C10 N5 104.2(3) . . ? N4 C10 Pd1 119.5(3) . . ? N5 C10 Pd1 136.0(3) . . ? C14B C11 C13B 111.6(8) . . ? C14B C11 N1 113.9(6) . . ? C13B C11 N1 109.9(6) . . ? C14B C11 C13A 133.7(6) . . ? C13B C11 C13A 50.7(6) . . ? N1 C11 C13A 112.4(5) . . ? C14B C11 C14A 58.2(7) . . ? C13B C11 C14A 61.7(6) . . ? N1 C11 C14A 104.7(5) . . ? C13A C11 C14A 110.0(6) . . ? C14B C11 C12B 109.5(8) . . ? C13B C11 C12B 108.2(7) . . ? N1 C11 C12B 103.3(5) . . ? C13A C11 C12B 58.1(6) . . ? C14A C11 C12B 152.0(6) . . ? C14B C11 C12A 53.0(7) . . ? C13B C11 C12A 137.8(6) . . ? N1 C11 C12A 112.1(4) . . ? C13A C11 C12A 107.6(6) . . ? C14A C11 C12A 110.1(6) . . ? C12B C11 C12A 58.1(6) . . ? C11 C12A H12A 109.5 . . ? C11 C12A H12B 109.5 . . ? C11 C12A H12C 109.5 . . ? C11 C13A H13A 109.5 . . ? C11 C13A H13B 109.5 . . ? C11 C13A H13C 109.5 . . ? C11 C14A H14A 109.5 . . ? C11 C14A H14B 109.5 . . ? C11 C14A H14C 109.5 . . ? C11 C12B H12D 109.5 . . ? C11 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11 C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C11 C13B H13D 109.5 . . ? C11 C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C11 C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C11 C14B H14D 109.5 . . ? C11 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C11 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? N5 C15 C16 110.4(4) . . ? N5 C15 C17 107.8(4) . . ? C16 C15 C17 110.9(4) . . ? N5 C15 C18 107.9(4) . . ? C16 C15 C18 109.1(4) . . ? C17 C15 C18 110.7(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 112.3(4) . . ? N3 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N3 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C25 C20 C21 118.0(4) . . ? C25 C20 C19 121.2(4) . . ? C21 C20 C19 120.7(4) . . ? C22 C21 C20 121.3(5) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.9(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.5(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 119.7(5) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C20 C25 C24 121.6(4) . . ? C20 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? N6 C26 N7 105.4(4) . . ? N6 C26 Pd2 135.7(3) . . ? N7 C26 Pd2 119.0(3) . . ? C28 C27 N6 107.9(4) . . ? C28 C27 H27 126.0 . . ? N6 C27 H27 126.0 . . ? C27 C28 N7 106.8(4) . . ? C27 C28 H28 126.6 . . ? N7 C28 H28 126.6 . . ? N7 C29 C30 113.8(3) . . ? N7 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? N7 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N8 C30 C29 110.4(3) . . ? N8 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? N8 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? N8 C31 C32 114.3(4) . . ? N8 C31 H31A 108.7 . . ? C32 C31 H31A 108.7 . . ? N8 C31 H31B 108.7 . . ? C32 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N9 C32 C31 112.2(4) . . ? N9 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? N9 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C34 C33 N9 106.6(4) . . ? C34 C33 H33 126.7 . . ? N9 C33 H33 126.7 . . ? C33 C34 N10 107.1(4) . . ? C33 C34 H34 126.4 . . ? N10 C34 H34 126.4 . . ? N9 C35 N10 105.2(4) . . ? N9 C35 Pd2 118.2(3) . . ? N10 C35 Pd2 136.5(3) . . ? N6 C36 C38 108.7(4) . . ? N6 C36 C39 111.9(4) . . ? C38 C36 C39 110.8(5) . . ? N6 C36 C37 106.0(4) . . ? C38 C36 C37 111.8(5) . . ? C39 C36 C37 107.7(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N10 C40 C42 110.1(4) . . ? N10 C40 C41 108.1(4) . . ? C42 C40 C41 111.1(4) . . ? N10 C40 C43 109.1(4) . . ? C42 C40 C43 109.6(4) . . ? C41 C40 C43 108.7(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N8 C44 C45 112.5(4) . . ? N8 C44 H44A 109.1 . . ? C45 C44 H44A 109.1 . . ? N8 C44 H44B 109.1 . . ? C45 C44 H44B 109.1 . . ? H44A C44 H44B 107.8 . . ? C46 C45 C50 118.6(4) . . ? C46 C45 C44 121.0(4) . . ? C50 C45 C44 120.3(4) . . ? C45 C46 C47 120.9(4) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 119.9(4) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 119.9(5) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? C48 C49 C50 120.0(5) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C45 C50 C49 120.7(4) . . ? C45 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C1 N1 C2 110.5(4) . . ? C1 N1 C11 125.6(4) . . ? C2 N1 C11 123.5(4) . . ? C1 N2 C3 111.7(4) . . ? C1 N2 C4 123.7(4) . . ? C3 N2 C4 124.4(4) . . ? C19 N3 C5 112.2(3) . . ? C19 N3 C6 111.8(3) . . ? C5 N3 C6 112.1(3) . . ? C10 N4 C8 111.4(4) . . ? C10 N4 C7 125.1(4) . . ? C8 N4 C7 123.5(4) . . ? C10 N5 C9 110.2(4) . . ? C10 N5 C15 128.1(3) . . ? C9 N5 C15 121.6(4) . . ? C26 N6 C27 109.8(4) . . ? C26 N6 C36 128.9(4) . . ? C27 N6 C36 121.1(4) . . ? C26 N7 C28 110.2(4) . . ? C26 N7 C29 125.2(4) . . ? C28 N7 C29 124.0(4) . . ? C31 N8 C44 111.6(4) . . ? C31 N8 C30 113.2(3) . . ? C44 N8 C30 112.0(4) . . ? C35 N9 C33 110.9(4) . . ? C35 N9 C32 125.9(4) . . ? C33 N9 C32 123.2(4) . . ? C35 N10 C34 110.1(4) . . ? C35 N10 C40 127.3(4) . . ? C34 N10 C40 122.4(4) . . ? C26 Pd2 C35 170.09(18) . . ? C26 Pd2 Cl4 90.24(12) . . ? C35 Pd2 Cl4 88.51(12) . . ? C26 Pd2 Cl3 86.68(12) . . ? C35 Pd2 Cl3 95.19(12) . . ? Cl4 Pd2 Cl3 175.03(4) . . ? C1 Pd1 C10 170.48(17) . . ? C1 Pd1 Cl2 87.67(13) . . ? C10 Pd1 Cl2 89.96(12) . . ? C1 Pd1 Cl1 91.91(13) . . ? C10 Pd1 Cl1 90.15(12) . . ? Cl2 Pd1 Cl1 178.08(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.2(5) . . . . ? N2 C4 C5 N3 -154.6(4) . . . . ? N3 C6 C7 N4 -158.1(3) . . . . ? N4 C8 C9 N5 0.3(5) . . . . ? N3 C19 C20 C25 127.6(4) . . . . ? N3 C19 C20 C21 -48.5(6) . . . . ? C25 C20 C21 C22 0.2(7) . . . . ? C19 C20 C21 C22 176.4(4) . . . . ? C20 C21 C22 C23 0.3(8) . . . . ? C21 C22 C23 C24 -0.8(8) . . . . ? C22 C23 C24 C25 0.9(8) . . . . ? C21 C20 C25 C24 -0.2(7) . . . . ? C19 C20 C25 C24 -176.3(4) . . . . ? C23 C24 C25 C20 -0.4(8) . . . . ? N6 C27 C28 N7 0.3(5) . . . . ? N7 C29 C30 N8 153.7(4) . . . . ? N8 C31 C32 N9 158.2(4) . . . . ? N9 C33 C34 N10 -0.3(5) . . . . ? N8 C44 C45 C46 127.8(5) . . . . ? N8 C44 C45 C50 -55.7(6) . . . . ? C50 C45 C46 C47 -0.8(8) . . . . ? C44 C45 C46 C47 175.8(5) . . . . ? C45 C46 C47 C48 -0.5(8) . . . . ? C46 C47 C48 C49 1.0(8) . . . . ? C47 C48 C49 C50 -0.2(8) . . . . ? C46 C45 C50 C49 1.6(7) . . . . ? C44 C45 C50 C49 -175.0(5) . . . . ? C48 C49 C50 C45 -1.2(8) . . . . ? N2 C1 N1 C2 0.7(5) . . . . ? Pd1 C1 N1 C2 -167.3(4) . . . . ? N2 C1 N1 C11 -171.4(4) . . . . ? Pd1 C1 N1 C11 20.6(7) . . . . ? C3 C2 N1 C1 -0.4(5) . . . . ? C3 C2 N1 C11 172.0(4) . . . . ? C14B C11 N1 C1 5.2(9) . . . . ? C13B C11 N1 C1 131.3(7) . . . . ? C13A C11 N1 C1 -174.1(6) . . . . ? C14A C11 N1 C1 66.5(6) . . . . ? C12B C11 N1 C1 -113.4(7) . . . . ? C12A C11 N1 C1 -52.8(7) . . . . ? C14B C11 N1 C2 -166.0(8) . . . . ? C13B C11 N1 C2 -39.9(8) . . . . ? C13A C11 N1 C2 14.7(7) . . . . ? C14A C11 N1 C2 -104.7(6) . . . . ? C12B C11 N1 C2 75.4(7) . . . . ? C12A C11 N1 C2 136.0(6) . . . . ? N1 C1 N2 C3 -0.8(5) . . . . ? Pd1 C1 N2 C3 169.3(3) . . . . ? N1 C1 N2 C4 175.8(4) . . . . ? Pd1 C1 N2 C4 -14.0(6) . . . . ? C2 C3 N2 C1 0.6(5) . . . . ? C2 C3 N2 C4 -176.0(4) . . . . ? C5 C4 N2 C1 83.4(5) . . . . ? C5 C4 N2 C3 -100.3(5) . . . . ? C20 C19 N3 C5 178.3(4) . . . . ? C20 C19 N3 C6 -54.7(5) . . . . ? C4 C5 N3 C19 -157.4(4) . . . . ? C4 C5 N3 C6 75.7(4) . . . . ? C7 C6 N3 C19 -57.6(5) . . . . ? C7 C6 N3 C5 69.5(5) . . . . ? N5 C10 N4 C8 -0.8(5) . . . . ? Pd1 C10 N4 C8 174.8(3) . . . . ? N5 C10 N4 C7 179.9(4) . . . . ? Pd1 C10 N4 C7 -4.5(6) . . . . ? C9 C8 N4 C10 0.3(5) . . . . ? C9 C8 N4 C7 179.6(4) . . . . ? C6 C7 N4 C10 72.4(5) . . . . ? C6 C7 N4 C8 -106.9(5) . . . . ? N4 C10 N5 C9 1.0(5) . . . . ? Pd1 C10 N5 C9 -173.5(3) . . . . ? N4 C10 N5 C15 178.6(4) . . . . ? Pd1 C10 N5 C15 4.2(7) . . . . ? C8 C9 N5 C10 -0.9(5) . . . . ? C8 C9 N5 C15 -178.7(4) . . . . ? C16 C15 N5 C10 19.2(6) . . . . ? C17 C15 N5 C10 -102.0(5) . . . . ? C18 C15 N5 C10 138.4(4) . . . . ? C16 C15 N5 C9 -163.4(4) . . . . ? C17 C15 N5 C9 75.4(5) . . . . ? C18 C15 N5 C9 -44.2(5) . . . . ? N7 C26 N6 C27 0.0(5) . . . . ? Pd2 C26 N6 C27 178.8(3) . . . . ? N7 C26 N6 C36 175.3(4) . . . . ? Pd2 C26 N6 C36 -5.9(7) . . . . ? C28 C27 N6 C26 -0.2(5) . . . . ? C28 C27 N6 C36 -175.9(4) . . . . ? C38 C36 N6 C26 128.4(5) . . . . ? C39 C36 N6 C26 5.8(6) . . . . ? C37 C36 N6 C26 -111.3(5) . . . . ? C38 C36 N6 C27 -56.7(6) . . . . ? C39 C36 N6 C27 -179.3(4) . . . . ? C37 C36 N6 C27 63.6(5) . . . . ? N6 C26 N7 C28 0.2(5) . . . . ? Pd2 C26 N7 C28 -178.9(3) . . . . ? N6 C26 N7 C29 -171.5(4) . . . . ? Pd2 C26 N7 C29 9.5(5) . . . . ? C27 C28 N7 C26 -0.3(5) . . . . ? C27 C28 N7 C29 171.5(4) . . . . ? C30 C29 N7 C26 -80.5(5) . . . . ? C30 C29 N7 C28 109.0(5) . . . . ? C32 C31 N8 C44 58.7(5) . . . . ? C32 C31 N8 C30 -68.7(5) . . . . ? C45 C44 N8 C31 156.1(4) . . . . ? C45 C44 N8 C30 -75.8(5) . . . . ? C29 C30 N8 C31 -75.2(4) . . . . ? C29 C30 N8 C44 157.5(4) . . . . ? N10 C35 N9 C33 -0.8(5) . . . . ? Pd2 C35 N9 C33 178.0(3) . . . . ? N10 C35 N9 C32 179.7(4) . . . . ? Pd2 C35 N9 C32 -1.5(5) . . . . ? C34 C33 N9 C35 0.7(5) . . . . ? C34 C33 N9 C32 -179.8(4) . . . . ? C31 C32 N9 C35 -69.8(5) . . . . ? C31 C32 N9 C33 110.7(4) . . . . ? N9 C35 N10 C34 0.6(5) . . . . ? Pd2 C35 N10 C34 -177.9(3) . . . . ? N9 C35 N10 C40 -174.0(4) . . . . ? Pd2 C35 N10 C40 7.6(7) . . . . ? C33 C34 N10 C35 -0.2(5) . . . . ? C33 C34 N10 C40 174.7(4) . . . . ? C42 C40 N10 C35 -31.8(6) . . . . ? C41 C40 N10 C35 89.7(5) . . . . ? C43 C40 N10 C35 -152.1(5) . . . . ? C42 C40 N10 C34 154.3(4) . . . . ? C41 C40 N10 C34 -84.2(5) . . . . ? C43 C40 N10 C34 33.9(6) . . . . ? N6 C26 Pd2 Cl4 -78.2(4) . . . . ? N7 C26 Pd2 Cl4 100.5(3) . . . . ? N6 C26 Pd2 Cl3 97.9(4) . . . . ? N7 C26 Pd2 Cl3 -83.4(3) . . . . ? N9 C35 Pd2 Cl4 -71.5(3) . . . . ? N10 C35 Pd2 Cl4 106.8(4) . . . . ? N9 C35 Pd2 Cl3 111.8(3) . . . . ? N10 C35 Pd2 Cl3 -69.8(4) . . . . ? N2 C1 Pd1 Cl2 -96.0(4) . . . . ? N1 C1 Pd1 Cl2 70.5(5) . . . . ? N2 C1 Pd1 Cl1 82.1(4) . . . . ? N1 C1 Pd1 Cl1 -111.4(5) . . . . ? N4 C10 Pd1 Cl2 74.1(3) . . . . ? N5 C10 Pd1 Cl2 -112.1(4) . . . . ? N4 C10 Pd1 Cl1 -104.0(3) . . . . ? N5 C10 Pd1 Cl1 69.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.322 _refine_diff_density_min -0.969 _refine_diff_density_rms 0.130 #============= Material Relevant to Compound(17)===================== data_compound17 _database_code_depnum_ccdc_archive 'CCDC 639057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H34 N6 Pd, C2 H3 N, 2(B F4)' _chemical_formula_sum 'C22 H37 B2 F8 N7 Pd' _chemical_formula_weight 679.61 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 13.3436(9) _cell_length_b 12.2206(9) _cell_length_c 18.1927(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.253(2) _cell_angle_gamma 90.00 _cell_volume 2958.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2450 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 22.44 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16217 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5203 _reflns_number_gt 4142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H3' was placed (on central bridging nitrogen N3) by difference map after positioning of other hydrogens using riding models ; _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^)+(0.0401P)^2^+5.9577P] 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 5203 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 B1 B 0.8912(5) 0.4706(5) 0.2086(4) 0.0381(15) Uani 1 1 d . . . B2 B 0.3992(4) 0.4192(4) 0.1986(3) 0.0212(11) Uani 1 1 d . . . C1 C 0.7061(3) 0.2224(3) 0.0201(2) 0.0166(9) Uani 1 1 d . . . C2 C 0.6812(3) 0.3923(4) -0.0240(3) 0.0224(10) Uani 1 1 d . . . H2 H 0.6815 0.4527 -0.0552 0.027 Uiso 1 1 calc R . . C3 C 0.6395(3) 0.3873(4) 0.0406(3) 0.0215(10) Uani 1 1 d . . . H3 H 0.6065 0.4435 0.0633 0.026 Uiso 1 1 calc R . . C4 C 0.6375(4) 0.2456(4) 0.1416(3) 0.0275(11) Uani 1 1 d . . . H4A H 0.5915 0.1841 0.1391 0.033 Uiso 1 1 calc R . . H4B H 0.6077 0.3042 0.1686 0.033 Uiso 1 1 calc R . . C5 C 0.7364(4) 0.2119(4) 0.1808(3) 0.0329(12) Uani 1 1 d . . . H5A H 0.7861 0.2682 0.1738 0.040 Uiso 1 1 calc R . . H5B H 0.7283 0.2062 0.2332 0.040 Uiso 1 1 calc R . . C6 C 0.8790(3) 0.0829(4) 0.1769(3) 0.0253(11) Uani 1 1 d . . . H6A H 0.8840 0.0591 0.2279 0.030 Uiso 1 1 calc R . . H6B H 0.9179 0.1496 0.1739 0.030 Uiso 1 1 calc R . . C7 C 0.9231(3) -0.0042(4) 0.1299(3) 0.0226(10) Uani 1 1 d . . . H7A H 0.9334 0.0259 0.0817 0.027 Uiso 1 1 calc R . . H7B H 0.9880 -0.0264 0.1526 0.027 Uiso 1 1 calc R . . C8 C 0.8788(3) -0.2060(4) 0.1432(2) 0.0199(10) Uani 1 1 d . . . H8 H 0.9386 -0.2320 0.1663 0.024 Uiso 1 1 calc R . . C9 C 0.7964(3) -0.2637(4) 0.1244(2) 0.0196(10) Uani 1 1 d . . . H9 H 0.7886 -0.3386 0.1312 0.023 Uiso 1 1 calc R . . C10 C 0.7636(3) -0.0913(3) 0.0891(2) 0.0152(9) Uani 1 1 d . . . C11 C 0.7828(3) 0.2682(4) -0.1017(2) 0.0201(10) Uani 1 1 d . . . C12 C 0.8613(3) 0.1797(4) -0.0826(3) 0.0220(10) Uani 1 1 d . . . H12A H 0.9070 0.2047 -0.0428 0.033 Uiso 1 1 calc R . . H12B H 0.8978 0.1646 -0.1249 0.033 Uiso 1 1 calc R . . H12C H 0.8283 0.1143 -0.0679 0.033 Uiso 1 1 calc R . . C13 C 0.7089(3) 0.2362(4) -0.1664(2) 0.0252(11) Uani 1 1 d . . . H13A H 0.6706 0.1738 -0.1530 0.038 Uiso 1 1 calc R . . H13B H 0.7454 0.2184 -0.2083 0.038 Uiso 1 1 calc R . . H13C H 0.6644 0.2963 -0.1785 0.038 Uiso 1 1 calc R . . C14 C 0.8398(3) 0.3713(4) -0.1207(3) 0.0286(11) Uani 1 1 d . . . H14A H 0.7930 0.4263 -0.1388 0.043 Uiso 1 1 calc R . . H14B H 0.8850 0.3546 -0.1578 0.043 Uiso 1 1 calc R . . H14C H 0.8774 0.3979 -0.0773 0.043 Uiso 1 1 calc R . . C15 C 0.6197(3) -0.2309(4) 0.0686(2) 0.0179(9) Uani 1 1 d . . . C16 C 0.5846(3) -0.3082(4) 0.1267(3) 0.0260(11) Uani 1 1 d . . . H16A H 0.6272 -0.3716 0.1299 0.039 Uiso 1 1 calc R . . H16B H 0.5166 -0.3303 0.1133 0.039 Uiso 1 1 calc R . . H16C H 0.5877 -0.2717 0.1735 0.039 Uiso 1 1 calc R . . C17 C 0.5477(3) -0.1340(4) 0.0624(3) 0.0255(11) Uani 1 1 d . . . H17A H 0.5513 -0.0948 0.1082 0.038 Uiso 1 1 calc R . . H17B H 0.4803 -0.1600 0.0513 0.038 Uiso 1 1 calc R . . H17C H 0.5660 -0.0862 0.0237 0.038 Uiso 1 1 calc R . . C18 C 0.6256(4) -0.2899(4) -0.0052(3) 0.0272(11) Uani 1 1 d . . . H18A H 0.6456 -0.2389 -0.0415 0.041 Uiso 1 1 calc R . . H18B H 0.5610 -0.3197 -0.0208 0.041 Uiso 1 1 calc R . . H18C H 0.6741 -0.3479 0.0004 0.041 Uiso 1 1 calc R . . C19 C 0.6762(3) -0.0370(4) -0.1093(3) 0.0219(10) Uani 1 1 d . . . C20 C 0.6637(4) -0.0823(5) -0.1836(3) 0.0374(13) Uani 1 1 d . . . H20A H 0.6026 -0.0549 -0.2081 0.056 Uiso 1 1 calc R . . H20B H 0.6606 -0.1606 -0.1808 0.056 Uiso 1 1 calc R . . H20C H 0.7196 -0.0611 -0.2107 0.056 Uiso 1 1 calc R . . C21 C 0.0960(4) 0.2344(5) 0.0587(3) 0.0412(14) Uani 1 1 d . . . C22 C 0.0913(5) 0.3543(5) 0.0604(4) 0.062(2) Uani 1 1 d . . . H22A H 0.0911 0.3823 0.0111 0.093 Uiso 1 1 calc R . . H22B H 0.1487 0.3822 0.0894 0.093 Uiso 1 1 calc R . . H22C H 0.0310 0.3768 0.0819 0.093 Uiso 1 1 calc R . . F1 F 0.9014(5) 0.5011(5) 0.1395(3) 0.153(3) Uani 1 1 d . . . F2 F 0.9397(3) 0.3779(3) 0.2203(3) 0.0954(16) Uani 1 1 d . . . F3 F 0.7912(3) 0.4699(3) 0.2178(3) 0.0969(18) Uani 1 1 d . . . F4 F 0.9303(4) 0.5543(5) 0.2505(4) 0.154(3) Uani 1 1 d . . . F5 F 0.4722(2) 0.4574(2) 0.15547(19) 0.0485(9) Uani 1 1 d . . . F6 F 0.3125(2) 0.3954(3) 0.15397(17) 0.0429(8) Uani 1 1 d . . . F7 F 0.4331(2) 0.3242(2) 0.23435(15) 0.0314(6) Uani 1 1 d . . . F8 F 0.3766(2) 0.4968(3) 0.24998(16) 0.0429(8) Uani 1 1 d . . . H3' H 0.733(5) 0.054(5) 0.183(4) 0.07(2) Uiso 1 1 d . . . N1 N 0.7240(3) 0.2907(3) -0.03591(19) 0.0178(8) Uani 1 1 d . . . N2 N 0.6550(3) 0.2828(3) 0.0669(2) 0.0188(8) Uani 1 1 d . . . N3 N 0.7734(3) 0.1064(4) 0.1540(2) 0.0290(10) Uani 1 1 d . . . N4 N 0.8577(2) -0.0994(3) 0.12144(19) 0.0152(8) Uani 1 1 d . . . N5 N 0.7239(2) -0.1929(3) 0.09276(19) 0.0158(8) Uani 1 1 d . . . N6 N 0.6870(3) 0.0007(3) -0.0526(2) 0.0179(8) Uani 1 1 d . . . N7 N 0.0993(3) 0.1421(4) 0.0547(3) 0.0475(13) Uani 1 1 d . . . Pd1 Pd 0.72873(2) 0.06072(3) 0.048199(17) 0.01358(11) 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 B1 0.039(4) 0.026(3) 0.051(4) 0.006(3) 0.009(3) 0.004(3) B2 0.019(3) 0.021(3) 0.024(3) -0.002(2) 0.003(2) 0.004(2) C1 0.015(2) 0.017(2) 0.017(2) 0.0004(18) -0.0038(17) -0.0005(17) C2 0.024(2) 0.013(2) 0.030(3) 0.004(2) 0.000(2) 0.0003(18) C3 0.023(2) 0.012(2) 0.030(3) -0.001(2) 0.002(2) 0.0046(18) C4 0.035(3) 0.025(3) 0.024(3) 0.005(2) 0.010(2) 0.009(2) C5 0.048(3) 0.028(3) 0.022(3) -0.007(2) -0.002(2) 0.012(2) C6 0.027(2) 0.021(3) 0.026(3) -0.007(2) -0.007(2) -0.0029(19) C7 0.013(2) 0.018(3) 0.036(3) 0.002(2) -0.007(2) -0.0038(18) C8 0.017(2) 0.022(3) 0.020(2) 0.0042(19) -0.0025(19) 0.0061(18) C9 0.021(2) 0.015(2) 0.022(2) 0.0036(19) -0.0007(19) 0.0054(18) C10 0.017(2) 0.016(2) 0.012(2) -0.0007(17) 0.0021(18) 0.0010(17) C11 0.020(2) 0.018(2) 0.022(2) 0.0011(19) 0.0055(19) 0.0034(18) C12 0.017(2) 0.022(3) 0.027(3) 0.002(2) 0.0027(19) 0.0010(19) C13 0.029(2) 0.028(3) 0.019(2) 0.000(2) 0.002(2) 0.005(2) C14 0.026(2) 0.024(3) 0.037(3) 0.009(2) 0.010(2) 0.002(2) C15 0.016(2) 0.017(2) 0.020(2) 0.0021(18) -0.0018(18) -0.0029(17) C16 0.025(2) 0.020(3) 0.033(3) 0.005(2) 0.002(2) -0.007(2) C17 0.018(2) 0.024(3) 0.034(3) 0.005(2) -0.002(2) 0.0012(19) C18 0.027(2) 0.029(3) 0.026(3) -0.003(2) -0.001(2) -0.006(2) C19 0.022(2) 0.017(3) 0.027(3) 0.002(2) 0.001(2) -0.0052(18) C20 0.048(3) 0.042(4) 0.023(3) -0.012(2) 0.004(2) -0.014(3) C21 0.025(3) 0.042(4) 0.057(4) -0.010(3) 0.006(3) -0.002(2) C22 0.044(4) 0.041(4) 0.100(6) -0.022(4) 0.004(4) 0.000(3) F1 0.199(6) 0.156(6) 0.114(4) 0.072(4) 0.079(4) 0.132(5) F2 0.090(3) 0.054(3) 0.146(4) 0.044(3) 0.042(3) 0.037(2) F3 0.041(2) 0.056(3) 0.197(5) -0.063(3) 0.032(3) -0.0138(18) F4 0.061(3) 0.140(5) 0.254(8) -0.122(5) -0.027(4) 0.003(3) F5 0.0488(19) 0.0340(19) 0.067(2) 0.0131(16) 0.0324(17) -0.0006(14) F6 0.0369(17) 0.047(2) 0.0418(18) -0.0096(15) -0.0160(14) 0.0072(14) F7 0.0360(15) 0.0262(16) 0.0314(16) 0.0091(13) -0.0009(13) 0.0085(12) F8 0.0466(18) 0.0417(19) 0.0394(18) -0.0170(15) -0.0038(15) 0.0175(15) N1 0.0212(18) 0.0133(19) 0.019(2) 0.0011(15) 0.0020(16) 0.0015(15) N2 0.0202(18) 0.017(2) 0.020(2) -0.0014(16) 0.0028(16) 0.0020(15) N3 0.032(2) 0.032(2) 0.022(2) -0.0093(19) -0.0068(19) 0.0099(19) N4 0.0137(17) 0.0135(19) 0.0183(19) 0.0014(15) 0.0006(15) 0.0004(14) N5 0.0174(18) 0.0149(19) 0.0151(19) 0.0024(15) 0.0000(15) 0.0020(15) N6 0.0221(19) 0.012(2) 0.019(2) -0.0001(16) 0.0014(16) 0.0006(15) N7 0.042(3) 0.041(3) 0.061(3) 0.005(3) 0.015(2) -0.005(2) Pd1 0.01616(17) 0.01067(17) 0.01365(17) -0.00075(14) -0.00079(12) 0.00021(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 B1 F2 1.315(7) . ? B1 F1 1.328(8) . ? B1 F3 1.356(7) . ? B1 F4 1.356(8) . ? B2 F5 1.377(6) . ? B2 F8 1.382(6) . ? B2 F7 1.390(6) . ? B2 F6 1.394(6) . ? C1 N2 1.349(5) . ? C1 N1 1.352(5) . ? C1 Pd1 2.058(4) . ? C2 C3 1.338(6) . ? C2 N1 1.390(6) . ? C2 H2 0.9300 . ? C3 N2 1.374(6) . ? C3 H3 0.9300 . ? C4 N2 1.469(6) . ? C4 C5 1.509(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.477(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N3 1.468(6) . ? C6 C7 1.511(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N4 1.455(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.330(6) . ? C8 N4 1.384(5) . ? C8 H8 0.9300 . ? C9 N5 1.390(5) . ? C9 H9 0.9300 . ? C10 N4 1.350(5) . ? C10 N5 1.353(5) . ? C10 Pd1 2.043(4) . ? C11 N1 1.505(5) . ? C11 C14 1.524(6) . ? C11 C12 1.528(6) . ? C11 C13 1.529(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N5 1.501(5) . ? C15 C16 1.517(6) . ? C15 C17 1.524(6) . ? C15 C18 1.531(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N6 1.130(5) . ? C19 C20 1.458(7) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N7 1.131(7) . ? C21 C22 1.467(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N3 Pd1 2.049(4) . ? N3 H3' 1.01(7) . ? N6 Pd1 2.014(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 F2 B1 F1 108.1(6) . . ? F2 B1 F3 116.8(5) . . ? F1 B1 F3 106.9(6) . . ? F2 B1 F4 113.2(6) . . ? F1 B1 F4 105.0(7) . . ? F3 B1 F4 106.1(5) . . ? F5 B2 F8 110.6(4) . . ? F5 B2 F7 109.3(4) . . ? F8 B2 F7 109.7(4) . . ? F5 B2 F6 109.3(4) . . ? F8 B2 F6 108.9(4) . . ? F7 B2 F6 109.0(4) . . ? N2 C1 N1 105.3(4) . . ? N2 C1 Pd1 116.1(3) . . ? N1 C1 Pd1 138.6(3) . . ? C3 C2 N1 107.3(4) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 106.7(4) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 C5 109.2(4) . . ? N2 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? N3 C5 C4 112.6(4) . . ? N3 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N3 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N3 C6 C7 112.5(4) . . ? N3 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N3 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N4 C7 C6 111.5(4) . . ? N4 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N4 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C9 C8 N4 106.2(4) . . ? C9 C8 H8 126.9 . . ? N4 C8 H8 126.9 . . ? C8 C9 N5 108.2(4) . . ? C8 C9 H9 125.9 . . ? N5 C9 H9 125.9 . . ? N4 C10 N5 105.5(3) . . ? N4 C10 Pd1 113.8(3) . . ? N5 C10 Pd1 140.6(3) . . ? N1 C11 C14 109.1(4) . . ? N1 C11 C12 109.7(3) . . ? C14 C11 C12 106.9(4) . . ? N1 C11 C13 108.4(3) . . ? C14 C11 C13 110.0(4) . . ? C12 C11 C13 112.7(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 C16 108.4(3) . . ? N5 C15 C17 110.3(3) . . ? C16 C15 C17 108.0(4) . . ? N5 C15 C18 107.2(3) . . ? C16 C15 C18 110.9(4) . . ? C17 C15 C18 112.0(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 178.1(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 C22 177.6(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 N1 C2 109.7(4) . . ? C1 N1 C11 128.2(3) . . ? C2 N1 C11 122.1(3) . . ? C1 N2 C3 111.0(4) . . ? C1 N2 C4 122.5(4) . . ? C3 N2 C4 125.4(4) . . ? C6 N3 C5 114.5(4) . . ? C6 N3 Pd1 114.8(3) . . ? C5 N3 Pd1 117.9(3) . . ? C6 N3 H3' 105(4) . . ? C5 N3 H3' 101(4) . . ? Pd1 N3 H3' 100(4) . . ? C10 N4 C8 110.8(3) . . ? C10 N4 C7 121.3(3) . . ? C8 N4 C7 127.9(3) . . ? C10 N5 C9 109.2(3) . . ? C10 N5 C15 128.8(3) . . ? C9 N5 C15 122.0(3) . . ? C19 N6 Pd1 171.1(4) . . ? N6 Pd1 C10 92.33(15) . . ? N6 Pd1 N3 174.44(16) . . ? C10 Pd1 N3 82.12(17) . . ? N6 Pd1 C1 95.61(16) . . ? C10 Pd1 C1 171.66(16) . . ? N3 Pd1 C1 89.95(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -1.3(5) . . . . ? N2 C4 C5 N3 -73.9(5) . . . . ? N3 C6 C7 N4 -48.4(5) . . . . ? N4 C8 C9 N5 -1.4(5) . . . . ? N2 C1 N1 C2 -1.6(5) . . . . ? Pd1 C1 N1 C2 174.9(4) . . . . ? N2 C1 N1 C11 176.8(4) . . . . ? Pd1 C1 N1 C11 -6.7(7) . . . . ? C3 C2 N1 C1 1.8(5) . . . . ? C3 C2 N1 C11 -176.6(4) . . . . ? C14 C11 N1 C1 -143.6(4) . . . . ? C12 C11 N1 C1 -26.8(6) . . . . ? C13 C11 N1 C1 96.7(5) . . . . ? C14 C11 N1 C2 34.6(5) . . . . ? C12 C11 N1 C2 151.4(4) . . . . ? C13 C11 N1 C2 -85.2(5) . . . . ? N1 C1 N2 C3 0.8(5) . . . . ? Pd1 C1 N2 C3 -176.6(3) . . . . ? N1 C1 N2 C4 -168.1(4) . . . . ? Pd1 C1 N2 C4 14.5(5) . . . . ? C2 C3 N2 C1 0.3(5) . . . . ? C2 C3 N2 C4 168.8(4) . . . . ? C5 C4 N2 C1 51.8(6) . . . . ? C5 C4 N2 C3 -115.5(5) . . . . ? C7 C6 N3 C5 -161.4(4) . . . . ? C7 C6 N3 Pd1 -20.5(5) . . . . ? C4 C5 N3 C6 166.0(4) . . . . ? C4 C5 N3 Pd1 26.3(6) . . . . ? N5 C10 N4 C8 2.0(5) . . . . ? Pd1 C10 N4 C8 -175.7(3) . . . . ? N5 C10 N4 C7 -178.0(4) . . . . ? Pd1 C10 N4 C7 4.3(5) . . . . ? C9 C8 N4 C10 -0.3(5) . . . . ? C9 C8 N4 C7 179.6(4) . . . . ? C6 C7 N4 C10 61.0(5) . . . . ? C6 C7 N4 C8 -118.9(5) . . . . ? N4 C10 N5 C9 -2.8(4) . . . . ? Pd1 C10 N5 C9 173.9(4) . . . . ? N4 C10 N5 C15 176.8(4) . . . . ? Pd1 C10 N5 C15 -6.5(7) . . . . ? C8 C9 N5 C10 2.7(5) . . . . ? C8 C9 N5 C15 -177.0(4) . . . . ? C16 C15 N5 C10 -138.0(4) . . . . ? C17 C15 N5 C10 -19.9(6) . . . . ? C18 C15 N5 C10 102.2(5) . . . . ? C16 C15 N5 C9 41.6(5) . . . . ? C17 C15 N5 C9 159.7(4) . . . . ? C18 C15 N5 C9 -78.2(5) . . . . ? N4 C10 Pd1 N6 126.1(3) . . . . ? N5 C10 Pd1 N6 -50.4(5) . . . . ? N4 C10 Pd1 N3 -54.2(3) . . . . ? N5 C10 Pd1 N3 129.3(5) . . . . ? C6 N3 Pd1 C10 62.8(3) . . . . ? C5 N3 Pd1 C10 -157.7(4) . . . . ? C6 N3 Pd1 C1 -114.7(4) . . . . ? C5 N3 Pd1 C1 24.8(4) . . . . ? N2 C1 Pd1 N6 133.2(3) . . . . ? N1 C1 Pd1 N6 -43.0(5) . . . . ? N2 C1 Pd1 N3 -46.7(3) . . . . ? N1 C1 Pd1 N3 137.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.047 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.101 #==END==#