Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' #============================================================================== # (Publishing Staff Use Only) _journal_coden_Cambridge 0222 _audit_creation_method SHELXL-97 _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _publ_section_title 'Chiral NHC ligands based on a biisoquinoline template' _publ_contact_author_name 'K.J. Cavell' _publ_contact_author_address ; School of Chemistry Cardiff University Park Place Cardiff, CF10 3AT Wales UK ; _publ_contact_author_email cavellkj@cf.ac.uk _publ_contact_author_fax (+44)_29_20875899 _publ_contact_author_phone (+44)_29_20875899 loop_ _publ_author_name 'Kingsley Cavell' 'Mark Elliott' 'David J. Nielsen' 'James S.Paine' #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_611607 _database_code_depnum_ccdc_archive 'CCDC 611607' _chemical_name_systematic ; Compound 2 ; _chemical_name_common 'Compound 2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 B F4 N2' _chemical_formula_weight 362.17 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' _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 7.5518(15) _cell_length_b 8.1740(16) _cell_length_c 14.052(3) _cell_angle_alpha 100.08(3) _cell_angle_beta 101.81(3) _cell_angle_gamma 96.24(3) _cell_volume 826.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6741 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3588 _reflns_number_gt 2648 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+1.1234P] 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 3588 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1979 _refine_ls_wR_factor_gt 0.1828 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F -0.4757(3) 0.2830(2) 0.21791(14) 0.0441(5) Uani 1 1 d . . . N1 N -0.1699(3) -0.0378(3) 0.20234(16) 0.0233(5) Uani 1 1 d . . . C1 C -0.1114(4) 0.1168(3) 0.2501(2) 0.0245(6) Uani 1 1 d . . . H1 H -0.1867 0.2027 0.2505 0.029 Uiso 1 1 calc R . . B1 B -0.4168(5) 0.4547(4) 0.2451(3) 0.0309(7) Uani 1 1 d . . . F2 F -0.2305(3) 0.4835(2) 0.28874(15) 0.0447(5) Uani 1 1 d . . . N2 N 0.0607(3) 0.1424(3) 0.29753(17) 0.0244(5) Uani 1 1 d . . . C2 C -0.0202(3) -0.1406(3) 0.21148(19) 0.0213(5) Uani 1 1 d . . . H2 H -0.0551 -0.2384 0.2412 0.026 Uiso 1 1 calc R . . F3 F -0.5110(3) 0.5250(3) 0.3103(2) 0.0863(10) Uani 1 1 d . . . C3 C 0.1385(3) -0.0160(3) 0.28754(19) 0.0214(5) Uani 1 1 d . . . H3 H 0.2464 -0.0023 0.2571 0.026 Uiso 1 1 calc R . . F4 F -0.4447(4) 0.5179(4) 0.1590(2) 0.0813(9) Uani 1 1 d . . . C4 C -0.3349(4) -0.1000(4) 0.1235(2) 0.0282(6) Uani 1 1 d . . . H4A H -0.4239 -0.0200 0.1270 0.034 Uiso 1 1 calc R . . H4B H -0.3926 -0.2098 0.1316 0.034 Uiso 1 1 calc R . . C5 C -0.2820(4) -0.1191(4) 0.0235(2) 0.0272(6) Uani 1 1 d . . . H5A H -0.3843 -0.1888 -0.0283 0.033 Uiso 1 1 calc R . . H5B H -0.2625 -0.0069 0.0066 0.033 Uiso 1 1 calc R . . C6 C -0.1104(4) -0.1992(3) 0.0230(2) 0.0229(6) Uani 1 1 d . . . C7 C -0.0746(4) -0.2697(3) -0.0680(2) 0.0267(6) Uani 1 1 d . . . H7 H -0.1592 -0.2674 -0.1277 0.032 Uiso 1 1 calc R . . C8 C 0.0811(4) -0.3426(3) -0.0730(2) 0.0286(6) Uani 1 1 d . . . H8 H 0.1018 -0.3907 -0.1356 0.034 Uiso 1 1 calc R . . C9 C 0.2071(4) -0.3454(3) 0.0137(2) 0.0271(6) Uani 1 1 d . . . H9 H 0.3148 -0.3943 0.0108 0.033 Uiso 1 1 calc R . . C10 C 0.1739(4) -0.2759(3) 0.1051(2) 0.0257(6) Uani 1 1 d . . . H10 H 0.2598 -0.2776 0.1645 0.031 Uiso 1 1 calc R . . C11 C 0.0169(3) -0.2040(3) 0.1103(2) 0.0217(6) Uani 1 1 d . . . C12 C 0.1563(4) 0.2856(3) 0.3759(2) 0.0282(6) Uani 1 1 d . . . H12A H 0.0873 0.3817 0.3738 0.034 Uiso 1 1 calc R . . H12B H 0.2795 0.3206 0.3655 0.034 Uiso 1 1 calc R . . C13 C 0.1731(4) 0.2349(3) 0.4761(2) 0.0272(6) Uani 1 1 d . . . H13A H 0.2669 0.3175 0.5264 0.033 Uiso 1 1 calc R . . H13B H 0.0550 0.2387 0.4960 0.033 Uiso 1 1 calc R . . C14 C 0.2247(3) 0.0610(3) 0.4756(2) 0.0242(6) Uani 1 1 d . . . C15 C 0.2978(4) 0.0177(4) 0.5661(2) 0.0273(6) Uani 1 1 d . . . H15 H 0.3161 0.0987 0.6259 0.033 Uiso 1 1 calc R . . C16 C 0.3439(4) -0.1401(4) 0.5703(2) 0.0300(6) Uani 1 1 d . . . H16 H 0.3942 -0.1666 0.6325 0.036 Uiso 1 1 calc R . . C17 C 0.3165(4) -0.2604(4) 0.4832(2) 0.0285(6) Uani 1 1 d . . . H17 H 0.3468 -0.3696 0.4857 0.034 Uiso 1 1 calc R . . C18 C 0.2452(4) -0.2201(3) 0.3933(2) 0.0262(6) Uani 1 1 d . . . H18 H 0.2267 -0.3022 0.3339 0.031 Uiso 1 1 calc R . . C19 C 0.1997(3) -0.0600(3) 0.3884(2) 0.0224(6) 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 F1 0.0509(12) 0.0316(10) 0.0407(11) 0.0032(8) -0.0077(9) 0.0086(8) N1 0.0232(11) 0.0261(12) 0.0199(11) 0.0035(9) 0.0030(9) 0.0053(9) C1 0.0301(14) 0.0275(14) 0.0201(13) 0.0090(11) 0.0087(11) 0.0100(11) B1 0.0318(17) 0.0259(16) 0.0374(19) 0.0049(14) 0.0119(14) 0.0094(14) F2 0.0367(10) 0.0438(11) 0.0485(12) -0.0036(9) 0.0080(9) 0.0084(9) N2 0.0296(12) 0.0190(11) 0.0243(12) 0.0039(9) 0.0053(10) 0.0043(9) C2 0.0212(12) 0.0225(13) 0.0193(13) 0.0037(10) 0.0029(10) 0.0039(10) F3 0.0566(14) 0.0785(18) 0.111(2) -0.0430(16) 0.0489(15) -0.0015(13) C3 0.0206(12) 0.0218(13) 0.0207(13) 0.0029(10) 0.0030(10) 0.0034(10) F4 0.0790(17) 0.0856(19) 0.093(2) 0.0669(17) 0.0072(15) 0.0145(15) C4 0.0210(13) 0.0295(14) 0.0302(15) 0.0026(12) 0.0014(11) 0.0012(11) C5 0.0265(14) 0.0271(14) 0.0241(14) 0.0038(11) -0.0007(11) 0.0021(11) C6 0.0266(13) 0.0182(12) 0.0218(13) 0.0034(10) 0.0035(11) -0.0001(10) C7 0.0342(15) 0.0243(14) 0.0188(13) 0.0031(11) 0.0036(11) -0.0014(12) C8 0.0382(16) 0.0226(13) 0.0241(14) 0.0000(11) 0.0120(12) -0.0016(12) C9 0.0307(14) 0.0195(13) 0.0314(15) 0.0025(11) 0.0106(12) 0.0027(11) C10 0.0288(14) 0.0217(13) 0.0255(14) 0.0039(11) 0.0050(11) 0.0030(11) C11 0.0230(13) 0.0158(12) 0.0234(13) 0.0009(10) 0.0040(10) -0.0015(10) C12 0.0353(15) 0.0200(13) 0.0258(15) 0.0004(11) 0.0050(12) 0.0000(11) C13 0.0283(14) 0.0262(14) 0.0245(14) -0.0013(11) 0.0063(11) 0.0023(11) C14 0.0195(12) 0.0271(14) 0.0244(14) 0.0031(11) 0.0054(10) -0.0013(11) C15 0.0236(13) 0.0363(16) 0.0185(13) 0.0011(12) 0.0040(11) -0.0013(12) C16 0.0246(14) 0.0409(17) 0.0251(15) 0.0117(13) 0.0031(11) 0.0042(12) C17 0.0235(13) 0.0295(15) 0.0334(16) 0.0107(12) 0.0037(12) 0.0061(11) C18 0.0248(13) 0.0250(14) 0.0266(14) 0.0028(11) 0.0033(11) 0.0040(11) C19 0.0178(12) 0.0251(13) 0.0231(13) 0.0031(11) 0.0037(10) 0.0029(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 B1 1.386(4) . ? N1 C1 1.305(4) . ? N1 C4 1.462(3) . ? N1 C2 1.478(3) . ? C1 N2 1.310(4) . ? B1 F3 1.359(4) . ? B1 F4 1.383(4) . ? B1 F2 1.391(4) . ? N2 C12 1.464(4) . ? N2 C3 1.475(3) . ? C2 C11 1.518(4) . ? C2 C3 1.564(4) . ? C3 C19 1.516(4) . ? C4 C5 1.525(4) . ? C5 C6 1.515(4) . ? C6 C7 1.398(4) . ? C6 C11 1.405(4) . ? C7 C8 1.383(4) . ? C8 C9 1.389(4) . ? C9 C10 1.393(4) . ? C10 C11 1.388(4) . ? C12 C13 1.522(4) . ? C13 C14 1.513(4) . ? C14 C19 1.398(4) . ? C14 C15 1.399(4) . ? C15 C16 1.380(4) . ? C16 C17 1.392(4) . ? C17 C18 1.379(4) . ? C18 C19 1.398(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 C1 N1 C4 127.6(2) . . ? C1 N1 C2 110.9(2) . . ? C4 N1 C2 118.7(2) . . ? N1 C1 N2 113.7(2) . . ? F3 B1 F4 112.1(3) . . ? F3 B1 F1 109.6(3) . . ? F4 B1 F1 107.2(3) . . ? F3 B1 F2 110.0(3) . . ? F4 B1 F2 108.8(3) . . ? F1 B1 F2 109.1(3) . . ? C1 N2 C12 127.5(2) . . ? C1 N2 C3 110.7(2) . . ? C12 N2 C3 119.2(2) . . ? N1 C2 C11 110.4(2) . . ? N1 C2 C3 101.9(2) . . ? C11 C2 C3 115.9(2) . . ? N2 C3 C19 110.4(2) . . ? N2 C3 C2 102.20(19) . . ? C19 C3 C2 116.7(2) . . ? N1 C4 C5 108.7(2) . . ? C6 C5 C4 112.7(2) . . ? C7 C6 C11 118.1(2) . . ? C7 C6 C5 119.1(2) . . ? C11 C6 C5 122.8(2) . . ? C8 C7 C6 121.6(3) . . ? C7 C8 C9 119.9(3) . . ? C8 C9 C10 119.4(3) . . ? C11 C10 C9 120.8(3) . . ? C10 C11 C6 120.2(2) . . ? C10 C11 C2 119.0(2) . . ? C6 C11 C2 120.7(2) . . ? N2 C12 C13 109.1(2) . . ? C14 C13 C12 113.1(2) . . ? C19 C14 C15 118.3(3) . . ? C19 C14 C13 122.8(2) . . ? C15 C14 C13 118.9(2) . . ? C16 C15 C14 121.5(3) . . ? C15 C16 C17 119.8(3) . . ? C18 C17 C16 119.6(3) . . ? C17 C18 C19 120.8(3) . . ? C18 C19 C14 120.0(3) . . ? C18 C19 C3 119.0(2) . . ? C14 C19 C3 120.8(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.657 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.075 #==>END data_611608 _database_code_depnum_ccdc_archive 'CCDC 611608' _chemical_name_systematic ; Compound 4 ; _chemical_name_common 'Compound 4' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H27 B F4 N2' _chemical_formula_weight 418.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 8.0210(16) _cell_length_b 10.697(2) _cell_length_c 12.929(3) _cell_angle_alpha 71.95(3) _cell_angle_beta 86.98(3) _cell_angle_gamma 74.82(3) _cell_volume 1017.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7948 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.99 _reflns_number_total 4381 _reflns_number_gt 3049 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.4072P] 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 4381 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.04940(19) 0.25921(14) 0.54083(10) 0.0460(4) Uani 1 1 d . . . N1 N 0.3752(2) 0.34190(15) 0.28731(13) 0.0224(4) Uani 1 1 d . . . C1 C 0.3055(2) 0.24451(19) 0.34483(16) 0.0225(4) Uani 1 1 d . . . H1 H 0.2421 0.2485 0.4084 0.027 Uiso 1 1 calc R . . B1 B 0.1299(3) 0.2284(3) 0.6418(2) 0.0306(6) Uani 1 1 d . . . F2 F 0.1774(3) 0.33809(18) 0.65131(12) 0.0810(6) Uani 1 1 d . . . N2 N 0.3314(2) 0.14190(15) 0.30632(12) 0.0216(4) Uani 1 1 d . . . C2 C 0.4537(2) 0.31064(19) 0.18948(15) 0.0205(4) Uani 1 1 d . . . H2 H 0.3779 0.3710 0.1248 0.025 Uiso 1 1 calc R . . F3 F 0.01941(18) 0.19226(16) 0.72246(11) 0.0534(4) Uani 1 1 d . . . C3 C 0.4426(2) 0.16256(19) 0.20940(15) 0.0212(4) Uani 1 1 d . . . H3 H 0.5602 0.0988 0.2290 0.025 Uiso 1 1 calc R . . F4 F 0.2715(2) 0.1220(2) 0.65030(18) 0.0933(7) Uani 1 1 d . . . C4 C 0.3881(3) 0.46740(19) 0.30900(16) 0.0245(4) Uani 1 1 d . . . C5 C 0.5813(3) 0.4533(2) 0.31973(16) 0.0264(4) Uani 1 1 d . . . H5A H 0.5980 0.5417 0.3201 0.032 Uiso 1 1 calc R . . H5B H 0.6259 0.3855 0.3906 0.032 Uiso 1 1 calc R . . C6 C 0.6867(3) 0.41035(19) 0.22998(16) 0.0238(4) Uani 1 1 d . . . C7 C 0.8462(3) 0.4412(2) 0.20555(17) 0.0276(5) Uani 1 1 d . . . H7 H 0.8855 0.4914 0.2438 0.033 Uiso 1 1 calc R . . C8 C 0.9473(3) 0.3994(2) 0.12633(17) 0.0299(5) Uani 1 1 d . . . H8 H 1.0545 0.4223 0.1099 0.036 Uiso 1 1 calc R . . C9 C 0.8931(3) 0.3242(2) 0.07076(17) 0.0289(5) Uani 1 1 d . . . H9 H 0.9634 0.2945 0.0171 0.035 Uiso 1 1 calc R . . C10 C 0.7361(3) 0.29297(19) 0.09413(16) 0.0251(4) Uani 1 1 d . . . H10 H 0.6990 0.2412 0.0564 0.030 Uiso 1 1 calc R . . C11 C 0.6315(2) 0.33642(18) 0.17251(15) 0.0216(4) Uani 1 1 d . . . C12 C 0.2975(3) 0.4790(2) 0.41311(18) 0.0339(5) Uani 1 1 d . . . H12A H 0.1748 0.4840 0.4053 0.051 Uiso 1 1 calc R . . H12B H 0.3088 0.5614 0.4271 0.051 Uiso 1 1 calc R . . H12C H 0.3504 0.3990 0.4741 0.051 Uiso 1 1 calc R . . C13 C 0.3055(3) 0.5893(2) 0.21181(17) 0.0332(5) Uani 1 1 d . . . H13A H 0.3661 0.5802 0.1456 0.050 Uiso 1 1 calc R . . H13B H 0.3139 0.6734 0.2241 0.050 Uiso 1 1 calc R . . H13C H 0.1837 0.5924 0.2034 0.050 Uiso 1 1 calc R . . C14 C 0.2539(2) 0.02282(19) 0.34648(15) 0.0229(4) Uani 1 1 d . . . C15 C 0.3119(3) -0.06278(19) 0.26827(16) 0.0238(4) Uani 1 1 d . . . H15A H 0.4342 -0.1143 0.2857 0.029 Uiso 1 1 calc R . . H15B H 0.2421 -0.1297 0.2806 0.029 Uiso 1 1 calc R . . C16 C 0.2945(2) 0.02041(19) 0.15017(16) 0.0223(4) Uani 1 1 d . . . C17 C 0.2197(3) -0.0129(2) 0.07080(17) 0.0268(5) Uani 1 1 d . . . H17 H 0.1706 -0.0885 0.0914 0.032 Uiso 1 1 calc R . . C18 C 0.2163(3) 0.0632(2) -0.03802(17) 0.0294(5) Uani 1 1 d . . . H18 H 0.1670 0.0384 -0.0915 0.035 Uiso 1 1 calc R . . C19 C 0.2845(3) 0.1753(2) -0.06884(17) 0.0293(5) Uani 1 1 d . . . H19 H 0.2827 0.2270 -0.1434 0.035 Uiso 1 1 calc R . . C20 C 0.3558(2) 0.2118(2) 0.00999(16) 0.0258(4) Uani 1 1 d . . . H20 H 0.4004 0.2898 -0.0107 0.031 Uiso 1 1 calc R . . C21 C 0.3616(2) 0.13466(19) 0.11846(15) 0.0210(4) Uani 1 1 d . . . C22 C 0.3233(3) -0.0619(2) 0.46133(16) 0.0300(5) Uani 1 1 d . . . H22A H 0.4497 -0.0916 0.4613 0.045 Uiso 1 1 calc R . . H22B H 0.2764 -0.1418 0.4858 0.045 Uiso 1 1 calc R . . H22C H 0.2883 -0.0068 0.5107 0.045 Uiso 1 1 calc R . . C23 C 0.0577(2) 0.0752(2) 0.34424(17) 0.0269(5) Uani 1 1 d . . . H23A H 0.0252 0.1349 0.3902 0.040 Uiso 1 1 calc R . . H23B H 0.0062 -0.0020 0.3718 0.040 Uiso 1 1 calc R . . H23C H 0.0157 0.1263 0.2693 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0642(10) 0.0518(8) 0.0289(7) -0.0158(6) 0.0017(6) -0.0228(7) N1 0.0253(9) 0.0218(8) 0.0248(9) -0.0124(7) 0.0072(7) -0.0087(7) C1 0.0219(10) 0.0254(10) 0.0227(10) -0.0097(8) 0.0028(8) -0.0078(8) B1 0.0333(13) 0.0357(14) 0.0310(14) -0.0179(11) 0.0073(11) -0.0148(11) F2 0.1571(19) 0.0841(12) 0.0395(9) -0.0228(8) 0.0126(10) -0.0926(13) N2 0.0249(9) 0.0223(8) 0.0211(8) -0.0085(7) 0.0046(7) -0.0107(7) C2 0.0210(10) 0.0235(10) 0.0193(10) -0.0094(8) 0.0038(8) -0.0070(8) F3 0.0489(9) 0.0870(11) 0.0333(8) -0.0176(7) 0.0123(7) -0.0361(8) C3 0.0194(10) 0.0229(10) 0.0230(10) -0.0092(8) 0.0053(8) -0.0067(8) F4 0.0395(10) 0.1266(17) 0.1260(17) -0.0909(15) -0.0220(10) 0.0253(10) C4 0.0315(11) 0.0211(10) 0.0265(11) -0.0120(8) 0.0062(9) -0.0118(8) C5 0.0338(11) 0.0257(10) 0.0249(11) -0.0112(9) 0.0027(9) -0.0127(9) C6 0.0268(11) 0.0204(10) 0.0249(11) -0.0057(8) 0.0000(8) -0.0085(8) C7 0.0283(11) 0.0244(10) 0.0321(12) -0.0061(9) -0.0031(9) -0.0127(9) C8 0.0211(10) 0.0297(11) 0.0374(12) -0.0048(9) 0.0021(9) -0.0106(9) C9 0.0257(11) 0.0322(11) 0.0272(11) -0.0079(9) 0.0056(9) -0.0070(9) C10 0.0256(11) 0.0265(10) 0.0247(11) -0.0085(9) 0.0021(8) -0.0088(9) C11 0.0216(10) 0.0207(9) 0.0214(10) -0.0039(8) 0.0021(8) -0.0071(8) C12 0.0410(13) 0.0334(12) 0.0363(13) -0.0205(10) 0.0111(10) -0.0149(10) C13 0.0385(13) 0.0232(10) 0.0368(13) -0.0113(9) 0.0021(10) -0.0039(9) C14 0.0264(10) 0.0204(9) 0.0240(10) -0.0066(8) 0.0038(8) -0.0104(8) C15 0.0245(10) 0.0190(9) 0.0290(11) -0.0090(8) -0.0004(8) -0.0056(8) C16 0.0186(9) 0.0214(10) 0.0286(11) -0.0121(8) 0.0029(8) -0.0031(8) C17 0.0251(11) 0.0263(10) 0.0345(12) -0.0167(9) 0.0034(9) -0.0078(9) C18 0.0290(11) 0.0360(12) 0.0288(11) -0.0178(9) -0.0009(9) -0.0079(9) C19 0.0282(11) 0.0360(12) 0.0254(11) -0.0133(9) 0.0046(9) -0.0077(9) C20 0.0243(10) 0.0297(11) 0.0287(11) -0.0139(9) 0.0056(8) -0.0107(9) C21 0.0168(9) 0.0245(10) 0.0245(10) -0.0129(8) 0.0043(8) -0.0043(8) C22 0.0360(12) 0.0265(11) 0.0281(11) -0.0057(9) -0.0007(9) -0.0118(9) C23 0.0273(11) 0.0251(10) 0.0302(11) -0.0092(9) 0.0043(9) -0.0099(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F1 B1 1.393(3) . ? N1 C1 1.316(2) . ? N1 C2 1.475(2) . ? N1 C4 1.483(2) . ? C1 N2 1.305(2) . ? B1 F3 1.362(3) . ? B1 F4 1.362(3) . ? B1 F2 1.366(3) . ? N2 C3 1.493(2) . ? N2 C14 1.500(2) . ? C2 C11 1.514(2) . ? C2 C3 1.550(2) . ? C3 C21 1.514(3) . ? C4 C12 1.519(3) . ? C4 C5 1.527(3) . ? C4 C13 1.529(3) . ? C5 C6 1.515(3) . ? C6 C11 1.399(3) . ? C6 C7 1.400(3) . ? C7 C8 1.383(3) . ? C8 C9 1.388(3) . ? C9 C10 1.380(3) . ? C10 C11 1.395(3) . ? C14 C23 1.524(3) . ? C14 C22 1.525(3) . ? C14 C15 1.542(3) . ? C15 C16 1.503(3) . ? C16 C17 1.394(3) . ? C16 C21 1.401(3) . ? C17 C18 1.388(3) . ? C18 C19 1.385(3) . ? C19 C20 1.394(3) . ? C20 C21 1.386(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 110.31(14) . . ? C1 N1 C4 130.10(16) . . ? C2 N1 C4 119.57(14) . . ? N2 C1 N1 113.72(16) . . ? F3 B1 F4 109.8(2) . . ? F3 B1 F2 108.64(18) . . ? F4 B1 F2 110.3(2) . . ? F3 B1 F1 109.70(19) . . ? F4 B1 F1 107.54(18) . . ? F2 B1 F1 110.9(2) . . ? C1 N2 C3 110.35(14) . . ? C1 N2 C14 126.38(15) . . ? C3 N2 C14 123.16(14) . . ? N1 C2 C11 111.40(15) . . ? N1 C2 C3 102.73(14) . . ? C11 C2 C3 117.06(15) . . ? N2 C3 C21 109.21(14) . . ? N2 C3 C2 101.88(13) . . ? C21 C3 C2 116.68(16) . . ? N1 C4 C12 110.36(15) . . ? N1 C4 C5 105.50(15) . . ? C12 C4 C5 111.02(17) . . ? N1 C4 C13 108.15(16) . . ? C12 C4 C13 110.72(17) . . ? C5 C4 C13 110.93(16) . . ? C6 C5 C4 114.08(16) . . ? C11 C6 C7 118.61(18) . . ? C11 C6 C5 121.70(17) . . ? C7 C6 C5 119.66(17) . . ? C8 C7 C6 120.80(18) . . ? C7 C8 C9 120.32(18) . . ? C10 C9 C8 119.48(18) . . ? C9 C10 C11 120.80(18) . . ? C10 C11 C6 119.97(17) . . ? C10 C11 C2 119.42(16) . . ? C6 C11 C2 120.49(16) . . ? N2 C14 C23 108.97(15) . . ? N2 C14 C22 109.84(15) . . ? C23 C14 C22 110.90(16) . . ? N2 C14 C15 106.15(14) . . ? C23 C14 C15 111.31(16) . . ? C22 C14 C15 109.55(16) . . ? C16 C15 C14 113.67(15) . . ? C17 C16 C21 118.77(18) . . ? C17 C16 C15 123.23(17) . . ? C21 C16 C15 117.97(17) . . ? C18 C17 C16 120.66(18) . . ? C19 C18 C17 120.20(19) . . ? C18 C19 C20 119.75(19) . . ? C21 C20 C19 120.09(18) . . ? C20 C21 C16 120.50(17) . . ? C20 C21 C3 124.10(16) . . ? C16 C21 C3 115.38(17) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.377 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.055 #==>END data_611609 _database_code_depnum_ccdc_archive 'CCDC 611609' _chemical_name_systematic ; Complex 5 ; _chemical_name_common 'Complex 5' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H49 I2 N4 O1.50 Pd' _chemical_formula_weight 1018.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4100(3) _cell_length_b 12.7960(3) _cell_length_c 15.1290(4) _cell_angle_alpha 100.433(1) _cell_angle_beta 99.417(1) _cell_angle_gamma 111.286(1) _cell_volume 2131.48(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25404 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 1.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6998 _exptl_absorpt_correction_T_max 0.7614 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32768 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8678 _reflns_number_gt 5722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'Dirdif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0605P)^2^+6.3363P] 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 8678 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1470 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0734(6) -0.1430(5) 0.1341(5) 0.0255(15) Uani 1 1 d . . . C2 C -0.0668(7) -0.0226(6) 0.2845(5) 0.0400(19) Uani 1 1 d . . . H2A H -0.0246 -0.0653 0.3132 0.048 Uiso 1 1 calc R . . H2B H -0.1332 -0.0256 0.3138 0.048 Uiso 1 1 calc R . . C3 C 0.0178(7) 0.1012(6) 0.3004(5) 0.046(2) Uani 1 1 d . . . H3A H 0.0938 0.1030 0.2868 0.056 Uiso 1 1 calc R . . H3B H 0.0356 0.1419 0.3667 0.056 Uiso 1 1 calc R . . C4 C -0.0304(6) 0.1652(6) 0.2415(5) 0.0333(17) Uani 1 1 d . . . C5 C 0.0177(6) 0.2872(6) 0.2676(5) 0.0386(18) Uani 1 1 d . . . H5 H 0.0813 0.3283 0.3218 0.046 Uiso 1 1 calc R . . C6 C -0.0253(6) 0.3482(6) 0.2163(5) 0.0363(18) Uani 1 1 d . . . H6 H 0.0061 0.4306 0.2365 0.044 Uiso 1 1 calc R . . C7 C -0.1142(7) 0.2898(6) 0.1355(5) 0.0345(17) Uani 1 1 d . . . H7 H -0.1421 0.3319 0.0986 0.041 Uiso 1 1 calc R . . C8 C -0.1633(6) 0.1682(6) 0.1079(5) 0.0287(15) Uani 1 1 d . . . H8 H -0.2255 0.1277 0.0527 0.034 Uiso 1 1 calc R . . C9 C -0.1210(6) 0.1060(5) 0.1615(5) 0.0252(15) Uani 1 1 d . . . C10 C -0.1824(6) -0.0269(5) 0.1333(5) 0.0265(15) Uani 1 1 d . . . H10 H -0.2639 -0.0517 0.1450 0.032 Uiso 1 1 calc R . . C11 C -0.1926(5) -0.0866(5) 0.0326(4) 0.0232(14) Uani 1 1 d . . . H11 H -0.1565 -0.0259 0.0003 0.028 Uiso 1 1 calc R . . C12 C -0.3193(6) -0.1678(5) -0.0255(5) 0.0267(15) Uani 1 1 d . . . C13 C -0.4090(6) -0.1283(6) -0.0336(5) 0.0356(17) Uani 1 1 d . . . H13 H -0.3919 -0.0507 -0.0018 0.043 Uiso 1 1 calc R . . C14 C -0.5230(7) -0.1987(7) -0.0868(5) 0.0414(19) Uani 1 1 d . . . H14 H -0.5840 -0.1703 -0.0900 0.050 Uiso 1 1 calc R . . C15 C -0.5479(7) -0.3091(7) -0.1348(6) 0.046(2) Uani 1 1 d . . . H15 H -0.6257 -0.3572 -0.1730 0.056 Uiso 1 1 calc R . . C16 C -0.4598(7) -0.3501(6) -0.1277(5) 0.043(2) Uani 1 1 d . . . H16 H -0.4786 -0.4279 -0.1600 0.052 Uiso 1 1 calc R . . C17 C -0.3432(6) -0.2811(6) -0.0743(5) 0.0326(16) Uani 1 1 d . . . C18 C -0.2488(7) -0.3296(6) -0.0684(5) 0.0417(19) Uani 1 1 d . . . H18A H -0.2583 -0.3782 -0.1304 0.050 Uiso 1 1 calc R . . H18B H -0.2611 -0.3803 -0.0254 0.050 Uiso 1 1 calc R . . C19 C -0.1227(6) -0.2363(6) -0.0350(5) 0.0336(17) Uani 1 1 d . . . H19A H -0.0656 -0.2714 -0.0185 0.040 Uiso 1 1 calc R . . H19B H -0.1015 -0.1985 -0.0850 0.040 Uiso 1 1 calc R . . C20 C 0.1463(6) -0.2806(5) 0.2459(5) 0.0242(14) Uani 1 1 d . . . C21 C 0.1533(6) -0.4108(6) 0.1059(5) 0.0308(16) Uani 1 1 d . . . H21A H 0.0886 -0.3944 0.0719 0.037 Uiso 1 1 calc R . . H21B H 0.1294 -0.4960 0.0894 0.037 Uiso 1 1 calc R . . C22 C 0.2674(6) -0.3521(6) 0.0789(5) 0.0336(17) Uani 1 1 d . . . H22A H 0.2777 -0.2719 0.0778 0.040 Uiso 1 1 calc R . . H22B H 0.2615 -0.3944 0.0154 0.040 Uiso 1 1 calc R . . C23 C 0.3762(6) -0.3476(5) 0.1452(5) 0.0266(15) Uani 1 1 d . . . C24 C 0.4825(7) -0.3245(6) 0.1167(5) 0.0374(18) Uani 1 1 d . . . H24 H 0.4847 -0.3121 0.0569 0.045 Uiso 1 1 calc R . . C25 C 0.5838(7) -0.3194(6) 0.1736(6) 0.0397(18) Uani 1 1 d . . . H25 H 0.6544 -0.3050 0.1523 0.048 Uiso 1 1 calc R . . C26 C 0.5832(6) -0.3350(6) 0.2613(5) 0.0371(18) Uani 1 1 d . . . H26 H 0.6531 -0.3313 0.3008 0.044 Uiso 1 1 calc R . . C27 C 0.4788(6) -0.3564(6) 0.2911(5) 0.0304(16) Uani 1 1 d . . . H27 H 0.4781 -0.3670 0.3516 0.036 Uiso 1 1 calc R . . C28 C 0.3742(6) -0.3626(5) 0.2334(5) 0.0243(14) Uani 1 1 d . . . C29 C 0.2625(5) -0.3885(5) 0.2680(4) 0.0219(14) Uani 1 1 d . . . H29 H 0.2297 -0.4713 0.2707 0.026 Uiso 1 1 calc R . . C30 C 0.2750(6) -0.3087(5) 0.3625(4) 0.0256(15) Uani 1 1 d . . . H30 H 0.3608 -0.2541 0.3886 0.031 Uiso 1 1 calc R . . C31 C 0.2310(6) -0.3672(6) 0.4356(5) 0.0327(16) Uani 1 1 d . . . C32 C 0.2680(7) -0.4523(6) 0.4587(5) 0.0401(19) Uani 1 1 d . . . H32 H 0.3158 -0.4776 0.4245 0.048 Uiso 1 1 calc R . . C33 C 0.2362(8) -0.4999(7) 0.5304(6) 0.052(2) Uani 1 1 d . . . H33 H 0.2616 -0.5577 0.5450 0.063 Uiso 1 1 calc R . . C34 C 0.1673(9) -0.4632(9) 0.5807(7) 0.066(3) Uani 1 1 d . . . H34 H 0.1463 -0.4948 0.6307 0.079 Uiso 1 1 calc R . . C35 C 0.1294(9) -0.3809(9) 0.5582(6) 0.065(3) Uani 1 1 d . . . H35 H 0.0809 -0.3574 0.5928 0.078 Uiso 1 1 calc R . . C36 C 0.1595(7) -0.3304(7) 0.4863(5) 0.0423(19) Uani 1 1 d . . . C37 C 0.1117(8) -0.2428(7) 0.4615(6) 0.049(2) Uani 1 1 d . . . H37A H 0.0283 -0.2848 0.4234 0.059 Uiso 1 1 calc R . . H37B H 0.1111 -0.1923 0.5191 0.059 Uiso 1 1 calc R . . C38 C 0.1857(7) -0.1686(6) 0.4086(5) 0.0365(17) Uani 1 1 d . . . H38A H 0.1431 -0.1249 0.3820 0.044 Uiso 1 1 calc R . . H38B H 0.2628 -0.1119 0.4511 0.044 Uiso 1 1 calc R . . N1 N -0.1137(5) -0.0768(4) 0.1861(4) 0.0275(13) Uani 1 1 d . . . N2 N -0.1158(5) -0.1501(4) 0.0462(4) 0.0272(13) Uani 1 1 d . . . N3 N 0.1716(4) -0.3678(4) 0.2057(4) 0.0252(12) Uani 1 1 d . . . N4 N 0.2068(5) -0.2424(4) 0.3349(4) 0.0265(12) Uani 1 1 d . . . Pd1 Pd 0.03564(4) -0.21591(4) 0.18664(3) 0.02231(14) Uani 1 1 d . . . I1 I -0.14445(4) -0.39787(4) 0.19018(4) 0.03491(15) Uani 1 1 d . . . I2 I 0.22025(4) -0.04190(4) 0.17811(3) 0.03281(15) Uani 1 1 d . . . O1 O -0.3508(7) 0.0833(7) 0.2812(6) 0.096(2) Uiso 1 1 d . . . C41 C -0.4843(8) -0.0168(7) 0.3888(6) 0.046(2) Uiso 1 1 d . . . H41A H -0.5716 -0.0630 0.3726 0.055 Uiso 1 1 calc R . . H41B H -0.4453 -0.0373 0.4415 0.055 Uiso 1 1 calc R . . C39 C -0.4267(12) 0.1505(11) 0.3334(9) 0.103(4) Uiso 1 1 d . . . H39A H -0.3762 0.2342 0.3610 0.123 Uiso 1 1 calc R . . H39B H -0.4991 0.1419 0.2887 0.123 Uiso 1 1 calc R . . C40 C -0.4582(12) 0.0912(10) 0.4052(9) 0.093(4) Uiso 1 1 d . . . H40A H -0.3905 0.1302 0.4610 0.112 Uiso 1 1 calc R . . H40B H -0.5272 0.1043 0.4216 0.112 Uiso 1 1 calc R . . C42 C -0.4328(15) -0.0310(14) 0.3075(12) 0.139(6) Uiso 1 1 d . . . H42A H -0.5000 -0.0787 0.2524 0.166 Uiso 1 1 calc R . . H42B H -0.3846 -0.0766 0.3180 0.166 Uiso 1 1 calc R . . O2 O 0.3129(9) -0.7320(8) 0.4754(7) 0.037(2) Uiso 0.50 1 d P . . C43 C 0.2825(13) -0.8440(12) 0.4813(11) 0.038(3) Uiso 0.50 1 d P . . H43A H 0.2539 -0.8957 0.4175 0.045 Uiso 0.50 1 calc PR . . H43B H 0.3554 -0.8511 0.5120 0.045 Uiso 0.50 1 calc PR . . C44 C 0.2060(10) -0.8790(9) 0.5233(8) 0.017(2) Uiso 0.50 1 d P . . H44A H 0.2408 -0.8440 0.5901 0.026 Uiso 0.50 1 calc PR . . H44B H 0.1762 -0.9638 0.5107 0.026 Uiso 0.50 1 calc PR . . H44C H 0.1399 -0.8573 0.5029 0.026 Uiso 0.50 1 calc PR . . C45 C 0.3912(12) -0.6902(11) 0.4343(9) 0.029(3) Uiso 0.50 1 d P . . H45A H 0.4424 -0.7340 0.4380 0.035 Uiso 0.50 1 calc PR . . H45B H 0.4415 -0.6099 0.4726 0.035 Uiso 0.50 1 calc PR . . C46 C 0.3685(14) -0.6831(13) 0.3435(10) 0.039(4) Uiso 0.50 1 d P . . H46A H 0.3527 -0.7578 0.3014 0.058 Uiso 0.50 1 calc PR . . H46B H 0.4381 -0.6222 0.3344 0.058 Uiso 0.50 1 calc PR . . H46C H 0.2988 -0.6642 0.3304 0.058 Uiso 0.50 1 calc PR . . 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 0.023(3) 0.017(3) 0.033(4) 0.007(3) 0.004(3) 0.006(3) C2 0.053(5) 0.054(5) 0.031(4) 0.017(4) 0.014(4) 0.038(4) C3 0.054(5) 0.048(5) 0.036(5) -0.003(4) -0.008(4) 0.033(4) C4 0.033(4) 0.032(4) 0.039(4) 0.003(3) 0.009(3) 0.022(3) C5 0.028(4) 0.033(4) 0.044(5) -0.006(3) 0.001(3) 0.012(3) C6 0.029(4) 0.025(4) 0.051(5) 0.007(3) 0.012(4) 0.007(3) C7 0.039(4) 0.025(4) 0.045(5) 0.011(3) 0.017(4) 0.015(3) C8 0.023(4) 0.034(4) 0.032(4) 0.013(3) 0.009(3) 0.013(3) C9 0.024(4) 0.025(3) 0.027(4) 0.005(3) 0.006(3) 0.011(3) C10 0.021(3) 0.028(3) 0.036(4) 0.016(3) 0.009(3) 0.012(3) C11 0.022(3) 0.021(3) 0.027(4) 0.008(3) 0.005(3) 0.009(3) C12 0.023(3) 0.032(4) 0.031(4) 0.018(3) 0.008(3) 0.012(3) C13 0.032(4) 0.031(4) 0.046(5) 0.012(3) 0.007(4) 0.015(3) C14 0.028(4) 0.048(5) 0.049(5) 0.024(4) 0.005(4) 0.014(4) C15 0.030(4) 0.047(5) 0.050(5) 0.016(4) -0.001(4) 0.005(4) C16 0.041(5) 0.033(4) 0.036(5) 0.002(3) 0.001(4) 0.001(4) C17 0.037(4) 0.034(4) 0.025(4) 0.007(3) 0.009(3) 0.012(3) C18 0.054(5) 0.029(4) 0.036(5) 0.000(3) 0.002(4) 0.017(4) C19 0.039(4) 0.035(4) 0.034(4) 0.005(3) 0.013(3) 0.023(3) C20 0.022(3) 0.018(3) 0.034(4) 0.010(3) 0.012(3) 0.006(3) C21 0.026(4) 0.037(4) 0.025(4) 0.003(3) -0.002(3) 0.014(3) C22 0.035(4) 0.046(4) 0.026(4) 0.014(3) 0.009(3) 0.022(4) C23 0.023(4) 0.024(3) 0.033(4) 0.005(3) 0.007(3) 0.012(3) C24 0.040(4) 0.040(4) 0.040(5) 0.017(3) 0.018(4) 0.019(4) C25 0.031(4) 0.039(4) 0.055(5) 0.015(4) 0.020(4) 0.016(3) C26 0.029(4) 0.037(4) 0.042(5) 0.003(3) 0.001(3) 0.016(3) C27 0.027(4) 0.034(4) 0.029(4) 0.009(3) 0.001(3) 0.012(3) C28 0.023(3) 0.024(3) 0.027(4) 0.009(3) 0.008(3) 0.010(3) C29 0.019(3) 0.024(3) 0.027(4) 0.012(3) 0.007(3) 0.010(3) C30 0.025(4) 0.027(3) 0.027(4) 0.009(3) 0.010(3) 0.010(3) C31 0.032(4) 0.036(4) 0.027(4) 0.012(3) 0.006(3) 0.010(3) C32 0.046(5) 0.042(4) 0.030(4) 0.014(3) 0.004(4) 0.016(4) C33 0.054(6) 0.049(5) 0.048(6) 0.027(4) 0.004(5) 0.012(4) C34 0.070(7) 0.079(7) 0.051(6) 0.043(5) 0.023(5) 0.019(6) C35 0.079(7) 0.086(7) 0.050(6) 0.039(5) 0.040(5) 0.037(6) C36 0.043(5) 0.053(5) 0.033(5) 0.014(4) 0.016(4) 0.017(4) C37 0.049(5) 0.065(5) 0.046(5) 0.012(4) 0.020(4) 0.034(5) C38 0.042(5) 0.039(4) 0.032(4) 0.007(3) 0.007(3) 0.022(4) N1 0.031(3) 0.028(3) 0.029(3) 0.010(2) 0.010(3) 0.017(3) N2 0.023(3) 0.024(3) 0.035(4) 0.004(2) 0.006(3) 0.014(2) N3 0.015(3) 0.028(3) 0.032(3) 0.006(2) 0.003(2) 0.009(2) N4 0.027(3) 0.029(3) 0.027(3) 0.007(2) 0.010(3) 0.015(2) Pd1 0.0203(3) 0.0221(3) 0.0276(3) 0.0093(2) 0.0074(2) 0.0100(2) I1 0.0237(3) 0.0304(3) 0.0555(3) 0.0212(2) 0.0126(2) 0.0107(2) I2 0.0272(3) 0.0301(2) 0.0383(3) 0.0149(2) 0.0074(2) 0.0060(2) _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 1.321(8) . ? C1 N1 1.336(8) . ? C1 Pd1 2.041(6) . ? C2 N1 1.443(9) . ? C2 C3 1.497(11) . ? C3 C4 1.506(10) . ? C4 C9 1.381(9) . ? C4 C5 1.404(9) . ? C5 C6 1.372(10) . ? C6 C7 1.379(10) . ? C7 C8 1.400(9) . ? C8 C9 1.402(9) . ? C9 C10 1.532(8) . ? C10 N1 1.460(8) . ? C10 C11 1.538(9) . ? C11 N2 1.473(7) . ? C11 C12 1.534(9) . ? C12 C13 1.378(9) . ? C12 C17 1.401(9) . ? C13 C14 1.378(10) . ? C14 C15 1.362(11) . ? C15 C16 1.371(11) . ? C16 C17 1.399(10) . ? C17 C18 1.511(10) . ? C18 C19 1.515(10) . ? C19 N2 1.463(8) . ? C20 N4 1.334(8) . ? C20 N3 1.336(8) . ? C20 Pd1 2.017(6) . ? C21 N3 1.459(8) . ? C21 C22 1.505(10) . ? C22 C23 1.521(9) . ? C23 C28 1.385(9) . ? C23 C24 1.401(10) . ? C24 C25 1.375(10) . ? C25 C26 1.377(10) . ? C26 C27 1.392(10) . ? C27 C28 1.409(9) . ? C28 C29 1.507(9) . ? C29 N3 1.479(8) . ? C29 C30 1.548(9) . ? C30 N4 1.463(8) . ? C30 C31 1.511(9) . ? C31 C32 1.402(10) . ? C31 C36 1.412(10) . ? C32 C33 1.381(11) . ? C33 C34 1.380(13) . ? C34 C35 1.373(13) . ? C35 C36 1.397(11) . ? C36 C37 1.520(11) . ? C37 C38 1.506(11) . ? C38 N4 1.450(8) . ? Pd1 I2 2.5924(6) . ? Pd1 I1 2.5933(6) . ? O1 C42 1.612(17) . ? O1 C39 1.684(14) . ? C41 C40 1.266(12) . ? C41 C42 1.488(17) . ? C39 C40 1.460(16) . ? O2 C45 1.249(15) . ? O2 C43 1.367(16) . ? C43 C44 1.223(17) . ? C45 C46 1.383(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 107.8(5) . . ? N2 C1 Pd1 128.2(5) . . ? N1 C1 Pd1 124.0(5) . . ? N1 C2 C3 109.9(6) . . ? C2 C3 C4 113.0(6) . . ? C9 C4 C5 119.1(6) . . ? C9 C4 C3 121.1(6) . . ? C5 C4 C3 119.8(6) . . ? C6 C5 C4 121.3(7) . . ? C5 C6 C7 119.9(6) . . ? C6 C7 C8 119.8(7) . . ? C7 C8 C9 120.1(6) . . ? C4 C9 C8 119.7(6) . . ? C4 C9 C10 121.2(6) . . ? C8 C9 C10 118.9(6) . . ? N1 C10 C9 111.0(5) . . ? N1 C10 C11 102.0(5) . . ? C9 C10 C11 115.9(5) . . ? N2 C11 C12 111.8(5) . . ? N2 C11 C10 101.7(5) . . ? C12 C11 C10 115.9(5) . . ? C13 C12 C17 119.4(6) . . ? C13 C12 C11 120.3(6) . . ? C17 C12 C11 120.2(6) . . ? C12 C13 C14 121.5(7) . . ? C15 C14 C13 119.9(7) . . ? C14 C15 C16 119.5(7) . . ? C15 C16 C17 122.1(7) . . ? C16 C17 C12 117.5(7) . . ? C16 C17 C18 120.5(6) . . ? C12 C17 C18 122.0(6) . . ? C17 C18 C19 113.1(6) . . ? N2 C19 C18 108.9(6) . . ? N4 C20 N3 107.9(5) . . ? N4 C20 Pd1 124.5(4) . . ? N3 C20 Pd1 127.6(5) . . ? N3 C21 C22 109.3(5) . . ? C21 C22 C23 112.4(6) . . ? C28 C23 C24 119.2(6) . . ? C28 C23 C22 122.1(6) . . ? C24 C23 C22 118.7(6) . . ? C25 C24 C23 121.4(7) . . ? C24 C25 C26 120.3(7) . . ? C25 C26 C27 119.1(7) . . ? C26 C27 C28 121.3(7) . . ? C23 C28 C27 118.8(6) . . ? C23 C28 C29 121.8(6) . . ? C27 C28 C29 119.4(6) . . ? N3 C29 C28 110.5(5) . . ? N3 C29 C30 101.5(5) . . ? C28 C29 C30 116.1(5) . . ? N4 C30 C31 111.5(5) . . ? N4 C30 C29 101.9(5) . . ? C31 C30 C29 117.1(5) . . ? C32 C31 C36 119.2(7) . . ? C32 C31 C30 120.5(6) . . ? C36 C31 C30 120.1(6) . . ? C33 C32 C31 121.1(8) . . ? C34 C33 C32 119.8(8) . . ? C35 C34 C33 119.8(8) . . ? C34 C35 C36 122.3(9) . . ? C35 C36 C31 117.8(8) . . ? C35 C36 C37 120.6(8) . . ? C31 C36 C37 121.6(7) . . ? C38 C37 C36 112.0(6) . . ? N4 C38 C37 109.2(6) . . ? C1 N1 C2 126.0(6) . . ? C1 N1 C10 114.0(5) . . ? C2 N1 C10 116.8(5) . . ? C1 N2 C19 126.7(5) . . ? C1 N2 C11 114.1(5) . . ? C19 N2 C11 116.8(5) . . ? C20 N3 C21 125.1(5) . . ? C20 N3 C29 113.5(5) . . ? C21 N3 C29 117.4(5) . . ? C20 N4 C38 126.4(5) . . ? C20 N4 C30 114.1(5) . . ? C38 N4 C30 117.0(5) . . ? C20 Pd1 C1 176.6(3) . . ? C20 Pd1 I2 89.13(17) . . ? C1 Pd1 I2 89.90(17) . . ? C20 Pd1 I1 88.95(17) . . ? C1 Pd1 I1 92.17(17) . . ? I2 Pd1 I1 176.72(3) . . ? C42 O1 C39 86.3(9) . . ? C40 C41 C42 99.0(10) . . ? C40 C39 O1 104.0(10) . . ? C41 C40 C39 119.1(11) . . ? C41 C42 O1 119.0(11) . . ? C45 O2 C43 119.2(11) . . ? C44 C43 O2 115.8(13) . . ? O2 C45 C46 124.8(13) . . ? 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 C4 46.4(9) . . . . ? C2 C3 C4 C9 -20.7(10) . . . . ? C2 C3 C4 C5 159.8(7) . . . . ? C9 C4 C5 C6 1.5(11) . . . . ? C3 C4 C5 C6 -179.0(7) . . . . ? C4 C5 C6 C7 -2.7(11) . . . . ? C5 C6 C7 C8 2.4(11) . . . . ? C6 C7 C8 C9 -1.0(10) . . . . ? C5 C4 C9 C8 0.0(10) . . . . ? C3 C4 C9 C8 -179.6(7) . . . . ? C5 C4 C9 C10 -175.8(6) . . . . ? C3 C4 C9 C10 4.6(10) . . . . ? C7 C8 C9 C4 -0.2(10) . . . . ? C7 C8 C9 C10 175.7(6) . . . . ? C4 C9 C10 N1 -14.5(9) . . . . ? C8 C9 C10 N1 169.7(6) . . . . ? C4 C9 C10 C11 -130.3(7) . . . . ? C8 C9 C10 C11 53.9(8) . . . . ? N1 C10 C11 N2 -6.2(6) . . . . ? C9 C10 C11 N2 114.5(6) . . . . ? N1 C10 C11 C12 115.3(5) . . . . ? C9 C10 C11 C12 -124.0(6) . . . . ? N2 C11 C12 C13 169.9(6) . . . . ? C10 C11 C12 C13 54.0(8) . . . . ? N2 C11 C12 C17 -13.2(9) . . . . ? C10 C11 C12 C17 -129.1(6) . . . . ? C17 C12 C13 C14 1.8(11) . . . . ? C11 C12 C13 C14 178.7(7) . . . . ? C12 C13 C14 C15 -1.8(12) . . . . ? C13 C14 C15 C16 1.8(12) . . . . ? C14 C15 C16 C17 -1.8(13) . . . . ? C15 C16 C17 C12 1.8(11) . . . . ? C15 C16 C17 C18 -179.9(8) . . . . ? C13 C12 C17 C16 -1.7(10) . . . . ? C11 C12 C17 C16 -178.6(6) . . . . ? C13 C12 C17 C18 -180.0(7) . . . . ? C11 C12 C17 C18 3.1(10) . . . . ? C16 C17 C18 C19 161.5(7) . . . . ? C12 C17 C18 C19 -20.3(10) . . . . ? C17 C18 C19 N2 46.6(8) . . . . ? N3 C21 C22 C23 44.9(7) . . . . ? C21 C22 C23 C28 -18.5(9) . . . . ? C21 C22 C23 C24 163.2(6) . . . . ? C28 C23 C24 C25 1.7(10) . . . . ? C22 C23 C24 C25 -180.0(6) . . . . ? C23 C24 C25 C26 -1.1(11) . . . . ? C24 C25 C26 C27 0.2(10) . . . . ? C25 C26 C27 C28 0.2(10) . . . . ? C24 C23 C28 C27 -1.3(9) . . . . ? C22 C23 C28 C27 -179.6(6) . . . . ? C24 C23 C28 C29 -179.5(6) . . . . ? C22 C23 C28 C29 2.2(9) . . . . ? C26 C27 C28 C23 0.4(10) . . . . ? C26 C27 C28 C29 178.7(6) . . . . ? C23 C28 C29 N3 -13.1(8) . . . . ? C27 C28 C29 N3 168.6(5) . . . . ? C23 C28 C29 C30 -128.0(6) . . . . ? C27 C28 C29 C30 53.8(8) . . . . ? N3 C29 C30 N4 -9.7(6) . . . . ? C28 C29 C30 N4 110.2(6) . . . . ? N3 C29 C30 C31 112.2(6) . . . . ? C28 C29 C30 C31 -127.9(6) . . . . ? N4 C30 C31 C32 167.7(6) . . . . ? C29 C30 C31 C32 50.9(9) . . . . ? N4 C30 C31 C36 -17.1(9) . . . . ? C29 C30 C31 C36 -133.9(7) . . . . ? C36 C31 C32 C33 -0.4(11) . . . . ? C30 C31 C32 C33 174.9(7) . . . . ? C31 C32 C33 C34 -0.3(12) . . . . ? C32 C33 C34 C35 1.0(14) . . . . ? C33 C34 C35 C36 -1.0(15) . . . . ? C34 C35 C36 C31 0.3(14) . . . . ? C34 C35 C36 C37 177.7(9) . . . . ? C32 C31 C36 C35 0.4(11) . . . . ? C30 C31 C36 C35 -174.9(7) . . . . ? C32 C31 C36 C37 -177.0(7) . . . . ? C30 C31 C36 C37 7.7(11) . . . . ? C35 C36 C37 C38 159.6(8) . . . . ? C31 C36 C37 C38 -23.1(11) . . . . ? C36 C37 C38 N4 47.4(9) . . . . ? N2 C1 N1 C2 -163.3(6) . . . . ? Pd1 C1 N1 C2 16.2(9) . . . . ? N2 C1 N1 C10 -4.2(7) . . . . ? Pd1 C1 N1 C10 175.3(4) . . . . ? C3 C2 N1 C1 97.3(8) . . . . ? C3 C2 N1 C10 -61.3(8) . . . . ? C9 C10 N1 C1 -117.3(6) . . . . ? C11 C10 N1 C1 6.8(7) . . . . ? C9 C10 N1 C2 43.9(8) . . . . ? C11 C10 N1 C2 167.9(6) . . . . ? N1 C1 N2 C19 -162.2(6) . . . . ? Pd1 C1 N2 C19 18.3(10) . . . . ? N1 C1 N2 C11 -0.6(7) . . . . ? Pd1 C1 N2 C11 179.9(4) . . . . ? C18 C19 N2 C1 99.7(8) . . . . ? C18 C19 N2 C11 -61.5(8) . . . . ? C12 C11 N2 C1 -119.7(6) . . . . ? C10 C11 N2 C1 4.6(7) . . . . ? C12 C11 N2 C19 43.9(8) . . . . ? C10 C11 N2 C19 168.1(5) . . . . ? N4 C20 N3 C21 -161.1(6) . . . . ? Pd1 C20 N3 C21 19.7(9) . . . . ? N4 C20 N3 C29 -4.3(7) . . . . ? Pd1 C20 N3 C29 176.5(4) . . . . ? C22 C21 N3 C20 94.5(7) . . . . ? C22 C21 N3 C29 -61.5(7) . . . . ? C28 C29 N3 C20 -114.6(6) . . . . ? C30 C29 N3 C20 9.2(7) . . . . ? C28 C29 N3 C21 44.1(7) . . . . ? C30 C29 N3 C21 167.9(5) . . . . ? N3 C20 N4 C38 -164.6(6) . . . . ? Pd1 C20 N4 C38 14.7(9) . . . . ? N3 C20 N4 C30 -3.1(7) . . . . ? Pd1 C20 N4 C30 176.1(4) . . . . ? C37 C38 N4 C20 98.2(8) . . . . ? C37 C38 N4 C30 -62.8(8) . . . . ? C31 C30 N4 C20 -117.2(6) . . . . ? C29 C30 N4 C20 8.5(7) . . . . ? C31 C30 N4 C38 46.1(8) . . . . ? C29 C30 N4 C38 171.8(5) . . . . ? N4 C20 Pd1 C1 5(5) . . . . ? N3 C20 Pd1 C1 -176(4) . . . . ? N4 C20 Pd1 I2 78.4(5) . . . . ? N3 C20 Pd1 I2 -102.5(5) . . . . ? N4 C20 Pd1 I1 -104.2(5) . . . . ? N3 C20 Pd1 I1 74.9(5) . . . . ? N2 C1 Pd1 C20 158(4) . . . . ? N1 C1 Pd1 C20 -22(5) . . . . ? N2 C1 Pd1 I2 84.0(6) . . . . ? N1 C1 Pd1 I2 -95.4(5) . . . . ? N2 C1 Pd1 I1 -93.5(6) . . . . ? N1 C1 Pd1 I1 87.1(5) . . . . ? C42 O1 C39 C40 30.4(11) . . . . ? C42 C41 C40 C39 17.3(16) . . . . ? O1 C39 C40 C41 -35.9(16) . . . . ? C40 C41 C42 O1 9.7(15) . . . . ? C39 O1 C42 C41 -26.0(13) . . . . ? C45 O2 C43 C44 179.3(13) . . . . ? C43 O2 C45 C46 98.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.621 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.153 #-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end