# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address J.D.Crowley ;Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; J.E.M.Lewis ;Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; E.L.Gavey ;Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; S.A.Cameron ;Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; _publ_contact_author_address ;Department of Chemistry University of Otago PO Box 56 Dunedin New Zealand ; _publ_contact_author_email jcrowley@chemistry.otago.ac.nz _publ_contact_author_phone '+64 3 479 7731' _publ_contact_author_name 'James Crowley' data_eg273 _database_code_depnum_ccdc_archive 'CCDC 853226' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.10 H48.40 F12 N6 O8.10 Pd Sb2' _chemical_formula_weight 1369.99 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' 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' Sb Sb -0.5866 1.5461 '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 12.850(5) _cell_length_b 15.422(5) _cell_length_c 16.768(5) _cell_angle_alpha 66.868(5) _cell_angle_beta 88.549(5) _cell_angle_gamma 80.667(5) _cell_volume 3012.7(18) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 8616 _cell_measurement_theta_min 2.3205 _cell_measurement_theta_max 20.4125 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.270 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6373 _exptl_absorpt_correction_T_max 0.7445 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55742 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 20.68 _reflns_number_total 6112 _reflns_number_gt 5014 _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^)+(0.0726P)^2^+21.2567P] 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 6112 _refine_ls_number_parameters 695 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.70839(5) 0.28211(5) 0.83513(4) 0.0221(2) Uani 1 1 d . . . C1 C 0.7358(7) 0.0720(7) 0.8916(6) 0.031(2) Uani 1 1 d . . . H1 H 0.7501 0.0723 0.9468 0.037 Uiso 1 1 calc R . . C2 C 0.7420(8) -0.0128(7) 0.8839(7) 0.037(3) Uani 1 1 d . . . H2 H 0.7617 -0.0710 0.9329 0.045 Uiso 1 1 calc R . . C3 C 0.7193(8) -0.0144(7) 0.8042(6) 0.037(3) Uani 1 1 d . . . H3 H 0.7218 -0.0734 0.7981 0.045 Uiso 1 1 calc R . . C4 C 0.6928(8) 0.0724(7) 0.7331(6) 0.032(3) Uani 1 1 d . . . C5 C 0.6875(8) 0.1567(7) 0.7450(6) 0.030(3) Uani 1 1 d . . . H5 H 0.6675 0.2160 0.6972 0.036 Uiso 1 1 calc R . . C6 C 0.6680(10) 0.0756(7) 0.6483(8) 0.047(3) Uani 1 1 d . . . C7 C 0.6446(10) 0.0784(8) 0.5787(9) 0.054(3) Uani 1 1 d . . . C8 C 0.6152(12) 0.0836(9) 0.4949(8) 0.067(4) Uani 1 1 d . . . C9 C 0.6432(16) 0.0067(10) 0.4718(10) 0.122(8) Uani 1 1 d . . . H9 H 0.6839 -0.0512 0.5106 0.146 Uiso 1 1 calc R . . C10 C 0.6103(17) 0.0165(10) 0.3903(10) 0.129(9) Uani 1 1 d . . . H10 H 0.6313 -0.0344 0.3719 0.155 Uiso 1 1 calc R . . C11 C 0.5480(13) 0.0983(8) 0.3358(8) 0.082(5) Uani 1 1 d . . . H11 H 0.5215 0.1041 0.2812 0.098 Uiso 1 1 calc R . . C12 C 0.5250(10) 0.1734(8) 0.3643(8) 0.054(3) Uani 1 1 d . . . C13 C 0.4625(10) 0.2636(9) 0.3073(8) 0.051(3) Uani 1 1 d . . . C14 C 0.4114(8) 0.3381(8) 0.2589(7) 0.035(3) Uani 1 1 d . . . C15 C 0.3517(7) 0.4239(7) 0.1985(6) 0.028(2) Uani 1 1 d . . . C16 C 0.3484(7) 0.5095(7) 0.2093(6) 0.025(2) Uani 1 1 d . . . H16 H 0.3856 0.5098 0.2574 0.030 Uiso 1 1 calc R . . C17 C 0.2955(8) 0.4254(7) 0.1278(7) 0.035(3) Uani 1 1 d . . . H17 H 0.2973 0.3682 0.1187 0.043 Uiso 1 1 calc R . . C18 C 0.2377(8) 0.5092(7) 0.0713(6) 0.033(3) Uani 1 1 d . . . H18 H 0.1979 0.5105 0.0238 0.040 Uiso 1 1 calc R . . C19 C 0.2388(8) 0.5914(7) 0.0850(6) 0.033(3) Uani 1 1 d . . . H19 H 0.1996 0.6497 0.0456 0.040 Uiso 1 1 calc R . . C20 C 0.9415(7) 0.2461(6) 0.8440(6) 0.026(2) Uani 1 1 d . . . H20 H 0.9316 0.2198 0.9047 0.032 Uiso 1 1 calc R . . C21 C 1.0431(8) 0.2433(7) 0.8147(6) 0.032(3) Uani 1 1 d . . . H21 H 1.1022 0.2173 0.8546 0.039 Uiso 1 1 calc R . . C22 C 1.0568(8) 0.2793(7) 0.7260(6) 0.032(3) Uani 1 1 d . . . H22 H 1.1258 0.2765 0.7045 0.039 Uiso 1 1 calc R . . C23 C 0.9692(7) 0.3195(6) 0.6685(6) 0.026(2) Uani 1 1 d . . . C24 C 0.8697(7) 0.3216(6) 0.7020(6) 0.024(2) Uani 1 1 d . . . H24 H 0.8097 0.3494 0.6631 0.029 Uiso 1 1 calc R . . C25 C 0.9782(7) 0.3595(7) 0.5760(7) 0.032(3) Uani 1 1 d . . . C26 C 0.9817(7) 0.3945(7) 0.4982(7) 0.029(2) Uani 1 1 d . . . C27 C 0.9853(8) 0.4338(7) 0.4055(6) 0.030(2) Uani 1 1 d . . . C28 C 1.0794(8) 0.4239(7) 0.3650(6) 0.035(3) Uani 1 1 d . . . H28 H 1.1437 0.3927 0.3978 0.042 Uiso 1 1 calc R . . C29 C 1.0761(8) 0.4613(7) 0.2743(6) 0.033(3) Uani 1 1 d . . . H29 H 1.1389 0.4545 0.2446 0.040 Uiso 1 1 calc R . . C30 C 0.9827(7) 0.5081(7) 0.2273(6) 0.031(2) Uani 1 1 d . . . H30 H 0.9798 0.5342 0.1656 0.037 Uiso 1 1 calc R . . C31 C 0.8926(7) 0.5155(7) 0.2737(7) 0.031(3) Uani 1 1 d . . . C32 C 0.7941(9) 0.5687(7) 0.2270(7) 0.033(3) Uani 1 1 d . . . C33 C 0.7146(9) 0.6140(7) 0.1847(6) 0.034(3) Uani 1 1 d . . . C34 C 0.6226(7) 0.6712(7) 0.1298(6) 0.028(2) Uani 1 1 d . . . C35 C 0.5235(7) 0.6716(6) 0.1638(6) 0.025(2) Uani 1 1 d . . . H35 H 0.5170 0.6346 0.2237 0.029 Uiso 1 1 calc R . . C36 C 0.6318(8) 0.7261(7) 0.0429(7) 0.040(3) Uani 1 1 d . . . H36 H 0.6990 0.7270 0.0179 0.048 Uiso 1 1 calc R . . C37 C 0.5425(8) 0.7794(8) -0.0070(6) 0.042(3) Uani 1 1 d . . . H37 H 0.5479 0.8183 -0.0666 0.050 Uiso 1 1 calc R . . C38 C 0.4451(8) 0.7763(7) 0.0299(6) 0.035(3) Uani 1 1 d . . . H38 H 0.3835 0.8125 -0.0050 0.041 Uiso 1 1 calc R . . N1 N 0.7099(6) 0.1566(5) 0.8228(5) 0.0239(19) Uani 1 1 d . . . N2 N 0.5567(8) 0.1673(6) 0.4413(5) 0.048(3) Uani 1 1 d . . . N3 N 0.2931(6) 0.5924(5) 0.1520(5) 0.0232(18) Uani 1 1 d . . . N4 N 0.8554(6) 0.2854(5) 0.7885(5) 0.0221(18) Uani 1 1 d . . . N5 N 0.8914(6) 0.4805(6) 0.3617(5) 0.030(2) Uani 1 1 d . . . N6 N 0.4359(6) 0.7226(5) 0.1149(5) 0.0220(18) Uani 1 1 d . . . Sb1 Sb 0.37625(6) 1.08588(5) 0.82064(5) 0.0408(3) Uani 1 1 d . . . F1 F 0.4834(5) 1.0875(5) 0.8919(5) 0.0604(19) Uani 1 1 d . A . F2 F 0.2684(6) 1.0876(5) 0.7467(4) 0.075(2) Uani 1 1 d . A . F3 F 0.4656(8) 1.0015(10) 0.7903(9) 0.109(5) Uani 0.75 1 d PD A 1 F4 F 0.3328(7) 0.9826(7) 0.9086(5) 0.065(3) Uani 0.75 1 d PD A 1 F5 F 0.2835(7) 1.1616(9) 0.8622(10) 0.115(5) Uani 0.75 1 d PDU A 1 F6 F 0.4218(12) 1.1911(9) 0.7396(7) 0.122(5) Uani 0.75 1 d PDU A 1 F7 F 0.333(3) 1.211(3) 0.791(3) 0.117(14) Uiso 0.25 1 d PD A 2 F8 F 0.469(2) 1.109(3) 0.729(2) 0.108(12) Uiso 0.25 1 d PD A 2 F9 F 0.287(2) 1.064(3) 0.9059(18) 0.082(9) Uiso 0.25 1 d PD A 2 F10 F 0.413(2) 0.957(2) 0.853(2) 0.089(10) Uiso 0.25 1 d PD A 2 Sb2 Sb 0.06935(6) 0.28402(5) 0.08780(4) 0.0360(3) Uani 1 1 d . . . F11 F 0.0743(6) 0.2157(4) 0.0178(4) 0.0620(19) Uani 1 1 d . . . F12 F 0.2143(4) 0.2402(4) 0.1147(4) 0.0404(14) Uani 1 1 d . . . F13 F -0.0768(5) 0.3261(5) 0.0627(5) 0.076(2) Uani 1 1 d . . . F14 F 0.1013(6) 0.3899(4) -0.0065(4) 0.067(2) Uani 1 1 d . . . F15 F 0.0679(5) 0.3518(4) 0.1578(4) 0.0521(17) Uani 1 1 d . . . F16 F 0.0420(5) 0.1753(4) 0.1816(4) 0.0535(17) Uani 1 1 d . . . O50 O 0.5141(6) 0.3287(5) 0.4806(5) 0.0441(18) Uani 1 1 d . . . H50X H 0.5264 0.2786 0.4683 0.053 Uiso 1 1 d . . . H50Y H 0.4463 0.3336 0.4840 0.053 Uiso 1 1 d . . . O51 O 0.2916(5) 0.4874(5) 0.5522(4) 0.0439(18) Uani 1 1 d . . . H51X H 0.3472 0.4884 0.5794 0.053 Uiso 1 1 d . . . H51Y H 0.2361 0.4974 0.5790 0.053 Uiso 1 1 d . . . O52 O 0.6337(6) 0.3760(5) 0.5929(5) 0.053(2) Uani 1 1 d . . . H52X H 0.5928 0.3521 0.5697 0.064 Uiso 1 1 d . . . H52Y H 0.6564 0.4179 0.5475 0.064 Uiso 1 1 d . . . O53 O 0.4727(7) 0.4897(6) 0.6388(5) 0.061(2) Uani 1 1 d . . . H53X H 0.5227 0.4552 0.6236 0.074 Uiso 1 1 d . . . H53Y H 0.4779 0.5462 0.6013 0.074 Uiso 1 1 d . . . O60 O 0.8161(6) 0.1668(5) 0.0220(5) 0.0437(19) Uani 1 1 d . . . C60 C 0.8431(10) 0.1155(9) 0.0953(9) 0.055(3) Uani 1 1 d . . . C61 C 0.9241(10) 0.0333(9) 0.1145(9) 0.068(4) Uani 1 1 d . . . H61A H 0.9507 0.0304 0.0602 0.081 Uiso 1 1 calc R . . H61B H 0.8948 -0.0247 0.1478 0.081 Uiso 1 1 calc R . . H61C H 0.9820 0.0383 0.1486 0.081 Uiso 1 1 calc R . . C62 C 0.7924(11) 0.1397(11) 0.1698(9) 0.076(4) Uani 1 1 d . . . H62A H 0.7479 0.2029 0.1457 0.091 Uiso 1 1 calc R . . H62B H 0.8479 0.1402 0.2085 0.091 Uiso 1 1 calc R . . H62C H 0.7491 0.0915 0.2024 0.091 Uiso 1 1 calc R . . O70 O 0.3007(6) 0.3451(5) 0.4917(5) 0.054(2) Uani 1 1 d . . . C70 C 0.2771(12) 0.2541(10) 0.5430(9) 0.079(4) Uani 1 1 d . . . H70A H 0.3207 0.2267 0.5970 0.095 Uiso 1 1 calc R . . H70B H 0.2918 0.2124 0.5112 0.095 Uiso 1 1 calc R . . H70C H 0.2023 0.2598 0.5567 0.095 Uiso 1 1 calc R . . H70X H 0.2977 0.3900 0.5108 0.095 Uiso 1 1 d . . . O80 O 1.116(2) 0.1608(17) 0.4319(16) 0.112(7) Uiso 0.50 1 d P . . C80 C 1.162(2) 0.1791(18) 0.3626(16) 0.060(7) Uiso 0.50 1 d P . . H80A H 1.1193 0.2335 0.3165 0.071 Uiso 0.50 1 calc PR . . H80B H 1.1709 0.1232 0.3473 0.071 Uiso 0.50 1 calc PR . . H80C H 1.2309 0.1949 0.3691 0.071 Uiso 0.50 1 calc PR . . H80X H 1.1343 0.1019 0.4663 0.071 Uiso 0.50 1 d P . . O90 O 1.085(3) 0.019(2) 0.600(2) 0.080(9) Uiso 0.30 1 d P . . C90 C 0.998(3) 0.054(3) 0.632(3) 0.055(11) Uiso 0.30 1 d P . . H90A H 0.9926 0.0115 0.6933 0.066 Uiso 0.30 1 calc PR . . H90B H 0.9356 0.0567 0.5988 0.066 Uiso 0.30 1 calc PR . . H90C H 1.0034 0.1180 0.6285 0.066 Uiso 0.30 1 calc PR . . H90X H 1.0894 -0.0369 0.5970 0.066 Uiso 0.30 1 d P . . O100 O 0.901(3) 0.160(2) 0.410(2) 0.078(9) Uiso 0.30 1 d P . . C100 C 0.847(3) 0.237(3) 0.366(3) 0.060(11) Uiso 0.30 1 d P . . H10A H 0.7987 0.2582 0.4031 0.072 Uiso 0.30 1 calc PR . . H10B H 0.8054 0.2290 0.3212 0.072 Uiso 0.30 1 calc PR . . H10C H 0.8925 0.2842 0.3377 0.072 Uiso 0.30 1 calc PR . . H100 H 0.9687 0.1596 0.4161 0.072 Uiso 0.30 1 d P . . O110 O 0.5324(19) 0.4982(16) 0.0464(14) 0.075(6) Uiso 0.40 1 d P B -1 C110 C 0.547(4) 0.404(3) 0.050(3) 0.104(14) Uiso 0.40 1 d P B -1 H11A H 0.6213 0.3751 0.0650 0.125 Uiso 0.40 1 calc PR B -1 H11B H 0.5274 0.4057 -0.0065 0.125 Uiso 0.40 1 calc PR B -1 H11C H 0.5025 0.3668 0.0943 0.125 Uiso 0.40 1 calc PR B -1 H110 H 0.4960 0.5426 0.0020 0.125 Uiso 0.40 1 d P C -1 O120 O 0.596(3) 0.354(3) 0.104(2) 0.093(11) Uiso 0.30 1 d P D 2 C120 C 0.638(3) 0.401(3) 0.137(2) 0.045(10) Uiso 0.30 1 d P D 2 H12A H 0.5982 0.4664 0.1180 0.055 Uiso 0.30 1 calc PR D 2 H12B H 0.7112 0.4045 0.1190 0.055 Uiso 0.30 1 calc PR D 2 H12C H 0.6383 0.3702 0.2007 0.055 Uiso 0.30 1 calc PR D 2 H120 H 0.5533 0.3946 0.0571 0.055 Uiso 0.30 1 d P E 2 O130 O 0.613(3) 0.435(2) 0.210(2) 0.078(9) Uiso 0.30 1 d P F 3 C130 C 0.697(5) 0.367(4) 0.220(4) 0.106(19) Uiso 0.30 1 d P F 3 H13A H 0.7506 0.3938 0.1789 0.127 Uiso 0.30 1 calc PR F 3 H13B H 0.6753 0.3145 0.2088 0.127 Uiso 0.30 1 calc PR F 3 H13C H 0.7275 0.3421 0.2794 0.127 Uiso 0.30 1 calc PR F 3 H130 H 0.6369 0.4941 0.2020 0.127 Uiso 0.30 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0188(5) 0.0208(4) 0.0228(4) -0.0044(3) -0.0039(3) -0.0029(3) C1 0.025(6) 0.032(7) 0.029(6) -0.007(6) -0.007(5) -0.001(5) C2 0.046(7) 0.019(6) 0.038(7) -0.005(5) -0.009(5) 0.001(5) C3 0.046(7) 0.032(7) 0.038(7) -0.020(6) -0.007(5) -0.001(5) C4 0.033(6) 0.025(6) 0.035(7) -0.012(6) -0.018(5) 0.005(5) C5 0.035(6) 0.018(6) 0.022(6) 0.005(5) 0.001(5) 0.004(5) C6 0.063(8) 0.024(6) 0.048(9) -0.013(6) -0.006(6) 0.008(5) C7 0.071(9) 0.032(7) 0.055(9) -0.023(6) -0.032(7) 0.021(6) C8 0.102(11) 0.048(9) 0.057(9) -0.035(7) -0.038(8) 0.018(8) C9 0.22(2) 0.052(9) 0.082(11) -0.049(9) -0.100(13) 0.078(11) C10 0.25(2) 0.058(10) 0.075(11) -0.049(9) -0.098(14) 0.071(12) C11 0.146(14) 0.037(8) 0.059(9) -0.032(7) -0.056(9) 0.040(8) C12 0.073(9) 0.028(7) 0.048(8) -0.011(6) -0.032(7) 0.025(6) C13 0.070(9) 0.040(8) 0.050(8) -0.026(7) -0.006(7) -0.011(7) C14 0.038(7) 0.026(7) 0.037(7) -0.009(6) -0.007(5) -0.006(6) C15 0.024(6) 0.024(6) 0.029(6) -0.004(5) -0.005(5) 0.000(5) C16 0.017(5) 0.028(6) 0.026(6) -0.008(5) -0.001(4) -0.002(5) C17 0.034(6) 0.026(6) 0.045(7) -0.015(6) -0.002(5) 0.001(5) C18 0.038(7) 0.032(7) 0.036(6) -0.018(6) -0.005(5) -0.011(5) C19 0.027(6) 0.029(6) 0.035(6) -0.003(5) -0.003(5) -0.004(5) C20 0.025(6) 0.030(6) 0.023(6) -0.007(5) 0.000(5) -0.007(5) C21 0.024(6) 0.045(7) 0.029(7) -0.019(5) -0.008(5) 0.001(5) C22 0.037(7) 0.026(6) 0.029(7) -0.007(5) 0.004(5) -0.003(5) C23 0.026(6) 0.025(6) 0.023(6) -0.007(5) -0.004(5) 0.002(5) C24 0.018(6) 0.023(5) 0.029(7) -0.009(5) -0.009(5) 0.001(4) C25 0.018(6) 0.035(6) 0.039(9) -0.014(6) 0.000(5) 0.004(5) C26 0.019(6) 0.035(6) 0.028(8) -0.007(5) 0.002(5) -0.003(5) C27 0.031(7) 0.025(6) 0.027(7) -0.004(5) -0.005(5) -0.004(5) C28 0.026(6) 0.042(7) 0.031(7) -0.012(5) -0.002(5) 0.006(5) C29 0.021(6) 0.044(7) 0.028(7) -0.011(5) 0.006(5) 0.002(5) C30 0.026(7) 0.042(6) 0.023(6) -0.012(5) -0.004(5) -0.003(5) C31 0.015(6) 0.033(6) 0.045(8) -0.015(5) 0.001(5) -0.006(5) C32 0.027(7) 0.039(6) 0.033(6) -0.015(5) 0.000(6) -0.003(6) C33 0.033(7) 0.040(7) 0.027(6) -0.010(5) 0.009(6) -0.011(6) C34 0.023(6) 0.032(6) 0.025(6) -0.007(5) 0.000(5) -0.002(5) C35 0.021(6) 0.027(6) 0.024(5) -0.008(5) -0.003(5) -0.006(5) C36 0.024(6) 0.050(7) 0.042(8) -0.013(6) 0.001(5) -0.003(5) C37 0.026(7) 0.057(7) 0.024(6) 0.002(5) 0.005(5) -0.004(6) C38 0.030(7) 0.039(6) 0.024(7) -0.003(5) -0.004(5) 0.000(5) N1 0.020(5) 0.028(5) 0.019(5) -0.006(4) -0.006(3) 0.002(4) N2 0.075(7) 0.025(5) 0.030(6) -0.003(4) -0.028(5) 0.012(5) N3 0.015(4) 0.030(5) 0.022(5) -0.008(4) -0.004(4) 0.000(4) N4 0.022(5) 0.018(4) 0.023(5) -0.005(4) -0.004(4) -0.001(4) N5 0.023(5) 0.037(5) 0.023(5) -0.009(4) 0.000(4) 0.001(4) N6 0.022(5) 0.018(4) 0.025(5) -0.006(4) -0.006(4) -0.005(4) Sb1 0.0357(5) 0.0334(5) 0.0453(5) -0.0057(4) -0.0033(4) -0.0087(3) F1 0.027(4) 0.072(5) 0.100(5) -0.053(4) -0.010(3) -0.007(3) F2 0.072(5) 0.085(5) 0.046(4) 0.004(4) -0.027(4) -0.030(4) F3 0.069(7) 0.185(13) 0.164(12) -0.162(12) 0.029(8) -0.033(8) F4 0.075(7) 0.062(6) 0.038(5) 0.018(5) -0.012(5) -0.049(5) F5 0.025(6) 0.122(10) 0.260(15) -0.144(11) -0.015(7) 0.001(6) F6 0.158(12) 0.096(9) 0.081(8) 0.029(7) -0.035(8) -0.090(9) Sb2 0.0367(5) 0.0309(4) 0.0382(5) -0.0115(4) -0.0108(3) -0.0032(3) F11 0.088(5) 0.046(4) 0.054(4) -0.024(3) -0.022(4) -0.004(4) F12 0.034(3) 0.033(3) 0.049(4) -0.010(3) 0.006(3) -0.006(3) F13 0.046(4) 0.068(5) 0.109(6) -0.034(4) -0.041(4) 0.004(4) F14 0.098(6) 0.042(4) 0.048(4) -0.001(3) -0.010(4) -0.016(4) F15 0.050(4) 0.050(4) 0.064(4) -0.033(3) 0.001(3) -0.002(3) F16 0.046(4) 0.051(4) 0.058(4) -0.010(3) 0.003(3) -0.021(3) O50 0.045(5) 0.034(4) 0.052(5) -0.017(4) 0.000(4) -0.002(3) O51 0.024(4) 0.058(5) 0.047(5) -0.018(4) 0.005(3) -0.005(3) O52 0.037(5) 0.049(5) 0.056(5) 0.002(4) -0.012(4) -0.018(4) O53 0.069(6) 0.061(5) 0.041(5) -0.001(4) -0.002(4) -0.021(4) O60 0.050(5) 0.046(5) 0.030(5) -0.006(4) 0.001(4) -0.017(4) C60 0.053(9) 0.053(8) 0.052(9) -0.007(7) -0.015(7) -0.026(7) C61 0.064(9) 0.047(8) 0.088(10) -0.025(8) 0.006(8) -0.005(7) C62 0.075(10) 0.101(12) 0.060(9) -0.035(9) 0.006(7) -0.032(9) O70 0.060(6) 0.041(5) 0.054(5) -0.014(4) -0.009(4) -0.005(4) C70 0.078(11) 0.069(10) 0.067(10) -0.008(8) -0.001(8) 0.004(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 Pd1 N6 2.016(7) 2_666 ? Pd1 N1 2.022(7) . ? Pd1 N4 2.026(7) . ? Pd1 N3 2.027(7) 2_666 ? C1 C2 1.354(13) . ? C1 N1 1.356(12) . ? C1 H1 0.9500 . ? C2 C3 1.384(14) . ? C2 H2 0.9500 . ? C3 C4 1.397(14) . ? C3 H3 0.9500 . ? C4 C5 1.382(13) . ? C4 C6 1.445(16) . ? C5 N1 1.342(12) . ? C5 H5 0.9500 . ? C6 C7 1.196(15) . ? C7 C8 1.431(17) . ? C8 N2 1.359(14) . ? C8 C9 1.379(16) . ? C9 C10 1.385(18) . ? C9 H9 0.9500 . ? C10 C11 1.368(17) . ? C10 H10 0.9500 . ? C11 C12 1.404(15) . ? C11 H11 0.9500 . ? C12 N2 1.327(13) . ? C12 C13 1.458(17) . ? C13 C14 1.207(15) . ? C14 C15 1.422(15) . ? C15 C17 1.395(14) . ? C15 C16 1.395(13) . ? C16 N3 1.355(11) . ? C16 H16 0.9500 . ? C17 C18 1.372(14) . ? C17 H17 0.9500 . ? C18 C19 1.377(13) . ? C18 H18 0.9500 . ? C19 N3 1.344(12) . ? C19 H19 0.9500 . ? C20 N4 1.359(12) . ? C20 C21 1.383(13) . ? C20 H20 0.9500 . ? C21 C22 1.385(13) . ? C21 H21 0.9500 . ? C22 C23 1.393(13) . ? C22 H22 0.9500 . ? C23 C24 1.384(13) . ? C23 C25 1.437(15) . ? C24 N4 1.355(11) . ? C24 H24 0.9500 . ? C25 C26 1.202(13) . ? C26 C27 1.432(15) . ? C27 N5 1.365(12) . ? C27 C28 1.388(14) . ? C28 C29 1.399(13) . ? C28 H28 0.9500 . ? C29 C30 1.380(13) . ? C29 H29 0.9500 . ? C30 C31 1.393(13) . ? C30 H30 0.9500 . ? C31 N5 1.358(12) . ? C31 C32 1.448(15) . ? C32 C33 1.204(14) . ? C33 C34 1.450(16) . ? C34 C36 1.381(13) . ? C34 C35 1.382(13) . ? C35 N6 1.345(11) . ? C35 H35 0.9500 . ? C36 C37 1.377(14) . ? C36 H36 0.9500 . ? C37 C38 1.382(14) . ? C37 H37 0.9500 . ? C38 N6 1.352(12) . ? C38 H38 0.9500 . ? N3 Pd1 2.027(7) 2_666 ? N6 Pd1 2.016(7) 2_666 ? Sb1 F9 1.77(3) . ? Sb1 F7 1.79(4) . ? Sb1 F3 1.810(10) . ? Sb1 F10 1.82(3) . ? Sb1 F6 1.832(10) . ? Sb1 F5 1.848(10) . ? Sb1 F4 1.851(7) . ? Sb1 F1 1.855(6) . ? Sb1 F2 1.872(6) . ? Sb1 F8 1.87(4) . ? Sb2 F15 1.851(6) . ? Sb2 F11 1.854(6) . ? Sb2 F14 1.868(6) . ? Sb2 F16 1.870(6) . ? Sb2 F12 1.878(5) . ? Sb2 F13 1.886(6) . ? O50 H50X 0.8648 . ? O50 H50Y 0.8636 . ? O51 H51X 0.8634 . ? O51 H51Y 0.8584 . ? O52 H52X 0.8646 . ? O52 H52Y 0.8637 . ? O53 H53X 0.8650 . ? O53 H53Y 0.8629 . ? O60 C60 1.194(13) . ? C60 C61 1.435(17) . ? C60 C62 1.540(18) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O70 C70 1.406(15) . ? O70 H70X 0.8653 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? O80 C80 1.24(3) . ? O80 H80X 0.8596 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? O90 C90 1.35(4) . ? O90 H90X 0.8820 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? O100 C100 1.22(4) . ? O100 H100 0.8824 . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? O110 C110 1.41(4) . ? O110 H110 0.8695 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C110 H120 0.1597 . ? O120 C120 1.26(5) . ? O120 H120 0.9163 . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? O130 C130 1.34(6) . ? O130 H130 0.9637 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? 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 N6 Pd1 N1 91.5(3) 2_666 . ? N6 Pd1 N4 178.3(3) 2_666 . ? N1 Pd1 N4 88.8(3) . . ? N6 Pd1 N3 88.4(3) 2_666 2_666 ? N1 Pd1 N3 179.8(3) . 2_666 ? N4 Pd1 N3 91.3(3) . 2_666 ? C2 C1 N1 121.9(9) . . ? C2 C1 H1 119.0 . . ? N1 C1 H1 119.0 . . ? C1 C2 C3 119.7(9) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 118.7(9) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.0(9) . . ? C5 C4 C6 119.7(9) . . ? C3 C4 C6 121.3(9) . . ? N1 C5 C4 121.4(8) . . ? N1 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C7 C6 C4 178.2(13) . . ? C6 C7 C8 178.8(12) . . ? N2 C8 C9 122.7(10) . . ? N2 C8 C7 116.1(10) . . ? C9 C8 C7 121.2(11) . . ? C8 C9 C10 117.9(12) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? C11 C10 C9 121.1(12) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 116.9(11) . . ? C10 C11 H11 121.6 . . ? C12 C11 H11 121.6 . . ? N2 C12 C11 123.7(9) . . ? N2 C12 C13 117.1(9) . . ? C11 C12 C13 119.2(10) . . ? C14 C13 C12 178.9(13) . . ? C13 C14 C15 177.1(11) . . ? C17 C15 C16 118.3(8) . . ? C17 C15 C14 121.7(9) . . ? C16 C15 C14 119.9(9) . . ? N3 C16 C15 121.0(8) . . ? N3 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C18 C17 C15 120.3(9) . . ? C18 C17 H17 119.9 . . ? C15 C17 H17 119.9 . . ? C17 C18 C19 118.5(9) . . ? C17 C18 H18 120.8 . . ? C19 C18 H18 120.8 . . ? N3 C19 C18 122.6(9) . . ? N3 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? N4 C20 C21 122.0(9) . . ? N4 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C22 118.7(9) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C21 C22 C23 119.9(9) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 118.6(9) . . ? C24 C23 C25 118.8(8) . . ? C22 C23 C25 122.6(9) . . ? N4 C24 C23 122.0(8) . . ? N4 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C26 C25 C23 177.5(10) . . ? C25 C26 C27 178.4(10) . . ? N5 C27 C28 123.6(9) . . ? N5 C27 C26 115.5(8) . . ? C28 C27 C26 120.9(9) . . ? C27 C28 C29 117.6(9) . . ? C27 C28 H28 121.2 . . ? C29 C28 H28 121.2 . . ? C30 C29 C28 120.7(9) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 117.5(9) . . ? C29 C30 H30 121.3 . . ? C31 C30 H30 121.3 . . ? N5 C31 C30 124.2(9) . . ? N5 C31 C32 116.4(8) . . ? C30 C31 C32 119.2(9) . . ? C33 C32 C31 177.0(10) . . ? C32 C33 C34 176.8(11) . . ? C36 C34 C35 118.6(9) . . ? C36 C34 C33 121.0(9) . . ? C35 C34 C33 120.3(8) . . ? N6 C35 C34 122.3(9) . . ? N6 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C37 C36 C34 119.2(9) . . ? C37 C36 H36 120.4 . . ? C34 C36 H36 120.4 . . ? C36 C37 C38 119.8(9) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? N6 C38 C37 121.0(9) . . ? N6 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C5 N1 C1 119.3(8) . . ? C5 N1 Pd1 119.7(6) . . ? C1 N1 Pd1 121.0(6) . . ? C12 N2 C8 117.7(9) . . ? C19 N3 C16 119.3(8) . . ? C19 N3 Pd1 119.3(6) . 2_666 ? C16 N3 Pd1 121.3(6) . 2_666 ? C24 N4 C20 118.9(8) . . ? C24 N4 Pd1 120.9(6) . . ? C20 N4 Pd1 120.1(6) . . ? C31 N5 C27 116.4(8) . . ? C35 N6 C38 119.0(8) . . ? C35 N6 Pd1 121.5(6) . 2_666 ? C38 N6 Pd1 119.4(6) . 2_666 ? F9 Sb1 F7 88(2) . . ? F9 Sb1 F3 129.1(14) . . ? F7 Sb1 F3 142.6(18) . . ? F9 Sb1 F10 88.6(18) . . ? F7 Sb1 F10 177(2) . . ? F3 Sb1 F10 40.6(12) . . ? F9 Sb1 F6 136.4(14) . . ? F7 Sb1 F6 48.4(16) . . ? F3 Sb1 F6 94.3(8) . . ? F10 Sb1 F6 134.8(14) . . ? F9 Sb1 F5 45.1(13) . . ? F7 Sb1 F5 43.2(16) . . ? F3 Sb1 F5 174.1(7) . . ? F10 Sb1 F5 133.7(14) . . ? F6 Sb1 F5 91.3(7) . . ? F9 Sb1 F4 41.2(12) . . ? F7 Sb1 F4 129.5(17) . . ? F3 Sb1 F4 88.0(6) . . ? F10 Sb1 F4 47.4(13) . . ? F6 Sb1 F4 175.9(5) . . ? F5 Sb1 F4 86.3(6) . . ? F9 Sb1 F1 91.6(6) . . ? F7 Sb1 F1 90.2(6) . . ? F3 Sb1 F1 89.1(3) . . ? F10 Sb1 F1 91.3(5) . . ? F6 Sb1 F1 84.8(4) . . ? F5 Sb1 F1 89.6(3) . . ? F4 Sb1 F1 91.7(3) . . ? F9 Sb1 F2 89.2(6) . . ? F7 Sb1 F2 88.5(6) . . ? F3 Sb1 F2 91.5(4) . . ? F10 Sb1 F2 90.0(6) . . ? F6 Sb1 F2 93.7(4) . . ? F5 Sb1 F2 90.0(4) . . ? F4 Sb1 F2 89.7(3) . . ? F1 Sb1 F2 178.5(3) . . ? F9 Sb1 F8 179.0(8) . . ? F7 Sb1 F8 92(2) . . ? F3 Sb1 F8 50.8(14) . . ? F10 Sb1 F8 91.4(19) . . ? F6 Sb1 F8 43.7(13) . . ? F5 Sb1 F8 134.9(15) . . ? F4 Sb1 F8 138.8(15) . . ? F1 Sb1 F8 89.4(6) . . ? F2 Sb1 F8 89.9(6) . . ? F15 Sb2 F11 178.6(3) . . ? F15 Sb2 F14 89.6(3) . . ? F11 Sb2 F14 90.1(3) . . ? F15 Sb2 F16 91.5(3) . . ? F11 Sb2 F16 88.8(3) . . ? F14 Sb2 F16 177.9(3) . . ? F15 Sb2 F12 89.4(3) . . ? F11 Sb2 F12 89.3(3) . . ? F14 Sb2 F12 89.4(3) . . ? F16 Sb2 F12 88.8(2) . . ? F15 Sb2 F13 90.5(3) . . ? F11 Sb2 F13 90.8(3) . . ? F14 Sb2 F13 91.7(3) . . ? F16 Sb2 F13 90.2(3) . . ? F12 Sb2 F13 178.9(3) . . ? H50X O50 H50Y 98.8 . . ? H51X O51 H51Y 110.2 . . ? H52X O52 H52Y 101.6 . . ? H53X O53 H53Y 101.0 . . ? O60 C60 C61 120.9(13) . . ? O60 C60 C62 119.3(12) . . ? C61 C60 C62 119.8(12) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C70 O70 H70X 122.6 . . ? O70 C70 H70A 109.5 . . ? O70 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O70 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C80 O80 H80X 111.0 . . ? O80 C80 H80A 109.5 . . ? O80 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O80 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C90 O90 H90X 119.0 . . ? O90 C90 H90A 109.5 . . ? O90 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? O90 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C100 O100 H100 117.3 . . ? O100 C100 H10A 109.5 . . ? O100 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? O100 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C110 O110 H110 117.1 . . ? O110 C110 H120 130.5 . . ? H11A C110 H120 43.7 . . ? H11B C110 H120 118.5 . . ? H11C C110 H120 66.3 . . ? C120 O120 H120 110.6 . . ? O120 C120 H12A 109.5 . . ? O120 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? O120 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? C130 O130 H130 109.6 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 20.68 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.144 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.133 # Attachment 'jl32.cif' data_jl_merged _database_code_depnum_ccdc_archive 'CCDC 853227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H56 Cl4 N16 Pd2 Pt2' _chemical_formula_weight 1938.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pt Pt -1.7033 8.3905 '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 11.9663(19) _cell_length_b 12.3450(19) _cell_length_c 17.495(3) _cell_angle_alpha 76.455(9) _cell_angle_beta 83.846(10) _cell_angle_gamma 85.135(10) _cell_volume 2493.3(7) _cell_formula_units_Z 1 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 7324 _cell_measurement_theta_min 2.340 _cell_measurement_theta_max 22.333 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 3.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4183 _exptl_absorpt_correction_T_max 0.4278 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53506 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 26.47 _reflns_number_total 10143 _reflns_number_gt 7248 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1493P)^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 10143 _refine_ls_number_parameters 454 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2379 _refine_ls_wR_factor_gt 0.2226 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd -0.11598(6) -0.23178(7) 0.82641(4) 0.0359(2) Uani 1 1 d . . . C1 C 0.0868(11) -0.3293(13) 0.9024(7) 0.067(4) Uani 1 1 d U . . H1 H 0.0347 -0.3416 0.9480 0.080 Uiso 1 1 calc R . . C2 C 0.2021(11) -0.3660(14) 0.9104(8) 0.074(4) Uani 1 1 d U . . H2 H 0.2256 -0.4100 0.9589 0.089 Uiso 1 1 calc R . . C3 C 0.2757(9) -0.3363(12) 0.8476(7) 0.058(3) Uani 1 1 d U . . H3 H 0.3540 -0.3526 0.8522 0.069 Uiso 1 1 calc R . . C4 C 0.2379(8) -0.2817(8) 0.7757(6) 0.035(2) Uani 1 1 d . . . C5 C 0.1246(8) -0.2529(8) 0.7720(6) 0.032(2) Uani 1 1 d . . . H5 H 0.0989 -0.2128 0.7231 0.039 Uiso 1 1 calc R . . C6 C 0.3174(8) -0.2541(9) 0.7054(5) 0.031(2) Uani 1 1 d . . . C7 C 0.3857(8) -0.2388(9) 0.6519(6) 0.035(2) Uani 1 1 d . . . C8 C 0.4734(8) -0.2157(8) 0.5886(6) 0.031(2) Uani 1 1 d . . . C9 C 0.5817(8) -0.2618(8) 0.5988(6) 0.035(2) Uani 1 1 d . . . H9 H 0.6003 -0.3109 0.6469 0.042 Uiso 1 1 calc R . . C10 C 0.6651(8) -0.2317(9) 0.5329(6) 0.036(2) Uani 1 1 d . . . H10 H 0.7411 -0.2593 0.5378 0.044 Uiso 1 1 calc R . . C11 C 0.6356(8) -0.1639(8) 0.4636(6) 0.036(2) Uani 1 1 d . . . H11 H 0.6897 -0.1450 0.4195 0.043 Uiso 1 1 calc R . . C12 C 0.5220(8) -0.1226(8) 0.4594(5) 0.029(2) Uani 1 1 d . . . C13 C 0.4891(8) -0.0487(9) 0.3868(7) 0.040(3) Uani 1 1 d . . . C14 C 0.4622(8) 0.0110(9) 0.3281(6) 0.037(2) Uani 1 1 d . . . C15 C 0.4304(8) 0.0860(8) 0.2569(6) 0.035(2) Uani 1 1 d . . . C16 C 0.5083(9) 0.1298(11) 0.1938(7) 0.057(3) Uani 1 1 d . . . H16 H 0.5861 0.1082 0.1966 0.068 Uiso 1 1 calc R . . C17 C 0.4735(11) 0.2024(13) 0.1294(8) 0.067(4) Uani 1 1 d . . . H17 H 0.5265 0.2364 0.0882 0.081 Uiso 1 1 calc R . . C18 C 0.3618(9) 0.2263(11) 0.1242(7) 0.054(3) Uani 1 1 d . . . H18 H 0.3384 0.2742 0.0771 0.065 Uiso 1 1 calc R . . C19 C 0.3159(8) 0.1148(8) 0.2488(6) 0.033(2) Uani 1 1 d . . . H19 H 0.2616 0.0843 0.2903 0.039 Uiso 1 1 calc R . . N1 N 0.0503(7) -0.2790(8) 0.8341(5) 0.042(2) Uani 1 1 d . . . N2 N 0.4435(6) -0.1478(7) 0.5192(5) 0.0316(18) Uani 1 1 d . . . N3 N 0.2810(7) 0.1860(7) 0.1823(5) 0.0372(19) Uani 1 1 d . . . C21 C -0.1161(10) -0.0647(10) 0.9174(7) 0.053(3) Uani 1 1 d . . . H21 H -0.1467 -0.1235 0.9574 0.063 Uiso 1 1 calc R . . C22 C -0.0997(12) 0.0346(13) 0.9367(8) 0.070(4) Uani 1 1 d . . . H22 H -0.1154 0.0441 0.9892 0.084 Uiso 1 1 calc R . . C23 C -0.0592(10) 0.1193(10) 0.8763(8) 0.054(3) Uani 1 1 d . . . H23 H -0.0509 0.1898 0.8873 0.064 Uiso 1 1 calc R . . C24 C -0.0315(9) 0.1059(10) 0.8031(6) 0.043(3) Uani 1 1 d . . . C25 C -0.0509(8) 0.0024(9) 0.7879(7) 0.040(2) Uani 1 1 d . . . H25 H -0.0354 -0.0087 0.7358 0.048 Uiso 1 1 calc R . . C26 C 0.0103(9) 0.1925(9) 0.7399(6) 0.041(2) Uani 1 1 d . . . C27 C 0.0471(9) 0.2713(9) 0.6934(6) 0.040(2) Uani 1 1 d . . . C28 C 0.0950(9) 0.3731(8) 0.6420(6) 0.037(2) Uani 1 1 d . . . C29 C 0.1251(11) 0.4579(10) 0.6776(7) 0.054(3) Uani 1 1 d . . . H29 H 0.1157 0.4498 0.7333 0.065 Uiso 1 1 calc R . . C30 C 0.1667(12) 0.5485(11) 0.6303(8) 0.060(4) Uani 1 1 d . . . H30 H 0.1897 0.6056 0.6523 0.072 Uiso 1 1 calc R . . C31 C 0.1769(11) 0.5607(9) 0.5507(8) 0.053(3) Uani 1 1 d . . . H31 H 0.2040 0.6267 0.5165 0.063 Uiso 1 1 calc R . . C32 C 0.1462(8) 0.4730(8) 0.5206(6) 0.034(2) Uani 1 1 d . . . C33 C 0.1583(10) 0.4858(9) 0.4362(7) 0.045(3) Uani 1 1 d . . . C34 C 0.1616(10) 0.4951(10) 0.3669(7) 0.046(3) Uani 1 1 d . . . C35 C 0.1654(9) 0.4933(11) 0.2863(7) 0.047(3) Uani 1 1 d . . . C36 C 0.1878(15) 0.5845(11) 0.2213(8) 0.077(5) Uani 1 1 d . . . H36 H 0.2013 0.6551 0.2302 0.092 Uiso 1 1 calc R . . C37 C 0.1898(13) 0.5710(10) 0.1483(7) 0.065(4) Uani 1 1 d . . . H37 H 0.2068 0.6321 0.1053 0.078 Uiso 1 1 calc R . . C38 C 0.1692(11) 0.4763(10) 0.1336(6) 0.053(3) Uani 1 1 d . . . H38 H 0.1732 0.4705 0.0802 0.064 Uiso 1 1 calc R . . C39 C 0.1436(9) 0.4014(11) 0.2662(6) 0.050(3) Uani 1 1 d . . . H39 H 0.1271 0.3395 0.3086 0.059 Uiso 1 1 calc R . . N21 N -0.0911(7) -0.0811(7) 0.8458(5) 0.039(2) Uani 1 1 d . . . N22 N 0.1033(7) 0.3796(6) 0.5663(5) 0.0294(17) Uani 1 1 d . . . N23 N 0.1418(7) 0.3837(8) 0.1926(5) 0.039(2) Uani 1 1 d . . . Pt50 Pt 0.08567(3) -0.10681(3) 0.53918(2) 0.03839(18) Uani 1 1 d . . . Cl50 Cl 0.1502(2) -0.0146(2) 0.62492(15) 0.0430(6) Uani 1 1 d . . . Cl51 Cl -0.0761(2) -0.1529(2) 0.62132(15) 0.0428(6) Uani 1 1 d . . . N50 N 0.2276(7) -0.0625(7) 0.4668(5) 0.039(2) Uani 1 1 d . . . H50A H 0.2207 -0.0746 0.4183 0.047 Uiso 1 1 calc R . . H50B H 0.2883 -0.1043 0.4875 0.047 Uiso 1 1 calc R . . H50C H 0.2373 0.0111 0.4624 0.047 Uiso 1 1 calc R . . N51 N 0.0283(8) -0.1843(7) 0.4581(5) 0.043(2) Uani 1 1 d . . . H51A H -0.0244 -0.1381 0.4308 0.051 Uiso 1 1 calc R . . H51B H -0.0027 -0.2490 0.4842 0.051 Uiso 1 1 calc R . . H51C H 0.0871 -0.1995 0.4239 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0191(4) 0.0519(5) 0.0236(4) 0.0157(3) -0.0009(3) 0.0025(3) C1 0.040(7) 0.107(10) 0.032(6) 0.023(6) 0.005(5) 0.002(7) C2 0.046(7) 0.117(11) 0.038(7) 0.016(7) -0.014(6) 0.028(7) C3 0.021(5) 0.101(9) 0.039(6) 0.002(6) -0.006(5) 0.017(6) C4 0.032(5) 0.044(5) 0.026(5) -0.002(4) -0.008(4) 0.001(4) C5 0.031(5) 0.041(5) 0.021(5) -0.003(4) 0.000(4) 0.003(4) C6 0.021(5) 0.057(6) 0.018(5) -0.011(4) -0.006(4) -0.003(4) C7 0.028(5) 0.046(6) 0.034(6) -0.010(5) -0.008(5) -0.008(4) C8 0.030(5) 0.032(5) 0.030(5) -0.010(4) -0.003(4) 0.001(4) C9 0.032(5) 0.042(5) 0.029(5) -0.005(4) -0.006(4) 0.004(4) C10 0.027(5) 0.046(6) 0.033(5) -0.009(5) -0.001(4) 0.012(4) C11 0.025(5) 0.038(5) 0.041(6) -0.009(5) 0.002(4) 0.007(4) C12 0.028(5) 0.035(5) 0.026(5) -0.007(4) -0.004(4) 0.002(4) C13 0.015(5) 0.056(6) 0.050(7) -0.023(6) 0.009(4) 0.003(4) C14 0.024(5) 0.046(6) 0.037(6) -0.002(5) -0.010(4) 0.008(4) C15 0.023(5) 0.042(5) 0.033(5) 0.003(4) -0.001(4) 0.006(4) C16 0.024(6) 0.073(8) 0.055(8) 0.012(6) 0.000(5) 0.017(5) C17 0.048(8) 0.100(11) 0.041(7) 0.005(7) 0.016(6) -0.011(7) C18 0.027(6) 0.080(8) 0.037(6) 0.016(6) 0.005(5) 0.011(6) C19 0.022(5) 0.038(5) 0.040(6) -0.013(4) -0.001(4) -0.001(4) N1 0.022(4) 0.068(6) 0.024(4) 0.013(4) -0.004(3) 0.004(4) N2 0.022(4) 0.036(4) 0.038(5) -0.012(4) -0.009(3) 0.006(3) N3 0.032(5) 0.046(5) 0.025(4) 0.009(4) -0.004(3) -0.003(4) C21 0.045(7) 0.056(7) 0.045(7) 0.018(6) -0.009(5) -0.010(6) C22 0.067(9) 0.100(11) 0.039(7) 0.004(7) -0.019(6) -0.018(8) C23 0.045(7) 0.056(7) 0.059(8) 0.001(6) -0.024(6) -0.015(6) C24 0.027(5) 0.067(7) 0.027(6) 0.008(5) -0.009(4) 0.003(5) C25 0.026(5) 0.045(6) 0.039(6) 0.014(5) -0.006(4) -0.004(4) C26 0.040(6) 0.046(6) 0.038(6) -0.006(5) -0.013(5) -0.005(5) C27 0.048(7) 0.043(6) 0.030(6) -0.005(5) -0.016(5) -0.004(5) C28 0.041(6) 0.035(5) 0.035(6) -0.002(4) -0.016(5) -0.005(4) C29 0.070(8) 0.064(7) 0.040(7) -0.029(6) -0.015(6) -0.015(7) C30 0.075(9) 0.058(7) 0.058(8) -0.032(7) 0.001(7) -0.029(7) C31 0.067(8) 0.033(5) 0.057(8) -0.004(5) 0.000(6) -0.017(5) C32 0.038(6) 0.033(5) 0.031(5) -0.005(4) -0.012(4) 0.004(4) C33 0.045(7) 0.037(5) 0.045(7) 0.002(5) -0.010(5) 0.010(5) C34 0.039(6) 0.052(6) 0.039(7) 0.004(5) -0.002(5) 0.010(5) C35 0.033(6) 0.063(7) 0.042(7) -0.016(6) 0.004(5) 0.008(5) C36 0.121(13) 0.051(7) 0.040(7) 0.001(6) 0.011(8) 0.039(8) C37 0.111(12) 0.038(6) 0.029(6) 0.009(5) 0.009(7) 0.026(7) C38 0.066(8) 0.054(7) 0.023(6) 0.015(5) 0.004(5) 0.011(6) C39 0.024(6) 0.077(8) 0.028(6) 0.023(6) -0.001(4) 0.006(5) N21 0.030(5) 0.049(5) 0.030(5) 0.011(4) -0.010(4) 0.001(4) N22 0.035(4) 0.031(4) 0.026(4) -0.011(3) -0.012(3) 0.006(3) N23 0.024(4) 0.063(6) 0.021(4) 0.006(4) -0.001(3) 0.012(4) Pt50 0.0377(3) 0.0430(3) 0.0325(3) -0.00294(18) -0.00835(18) -0.00092(18) Cl50 0.0457(15) 0.0513(15) 0.0323(13) -0.0061(12) -0.0096(11) -0.0071(12) Cl51 0.0382(14) 0.0498(14) 0.0334(13) 0.0046(11) -0.0037(11) -0.0031(11) N50 0.043(5) 0.034(4) 0.036(5) -0.001(4) -0.015(4) 0.007(4) N51 0.058(6) 0.044(5) 0.023(4) -0.004(4) 0.004(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N21 2.018(9) . ? Pd1 N3 2.020(8) 2_556 ? Pd1 N23 2.034(10) 2_556 ? Pd1 N1 2.035(8) . ? C1 N1 1.313(14) . ? C1 C2 1.426(18) . ? C1 H1 0.9500 . ? C2 C3 1.333(17) . ? C2 H2 0.9500 . ? C3 C4 1.383(14) . ? C3 H3 0.9500 . ? C4 C5 1.377(14) . ? C4 C6 1.464(14) . ? C5 N1 1.323(12) . ? C5 H5 0.9500 . ? C6 C7 1.165(13) . ? C7 C8 1.437(14) . ? C8 N2 1.368(12) . ? C8 C9 1.384(14) . ? C9 C10 1.442(14) . ? C9 H9 0.9500 . ? C10 C11 1.365(14) . ? C10 H10 0.9500 . ? C11 C12 1.414(13) . ? C11 H11 0.9500 . ? C12 N2 1.326(12) . ? C12 C13 1.451(15) . ? C13 C14 1.174(15) . ? C14 C15 1.435(14) . ? C15 C19 1.400(13) . ? C15 C16 1.401(15) . ? C16 C17 1.346(18) . ? C16 H16 0.9500 . ? C17 C18 1.351(17) . ? C17 H17 0.9500 . ? C18 N3 1.360(13) . ? C18 H18 0.9500 . ? C19 N3 1.365(13) . ? C19 H19 0.9500 . ? N3 Pd1 2.020(8) 2_556 ? C21 N21 1.315(15) . ? C21 C22 1.38(2) . ? C21 H21 0.9500 . ? C22 C23 1.380(17) . ? C22 H22 0.9500 . ? C23 C24 1.333(17) . ? C23 H23 0.9500 . ? C24 C25 1.407(16) . ? C24 C26 1.425(15) . ? C25 N21 1.346(12) . ? C25 H25 0.9500 . ? C26 C27 1.194(14) . ? C27 C28 1.483(14) . ? C28 N22 1.301(13) . ? C28 C29 1.426(14) . ? C29 C30 1.326(17) . ? C29 H29 0.9500 . ? C30 C31 1.358(17) . ? C30 H30 0.9500 . ? C31 C32 1.400(14) . ? C31 H31 0.9500 . ? C32 N22 1.347(12) . ? C32 C33 1.441(15) . ? C33 C34 1.188(16) . ? C34 C35 1.411(16) . ? C35 C39 1.318(18) . ? C35 C36 1.421(17) . ? C36 C37 1.324(18) . ? C36 H36 0.9500 . ? C37 C38 1.302(18) . ? C37 H37 0.9500 . ? C38 N23 1.385(13) . ? C38 H38 0.9500 . ? C39 N23 1.357(15) . ? C39 H39 0.9500 . ? N23 Pd1 2.034(10) 2_556 ? Pt50 N50 2.039(9) . ? Pt50 N51 2.086(9) . ? Pt50 Cl50 2.311(3) . ? Pt50 Cl51 2.311(3) . ? N50 H50A 0.9100 . ? N50 H50B 0.9100 . ? N50 H50C 0.9100 . ? N51 H51A 0.9100 . ? N51 H51B 0.9100 . ? N51 H51C 0.9100 . ? 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 N21 Pd1 N3 89.8(3) . 2_556 ? N21 Pd1 N23 179.7(3) . 2_556 ? N3 Pd1 N23 90.0(3) 2_556 2_556 ? N21 Pd1 N1 90.8(4) . . ? N3 Pd1 N1 179.3(4) 2_556 . ? N23 Pd1 N1 89.4(4) 2_556 . ? N1 C1 C2 122.2(11) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 117.7(11) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 119.9(10) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 118.7(9) . . ? C5 C4 C6 120.8(9) . . ? C3 C4 C6 120.5(9) . . ? N1 C5 C4 122.3(9) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C7 C6 C4 174.9(11) . . ? C6 C7 C8 176.3(10) . . ? N2 C8 C9 122.8(9) . . ? N2 C8 C7 116.7(9) . . ? C9 C8 C7 120.4(9) . . ? C8 C9 C10 116.7(9) . . ? C8 C9 H9 121.6 . . ? C10 C9 H9 121.6 . . ? C11 C10 C9 120.6(9) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 117.9(9) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? N2 C12 C11 123.1(9) . . ? N2 C12 C13 118.1(8) . . ? C11 C12 C13 118.9(9) . . ? C14 C13 C12 179.8(13) . . ? C13 C14 C15 178.7(12) . . ? C19 C15 C16 118.2(9) . . ? C19 C15 C14 118.6(9) . . ? C16 C15 C14 123.2(9) . . ? C17 C16 C15 120.4(11) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 118.9(11) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 N3 124.1(11) . . ? C17 C18 H18 117.9 . . ? N3 C18 H18 117.9 . . ? N3 C19 C15 121.0(9) . . ? N3 C19 H19 119.5 . . ? C15 C19 H19 119.5 . . ? C1 N1 C5 118.7(9) . . ? C1 N1 Pd1 120.2(7) . . ? C5 N1 Pd1 121.0(6) . . ? C12 N2 C8 118.9(8) . . ? C18 N3 C19 117.3(9) . . ? C18 N3 Pd1 122.2(7) . 2_556 ? C19 N3 Pd1 120.5(6) . 2_556 ? N21 C21 C22 122.6(11) . . ? N21 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C23 C22 C21 116.9(13) . . ? C23 C22 H22 121.6 . . ? C21 C22 H22 121.6 . . ? C24 C23 C22 122.5(12) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C23 C24 C25 117.2(10) . . ? C23 C24 C26 123.3(11) . . ? C25 C24 C26 119.5(10) . . ? N21 C25 C24 121.3(10) . . ? N21 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C27 C26 C24 172.6(11) . . ? C26 C27 C28 174.7(10) . . ? N22 C28 C29 124.6(10) . . ? N22 C28 C27 116.7(8) . . ? C29 C28 C27 118.7(10) . . ? C30 C29 C28 117.5(10) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C29 C30 C31 120.8(10) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 118.0(10) . . ? C30 C31 H31 121.0 . . ? C32 C31 H31 121.0 . . ? N22 C32 C31 123.4(9) . . ? N22 C32 C33 118.8(8) . . ? C31 C32 C33 117.8(10) . . ? C34 C33 C32 176.1(12) . . ? C33 C34 C35 173.8(13) . . ? C39 C35 C34 119.6(11) . . ? C39 C35 C36 114.2(11) . . ? C34 C35 C36 126.2(12) . . ? C37 C36 C35 119.9(14) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 121.9(12) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 N23 122.7(11) . . ? C37 C38 H38 118.6 . . ? N23 C38 H38 118.6 . . ? C35 C39 N23 128.3(11) . . ? C35 C39 H39 115.8 . . ? N23 C39 H39 115.8 . . ? C21 N21 C25 119.5(10) . . ? C21 N21 Pd1 118.4(7) . . ? C25 N21 Pd1 122.2(8) . . ? C28 N22 C32 115.7(8) . . ? C39 N23 C38 112.9(10) . . ? C39 N23 Pd1 122.4(8) . 2_556 ? C38 N23 Pd1 124.5(7) . 2_556 ? N50 Pt50 N51 91.7(3) . . ? N50 Pt50 Cl50 86.9(3) . . ? N51 Pt50 Cl50 177.7(2) . . ? N50 Pt50 Cl51 178.7(2) . . ? N51 Pt50 Cl51 89.1(3) . . ? Cl50 Pt50 Cl51 92.36(10) . . ? Pt50 N50 H50A 109.5 . . ? Pt50 N50 H50B 109.5 . . ? H50A N50 H50B 109.5 . . ? Pt50 N50 H50C 109.5 . . ? H50A N50 H50C 109.5 . . ? H50B N50 H50C 109.5 . . ? Pt50 N51 H51A 109.5 . . ? Pt50 N51 H51B 109.5 . . ? H51A N51 H51B 109.5 . . ? Pt50 N51 H51C 109.5 . . ? H51A N51 H51C 109.5 . . ? H51B N51 H51C 109.5 . . ? 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 C1 C2 C3 8(3) . . . . ? C1 C2 C3 C4 -6(2) . . . . ? C2 C3 C4 C5 4(2) . . . . ? C2 C3 C4 C6 -176.7(14) . . . . ? C3 C4 C5 N1 -2.5(17) . . . . ? C6 C4 C5 N1 178.4(10) . . . . ? C5 C4 C6 C7 -153(11) . . . . ? C3 C4 C6 C7 28(12) . . . . ? C4 C6 C7 C8 -89(23) . . . . ? C6 C7 C8 N2 -110(18) . . . . ? C6 C7 C8 C9 71(18) . . . . ? N2 C8 C9 C10 2.3(14) . . . . ? C7 C8 C9 C10 -178.4(9) . . . . ? C8 C9 C10 C11 -2.2(15) . . . . ? C9 C10 C11 C12 1.4(15) . . . . ? C10 C11 C12 N2 -0.7(15) . . . . ? C10 C11 C12 C13 178.9(9) . . . . ? N2 C12 C13 C14 -19(100) . . . . ? C11 C12 C13 C14 161(100) . . . . ? C12 C13 C14 C15 122(100) . . . . ? C13 C14 C15 C19 -112(52) . . . . ? C13 C14 C15 C16 70(52) . . . . ? C19 C15 C16 C17 3.6(19) . . . . ? C14 C15 C16 C17 -178.1(13) . . . . ? C15 C16 C17 C18 -5(2) . . . . ? C16 C17 C18 N3 4(2) . . . . ? C16 C15 C19 N3 -1.8(15) . . . . ? C14 C15 C19 N3 179.9(9) . . . . ? C2 C1 N1 C5 -6(2) . . . . ? C2 C1 N1 Pd1 178.7(12) . . . . ? C4 C5 N1 C1 3.5(17) . . . . ? C4 C5 N1 Pd1 178.7(8) . . . . ? N21 Pd1 N1 C1 90.5(11) . . . . ? N3 Pd1 N1 C1 -127(27) 2_556 . . . ? N23 Pd1 N1 C1 -89.2(11) 2_556 . . . ? N21 Pd1 N1 C5 -84.6(9) . . . . ? N3 Pd1 N1 C5 58(28) 2_556 . . . ? N23 Pd1 N1 C5 95.6(9) 2_556 . . . ? C11 C12 N2 C8 0.9(14) . . . . ? C13 C12 N2 C8 -178.7(8) . . . . ? C9 C8 N2 C12 -1.7(13) . . . . ? C7 C8 N2 C12 179.0(8) . . . . ? C17 C18 N3 C19 -1.7(19) . . . . ? C17 C18 N3 Pd1 176.4(11) . . . 2_556 ? C15 C19 N3 C18 0.8(15) . . . . ? C15 C19 N3 Pd1 -177.4(7) . . . 2_556 ? N21 C21 C22 C23 2.5(19) . . . . ? C21 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 C25 3.5(17) . . . . ? C22 C23 C24 C26 180.0(11) . . . . ? C23 C24 C25 N21 -2.9(15) . . . . ? C26 C24 C25 N21 -179.5(9) . . . . ? C23 C24 C26 C27 14(10) . . . . ? C25 C24 C26 C27 -170(9) . . . . ? C24 C26 C27 C28 6(21) . . . . ? C26 C27 C28 N22 176(13) . . . . ? C26 C27 C28 C29 -7(14) . . . . ? N22 C28 C29 C30 -1.6(19) . . . . ? C27 C28 C29 C30 -179.3(12) . . . . ? C28 C29 C30 C31 2(2) . . . . ? C29 C30 C31 C32 -2(2) . . . . ? C30 C31 C32 N22 2.6(18) . . . . ? C30 C31 C32 C33 -179.4(12) . . . . ? N22 C32 C33 C34 52(18) . . . . ? C31 C32 C33 C34 -126(17) . . . . ? C32 C33 C34 C35 -74(23) . . . . ? C33 C34 C35 C39 13(12) . . . . ? C33 C34 C35 C36 -169(11) . . . . ? C39 C35 C36 C37 -3(2) . . . . ? C34 C35 C36 C37 179.4(13) . . . . ? C35 C36 C37 C38 2(2) . . . . ? C36 C37 C38 N23 1(2) . . . . ? C34 C35 C39 N23 179.2(10) . . . . ? C36 C35 C39 N23 1.0(18) . . . . ? C22 C21 N21 C25 -2.0(17) . . . . ? C22 C21 N21 Pd1 178.5(10) . . . . ? C24 C25 N21 C21 2.2(15) . . . . ? C24 C25 N21 Pd1 -178.4(7) . . . . ? N3 Pd1 N21 C21 81.1(8) 2_556 . . . ? N23 Pd1 N21 C21 31(69) 2_556 . . . ? N1 Pd1 N21 C21 -99.3(8) . . . . ? N3 Pd1 N21 C25 -98.3(8) 2_556 . . . ? N23 Pd1 N21 C25 -148(68) 2_556 . . . ? N1 Pd1 N21 C25 81.2(8) . . . . ? C29 C28 N22 C32 1.8(15) . . . . ? C27 C28 N22 C32 179.5(9) . . . . ? C31 C32 N22 C28 -2.3(15) . . . . ? C33 C32 N22 C28 179.8(10) . . . . ? C35 C39 N23 C38 1.5(16) . . . . ? C35 C39 N23 Pd1 175.9(9) . . . 2_556 ? C37 C38 N23 C39 -2.6(17) . . . . ? C37 C38 N23 Pd1 -177.0(10) . . . 2_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N50 H50B N2 0.91 1.99 2.866(11) 161.2 . N50 H50C Cl51 0.91 2.79 3.256(8) 113.3 2_556 N51 H51A Cl50 0.91 2.40 3.287(10) 166.4 2_556 N51 H51B N22 0.91 2.46 3.122(11) 129.8 2_556 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 4.948 _refine_diff_density_min -1.483 _refine_diff_density_rms 0.243 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.238 0.923 908 374 ' ' _platon_squeeze_details ; Highly disordered tetrafluoroborate anions and solvent. The number of electrons is consistent with a number of combinations of solvent (H2O, DMF, Et2O and/or MeCN). ;