# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Carlos Peinador' _publ_contact_author_email carlos.peinador@udc.es loop_ _publ_author_name 'Cristina Alvarino' 'Alessio Terenzi' 'Victor Blanco' 'Marcos Garcia' 'Carlos Peinador' 'Jose Quintela' # Attachment '- inclusion_complex.cif' data_0942687_b2_0s-sr _database_code_depnum_ccdc_archive 'CCDC 883118' #TrackingRef '- inclusion_complex.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H44 F18 N7 O7 P3 Pd' _chemical_formula_weight 1264.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1541(4) _cell_length_b 14.5559(5) _cell_length_c 17.0550(5) _cell_angle_alpha 81.470(2) _cell_angle_beta 73.532(2) _cell_angle_gamma 66.056(2) _cell_volume 2642.58(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17582 _cell_measurement_theta_min 4.985 _cell_measurement_theta_max 53.340 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8507 _exptl_absorpt_correction_T_max 0.9311 _exptl_absorpt_process_details 'SADABS 2004/1 (Sheldrick, 2004)' _exptl_special_details ; Data was collected using a X8 APEX II BRUKER-NONIUS diffractometer. A suitable crystal was chosen and mounted with glue on a glass fiber. Data were measured using omega scans of 0.5\% per frame for 10 s with a final resolution of 0.75 \%A. Data integration and reduction were performed using the Apex2 Service v2010, 1-2 (BRUKER AXS) suite software. Absorption corrections were applied using SADABS (2008) of the suite software. The structures are solved by the direct method using the SHELX-XS Version 2008/1 program and refined by least squares method on F2 SHELXL Version 2008/4 , incorporated in the Apex2 suite software. ; _diffrn_ambient_temperature 100(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 'APEXII area detector' _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 69366 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.37 _reflns_number_total 13029 _reflns_number_gt 9826 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Apex2 V.1.0-27 (Bruker Nonius, 2005)' _computing_cell_refinement 'SAINT V7.12A in Apex2 suite.' _computing_data_reduction 'SAINT and XPREP Ver. 6.14 2003 Bruker-AXS' _computing_structure_solution 'SHELXS-97 in SHELXTL suite Ver. 6.12' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. DFIX and DANG restrictions were applied to correct wrong geometries on both nitromethane molecules and one of the PF6 counterions. The disorder on the terminal OH group and one CH2 in the ethylenediamine moiety was treated by splitting the atoms involved into two positions. The crystal lattice contains large voids filled with scattered electron density, the SQUEEZE protocol inside PLATON was used to remove the void electron density. ; _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^)+(0.1463P)^2^+4.0865P] 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 13029 _refine_ls_number_parameters 698 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2422 _refine_ls_wR_factor_gt 0.2267 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.003 _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 0.4114(5) 0.1559(4) 0.1540(3) 0.0481(12) Uani 1 1 d . . . H1 H 0.3794 0.1043 0.1673 0.058 Uiso 1 1 calc R . . C2 C 0.4993(5) 0.1535(4) 0.1912(4) 0.0514(13) Uani 1 1 d . . . H2 H 0.5269 0.1006 0.2297 0.062 Uiso 1 1 calc R . . C3 C 0.5478(4) 0.2270(3) 0.1733(3) 0.0385(10) Uani 1 1 d . . . C4 C 0.5059(5) 0.3011(4) 0.1146(3) 0.0501(12) Uani 1 1 d . . . H4 H 0.5377 0.3527 0.0990 0.060 Uiso 1 1 calc R . . C5 C 0.4187(5) 0.2988(4) 0.0796(3) 0.0502(12) Uani 1 1 d . . . H5 H 0.3918 0.3494 0.0393 0.060 Uiso 1 1 calc R . . C6 C 0.6367(4) 0.2315(4) 0.2167(3) 0.0449(11) Uani 1 1 d . . . H6A H 0.6896 0.2656 0.1807 0.054 Uiso 1 1 calc R . . H6B H 0.6913 0.1626 0.2303 0.054 Uiso 1 1 calc R . . C7 C 0.5636(4) 0.2891(4) 0.2945(3) 0.0400(10) Uani 1 1 d . . . C8 C 0.4940(5) 0.3920(4) 0.2894(3) 0.0446(11) Uani 1 1 d . . . H8 H 0.4987 0.4267 0.2375 0.054 Uiso 1 1 calc R . . C9 C 0.4179(4) 0.4446(4) 0.3593(3) 0.0408(10) Uani 1 1 d . . . H9 H 0.3704 0.5148 0.3557 0.049 Uiso 1 1 calc R . . C10 C 0.4126(4) 0.3924(4) 0.4346(3) 0.0374(9) Uani 1 1 d . . . C11 C 0.4831(5) 0.2905(4) 0.4412(3) 0.0456(11) Uani 1 1 d . . . H11 H 0.4804 0.2560 0.4931 0.055 Uiso 1 1 calc R . . C12 C 0.5578(5) 0.2397(4) 0.3702(3) 0.0473(11) Uani 1 1 d . . . H12 H 0.6057 0.1696 0.3739 0.057 Uiso 1 1 calc R . . C13 C 0.2609(4) 0.3973(4) 0.5619(3) 0.0365(9) Uani 1 1 d . . . H13 H 0.2730 0.3308 0.5525 0.044 Uiso 1 1 calc R . . C14 C 0.1770(4) 0.4433(4) 0.6313(3) 0.0368(9) Uani 1 1 d . . . C15 C 0.1567(4) 0.5434(3) 0.6417(3) 0.0335(8) Uani 1 1 d . . . C16 C 0.2244(4) 0.5930(4) 0.5838(3) 0.0386(9) Uani 1 1 d . . . C17 C 0.3106(4) 0.5405(4) 0.5160(3) 0.0382(9) Uani 1 1 d . . . H17 H 0.3583 0.5718 0.4764 0.046 Uiso 1 1 calc R . . C18 C 0.1088(4) 0.3933(4) 0.6914(3) 0.0402(10) Uani 1 1 d . . . H18 H 0.1236 0.3252 0.6849 0.048 Uiso 1 1 calc R . . C19 C 0.0235(5) 0.4425(4) 0.7571(3) 0.0434(11) Uani 1 1 d . . . H19 H -0.0213 0.4085 0.7963 0.052 Uiso 1 1 calc R . . C20 C -0.0007(4) 0.5448(4) 0.7689(3) 0.0379(9) Uani 1 1 d . . . C21 C 0.0662(4) 0.5959(3) 0.7104(3) 0.0361(9) Uani 1 1 d . . . C22 C 0.2005(5) 0.6965(4) 0.5950(3) 0.0462(11) Uani 1 1 d . . . H22 H 0.2453 0.7303 0.5557 0.055 Uiso 1 1 calc R . . C23 C 0.1149(5) 0.7454(4) 0.6609(3) 0.0474(12) Uani 1 1 d . . . H23 H 0.1009 0.8133 0.6675 0.057 Uiso 1 1 calc R . . C24 C 0.0444(4) 0.6963(4) 0.7214(3) 0.0400(10) Uani 1 1 d . . . C25 C -0.0443(5) 0.7422(4) 0.7904(3) 0.0440(11) Uani 1 1 d . . . H25 H -0.0620 0.8104 0.7987 0.053 Uiso 1 1 calc R . . C26 C -0.0863(4) 0.5978(4) 0.8352(3) 0.0421(10) Uani 1 1 d . . . H26 H -0.1329 0.5655 0.8747 0.051 Uiso 1 1 calc R . . C27 C -0.1246(6) 0.5487(7) 0.5956(5) 0.072(2) Uani 1 1 d . . . H27 H -0.1742 0.5247 0.6405 0.086 Uiso 1 1 calc R . . C28 C -0.1374(7) 0.6455(7) 0.5916(5) 0.078(2) Uani 1 1 d . . . H28 H -0.1961 0.6881 0.6342 0.094 Uiso 1 1 calc R . . C29 C -0.0681(7) 0.6852(7) 0.5275(5) 0.078(2) Uani 1 1 d . . . H29 H -0.0807 0.7543 0.5254 0.094 Uiso 1 1 calc R . . C30 C 0.0218(6) 0.6209(6) 0.4651(5) 0.072(2) Uani 1 1 d . . . C31 C 0.0360(6) 0.5195(6) 0.4677(4) 0.070(2) Uani 1 1 d . . . C32 C 0.0865(8) 0.7500(7) 0.3962(6) 0.093(3) Uani 1 1 d . . . H32A H 0.0953 0.7687 0.4470 0.112 Uiso 1 1 calc R . . H32B H 0.0040 0.7950 0.3875 0.112 Uiso 1 1 calc R . . C33 C 0.1891(8) 0.7591(9) 0.3236(7) 0.112(4) Uani 1 1 d . D . H33A H 0.1975 0.7212 0.2771 0.134 Uiso 1 1 calc R . . H33B H 0.1713 0.8304 0.3055 0.134 Uiso 1 1 calc R . . C34 C 0.4033(6) 0.7180(6) 0.2866(4) 0.0726(19) Uani 1 1 d D D . H34A H 0.3857 0.7863 0.2607 0.087 Uiso 1 1 calc R . . H34B H 0.4198 0.6707 0.2446 0.087 Uiso 1 1 calc R . . C35 C 0.5106(7) 0.6873(5) 0.3216(4) 0.077(2) Uani 1 1 d D . . H35A H 0.5826 0.6906 0.2777 0.093 Uiso 1 1 calc R A 1 H35B H 0.4920 0.7361 0.3630 0.093 Uiso 1 1 calc R A 1 C36 C -0.0677(8) 0.9828(8) 0.1231(7) 0.102(3) Uani 1 1 d . . . H36A H -0.0322 0.9355 0.1651 0.153 Uiso 1 1 calc R . . H36B H -0.0221 0.9553 0.0689 0.153 Uiso 1 1 calc R . . H36C H -0.1553 0.9934 0.1326 0.153 Uiso 1 1 calc R . . C37 C 0.6041(12) 0.4211(13) -0.0570(6) 0.156(7) Uani 1 1 d D . . H37A H 0.6079 0.4324 -0.0028 0.233 Uiso 1 1 calc R . . H37B H 0.5679 0.3707 -0.0521 0.233 Uiso 1 1 calc R . . H37C H 0.5524 0.4843 -0.0802 0.233 Uiso 1 1 calc R . . C38 C 0.1541(5) 0.2164(6) -0.0862(4) 0.0699(19) Uani 1 1 d . . . H38A H 0.1014 0.1864 -0.0989 0.084 Uiso 1 1 calc R B 3 H38B H 0.1533 0.2738 -0.1255 0.084 Uiso 1 1 calc R B 3 N1 N 0.3700(3) 0.2294(3) 0.0995(2) 0.0381(8) Uani 1 1 d . . . N2 N 0.3265(3) 0.4446(3) 0.5066(2) 0.0354(8) Uani 1 1 d . . . N3 N -0.1064(4) 0.6924(3) 0.8463(2) 0.0411(9) Uani 1 1 d . . . N4 N 0.0967(4) 0.2554(4) -0.0053(3) 0.0478(10) Uani 1 1 d . E . H4A H 0.0489 0.2208 0.0249 0.057 Uiso 1 1 calc R . . H4B H 0.0459 0.3222 -0.0087 0.057 Uiso 1 1 calc R . . N5 N 0.3498(3) 0.1740(3) -0.0535(2) 0.0390(8) Uani 1 1 d . . . H5A H 0.3826 0.2179 -0.0855 0.047 Uiso 1 1 calc R C 3 H5B H 0.4141 0.1178 -0.0412 0.047 Uiso 1 1 calc R C 3 N6 N -0.0582(7) 1.0740(5) 0.1268(4) 0.149(5) Uani 1 1 d D . . N7 N 0.7216(13) 0.3872(7) -0.1073(7) 0.161(6) Uani 1 1 d D . . O1 O 0.0994(5) 0.6485(5) 0.4021(3) 0.0853(17) Uani 1 1 d . . . O2 O 0.2999(5) 0.7169(5) 0.3527(3) 0.0853(16) Uani 1 1 d . . . O3A O 0.5442(5) 0.5890(4) 0.3588(3) 0.0515(19) Uani 0.743(15) 1 d PD D 1 H3A H 0.5621 0.5469 0.3239 0.077 Uiso 0.743(15) 1 calc PR D 1 O3B O 0.4799(19) 0.660(2) 0.4069(7) 0.132(15) Uani 0.257(15) 1 d PD D 2 H3B H 0.5430 0.6416 0.4253 0.198 Uiso 0.257(15) 1 calc PR D 2 O4 O -0.0583(7) 1.1393(6) 0.0642(5) 0.117(3) Uani 1 1 d D . . O5 O -0.0551(7) 1.0924(8) 0.1994(4) 0.212(7) Uani 1 1 d D . . O6 O 0.8193(16) 0.3105(7) -0.0914(12) 0.321(13) Uani 1 1 d D . . O7 O 0.7357(6) 0.4439(7) -0.1689(5) 0.139(3) Uani 1 1 d D . . F1 F 0.1505(6) 0.1586(4) 0.7170(5) 0.152(3) Uani 1 1 d D . . F2A F 0.3057(6) 0.0283(5) 0.7376(4) 0.174(4) Uani 1 1 d D . . F3 F 0.2137(10) 0.0204(6) 0.6435(6) 0.211(5) Uani 1 1 d D . . F4 F 0.2458(7) 0.1603(4) 0.5895(4) 0.161(3) Uani 1 1 d D . . F5 F 0.3383(7) 0.1692(5) 0.6831(5) 0.172(3) Uani 1 1 d D . . F6 F 0.4112(6) 0.0185(6) 0.6049(5) 0.179(4) Uani 1 1 d D . . F7 F 0.7275(3) 0.5027(3) 0.1973(2) 0.0622(9) Uani 1 1 d . . . F8 F 0.6528(4) 0.6145(2) 0.0997(2) 0.0639(9) Uani 1 1 d . . . F9 F 0.8597(4) 0.5438(3) 0.0887(3) 0.0731(11) Uani 1 1 d . . . F10 F 0.7791(3) 0.5006(3) 0.00300(18) 0.0548(8) Uani 1 1 d . . . F11 F 0.8537(3) 0.3904(2) 0.1023(2) 0.0620(9) Uani 1 1 d . . . F12 F 0.6469(3) 0.4609(3) 0.1107(2) 0.0609(9) Uani 1 1 d . . . F13 F 0.2522(5) 0.9151(4) 0.0186(3) 0.0850(13) Uani 1 1 d . . . F14 F 0.4028(3) 0.8171(2) 0.0820(3) 0.0690(10) Uani 1 1 d . . . F15 F 0.2072(4) 0.8897(3) 0.1538(3) 0.0804(12) Uani 1 1 d . . . F16 F 0.3547(6) 0.9439(4) 0.1597(3) 0.1072(18) Uani 1 1 d . . . F17 F 0.2024(4) 1.0421(3) 0.0981(3) 0.0884(15) Uani 1 1 d . . . F18 F 0.3976(3) 0.9689(3) 0.0257(3) 0.0796(13) Uani 1 1 d . . . P1 P 0.2888(3) 0.09076(17) 0.65660(19) 0.1082(10) Uani 1 1 d . . . P2 P 0.75302(11) 0.50144(9) 0.10061(7) 0.0382(3) Uani 1 1 d . . . P3 P 0.30118(12) 0.92933(10) 0.08990(9) 0.0468(3) Uani 1 1 d . . . Pd01 Pd 0.23104(3) 0.24024(3) 0.050973(19) 0.03794(14) Uani 1 1 d . . . C39A C 0.2777(8) 0.1434(9) -0.1007(5) 0.042(3) Uani 0.60(2) 1 d P E 3 H39A H 0.3180 0.1413 -0.1601 0.051 Uiso 0.60(2) 1 calc PR E 3 H39B H 0.2775 0.0760 -0.0812 0.051 Uiso 0.60(2) 1 calc PR E 3 C39B C 0.2819(11) 0.2021(11) -0.1172(7) 0.036(4) Uani 0.40(2) 1 d P E 4 H39C H 0.2872 0.2651 -0.1456 0.043 Uiso 0.40(2) 1 calc PR E 4 H39D H 0.3220 0.1489 -0.1579 0.043 Uiso 0.40(2) 1 calc PR E 4 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 0.057(3) 0.040(3) 0.052(3) 0.007(2) -0.022(2) -0.020(2) C2 0.057(3) 0.038(3) 0.057(3) 0.005(2) -0.028(3) -0.010(2) C3 0.0281(19) 0.040(2) 0.035(2) -0.0125(17) -0.0008(16) -0.0019(17) C4 0.056(3) 0.054(3) 0.046(3) 0.006(2) -0.014(2) -0.028(3) C5 0.056(3) 0.053(3) 0.043(3) 0.014(2) -0.017(2) -0.026(3) C6 0.026(2) 0.053(3) 0.043(2) -0.013(2) -0.0010(18) -0.0033(19) C7 0.0264(19) 0.049(3) 0.039(2) -0.0128(19) -0.0015(17) -0.0095(18) C8 0.041(2) 0.045(3) 0.038(2) -0.0045(19) 0.0068(19) -0.017(2) C9 0.036(2) 0.040(2) 0.037(2) -0.0032(18) 0.0044(18) -0.0141(19) C10 0.0270(19) 0.045(2) 0.038(2) -0.0117(18) -0.0017(16) -0.0117(18) C11 0.037(2) 0.050(3) 0.041(2) -0.005(2) -0.0115(19) -0.005(2) C12 0.035(2) 0.047(3) 0.050(3) -0.007(2) -0.013(2) -0.003(2) C13 0.033(2) 0.039(2) 0.037(2) 0.0014(17) -0.0077(17) -0.0150(18) C14 0.031(2) 0.042(2) 0.033(2) 0.0031(17) -0.0062(16) -0.0131(18) C15 0.0293(19) 0.040(2) 0.0286(19) 0.0011(16) -0.0065(15) -0.0123(17) C16 0.033(2) 0.052(3) 0.031(2) -0.0064(18) -0.0016(16) -0.0197(19) C17 0.033(2) 0.049(3) 0.032(2) -0.0046(18) -0.0015(16) -0.0189(19) C18 0.039(2) 0.035(2) 0.041(2) 0.0060(18) -0.0067(19) -0.0134(18) C19 0.039(2) 0.040(2) 0.038(2) 0.0103(19) -0.0024(19) -0.0119(19) C20 0.033(2) 0.045(2) 0.031(2) 0.0040(17) -0.0042(16) -0.0141(18) C21 0.032(2) 0.042(2) 0.0299(19) 0.0014(17) -0.0030(16) -0.0137(18) C22 0.049(3) 0.055(3) 0.039(2) -0.006(2) 0.005(2) -0.033(2) C23 0.052(3) 0.050(3) 0.042(2) -0.010(2) 0.004(2) -0.028(2) C24 0.036(2) 0.047(3) 0.033(2) -0.0037(18) 0.0000(17) -0.0170(19) C25 0.038(2) 0.050(3) 0.037(2) -0.007(2) 0.0024(19) -0.016(2) C26 0.033(2) 0.050(3) 0.034(2) 0.0066(19) -0.0027(17) -0.0128(19) C27 0.046(3) 0.106(6) 0.071(4) 0.018(4) -0.030(3) -0.034(4) C28 0.051(4) 0.111(6) 0.075(5) 0.016(4) -0.026(3) -0.033(4) C29 0.056(4) 0.086(5) 0.095(5) 0.023(4) -0.038(4) -0.025(4) C30 0.054(4) 0.098(5) 0.075(4) 0.031(4) -0.033(3) -0.040(4) C31 0.048(3) 0.098(5) 0.073(4) 0.030(4) -0.036(3) -0.033(3) C32 0.075(5) 0.107(7) 0.097(6) 0.038(5) -0.030(5) -0.044(5) C33 0.070(5) 0.138(8) 0.115(7) 0.071(7) -0.037(5) -0.044(5) C34 0.074(4) 0.081(5) 0.063(4) 0.025(3) -0.019(3) -0.039(4) C35 0.072(4) 0.104(6) 0.053(4) 0.011(4) -0.009(3) -0.040(4) C36 0.074(5) 0.112(7) 0.135(8) -0.052(6) 0.001(5) -0.051(5) C37 0.167(11) 0.32(2) 0.076(6) 0.058(9) -0.042(7) -0.199(14) C38 0.040(3) 0.097(5) 0.075(4) -0.043(4) -0.010(3) -0.017(3) N1 0.0304(17) 0.043(2) 0.0320(17) -0.0032(15) -0.0030(14) -0.0083(15) N2 0.0312(17) 0.042(2) 0.0304(17) -0.0026(14) -0.0032(14) -0.0137(15) N3 0.0356(19) 0.048(2) 0.0302(17) 0.0020(15) -0.0013(15) -0.0115(17) N4 0.033(2) 0.064(3) 0.037(2) -0.0018(19) -0.0042(16) -0.0126(19) N5 0.0301(18) 0.041(2) 0.0343(18) -0.0026(15) -0.0026(14) -0.0049(15) N6 0.043(4) 0.152(9) 0.260(15) -0.116(10) 0.004(6) -0.037(5) N7 0.296(18) 0.118(8) 0.157(10) 0.067(8) -0.157(12) -0.123(11) O1 0.070(3) 0.110(4) 0.087(4) 0.036(3) -0.031(3) -0.051(3) O2 0.066(3) 0.104(4) 0.082(3) 0.036(3) -0.019(3) -0.042(3) O3A 0.051(3) 0.061(4) 0.046(3) 0.004(2) -0.013(2) -0.027(3) O3B 0.12(2) 0.10(2) 0.14(3) 0.06(2) -0.04(2) -0.029(19) O4 0.091(5) 0.103(5) 0.162(7) 0.033(5) -0.028(5) -0.059(4) O5 0.079(5) 0.336(15) 0.240(11) -0.227(12) 0.053(6) -0.089(7) O6 0.45(2) 0.069(5) 0.52(3) -0.041(10) -0.41(2) 0.022(9) O7 0.066(4) 0.148(7) 0.151(7) 0.059(6) 0.001(4) -0.029(4) F1 0.175(7) 0.065(3) 0.179(7) 0.003(4) -0.045(6) -0.012(4) F2A 0.132(6) 0.120(5) 0.197(8) 0.056(5) -0.036(6) 0.003(5) F3 0.230(11) 0.142(7) 0.288(13) -0.056(8) -0.102(10) -0.057(7) F4 0.218(9) 0.121(5) 0.142(6) 0.004(4) -0.092(6) -0.036(5) F5 0.157(7) 0.152(7) 0.241(10) 0.021(7) -0.106(7) -0.064(6) F6 0.105(5) 0.143(7) 0.230(10) 0.013(6) -0.009(6) -0.019(5) F7 0.062(2) 0.066(2) 0.0427(16) -0.0047(15) -0.0134(15) -0.0072(17) F8 0.068(2) 0.0434(17) 0.065(2) -0.0009(15) -0.0250(18) -0.0006(15) F9 0.062(2) 0.079(3) 0.092(3) 0.014(2) -0.027(2) -0.041(2) F10 0.0519(17) 0.066(2) 0.0393(15) 0.0046(14) 0.0010(13) -0.0253(16) F11 0.0538(19) 0.0428(17) 0.064(2) -0.0006(15) -0.0052(16) -0.0004(14) F12 0.0526(18) 0.082(2) 0.0543(19) -0.0015(17) 0.0005(15) -0.0409(18) F13 0.098(3) 0.105(3) 0.075(3) 0.018(2) -0.037(2) -0.060(3) F14 0.0513(19) 0.0368(16) 0.109(3) -0.0019(17) -0.0115(19) -0.0125(14) F15 0.065(2) 0.070(2) 0.079(3) 0.016(2) 0.012(2) -0.0254(19) F16 0.170(5) 0.074(3) 0.111(4) 0.004(3) -0.076(4) -0.055(3) F17 0.053(2) 0.047(2) 0.114(4) 0.008(2) 0.012(2) 0.0050(16) F18 0.0381(17) 0.053(2) 0.126(4) 0.027(2) -0.0058(19) -0.0159(15) P1 0.151(3) 0.0500(11) 0.119(2) 0.0145(12) -0.069(2) -0.0167(13) P2 0.0338(6) 0.0356(6) 0.0397(6) 0.0038(4) -0.0065(5) -0.0113(5) P3 0.0351(6) 0.0371(6) 0.0594(8) 0.0015(5) -0.0053(5) -0.0103(5) Pd01 0.02950(19) 0.0462(2) 0.02826(18) -0.00101(13) -0.00131(12) -0.00873(14) C39A 0.044(4) 0.049(7) 0.036(4) -0.006(4) -0.013(3) -0.016(4) C39B 0.049(7) 0.029(8) 0.030(5) -0.003(4) 0.002(4) -0.022(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(6) . ? C1 C2 1.375(8) . ? C2 C3 1.377(8) . ? C3 C4 1.396(7) . ? C3 C6 1.499(7) . ? C4 C5 1.369(8) . ? C5 N1 1.325(7) . ? C6 C7 1.521(6) . ? C7 C12 1.379(7) . ? C7 C8 1.393(7) . ? C8 C9 1.391(6) . ? C9 C10 1.391(7) . ? C10 C11 1.386(7) . ? C10 N2 1.444(5) . ? C11 C12 1.391(7) . ? C13 N2 1.351(6) . ? C13 C14 1.373(6) . ? C14 C15 1.405(7) . ? C14 C18 1.434(6) . ? C15 C16 1.409(6) . ? C15 C21 1.422(6) . ? C16 C17 1.394(6) . ? C16 C22 1.444(7) . ? C17 N2 1.356(6) . ? C18 C19 1.349(7) . ? C19 C20 1.430(7) . ? C20 C26 1.377(6) . ? C20 C21 1.421(6) . ? C21 C24 1.408(7) . ? C22 C23 1.351(7) . ? C23 C24 1.445(7) . ? C24 C25 1.386(6) . ? C25 N3 1.355(6) . ? C26 N3 1.330(7) . ? C27 C28 1.347(12) . ? C27 C31 1.450(12) 2_566 ? C28 C29 1.388(11) . ? C29 C30 1.417(12) . ? C30 O1 1.346(8) . ? C30 C31 1.409(11) . ? C31 C31 1.405(13) 2_566 ? C31 C27 1.450(12) 2_566 ? C32 O1 1.413(11) . ? C32 C33 1.522(12) . ? C33 O2 1.435(10) . ? C34 O2 1.435(8) . ? C34 C35 1.465(10) . ? C35 O3A 1.422(5) . ? C35 O3B 1.434(5) . ? C36 N6 1.390(10) . ? C37 N7 1.371(13) . ? C38 C39A 1.421(10) . ? C38 C39B 1.428(13) . ? C38 N4 1.442(7) . ? N1 Pd01 2.025(4) . ? N3 Pd01 2.030(4) 2_566 ? N4 Pd01 2.041(4) . ? N5 C39B 1.460(13) . ? N5 C39A 1.561(10) . ? N5 Pd01 2.027(4) . ? N6 O5 1.3187(10) . ? N6 O4 1.3187(10) . ? N7 O7 1.251(10) . ? N7 O6 1.322(12) . ? F1 P1 1.683(7) . ? F2A P1 1.554(6) . ? F3 P1 1.695(8) . ? F4 P1 1.474(6) . ? F5 P1 1.653(7) . ? F6 P1 1.536(7) . ? F7 P2 1.592(3) . ? F8 P2 1.603(3) . ? F9 P2 1.602(4) . ? F10 P2 1.605(3) . ? F11 P2 1.585(3) . ? F12 P2 1.582(3) . ? F13 P3 1.568(5) . ? F14 P3 1.595(3) . ? F15 P3 1.571(4) . ? F16 P3 1.585(5) . ? F17 P3 1.590(4) . ? F18 P3 1.593(4) . ? Pd01 N3 2.030(4) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.4(5) . . ? C1 C2 C3 120.8(5) . . ? C2 C3 C4 116.8(5) . . ? C2 C3 C6 122.5(5) . . ? C4 C3 C6 120.6(5) . . ? C5 C4 C3 119.4(5) . . ? N1 C5 C4 123.0(5) . . ? C3 C6 C7 109.1(4) . . ? C12 C7 C8 119.2(4) . . ? C12 C7 C6 120.8(5) . . ? C8 C7 C6 119.8(4) . . ? C9 C8 C7 120.8(5) . . ? C8 C9 C10 118.6(4) . . ? C11 C10 C9 121.5(4) . . ? C11 C10 N2 119.4(4) . . ? C9 C10 N2 119.0(4) . . ? C10 C11 C12 118.6(5) . . ? C7 C12 C11 121.2(5) . . ? N2 C13 C14 121.4(4) . . ? C13 C14 C15 118.1(4) . . ? C13 C14 C18 122.0(4) . . ? C15 C14 C18 119.9(4) . . ? C14 C15 C16 120.5(4) . . ? C14 C15 C21 120.1(4) . . ? C16 C15 C21 119.4(4) . . ? C17 C16 C15 118.2(4) . . ? C17 C16 C22 122.3(4) . . ? C15 C16 C22 119.5(4) . . ? N2 C17 C16 120.1(4) . . ? C19 C18 C14 120.2(4) . . ? C18 C19 C20 121.3(4) . . ? C26 C20 C21 117.2(4) . . ? C26 C20 C19 123.4(4) . . ? C21 C20 C19 119.5(4) . . ? C24 C21 C20 120.3(4) . . ? C24 C21 C15 120.7(4) . . ? C20 C21 C15 119.0(4) . . ? C23 C22 C16 120.6(4) . . ? C22 C23 C24 121.1(5) . . ? C25 C24 C21 117.4(4) . . ? C25 C24 C23 124.0(5) . . ? C21 C24 C23 118.7(4) . . ? N3 C25 C24 121.8(5) . . ? N3 C26 C20 122.8(4) . . ? C28 C27 C31 120.9(7) . 2_566 ? C27 C28 C29 122.4(9) . . ? C28 C29 C30 118.7(8) . . ? O1 C30 C31 115.6(8) . . ? O1 C30 C29 124.6(8) . . ? C31 C30 C29 119.8(7) . . ? C31 C31 C30 121.0(10) 2_566 . ? C31 C31 C27 117.1(10) 2_566 2_566 ? C30 C31 C27 121.9(7) . 2_566 ? O1 C32 C33 106.4(9) . . ? O2 C33 C32 105.1(7) . . ? O2 C34 C35 106.9(5) . . ? O3A C35 O3B 52.2(12) . . ? O3A C35 C34 114.2(6) . . ? O3B C35 C34 111.2(8) . . ? C39A C38 C39B 35.8(6) . . ? C39A C38 N4 117.5(6) . . ? C39B C38 N4 115.5(6) . . ? C5 N1 C1 118.5(4) . . ? C5 N1 Pd01 119.6(3) . . ? C1 N1 Pd01 121.9(4) . . ? C13 N2 C17 121.7(4) . . ? C13 N2 C10 118.8(4) . . ? C17 N2 C10 119.5(4) . . ? C26 N3 C25 120.5(4) . . ? C26 N3 Pd01 118.6(3) . 2_566 ? C25 N3 Pd01 121.0(3) . 2_566 ? C38 N4 Pd01 109.5(3) . . ? C39B N5 C39A 33.5(5) . . ? C39B N5 Pd01 108.3(5) . . ? C39A N5 Pd01 109.0(4) . . ? O5 N6 O4 122.5(4) . . ? O5 N6 C36 114.4(7) . . ? O4 N6 C36 123.1(7) . . ? O7 N7 O6 119.6(15) . . ? O7 N7 C37 113.6(10) . . ? O6 N7 C37 126.2(14) . . ? C30 O1 C32 117.4(7) . . ? C33 O2 C34 108.9(6) . . ? F4 P1 F6 97.7(4) . . ? F4 P1 F2A 168.0(5) . . ? F6 P1 F2A 93.8(3) . . ? F4 P1 F5 91.4(3) . . ? F6 P1 F5 100.2(5) . . ? F2A P1 F5 89.6(3) . . ? F4 P1 F1 85.8(4) . . ? F6 P1 F1 173.6(4) . . ? F2A P1 F1 82.4(4) . . ? F5 P1 F1 84.9(3) . . ? F4 P1 F3 89.8(3) . . ? F6 P1 F3 90.2(5) . . ? F2A P1 F3 87.0(3) . . ? F5 P1 F3 169.2(5) . . ? F1 P1 F3 84.5(5) . . ? F12 P2 F11 91.4(2) . . ? F12 P2 F7 90.6(2) . . ? F11 P2 F7 89.41(19) . . ? F12 P2 F9 178.8(2) . . ? F11 P2 F9 89.3(2) . . ? F7 P2 F9 90.4(2) . . ? F12 P2 F8 89.6(2) . . ? F11 P2 F8 178.8(2) . . ? F7 P2 F8 89.99(19) . . ? F9 P2 F8 89.7(2) . . ? F12 P2 F10 89.75(19) . . ? F11 P2 F10 90.72(19) . . ? F7 P2 F10 179.6(2) . . ? F9 P2 F10 89.3(2) . . ? F8 P2 F10 89.88(19) . . ? F13 P3 F15 90.3(3) . . ? F13 P3 F16 178.0(3) . . ? F15 P3 F16 91.6(3) . . ? F13 P3 F17 90.0(3) . . ? F15 P3 F17 91.5(2) . . ? F16 P3 F17 90.5(3) . . ? F13 P3 F18 90.3(3) . . ? F15 P3 F18 179.3(3) . . ? F16 P3 F18 87.8(3) . . ? F17 P3 F18 88.9(2) . . ? F13 P3 F14 91.1(3) . . ? F15 P3 F14 89.4(2) . . ? F16 P3 F14 88.4(3) . . ? F17 P3 F14 178.5(3) . . ? F18 P3 F14 90.2(2) . . ? N1 Pd01 N5 93.18(15) . . ? N1 Pd01 N3 89.06(16) . 2_566 ? N5 Pd01 N3 177.75(16) . 2_566 ? N1 Pd01 N4 175.95(16) . . ? N5 Pd01 N4 84.19(16) . . ? N3 Pd01 N4 93.56(17) 2_566 . ? C38 C39A N5 107.8(7) . . ? C38 C39B N5 113.2(8) . . ? 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 -0.1(9) . . . . ? C1 C2 C3 C4 -1.7(8) . . . . ? C1 C2 C3 C6 175.5(5) . . . . ? C2 C3 C4 C5 1.4(8) . . . . ? C6 C3 C4 C5 -175.8(5) . . . . ? C3 C4 C5 N1 0.7(9) . . . . ? C2 C3 C6 C7 -86.0(6) . . . . ? C4 C3 C6 C7 91.1(6) . . . . ? C3 C6 C7 C12 106.7(5) . . . . ? C3 C6 C7 C8 -68.6(6) . . . . ? C12 C7 C8 C9 -1.0(8) . . . . ? C6 C7 C8 C9 174.3(5) . . . . ? C7 C8 C9 C10 0.1(8) . . . . ? C8 C9 C10 C11 1.3(7) . . . . ? C8 C9 C10 N2 -175.1(4) . . . . ? C9 C10 C11 C12 -1.7(8) . . . . ? N2 C10 C11 C12 174.7(4) . . . . ? C8 C7 C12 C11 0.5(8) . . . . ? C6 C7 C12 C11 -174.7(5) . . . . ? C10 C11 C12 C7 0.8(8) . . . . ? N2 C13 C14 C15 3.0(7) . . . . ? N2 C13 C14 C18 -178.6(4) . . . . ? C13 C14 C15 C16 -2.4(6) . . . . ? C18 C14 C15 C16 179.1(4) . . . . ? C13 C14 C15 C21 176.7(4) . . . . ? C18 C14 C15 C21 -1.8(6) . . . . ? C14 C15 C16 C17 0.5(7) . . . . ? C21 C15 C16 C17 -178.6(4) . . . . ? C14 C15 C16 C22 179.0(4) . . . . ? C21 C15 C16 C22 -0.2(7) . . . . ? C15 C16 C17 N2 0.8(7) . . . . ? C22 C16 C17 N2 -177.6(5) . . . . ? C13 C14 C18 C19 -177.3(5) . . . . ? C15 C14 C18 C19 1.2(7) . . . . ? C14 C18 C19 C20 -0.3(7) . . . . ? C18 C19 C20 C26 -179.6(5) . . . . ? C18 C19 C20 C21 0.0(7) . . . . ? C26 C20 C21 C24 0.2(7) . . . . ? C19 C20 C21 C24 -179.4(4) . . . . ? C26 C20 C21 C15 179.0(4) . . . . ? C19 C20 C21 C15 -0.6(7) . . . . ? C14 C15 C21 C24 -179.7(4) . . . . ? C16 C15 C21 C24 -0.5(7) . . . . ? C14 C15 C21 C20 1.5(6) . . . . ? C16 C15 C21 C20 -179.4(4) . . . . ? C17 C16 C22 C23 179.1(5) . . . . ? C15 C16 C22 C23 0.7(8) . . . . ? C16 C22 C23 C24 -0.5(9) . . . . ? C20 C21 C24 C25 -0.4(7) . . . . ? C15 C21 C24 C25 -179.3(4) . . . . ? C20 C21 C24 C23 179.6(5) . . . . ? C15 C21 C24 C23 0.7(7) . . . . ? C22 C23 C24 C25 179.8(5) . . . . ? C22 C23 C24 C21 -0.2(8) . . . . ? C21 C24 C25 N3 1.3(8) . . . . ? C23 C24 C25 N3 -178.7(5) . . . . ? C21 C20 C26 N3 -0.9(7) . . . . ? C19 C20 C26 N3 178.8(5) . . . . ? C31 C27 C28 C29 0.3(10) 2_566 . . . ? C27 C28 C29 C30 -1.8(10) . . . . ? C28 C29 C30 O1 -176.3(6) . . . . ? C28 C29 C30 C31 2.2(9) . . . . ? O1 C30 C31 C31 177.4(7) . . . 2_566 ? C29 C30 C31 C31 -1.3(10) . . . 2_566 ? O1 C30 C31 C27 -2.8(8) . . . 2_566 ? C29 C30 C31 C27 178.5(6) . . . 2_566 ? O1 C32 C33 O2 -77.3(10) . . . . ? O2 C34 C35 O3A 61.2(8) . . . . ? O2 C34 C35 O3B 4.3(16) . . . . ? C4 C5 N1 C1 -2.5(8) . . . . ? C4 C5 N1 Pd01 174.8(4) . . . . ? C2 C1 N1 C5 2.2(8) . . . . ? C2 C1 N1 Pd01 -175.0(4) . . . . ? C14 C13 N2 C17 -1.7(7) . . . . ? C14 C13 N2 C10 -179.6(4) . . . . ? C16 C17 N2 C13 -0.3(7) . . . . ? C16 C17 N2 C10 177.6(4) . . . . ? C11 C10 N2 C13 -38.8(6) . . . . ? C9 C10 N2 C13 137.6(5) . . . . ? C11 C10 N2 C17 143.2(5) . . . . ? C9 C10 N2 C17 -40.3(6) . . . . ? C20 C26 N3 C25 1.8(7) . . . . ? C20 C26 N3 Pd01 -177.9(4) . . . 2_566 ? C24 C25 N3 C26 -2.0(8) . . . . ? C24 C25 N3 Pd01 177.6(4) . . . 2_566 ? C39A C38 N4 Pd01 24.2(9) . . . . ? C39B C38 N4 Pd01 -15.9(10) . . . . ? C31 C30 O1 C32 178.7(6) . . . . ? C29 C30 O1 C32 -2.7(10) . . . . ? C33 C32 O1 C30 176.8(6) . . . . ? C32 C33 O2 C34 177.3(8) . . . . ? C35 C34 O2 C33 172.5(8) . . . . ? C5 N1 Pd01 N5 83.6(4) . . . . ? C1 N1 Pd01 N5 -99.2(4) . . . . ? C5 N1 Pd01 N3 -96.2(4) . . . 2_566 ? C1 N1 Pd01 N3 81.0(4) . . . 2_566 ? C5 N1 Pd01 N4 34(3) . . . . ? C1 N1 Pd01 N4 -149(2) . . . . ? C39B N5 Pd01 N1 -158.7(7) . . . . ? C39A N5 Pd01 N1 165.9(5) . . . . ? C39B N5 Pd01 N3 16(4) . . . 2_566 ? C39A N5 Pd01 N3 -19(4) . . . 2_566 ? C39B N5 Pd01 N4 18.2(7) . . . . ? C39A N5 Pd01 N4 -17.2(5) . . . . ? C38 N4 Pd01 N1 48(3) . . . . ? C38 N4 Pd01 N5 -1.9(5) . . . . ? C38 N4 Pd01 N3 178.0(5) . . . 2_566 ? C39B C38 C39A N5 57.8(10) . . . . ? N4 C38 C39A N5 -38.4(11) . . . . ? C39B N5 C39A C38 -61.4(10) . . . . ? Pd01 N5 C39A C38 33.4(9) . . . . ? C39A C38 C39B N5 -69.6(11) . . . . ? N4 C38 C39B N5 32.7(14) . . . . ? C39A N5 C39B C38 64.8(11) . . . . ? Pd01 N5 C39B C38 -32.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.568 _refine_diff_density_min -1.535 _refine_diff_density_rms 0.137 # 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 0.000 0.000 0.500 293 62 ' ' _platon_squeeze_details ; 'After refining the structure a large void in the structure filled with scattered electron density was present. Attempts to model the density were unsuccessful and the SQUEEZE routine inside PLATON was used to remove two ill defined nitromethane molecules from the data. The potential solvent volume was 294.6 A3 (11% of the cell volume) and accounted for a total of 62 electrons, this would be in good agreement with two heavily disordered nitromethane molecules into the unit cell (64 electrons).' ; data_0944010_b1_0s _database_code_depnum_ccdc_archive 'CCDC 883119' #TrackingRef '- catenane.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C192 H216 F72 N28 O36 P12 Pd4' _chemical_formula_weight 5657.17 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 30.8974(9) _cell_length_b 21.7294(6) _cell_length_c 20.8416(6) _cell_angle_alpha 90.000(0) _cell_angle_beta 118.4017(15) _cell_angle_gamma 90.000(0) _cell_volume 12308.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20096 _cell_measurement_theta_min 4.946 _cell_measurement_theta_max 50.929 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5728 _exptl_absorpt_coefficient_mu 0.490 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8245 _exptl_absorpt_correction_T_max 0.8999 _exptl_absorpt_process_details 'SADABS 2004/1 (Sheldrick, 2004)' _exptl_special_details ; Data was collected using a X8 APEX II BRUKER-NONIUS diffractometer. A suitable crystal was chosen and mounted with glue on a glass fiber. Data were measured using omega scans of 0.5\% per frame for 10 s with a final resolution of 0.75 \%A. Data integration and reduction were performed using the Apex2 Service v2010, 1-2 (BRUKER AXS) suite software. Absorption corrections were applied using SADABS (2008) of the suite software. The structures are solved by the direct method using the SHELX-XS Version 2008/1 program and refined by least squares method on F2 SHELXL Version 2008/4 , incorporated in the Apex2 suite software. ; _diffrn_ambient_temperature 100(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 'Apex2 V.1.0-27 (Bruker Nonius, 2005)' _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 81414 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.38 _reflns_number_total 29395 _reflns_number_gt 21393 _reflns_threshold_expression >2\s(I) _computing_data_collection "APEXII area detector'" _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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. The structure show some disorder in one of the ethylendiamine moieties, the poliether chain and the external naphtalene ring (which displayed a distorted geometry). This desorder has been treated using SIMU, DELU, DFIX, DANG and ISOR constraints to correct the geometry and get reasonable thermal ellipsoids. Also,SIMU, DELU, DFIX, DANG, ISOR and FLAT restrictions were used to model the disordered nitromethane solvent molecules and two disordered PF6 counterions. ; _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^)+(0.1986P)^2^+8.8973P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.19(3) _refine_ls_number_reflns 29395 _refine_ls_number_parameters 1614 _refine_ls_number_restraints 475 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2778 _refine_ls_wR_factor_gt 0.2375 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.002 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 0.2257(3) 0.0250(3) 0.8801(4) 0.0423(15) Uani 1 1 d . . . H1 H 0.2532 -0.0019 0.8963 0.051 Uiso 1 1 calc R . . C2 C 0.1798(3) 0.0026(4) 0.8320(5) 0.0526(19) Uani 1 1 d . . . H2 H 0.1762 -0.0386 0.8148 0.063 Uiso 1 1 calc R . . C3 C 0.1397(3) 0.0400(4) 0.8094(4) 0.0433(15) Uani 1 1 d . . . C4 C 0.1472(3) 0.0997(4) 0.8341(4) 0.0450(16) Uani 1 1 d . . . H4 H 0.1200 0.1271 0.8175 0.054 Uiso 1 1 calc R . . C5 C 0.1934(3) 0.1202(4) 0.8825(5) 0.0406(15) Uani 1 1 d . . . H5 H 0.1977 0.1611 0.9006 0.049 Uiso 1 1 calc R . . C6 C 0.0885(3) 0.0172(5) 0.7544(5) 0.058(2) Uani 1 1 d . . . H6A H 0.0893 -0.0279 0.7482 0.069 Uiso 1 1 calc R . . H6B H 0.0648 0.0262 0.7725 0.069 Uiso 1 1 calc R . . C7 C 0.0722(3) 0.0489(4) 0.6817(5) 0.0506(18) Uani 1 1 d . . . C8 C 0.0914(3) 0.0321(5) 0.6385(5) 0.055(2) Uani 1 1 d . . . H8 H 0.1118 -0.0034 0.6513 0.066 Uiso 1 1 calc R . . C9 C 0.0827(3) 0.0641(4) 0.5766(5) 0.0485(17) Uani 1 1 d . . . H9 H 0.0965 0.0507 0.5469 0.058 Uiso 1 1 calc R . . C10 C 0.0531(3) 0.1169(4) 0.5582(5) 0.0446(17) Uani 1 1 d . . . C11 C 0.0321(3) 0.1341(4) 0.6036(6) 0.053(2) Uani 1 1 d . . . H11 H 0.0117 0.1695 0.5921 0.064 Uiso 1 1 calc R . . C12 C 0.0416(3) 0.0995(5) 0.6640(5) 0.059(2) Uani 1 1 d . . . H12 H 0.0271 0.1103 0.6937 0.071 Uiso 1 1 calc R . . C13 C 0.0400(3) 0.1232(4) 0.4364(5) 0.0465(18) Uani 1 1 d . . . H13 H 0.0361 0.0798 0.4331 0.056 Uiso 1 1 calc R . . C14 C 0.0388(3) 0.1558(4) 0.3788(4) 0.0421(15) Uani 1 1 d . . . C15 C 0.0434(3) 0.2202(3) 0.3828(4) 0.0391(15) Uani 1 1 d . . . C16 C 0.0480(3) 0.2509(4) 0.4462(4) 0.0412(15) Uani 1 1 d . . . C17 C 0.0494(3) 0.2143(4) 0.5030(5) 0.0461(17) Uani 1 1 d . . . H17 H 0.0524 0.2335 0.5458 0.055 Uiso 1 1 calc R . . C18 C 0.0508(3) 0.3171(4) 0.4490(5) 0.0475(18) Uani 1 1 d . . . H18 H 0.0525 0.3384 0.4900 0.057 Uiso 1 1 calc R . . C19 C 0.0511(3) 0.3488(4) 0.3938(4) 0.0444(16) Uani 1 1 d . . . H19 H 0.0543 0.3923 0.3973 0.053 Uiso 1 1 calc R . . C20 C 0.0465(3) 0.3184(4) 0.3295(5) 0.0425(15) Uani 1 1 d . . . C21 C 0.0430(3) 0.2542(3) 0.3264(4) 0.0404(15) Uani 1 1 d . . . C22 C 0.0332(3) 0.1234(4) 0.3133(5) 0.0510(19) Uani 1 1 d . . . H22 H 0.0293 0.0799 0.3093 0.061 Uiso 1 1 calc R . . C23 C 0.0338(3) 0.1569(4) 0.2590(5) 0.0504(18) Uani 1 1 d . . . H23 H 0.0316 0.1363 0.2174 0.061 Uiso 1 1 calc R . . C24 C 0.0377(3) 0.2232(4) 0.2625(5) 0.0455(17) Uani 1 1 d . . . C25 C 0.0372(3) 0.2583(4) 0.2079(5) 0.0479(18) Uani 1 1 d . . . H25 H 0.0345 0.2381 0.1658 0.058 Uiso 1 1 calc R . . C26 C 0.0453(3) 0.3494(4) 0.2709(5) 0.0497(18) Uani 1 1 d . . . H26 H 0.0480 0.3930 0.2728 0.060 Uiso 1 1 calc R . . C27 C 0.1471(4) 0.3696(5) 0.2088(5) 0.057(2) Uani 1 1 d . . . H27 H 0.1441 0.3300 0.1877 0.068 Uiso 1 1 calc R . . C28 C 0.1934(4) 0.3909(5) 0.2555(6) 0.059(2) Uani 1 1 d . . . H28 H 0.2218 0.3673 0.2656 0.071 Uiso 1 1 calc R . . C29 C 0.1976(4) 0.4496(4) 0.2883(4) 0.0505(19) Uani 1 1 d . . . C30 C 0.1555(4) 0.4816(4) 0.2702(5) 0.056(2) Uani 1 1 d . . . H30 H 0.1569 0.5211 0.2907 0.067 Uiso 1 1 calc R . . C31 C 0.1105(4) 0.4560(5) 0.2214(5) 0.056(2) Uani 1 1 d . . . H31 H 0.0815 0.4790 0.2091 0.067 Uiso 1 1 calc R . . C32 C 0.2477(4) 0.4697(5) 0.3457(5) 0.060(2) Uani 1 1 d . . . H32A H 0.2480 0.5148 0.3527 0.072 Uiso 1 1 calc R . . H32B H 0.2725 0.4596 0.3300 0.072 Uiso 1 1 calc R . . C34 C 0.2601(3) 0.4367(4) 0.4169(5) 0.054(2) Uani 1 1 d . . . C35 C 0.2995(4) 0.3956(5) 0.4472(6) 0.061(2) Uani 1 1 d . . . H35 H 0.3196 0.3901 0.4247 0.074 Uiso 1 1 calc R . . C36 C 0.3095(3) 0.3628(5) 0.5098(5) 0.053(2) Uani 1 1 d . . . H36 H 0.3367 0.3354 0.5311 0.063 Uiso 1 1 calc R . . C37 C 0.2786(3) 0.3714(3) 0.5401(4) 0.0406(16) Uani 1 1 d . . . C38 C 0.2399(3) 0.4105(4) 0.5119(5) 0.0484(17) Uani 1 1 d . . . H38 H 0.2196 0.4155 0.5343 0.058 Uiso 1 1 calc R . . C39 C 0.2306(3) 0.4430(4) 0.4496(5) 0.0533(19) Uani 1 1 d . . . H39 H 0.2033 0.4703 0.4289 0.064 Uiso 1 1 calc R . . C40 C 0.2872(3) 0.3643(3) 0.6613(4) 0.0376(14) Uani 1 1 d . . . H40 H 0.2849 0.4079 0.6605 0.045 Uiso 1 1 calc R . . C41 C 0.2913(2) 0.3326(3) 0.7213(4) 0.0297(12) Uani 1 1 d . . . C42 C 0.2952(2) 0.2680(3) 0.7203(4) 0.0297(12) Uani 1 1 d . . . C43 C 0.2953(2) 0.2374(3) 0.6600(4) 0.0299(12) Uani 1 1 d . . . C44 C 0.2907(3) 0.2735(3) 0.6029(4) 0.0345(13) Uani 1 1 d . . . H44 H 0.2905 0.2549 0.5615 0.041 Uiso 1 1 calc R . . C45 C 0.2988(3) 0.1718(3) 0.6606(4) 0.0328(12) Uani 1 1 d . . . H45 H 0.2987 0.1516 0.6202 0.039 Uiso 1 1 calc R . . C46 C 0.3021(3) 0.1383(3) 0.7161(4) 0.0316(12) Uani 1 1 d . . . H46 H 0.3051 0.0949 0.7152 0.038 Uiso 1 1 calc R . . C47 C 0.3013(2) 0.1674(3) 0.7783(4) 0.0291(11) Uani 1 1 d . . . C48 C 0.2983(2) 0.2326(3) 0.7796(4) 0.0273(11) Uani 1 1 d . . . C49 C 0.2921(3) 0.3616(3) 0.7833(4) 0.0410(15) Uani 1 1 d . . . H49 H 0.2902 0.4052 0.7847 0.049 Uiso 1 1 calc R . . C50 C 0.2953(3) 0.3283(3) 0.8399(4) 0.0379(14) Uani 1 1 d . . . H50 H 0.2960 0.3486 0.8807 0.045 Uiso 1 1 calc R . . C51 C 0.2978(2) 0.2622(3) 0.8390(4) 0.0303(12) Uani 1 1 d . . . C52 C 0.3001(3) 0.2250(3) 0.8959(4) 0.0359(13) Uani 1 1 d . . . H52 H 0.3002 0.2439 0.9371 0.043 Uiso 1 1 calc R . . C53 C 0.3033(2) 0.1353(3) 0.8366(4) 0.0323(12) Uani 1 1 d . . . H53 H 0.3057 0.0917 0.8369 0.039 Uiso 1 1 calc R . . C54 C 0.3790(6) 0.1210(7) 1.1209(6) 0.101(5) Uani 1 1 d DU . . H54A H 0.3694 0.1552 1.1430 0.121 Uiso 1 1 calc R . . H54B H 0.4147 0.1139 1.1518 0.121 Uiso 1 1 calc R . . C55 C 0.3534(5) 0.0671(7) 1.1223(6) 0.105(5) Uani 1 1 d DU . . H55A H 0.3510 0.0663 1.1681 0.126 Uiso 1 1 calc R . . H55B H 0.3720 0.0303 1.1216 0.126 Uiso 1 1 calc R . . C56 C -0.0209(8) 0.3964(7) -0.0265(6) 0.126(6) Uani 1 1 d U . . H56A H -0.0426 0.4276 -0.0219 0.152 Uiso 1 1 calc R . . H56B H -0.0230 0.4020 -0.0751 0.152 Uiso 1 1 calc R . . C57 C -0.0397(6) 0.3382(8) -0.0249(7) 0.095(3) Uani 1 1 d U . . H57A H -0.0225 0.3051 -0.0365 0.114 Uiso 1 1 calc R . . H57B H -0.0755 0.3356 -0.0583 0.114 Uiso 1 1 calc R . . C58 C 0.1779(3) 0.1503(5) 0.5278(6) 0.059(2) Uani 1 1 d U . . C59 C 0.1785(3) 0.1699(5) 0.4663(6) 0.065(2) Uani 1 1 d U . . H59 H 0.1817 0.1408 0.4349 0.078 Uiso 1 1 calc R . . C60 C 0.1745(3) 0.2317(5) 0.4490(5) 0.060(2) Uani 1 1 d U . . H60 H 0.1748 0.2449 0.4058 0.072 Uiso 1 1 calc R . . C61 C 0.1698(3) 0.2755(5) 0.4960(5) 0.0507(17) Uani 1 1 d U . . H61 H 0.1668 0.3181 0.4843 0.061 Uiso 1 1 calc R . . C62 C 0.1699(3) 0.2553(4) 0.5594(4) 0.0442(15) Uani 1 1 d U . . C63 C 0.1655(3) 0.2990(4) 0.6081(4) 0.0429(16) Uani 1 1 d . . . C64 C 0.1646(3) 0.2786(4) 0.6688(4) 0.0477(18) Uani 1 1 d . . . H64 H 0.1622 0.3074 0.7011 0.057 Uiso 1 1 calc R . . C65 C 0.1674(3) 0.2163(4) 0.6847(5) 0.0501(19) Uani 1 1 d . . . H65 H 0.1655 0.2031 0.7267 0.060 Uiso 1 1 calc R . . C66 C 0.1728(3) 0.1732(4) 0.6401(5) 0.0492(18) Uani 1 1 d . . . H66 H 0.1759 0.1307 0.6523 0.059 Uiso 1 1 calc R . . C67 C 0.1736(3) 0.1932(5) 0.5768(5) 0.0544(18) Uani 1 1 d U . . C68 C 0.1871(4) 0.0438(5) 0.5056(8) 0.072(3) Uani 1 1 d . . . H68A H 0.2178 0.0521 0.5031 0.087 Uiso 1 1 calc R . . H68B H 0.1593 0.0444 0.4553 0.087 Uiso 1 1 calc R . . C69 C 0.1903(6) -0.0177(6) 0.5397(12) 0.106(6) Uani 1 1 d . . . H69A H 0.1607 -0.0232 0.5460 0.127 Uiso 1 1 calc R . . H69B H 0.1894 -0.0499 0.5055 0.127 Uiso 1 1 calc R . . C70 C 0.2271(8) -0.0242(7) 0.6697(13) 0.118(7) Uani 1 1 d . . . H70A H 0.1975 -0.0477 0.6617 0.142 Uiso 1 1 calc R . . H70B H 0.2218 0.0193 0.6786 0.142 Uiso 1 1 calc R . . C71 C 0.2703(8) -0.0486(6) 0.7356(11) 0.111(6) Uani 1 1 d . . . H71A H 0.2620 -0.0537 0.7757 0.134 Uiso 1 1 calc R . . H71B H 0.2795 -0.0894 0.7247 0.134 Uiso 1 1 calc R . . C74 C 0.4455(5) 0.0238(10) 0.7697(9) 0.117(7) Uani 1 1 d . . . H74A H 0.4735 0.0283 0.8195 0.140 Uiso 1 1 calc R . . H74B H 0.4566 -0.0013 0.7408 0.140 Uiso 1 1 calc R . . C75 C 0.4305(5) 0.0846(11) 0.7363(8) 0.116(6) Uani 1 1 d . . . H75A H 0.4542 0.0999 0.7205 0.139 Uiso 1 1 calc R . . H75B H 0.3975 0.0824 0.6931 0.139 Uiso 1 1 calc R . . C76 C 0.4232(3) 0.1880(7) 0.7719(4) 0.084(3) Uani 1 1 d DU . . C77 C 0.4172(3) 0.2118(5) 0.7060(4) 0.092(3) Uani 1 1 d DU . . H77 H 0.4158 0.1852 0.6689 0.111 Uiso 1 1 calc R . . C78 C 0.4131(4) 0.2777(6) 0.6951(4) 0.117(4) Uani 1 1 d DU . . H78 H 0.4108 0.2949 0.6516 0.141 Uiso 1 1 calc R . . C79 C 0.4127(4) 0.3162(5) 0.7489(5) 0.099(4) Uani 1 1 d DU . . H79 H 0.4091 0.3595 0.7417 0.119 Uiso 1 1 calc R . . C80 C 0.4178(3) 0.2898(4) 0.8137(4) 0.082(3) Uani 1 1 d DU . . C81 C 0.4187(4) 0.3266(6) 0.8695(5) 0.084(4) Uani 1 1 d D . . C82 C 0.4226(4) 0.3039(3) 0.9329(4) 0.078(3) Uani 1 1 d D . . H82 H 0.4217 0.3305 0.9684 0.094 Uiso 1 1 calc R . . C83 C 0.4280(3) 0.2405(3) 0.9446(3) 0.060(2) Uani 1 1 d D . . H83 H 0.4309 0.2235 0.9884 0.072 Uiso 1 1 calc R . . C84 C 0.4292(3) 0.2021(3) 0.8919(3) 0.0500(18) Uani 1 1 d D . . H84 H 0.4341 0.1591 0.9007 0.060 Uiso 1 1 calc R . . C85 C 0.4232(3) 0.2265(4) 0.8255(3) 0.067(2) Uani 1 1 d DU . . C86 C 0.4064(6) 0.4291(6) 0.9108(13) 0.134(6) Uani 1 1 d U . . H86A H 0.4358 0.4265 0.9594 0.161 Uiso 1 1 calc R . . H86B H 0.3769 0.4175 0.9149 0.161 Uiso 1 1 calc R . . C87 C 0.4010(6) 0.4937(7) 0.8768(15) 0.156(8) Uani 1 1 d U . . H87A H 0.4047 0.5252 0.9134 0.187 Uiso 1 1 calc R . . H87B H 0.4276 0.5000 0.8638 0.187 Uiso 1 1 calc R . . C88 C 0.3521(7) 0.5575(6) 0.7856(12) 0.119(7) Uani 1 1 d . . . H88A H 0.3781 0.5630 0.7712 0.142 Uiso 1 1 calc R . . H88B H 0.3564 0.5897 0.8218 0.142 Uiso 1 1 calc R . . C89 C 0.2984(7) 0.5653(7) 0.7144(8) 0.103(5) Uani 1 1 d U . . H89A H 0.2721 0.5518 0.7255 0.124 Uiso 1 1 calc R . . H89B H 0.2925 0.6089 0.6987 0.124 Uiso 1 1 calc R . . C90 C 0.2555(9) 0.5524(10) 0.5997(12) 0.146(7) Uani 1 1 d U . . H90A H 0.2600 0.5973 0.5974 0.175 Uiso 1 1 calc R . . H90B H 0.2552 0.5343 0.5559 0.175 Uiso 1 1 calc R . . C91 C 0.2098(7) 0.5442(6) 0.5920(9) 0.098(4) Uani 1 1 d U . . H91A H 0.1850 0.5508 0.5404 0.118 Uiso 1 1 calc R . . H91B H 0.2039 0.5746 0.6223 0.118 Uiso 1 1 calc R . . C92 C 0.1581(7) 0.4675(5) 0.5995(5) 0.095(5) Uani 1 1 d . . . H92A H 0.1366 0.4659 0.5460 0.114 Uiso 1 1 calc R . . H92B H 0.1454 0.5001 0.6194 0.114 Uiso 1 1 calc R . . C93 C 0.1566(4) 0.4063(4) 0.6327(5) 0.0522(19) Uani 1 1 d . . . H93A H 0.1829 0.4040 0.6840 0.063 Uiso 1 1 calc R . . H93B H 0.1244 0.4004 0.6313 0.063 Uiso 1 1 calc R . . C94 C 0.1149(10) 0.2207(10) 0.9912(11) 0.160(10) Uani 1 1 d DU . . H94A H 0.1501 0.2237 1.0061 0.240 Uiso 1 1 calc R . . H94B H 0.0966 0.2118 0.9388 0.240 Uiso 1 1 calc R . . H94C H 0.1095 0.1875 1.0184 0.240 Uiso 1 1 calc R . . C95 C 0.2616(8) 0.2628(8) 0.1313(11) 0.119(6) Uani 1 1 d D . . H95A H 0.2847 0.2885 0.1234 0.178 Uiso 1 1 calc R . . H95B H 0.2734 0.2580 0.1838 0.178 Uiso 1 1 calc R . . H95C H 0.2291 0.2825 0.1089 0.178 Uiso 1 1 calc R . . C96 C 0.3625(9) 0.7196(10) 0.9133(12) 0.165(9) Uani 1 1 d DU . . H96A H 0.3890 0.7468 0.9175 0.247 Uiso 1 1 calc . . . H96B H 0.3724 0.6766 0.9138 0.247 Uiso 1 1 calc . . . H96C H 0.3561 0.7268 0.9544 0.247 Uiso 1 1 calc . . . C97 C 0.9311(8) 0.2201(7) 0.8218(9) 0.114(6) Uani 1 1 d D . . H97A H 0.9546 0.2079 0.8051 0.171 Uiso 1 1 calc . . . H97B H 0.9020 0.1936 0.7989 0.171 Uiso 1 1 calc . . . H97C H 0.9464 0.2159 0.8749 0.171 Uiso 1 1 calc . . . N1 N 0.2333(2) 0.0821(3) 0.9047(3) 0.0335(11) Uani 1 1 d . . . N2 N 0.0468(2) 0.1529(3) 0.4977(4) 0.0420(13) Uani 1 1 d . . . N3 N 0.0402(3) 0.3194(3) 0.2107(4) 0.0487(15) Uani 1 1 d . . . N4 N 0.1061(3) 0.4011(4) 0.1913(4) 0.0509(16) Uani 1 1 d . . . N5 N 0.2865(2) 0.3354(3) 0.6054(3) 0.0385(12) Uani 1 1 d . . . N6 N 0.3020(2) 0.1635(3) 0.8930(3) 0.0317(11) Uani 1 1 d . . . N7 N 0.3708(3) 0.1398(3) 1.0514(4) 0.0432(13) Uani 1 1 d U . . H7A H 0.3939 0.1222 1.0412 0.052 Uiso 1 1 calc R . . H7B H 0.3737 0.1819 1.0504 0.052 Uiso 1 1 calc R . . N8 N 0.3043(2) 0.0654(3) 1.0602(4) 0.0386(12) Uani 1 1 d U . . H8A H 0.2822 0.0820 1.0733 0.046 Uiso 1 1 calc R . . H8B H 0.2953 0.0252 1.0465 0.046 Uiso 1 1 calc R . . N9 N 0.0368(3) 0.4115(5) 0.0366(4) 0.069(2) Uani 1 1 d U . . H9A H 0.0422 0.4531 0.0450 0.083 Uiso 1 1 calc R . . H9B H 0.0594 0.3955 0.0240 0.083 Uiso 1 1 calc R . . N10 N -0.0282(3) 0.3367(6) 0.0528(5) 0.077(3) Uani 1 1 d U . . H10A H -0.0316 0.2968 0.0646 0.092 Uiso 1 1 calc R . . H10B H -0.0512 0.3602 0.0578 0.092 Uiso 1 1 calc R . . N11 N 0.0988(5) 0.2758(6) 1.0055(9) 0.174(8) Uani 1 1 d DU . . N12 N 0.2581(4) 0.2078(5) 0.1012(8) 0.126(6) Uani 1 1 d D . . N13 N 0.3187(6) 0.7320(6) 0.8461(9) 0.149(6) Uani 1 1 d DU . . N14 N 0.9166(7) 0.2837(7) 0.8016(11) 0.129(5) Uani 1 1 d D . . O1 O 0.1801(3) 0.0896(3) 0.5486(5) 0.075(2) Uani 1 1 d . . . O2 O 0.2321(4) -0.0272(4) 0.6073(7) 0.092(3) Uani 1 1 d . . . O3 O 0.3088(4) -0.0087(3) 0.7564(6) 0.091(3) Uani 1 1 d . . . O4 O 0.4032(6) -0.0093(5) 0.7740(5) 0.127(5) Uani 1 1 d . . . O5 O 0.4296(3) 0.1255(4) 0.7903(4) 0.074(2) Uani 1 1 d . . . O6 O 0.4119(4) 0.3898(4) 0.8554(8) 0.123(5) Uani 1 1 d U . . O7 O 0.3568(4) 0.5014(4) 0.8163(8) 0.120(4) Uani 1 1 d U . . O8 O 0.2989(5) 0.5298(5) 0.6617(7) 0.109(3) Uani 1 1 d U . . O9 O 0.2050(4) 0.4815(4) 0.6145(5) 0.081(2) Uani 1 1 d U . . O10 O 0.1641(2) 0.3595(3) 0.5886(3) 0.0484(13) Uani 1 1 d . . . O11 O 0.1285(7) 0.3139(6) 1.0491(6) 0.192(8) Uani 1 1 d DU . . O12 O 0.0535(5) 0.2855(16) 0.977(2) 0.45(3) Uani 1 1 d DU . . O13 O 0.2852(7) 0.1730(8) 0.1525(8) 0.197(9) Uani 1 1 d D . . O14 O 0.2320(6) 0.1859(10) 0.0390(8) 0.237(13) Uani 1 1 d D . . O15 O 0.3000(11) 0.7844(8) 0.834(2) 0.48(3) Uani 1 1 d DU . . O16 O 0.3003(5) 0.6882(4) 0.8058(6) 0.107(3) Uani 1 1 d DU . . O17 O 0.9434(7) 0.3269(6) 0.8025(8) 0.187(9) Uani 1 1 d D . . O18 O 0.8777(9) 0.2943(10) 0.7920(16) 0.220(11) Uani 1 1 d . . . F1 F 0.3589(3) 0.1227(3) 0.4520(3) 0.0680(15) Uani 1 1 d . . . F2 F 0.2832(3) 0.1030(3) 0.4413(4) 0.0685(15) Uani 1 1 d . . . F3 F 0.3357(3) 0.1655(3) 0.5299(4) 0.080(2) Uani 1 1 d . . . F4 F 0.3943(2) 0.0905(3) 0.5697(3) 0.0743(17) Uani 1 1 d . . . F5 F 0.3196(3) 0.0711(2) 0.5587(3) 0.0641(15) Uani 1 1 d . . . F6 F 0.3406(2) 0.0282(2) 0.4794(3) 0.0534(11) Uani 1 1 d . . . F7 F 0.0527(3) 0.4225(5) 0.6516(5) 0.103(3) Uani 1 1 d . . . F8 F -0.0227(4) 0.3974(7) 0.6302(5) 0.147(5) Uani 1 1 d . . . F9 F -0.0061(3) 0.4913(6) 0.6037(6) 0.128(4) Uani 1 1 d . . . F10 F -0.0540(4) 0.4280(6) 0.5121(5) 0.137(4) Uani 1 1 d . . . F11 F 0.0065(5) 0.3573(6) 0.5593(5) 0.145(5) Uani 1 1 d . . . F12 F 0.0231(5) 0.4518(5) 0.5336(7) 0.140(4) Uani 1 1 d . . . F13 F 0.9984(4) 0.9672(7) 0.3201(7) 0.156(5) Uani 1 1 d . . . F14 F 1.0734(3) 0.9885(4) 0.4028(5) 0.101(2) Uani 1 1 d . . . F15 F 1.0695(4) 0.9156(8) 0.4751(9) 0.177(7) Uani 1 1 d . . . F16 F 0.9965(6) 0.8877(5) 0.3905(8) 0.157(6) Uani 1 1 d . . . F17 F 1.0588(9) 0.8917(5) 0.3663(15) 0.253(12) Uani 1 1 d . . . F18 F 1.0121(4) 0.9832(3) 0.4285(6) 0.109(3) Uani 1 1 d . . . F19 F 0.0315(5) 0.4150(4) 0.8373(8) 0.156(5) Uani 1 1 d . . . F20 F 0.0986(7) 0.4220(7) 0.8371(9) 0.178(6) Uani 1 1 d . . . F21 F 0.0618(5) 0.5062(4) 0.8264(6) 0.122(3) Uani 1 1 d . . . F22 F 0.1246(4) 0.4995(7) 0.9168(6) 0.145(4) Uani 1 1 d . . . F23 F 0.0562(4) 0.4877(5) 0.9237(4) 0.107(3) Uani 1 1 d . . . F24 F 0.1026(5) 0.4120(6) 0.9466(7) 0.145(4) Uani 1 1 d . . . F25 F 0.1485(8) 0.1383(7) 0.1393(8) 0.213(9) Uani 1 1 d . . . F26 F 0.1973(4) 0.1374(3) 0.2702(6) 0.109(3) Uani 1 1 d . . . F27 F 0.1488(4) 0.2173(5) 0.2671(5) 0.124(3) Uani 1 1 d . . . F28 F 0.1063(4) 0.2163(4) 0.1475(6) 0.112(3) Uani 1 1 d . . . F29 F 0.1163(6) 0.1260(6) 0.2030(7) 0.167(6) Uani 1 1 d . . . F30 F 0.1871(4) 0.2187(5) 0.1964(8) 0.148(5) Uani 1 1 d . . . F31 F 0.1271(3) 0.3136(6) 0.8643(9) 0.132(7) Uani 0.40 1 d PDU . . F32 F 0.1575(4) 0.4095(4) 0.8986(9) 0.077(4) Uani 0.40 1 d PDU . . F33 F 0.1599(7) 0.3658(6) 0.8034(4) 0.177(10) Uani 0.40 1 d PDU . . F34 F 0.1966(4) 0.2860(4) 0.8609(8) 0.064(3) Uani 0.40 1 d PDU . . F35 F 0.1964(7) 0.3314(12) 0.9705(4) 0.112(6) Uani 0.40 1 d PDU . . F37 F 0.3341(4) 0.2815(9) 0.0590(10) 0.200(7) Uani 0.60 1 d PDU . . F38 F 0.3934(7) 0.2596(4) 0.1595(6) 0.115(5) Uani 0.60 1 d PDU . . F39 F 0.3588(5) 0.3545(5) 0.1389(7) 0.110(4) Uani 0.60 1 d PDU . . F40 F 0.3781(14) 0.3689(7) 0.0477(13) 0.258(11) Uani 0.60 1 d PDU . . F41 F 0.4386(4) 0.3471(10) 0.1503(14) 0.233(10) Uani 0.60 1 d PDU . . F42 F 0.4085(6) 0.2723(4) 0.0645(7) 0.228(10) Uani 0.60 1 d PDU . . P1 P 0.33837(13) 0.09726(12) 0.50476(18) 0.0536(5) Uani 1 1 d . . . P2 P -0.00021(17) 0.4239(2) 0.5818(3) 0.1007(14) Uani 1 1 d . . . P3 P 1.03450(15) 0.93611(15) 0.3953(3) 0.0808(9) Uani 1 1 d . . . P4 P 0.0749(2) 0.45897(18) 0.8788(3) 0.1001(13) Uani 1 1 d . . . P5 P 0.15195(18) 0.17639(14) 0.2092(3) 0.0969(13) Uani 1 1 d . . . P6 P 0.17887(17) 0.3460(3) 0.8864(3) 0.0584(13) Uani 0.40 1 d PDU . . P7 P 0.3862(2) 0.31475(17) 0.1043(3) 0.101(2) Uani 0.60 1 d PDU . . Pd1 Pd 0.30176(8) 0.11324(2) 0.97510(13) 0.03376(12) Uani 1 1 d . . . Pd2 Pd 0.03861(9) 0.36650(3) 0.12460(13) 0.05438(19) Uani 1 1 d . . . F36 F 0.2289(5) 0.3844(9) 0.9162(18) 0.144(8) Uani 0.40 1 d PDU . . C72 C 0.3531(7) -0.0335(6) 0.8184(7) 0.110(6) Uani 1 1 d D . . H72A H 0.3602 -0.0755 0.8076 0.132 Uiso 1 1 calc R . . H72B H 0.3490 -0.0349 0.8627 0.132 Uiso 1 1 calc R . . C73A C 0.3932(6) 0.0098(7) 0.8284(6) 0.102(6) Uani 1 1 d D . . H73A H 0.3819 0.0531 0.8213 0.122 Uiso 1 1 calc R . . H73B H 0.4223 0.0052 0.8771 0.122 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.045(4) 0.041(4) 0.035(4) 0.001(3) 0.014(3) -0.002(3) C2 0.047(4) 0.053(5) 0.051(5) 0.002(3) 0.018(4) -0.005(3) C3 0.039(4) 0.048(4) 0.044(4) -0.001(3) 0.021(3) -0.003(3) C4 0.031(3) 0.063(5) 0.037(4) 0.008(3) 0.013(3) 0.009(3) C5 0.035(4) 0.042(4) 0.046(4) 0.003(3) 0.020(3) 0.001(3) C6 0.043(4) 0.069(5) 0.046(4) 0.004(4) 0.008(3) -0.022(4) C7 0.037(4) 0.069(5) 0.045(4) -0.006(4) 0.018(3) -0.012(3) C8 0.040(4) 0.065(5) 0.063(5) 0.004(4) 0.027(4) -0.005(4) C9 0.038(4) 0.057(5) 0.054(4) -0.001(3) 0.025(3) 0.002(3) C10 0.032(3) 0.056(4) 0.038(4) -0.004(3) 0.011(3) -0.003(3) C11 0.036(4) 0.062(5) 0.071(6) 0.014(4) 0.032(4) 0.010(3) C12 0.033(4) 0.098(7) 0.041(4) -0.007(4) 0.014(3) 0.000(4) C13 0.028(3) 0.050(4) 0.050(4) -0.012(3) 0.009(3) -0.001(3) C14 0.030(3) 0.044(4) 0.043(4) -0.008(3) 0.010(3) 0.002(3) C15 0.023(3) 0.041(3) 0.048(4) -0.006(3) 0.013(3) 0.009(2) C16 0.020(3) 0.055(4) 0.036(4) -0.003(3) 0.004(2) -0.001(3) C17 0.020(3) 0.062(5) 0.047(4) -0.009(3) 0.008(3) 0.002(3) C18 0.034(3) 0.047(4) 0.043(4) -0.015(3) 0.003(3) 0.005(3) C19 0.037(3) 0.042(4) 0.040(4) -0.009(3) 0.007(3) 0.006(3) C20 0.028(3) 0.046(4) 0.049(4) -0.002(3) 0.014(3) 0.005(3) C21 0.029(3) 0.039(3) 0.045(4) -0.003(3) 0.010(3) 0.010(3) C22 0.048(4) 0.043(4) 0.060(5) -0.019(3) 0.024(4) -0.006(3) C23 0.053(4) 0.043(4) 0.054(5) -0.016(3) 0.025(4) 0.002(3) C24 0.038(4) 0.050(4) 0.040(4) -0.010(3) 0.012(3) 0.008(3) C25 0.046(4) 0.056(5) 0.041(4) -0.010(3) 0.020(3) 0.005(3) C26 0.047(4) 0.042(4) 0.056(5) -0.011(3) 0.022(4) 0.008(3) C27 0.067(6) 0.061(5) 0.042(4) 0.018(4) 0.025(4) 0.016(4) C28 0.064(6) 0.066(5) 0.056(5) 0.025(4) 0.035(5) 0.021(4) C29 0.062(5) 0.060(5) 0.027(3) 0.017(3) 0.019(3) 0.007(4) C30 0.073(6) 0.056(5) 0.033(4) 0.010(3) 0.021(4) 0.004(4) C31 0.063(5) 0.068(5) 0.037(4) 0.013(3) 0.024(4) 0.019(4) C32 0.059(5) 0.079(6) 0.041(4) 0.025(4) 0.024(4) 0.003(4) C34 0.046(4) 0.063(5) 0.040(4) 0.024(4) 0.010(3) -0.001(4) C35 0.065(6) 0.083(7) 0.039(4) 0.018(4) 0.027(4) 0.005(5) C36 0.044(4) 0.071(6) 0.037(4) 0.018(4) 0.013(3) 0.006(4) C37 0.044(4) 0.040(3) 0.029(3) 0.004(3) 0.011(3) -0.001(3) C38 0.046(4) 0.050(4) 0.045(4) 0.012(3) 0.019(3) 0.001(3) C39 0.055(5) 0.050(4) 0.052(5) 0.021(3) 0.023(4) 0.009(4) C40 0.038(3) 0.031(3) 0.035(3) 0.001(2) 0.010(3) 0.003(3) C41 0.027(3) 0.025(3) 0.030(3) 0.001(2) 0.008(2) 0.001(2) C42 0.023(3) 0.032(3) 0.025(3) -0.003(2) 0.004(2) -0.002(2) C43 0.027(3) 0.033(3) 0.025(3) 0.004(2) 0.009(2) 0.002(2) C44 0.036(3) 0.035(3) 0.030(3) 0.003(2) 0.013(3) -0.002(2) C45 0.032(3) 0.038(3) 0.033(3) -0.002(2) 0.020(3) 0.002(2) C46 0.033(3) 0.028(3) 0.032(3) -0.002(2) 0.014(2) 0.002(2) C47 0.031(3) 0.030(3) 0.026(3) -0.003(2) 0.013(2) -0.003(2) C48 0.020(2) 0.028(3) 0.027(3) -0.005(2) 0.006(2) -0.005(2) C49 0.043(4) 0.039(3) 0.034(3) -0.005(3) 0.013(3) 0.003(3) C50 0.046(4) 0.036(3) 0.023(3) -0.002(2) 0.009(3) 0.000(3) C51 0.024(3) 0.036(3) 0.024(3) -0.005(2) 0.006(2) -0.001(2) C52 0.035(3) 0.037(3) 0.033(3) -0.006(2) 0.014(3) -0.001(3) C53 0.028(3) 0.027(3) 0.036(3) 0.002(2) 0.011(2) 0.000(2) C54 0.099(9) 0.157(12) 0.042(5) -0.014(6) 0.029(6) -0.068(8) C55 0.079(7) 0.147(11) 0.047(5) 0.035(6) -0.004(5) -0.052(7) C56 0.170(11) 0.093(8) 0.030(5) 0.012(5) -0.023(6) 0.023(7) C57 0.085(8) 0.131(9) 0.060(6) -0.010(7) 0.027(6) 0.017(6) C58 0.036(4) 0.065(5) 0.082(6) -0.031(4) 0.034(4) -0.016(4) C59 0.047(4) 0.085(5) 0.072(5) -0.041(5) 0.035(4) -0.013(4) C60 0.044(4) 0.089(5) 0.043(4) -0.031(4) 0.019(4) -0.013(4) C61 0.036(3) 0.075(5) 0.045(4) -0.023(3) 0.022(3) -0.008(3) C62 0.025(3) 0.068(4) 0.037(4) -0.013(3) 0.012(3) -0.003(3) C63 0.029(3) 0.060(5) 0.035(3) -0.010(3) 0.012(3) 0.006(3) C64 0.029(3) 0.072(5) 0.036(4) -0.015(3) 0.010(3) 0.003(3) C65 0.032(3) 0.074(5) 0.043(4) -0.014(4) 0.017(3) 0.002(3) C66 0.027(3) 0.057(4) 0.064(5) -0.015(4) 0.022(3) -0.008(3) C67 0.026(3) 0.077(5) 0.060(5) -0.022(4) 0.020(3) -0.006(3) C68 0.047(5) 0.076(6) 0.112(9) -0.041(6) 0.052(6) -0.012(4) C69 0.089(10) 0.074(8) 0.187(18) -0.043(10) 0.092(12) -0.008(7) C70 0.165(16) 0.068(7) 0.22(2) -0.047(11) 0.167(17) -0.044(9) C71 0.193(19) 0.059(7) 0.162(16) 0.024(8) 0.149(16) 0.008(9) C74 0.060(7) 0.161(16) 0.087(10) -0.064(10) 0.000(7) 0.025(9) C75 0.050(6) 0.22(2) 0.069(8) -0.021(10) 0.018(6) 0.022(9) C76 0.026(4) 0.179(9) 0.044(5) 0.012(5) 0.014(3) -0.009(5) C77 0.029(4) 0.183(10) 0.054(5) 0.024(6) 0.011(4) 0.008(6) C78 0.032(4) 0.208(12) 0.104(8) 0.064(8) 0.026(6) -0.007(7) C79 0.037(4) 0.134(9) 0.109(8) 0.063(7) 0.020(6) -0.004(6) C80 0.021(3) 0.112(7) 0.091(7) 0.046(6) 0.009(4) -0.005(4) C81 0.038(5) 0.083(7) 0.098(9) 0.029(7) 0.007(5) -0.010(5) C82 0.038(4) 0.080(7) 0.089(8) 0.019(6) 0.009(5) 0.001(4) C83 0.036(4) 0.064(5) 0.063(6) 0.004(4) 0.010(4) 0.000(4) C84 0.031(3) 0.060(5) 0.049(4) 0.003(3) 0.011(3) -0.004(3) C85 0.027(3) 0.098(6) 0.063(5) 0.022(4) 0.011(4) 0.002(4) C86 0.077(8) 0.049(6) 0.216(15) 0.017(7) 0.021(9) -0.002(6) C87 0.069(7) 0.060(6) 0.254(19) 0.021(8) 0.008(9) -0.005(6) C88 0.147(15) 0.061(7) 0.20(2) 0.027(9) 0.125(16) 0.028(8) C89 0.172(13) 0.092(8) 0.094(7) 0.050(6) 0.102(9) 0.058(9) C90 0.150(10) 0.116(12) 0.133(10) 0.024(9) 0.035(9) -0.061(10) C91 0.138(8) 0.052(5) 0.092(9) 0.002(5) 0.046(8) 0.000(7) C92 0.161(14) 0.071(7) 0.034(5) 0.003(4) 0.032(6) 0.062(8) C93 0.062(5) 0.062(5) 0.039(4) -0.005(3) 0.029(4) 0.016(4) C94 0.179(19) 0.121(13) 0.109(13) -0.029(11) 0.011(13) 0.065(13) C95 0.170(18) 0.092(11) 0.115(12) -0.032(9) 0.085(13) -0.032(11) C96 0.176(18) 0.149(15) 0.132(14) -0.036(12) 0.044(10) -0.094(13) C97 0.163(18) 0.089(10) 0.094(11) 0.016(8) 0.065(12) 0.029(10) N1 0.035(3) 0.036(3) 0.030(3) 0.009(2) 0.016(2) 0.000(2) N2 0.024(2) 0.053(4) 0.046(3) -0.003(3) 0.013(2) 0.001(2) N3 0.046(3) 0.054(4) 0.049(4) -0.005(3) 0.024(3) 0.011(3) N4 0.057(4) 0.061(4) 0.036(3) 0.007(3) 0.024(3) 0.017(3) N5 0.037(3) 0.040(3) 0.032(3) 0.003(2) 0.011(2) -0.001(2) N6 0.030(3) 0.035(3) 0.028(3) 0.001(2) 0.013(2) -0.002(2) N7 0.037(3) 0.054(4) 0.038(3) 0.005(3) 0.017(3) -0.005(3) N8 0.042(3) 0.039(3) 0.039(3) 0.010(2) 0.022(3) -0.004(2) N9 0.072(5) 0.090(6) 0.040(4) 0.002(4) 0.023(4) 0.032(4) N10 0.049(4) 0.119(8) 0.051(4) -0.014(4) 0.015(4) 0.024(5) N11 0.202(15) 0.136(13) 0.23(2) -0.066(13) 0.139(16) -0.001(11) N12 0.086(9) 0.080(8) 0.196(17) -0.028(10) 0.054(10) 0.025(6) N13 0.168(14) 0.129(10) 0.149(12) -0.086(10) 0.076(9) -0.036(9) N14 0.108(11) 0.129(14) 0.153(14) -0.020(11) 0.064(10) -0.017(10) O1 0.085(5) 0.057(4) 0.121(6) -0.032(4) 0.080(5) -0.016(4) O2 0.111(7) 0.060(4) 0.166(10) -0.005(5) 0.115(8) -0.008(4) O3 0.148(8) 0.045(4) 0.114(7) 0.026(4) 0.089(7) 0.012(4) O4 0.181(13) 0.086(6) 0.051(5) -0.011(4) 0.005(6) 0.033(7) O5 0.050(4) 0.093(5) 0.048(4) -0.008(3) -0.001(3) 0.011(4) O6 0.060(5) 0.067(5) 0.192(12) 0.041(6) 0.019(6) 0.005(4) O7 0.073(5) 0.053(4) 0.208(11) 0.044(6) 0.046(6) -0.002(4) O8 0.137(7) 0.093(7) 0.120(7) 0.000(5) 0.079(6) -0.010(6) O9 0.085(5) 0.055(4) 0.099(6) 0.020(4) 0.040(5) 0.015(4) O10 0.045(3) 0.060(3) 0.037(3) -0.017(2) 0.017(2) 0.007(2) O11 0.39(2) 0.109(8) 0.076(7) -0.008(6) 0.111(11) -0.056(12) O12 0.241(16) 0.37(4) 0.59(5) -0.22(4) 0.09(3) 0.14(2) O13 0.191(18) 0.171(16) 0.24(2) 0.107(16) 0.116(17) 0.067(15) O14 0.167(16) 0.31(3) 0.184(17) -0.054(18) 0.046(13) 0.155(19) O15 0.32(3) 0.190(17) 0.51(4) -0.22(2) -0.15(3) 0.09(2) O16 0.157(10) 0.077(5) 0.088(6) -0.023(5) 0.059(6) -0.014(6) O17 0.253(19) 0.095(8) 0.095(8) 0.015(7) -0.013(10) -0.059(11) O18 0.167(18) 0.164(17) 0.32(3) 0.038(18) 0.11(2) 0.061(14) F1 0.078(4) 0.094(4) 0.042(3) -0.004(2) 0.037(3) -0.022(3) F2 0.067(3) 0.051(3) 0.076(4) -0.006(3) 0.025(3) -0.009(2) F3 0.137(6) 0.055(3) 0.069(4) -0.021(3) 0.065(4) -0.031(3) F4 0.068(3) 0.104(5) 0.041(3) 0.000(3) 0.018(3) -0.032(3) F5 0.106(4) 0.051(3) 0.070(3) -0.012(2) 0.071(3) -0.019(3) F6 0.065(3) 0.058(3) 0.046(2) -0.006(2) 0.034(2) -0.002(2) F7 0.082(5) 0.135(7) 0.107(6) -0.057(5) 0.055(5) -0.049(5) F8 0.091(6) 0.256(14) 0.080(6) 0.006(7) 0.030(5) -0.092(8) F9 0.075(5) 0.204(11) 0.112(7) -0.038(7) 0.050(5) -0.042(6) F10 0.111(7) 0.204(12) 0.074(5) 0.001(6) 0.027(5) -0.081(7) F11 0.204(11) 0.159(9) 0.062(5) -0.052(5) 0.056(6) -0.118(9) F12 0.166(10) 0.134(8) 0.181(10) -0.041(7) 0.132(9) -0.079(7) F13 0.112(8) 0.196(13) 0.127(9) 0.030(8) 0.030(7) -0.053(8) F14 0.065(4) 0.107(6) 0.128(6) 0.013(5) 0.043(4) -0.020(4) F15 0.110(8) 0.213(14) 0.221(15) 0.113(12) 0.089(9) 0.045(9) F16 0.232(14) 0.099(6) 0.224(14) -0.072(7) 0.176(13) -0.091(8) F17 0.37(2) 0.085(7) 0.54(4) -0.020(12) 0.41(3) -0.013(10) F18 0.118(6) 0.064(4) 0.180(9) -0.022(5) 0.100(7) -0.017(4) F19 0.141(9) 0.072(5) 0.178(11) 0.001(6) 0.014(8) -0.029(6) F20 0.254(17) 0.174(12) 0.179(12) 0.026(10) 0.162(14) 0.059(12) F21 0.194(10) 0.080(5) 0.146(8) 0.029(5) 0.125(8) 0.008(6) F22 0.135(9) 0.205(13) 0.090(6) -0.018(7) 0.050(6) -0.051(8) F23 0.119(6) 0.142(7) 0.053(4) -0.013(4) 0.035(4) -0.040(6) F24 0.174(11) 0.138(9) 0.115(8) 0.032(7) 0.060(8) 0.036(8) F25 0.34(2) 0.180(13) 0.151(11) 0.024(10) 0.141(14) 0.153(15) F26 0.126(7) 0.069(4) 0.172(9) 0.042(5) 0.104(7) 0.039(4) F27 0.154(9) 0.126(7) 0.092(6) -0.003(5) 0.059(6) 0.063(6) F28 0.117(7) 0.086(5) 0.158(8) -0.013(5) 0.087(7) 0.021(5) F29 0.196(14) 0.123(8) 0.122(9) 0.014(7) 0.026(9) -0.065(8) F30 0.086(6) 0.133(8) 0.246(14) 0.089(9) 0.095(8) 0.026(5) F31 0.055(8) 0.154(15) 0.184(17) -0.082(15) 0.054(10) -0.024(9) F32 0.062(7) 0.103(8) 0.072(8) -0.019(7) 0.036(7) 0.016(7) F33 0.44(3) 0.044(7) 0.080(8) 0.002(6) 0.149(14) 0.063(12) F34 0.040(6) 0.051(6) 0.100(10) -0.003(6) 0.032(6) -0.001(5) F35 0.123(15) 0.134(16) 0.076(7) 0.009(8) 0.044(9) 0.000(12) F37 0.261(13) 0.131(13) 0.086(10) -0.051(8) -0.017(10) -0.040(12) F38 0.187(14) 0.076(7) 0.083(8) 0.005(5) 0.065(8) -0.014(7) F39 0.200(14) 0.063(6) 0.091(8) -0.021(5) 0.089(10) -0.017(7) F40 0.61(4) 0.088(10) 0.211(16) 0.037(10) 0.31(2) 0.026(15) F41 0.239(13) 0.131(15) 0.39(3) -0.119(15) 0.195(16) -0.106(14) F42 0.53(3) 0.059(7) 0.27(2) -0.046(10) 0.34(2) -0.046(12) P1 0.0664(14) 0.0608(12) 0.0417(11) -0.0127(9) 0.0323(11) -0.0219(11) P2 0.088(2) 0.138(3) 0.087(2) -0.041(2) 0.050(2) -0.071(2) P3 0.0791(19) 0.0693(17) 0.111(3) 0.0069(16) 0.059(2) -0.0039(14) P4 0.154(4) 0.081(2) 0.082(2) -0.0052(17) 0.070(3) -0.017(2) P5 0.114(3) 0.0504(14) 0.177(4) 0.0079(18) 0.110(3) 0.0148(16) P6 0.055(3) 0.060(3) 0.063(3) 0.001(3) 0.030(3) 0.001(2) P7 0.220(7) 0.0384(19) 0.075(3) -0.0217(19) 0.096(4) -0.025(3) Pd1 0.0354(2) 0.0356(2) 0.0313(2) 0.0021(2) 0.01666(18) -0.0001(2) Pd2 0.0519(4) 0.0667(4) 0.0387(3) 0.0027(3) 0.0167(3) 0.0195(3) F36 0.111(10) 0.073(11) 0.31(2) -0.033(13) 0.151(15) -0.029(8) C72 0.207(19) 0.064(7) 0.058(7) 0.031(6) 0.062(10) 0.036(10) C73A 0.141(13) 0.107(10) 0.032(5) 0.011(5) 0.021(6) 0.062(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.321(10) . ? C1 C2 1.378(11) . ? C2 C3 1.366(12) . ? C3 C4 1.374(12) . ? C3 C6 1.529(11) . ? C4 C5 1.372(11) . ? C5 N1 1.371(10) . ? C6 C7 1.516(12) . ? C7 C8 1.341(13) . ? C7 C12 1.380(14) . ? C8 C9 1.376(13) . ? C9 C10 1.404(12) . ? C10 N2 1.416(11) . ? C10 C11 1.428(13) . ? C11 C12 1.374(14) . ? C13 N2 1.354(10) . ? C13 C14 1.380(13) . ? C14 C15 1.404(11) . ? C14 C22 1.471(11) . ? C15 C21 1.383(11) . ? C15 C16 1.426(10) . ? C16 C17 1.408(12) . ? C16 C18 1.442(12) . ? C17 N2 1.338(11) . ? C18 C19 1.345(13) . ? C19 C20 1.441(11) . ? C20 C26 1.380(13) . ? C20 C21 1.397(11) . ? C21 C24 1.431(11) . ? C22 C23 1.355(14) . ? C23 C24 1.445(12) . ? C24 C25 1.363(13) . ? C25 N3 1.329(11) . ? C26 N3 1.355(11) . ? C27 N4 1.328(12) . ? C27 C28 1.374(16) . ? C28 C29 1.423(14) . ? C29 C30 1.360(14) . ? C29 C32 1.502(13) . ? C30 C31 1.389(14) . ? C31 N4 1.325(13) . ? C32 C34 1.525(10) . ? C34 C39 1.380(14) . ? C34 C35 1.394(14) . ? C35 C36 1.385(11) . ? C36 C37 1.388(13) . ? C37 C38 1.351(12) . ? C37 N5 1.485(9) . ? C38 C39 1.382(11) . ? C40 N5 1.315(10) . ? C40 C41 1.379(10) . ? C41 C42 1.411(9) . ? C41 C49 1.428(10) . ? C42 C48 1.420(9) . ? C42 C43 1.422(9) . ? C43 C44 1.375(9) . ? C43 C45 1.429(9) . ? C44 N5 1.356(9) . ? C45 C46 1.329(9) . ? C46 C47 1.454(8) . ? C47 C53 1.375(9) . ? C47 C48 1.419(9) . ? C48 C51 1.402(8) . ? C49 C50 1.346(11) . ? C50 C51 1.440(9) . ? C51 C52 1.409(10) . ? C52 N6 1.340(9) . ? C53 N6 1.343(9) . ? C54 N7 1.406(12) . ? C54 C55 1.422(5) . ? C55 N8 1.453(12) . ? C56 C57 1.40(2) . ? C56 N9 1.669(19) . ? C57 N10 1.484(16) . ? C58 C59 1.361(16) . ? C58 O1 1.379(14) . ? C58 C67 1.434(12) . ? C59 C60 1.379(17) . ? C60 C61 1.421(11) . ? C61 C62 1.392(12) . ? C62 C67 1.388(14) . ? C62 C63 1.442(10) . ? C63 C64 1.353(12) . ? C63 O10 1.371(11) . ? C64 C65 1.385(14) . ? C65 C66 1.385(11) . ? C66 C67 1.401(14) . ? C68 O1 1.423(11) . ? C68 C69 1.50(2) . ? C69 O2 1.40(2) . ? C70 O2 1.385(19) . ? C70 C71 1.49(3) . ? C71 O3 1.37(2) . ? C74 C75 1.46(3) . ? C74 O4 1.53(2) . ? C75 O5 1.444(18) . ? C76 C85 1.396(11) . ? C76 C77 1.395(5) . ? C76 O5 1.400(15) . ? C77 C78 1.445(14) . ? C78 C79 1.405(5) . ? C79 C80 1.405(5) . ? C80 C85 1.393(10) . ? C80 C81 1.400(11) . ? C81 C82 1.361(9) . ? C81 O6 1.401(15) . ? C82 C83 1.396(5) . ? C83 C84 1.393(5) . ? C84 C85 1.409(4) . ? C86 O6 1.51(3) . ? C86 C87 1.54(2) . ? C87 O7 1.36(2) . ? C88 O7 1.352(16) . ? C88 C89 1.63(3) . ? C89 O8 1.348(17) . ? C90 C91 1.35(3) . ? C90 O8 1.44(2) . ? C91 O9 1.472(15) . ? C92 O9 1.363(19) . ? C92 C93 1.510(17) . ? C93 O10 1.461(9) . ? C94 N11 1.38(2) . ? C95 N12 1.332(19) . ? C96 N13 1.436(17) . ? C97 N14 1.451(16) . ? N1 Pd1 2.032(6) . ? N3 Pd2 2.046(8) . ? N4 Pd2 2.022(8) . ? N6 Pd1 2.034(5) . ? N7 Pd1 2.046(6) . ? N8 Pd1 2.026(5) . ? N9 Pd2 2.057(9) . ? N10 Pd2 1.995(9) . ? N11 O11 1.2495(11) . ? N11 O12 1.2500(11) . ? N12 O14 1.2498(11) . ? N12 O13 1.2504(11) . ? N13 O16 1.217(15) . ? N13 O15 1.247(5) . ? N14 O18 1.14(2) . ? N14 O17 1.246(5) . ? O3 C72 1.466(18) . ? O4 C73A 1.371(18) . ? F1 P1 1.606(5) . ? F2 P1 1.588(7) . ? F3 P1 1.588(6) . ? F4 P1 1.617(7) . ? F5 P1 1.596(5) . ? F6 P1 1.602(6) . ? F7 P2 1.589(10) . ? F8 P2 1.580(9) . ? F9 P2 1.572(14) . ? F10 P2 1.607(10) . ? F11 P2 1.564(14) . ? F12 P2 1.609(9) . ? F13 P3 1.579(13) . ? F14 P3 1.607(8) . ? F15 P3 1.557(14) . ? F16 P3 1.542(9) . ? F17 P3 1.513(11) . ? F18 P3 1.570(9) . ? F19 P4 1.535(11) . ? F20 P4 1.595(12) . ? F20 F32 1.68(2) . ? F21 P4 1.411(9) . ? F22 P4 1.613(12) . ? F23 P4 1.454(10) . ? F24 P4 1.619(12) . ? F25 P5 1.635(13) . ? F26 P5 1.613(10) . ? F27 P5 1.538(9) . ? F28 P5 1.635(11) . ? F29 P5 1.514(13) . ? F30 P5 1.540(9) . ? F31 P6 1.6001(10) . ? F32 P6 1.6007(11) . ? F33 P6 1.5997(11) . ? F34 P6 1.6009(10) . ? F35 P6 1.5998(11) . ? F37 P7 1.6002(10) . ? F38 P7 1.6001(10) . ? F39 P7 1.5996(10) . ? F40 P7 1.5997(10) . ? F41 P7 1.5995(10) . ? F42 P7 1.6000(10) . ? P6 F36 1.6003(11) . ? C72 C73A 1.490(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.1(8) . . ? C3 C2 C1 119.4(8) . . ? C2 C3 C4 118.0(7) . . ? C2 C3 C6 120.8(8) . . ? C4 C3 C6 121.1(7) . . ? C5 C4 C3 120.9(7) . . ? N1 C5 C4 120.4(7) . . ? C7 C6 C3 109.5(7) . . ? C8 C7 C12 120.2(9) . . ? C8 C7 C6 120.2(9) . . ? C12 C7 C6 119.2(8) . . ? C7 C8 C9 122.7(9) . . ? C8 C9 C10 118.7(8) . . ? C9 C10 N2 119.4(7) . . ? C9 C10 C11 118.4(8) . . ? N2 C10 C11 122.2(7) . . ? C12 C11 C10 119.8(8) . . ? C11 C12 C7 120.1(8) . . ? N2 C13 C14 120.3(7) . . ? C13 C14 C15 119.9(7) . . ? C13 C14 C22 120.3(7) . . ? C15 C14 C22 119.8(8) . . ? C21 C15 C14 121.4(7) . . ? C21 C15 C16 119.6(7) . . ? C14 C15 C16 118.9(7) . . ? C17 C16 C15 117.7(7) . . ? C17 C16 C18 123.5(7) . . ? C15 C16 C18 118.8(7) . . ? N2 C17 C16 121.1(8) . . ? C19 C18 C16 120.1(7) . . ? C18 C19 C20 121.6(7) . . ? C26 C20 C21 118.6(7) . . ? C26 C20 C19 123.3(7) . . ? C21 C20 C19 118.1(8) . . ? C15 C21 C20 121.7(7) . . ? C15 C21 C24 119.4(7) . . ? C20 C21 C24 118.9(8) . . ? C23 C22 C14 118.3(7) . . ? C22 C23 C24 121.9(7) . . ? C25 C24 C21 117.7(7) . . ? C25 C24 C23 123.2(7) . . ? C21 C24 C23 119.1(8) . . ? N3 C25 C24 123.3(7) . . ? N3 C26 C20 121.7(8) . . ? N4 C27 C28 123.8(10) . . ? C27 C28 C29 117.9(9) . . ? C30 C29 C28 118.0(9) . . ? C30 C29 C32 124.0(9) . . ? C28 C29 C32 117.8(9) . . ? C29 C30 C31 119.3(9) . . ? N4 C31 C30 123.3(9) . . ? C29 C32 C34 109.0(7) . . ? C39 C34 C35 118.6(7) . . ? C39 C34 C32 121.0(8) . . ? C35 C34 C32 120.2(9) . . ? C36 C35 C34 120.8(9) . . ? C35 C36 C37 117.7(8) . . ? C38 C37 C36 123.0(7) . . ? C38 C37 N5 117.1(7) . . ? C36 C37 N5 119.9(7) . . ? C37 C38 C39 118.5(8) . . ? C34 C39 C38 121.4(8) . . ? N5 C40 C41 121.4(6) . . ? C40 C41 C42 117.1(6) . . ? C40 C41 C49 123.7(6) . . ? C42 C41 C49 119.1(6) . . ? C41 C42 C48 119.9(6) . . ? C41 C42 C43 120.9(6) . . ? C48 C42 C43 119.2(5) . . ? C44 C43 C42 117.1(6) . . ? C44 C43 C45 123.5(6) . . ? C42 C43 C45 119.3(6) . . ? N5 C44 C43 120.3(6) . . ? C46 C45 C43 121.9(6) . . ? C45 C46 C47 120.7(6) . . ? C53 C47 C48 117.8(6) . . ? C53 C47 C46 123.6(6) . . ? C48 C47 C46 118.6(5) . . ? C51 C48 C47 120.1(6) . . ? C51 C48 C42 119.7(5) . . ? C47 C48 C42 120.2(5) . . ? C50 C49 C41 121.2(6) . . ? C49 C50 C51 120.5(6) . . ? C48 C51 C52 117.6(6) . . ? C48 C51 C50 119.5(6) . . ? C52 C51 C50 122.9(6) . . ? N6 C52 C51 121.2(6) . . ? N6 C53 C47 122.2(6) . . ? N7 C54 C55 115.6(9) . . ? C54 C55 N8 111.0(10) . . ? C57 C56 N9 117.3(10) . . ? C56 C57 N10 99.2(12) . . ? C59 C58 O1 125.0(8) . . ? C59 C58 C67 120.9(10) . . ? O1 C58 C67 114.0(9) . . ? C58 C59 C60 120.8(8) . . ? C59 C60 C61 119.9(9) . . ? C62 C61 C60 119.2(9) . . ? C67 C62 C61 121.1(7) . . ? C67 C62 C63 118.7(8) . . ? C61 C62 C63 120.1(8) . . ? C64 C63 O10 125.5(7) . . ? C64 C63 C62 119.4(8) . . ? O10 C63 C62 115.0(7) . . ? C63 C64 C65 121.2(7) . . ? C64 C65 C66 120.9(8) . . ? C65 C66 C67 118.9(9) . . ? C62 C67 C66 120.7(8) . . ? C62 C67 C58 118.1(9) . . ? C66 C67 C58 121.2(9) . . ? O1 C68 C69 108.7(11) . . ? O2 C69 C68 115.4(11) . . ? O2 C70 C71 113.4(13) . . ? O3 C71 C70 109.3(10) . . ? C75 C74 O4 111.6(11) . . ? O5 C75 C74 107.6(13) . . ? C85 C76 C77 121.0(10) . . ? C85 C76 O5 114.6(6) . . ? C77 C76 O5 124.4(9) . . ? C76 C77 C78 118.9(7) . . ? C79 C78 C77 119.8(4) . . ? C80 C79 C78 119.0(6) . . ? C85 C80 C81 117.6(5) . . ? C85 C80 C79 121.5(5) . . ? C81 C80 C79 121.0(7) . . ? C82 C81 C80 123.9(10) . . ? C82 C81 O6 119.7(11) . . ? C80 C81 O6 116.3(10) . . ? C81 C82 C83 118.4(6) . . ? C84 C83 C82 120.0(4) . . ? C83 C84 C85 120.5(5) . . ? C80 C85 C76 119.7(6) . . ? C80 C85 C84 119.7(4) . . ? C76 C85 C84 120.6(7) . . ? O6 C86 C87 101(2) . . ? O7 C87 C86 112.3(12) . . ? O7 C88 C89 111.1(14) . . ? O8 C89 C88 106.4(12) . . ? C91 C90 O8 122.5(17) . . ? C90 C91 O9 110.0(14) . . ? O9 C92 C93 110.6(9) . . ? O10 C93 C92 106.0(7) . . ? C1 N1 C5 118.1(6) . . ? C1 N1 Pd1 121.7(5) . . ? C5 N1 Pd1 120.2(5) . . ? C17 N2 C13 121.9(7) . . ? C17 N2 C10 119.9(7) . . ? C13 N2 C10 118.1(7) . . ? C25 N3 C26 119.7(8) . . ? C25 N3 Pd2 119.3(6) . . ? C26 N3 Pd2 121.0(6) . . ? C31 N4 C27 117.7(9) . . ? C31 N4 Pd2 120.0(6) . . ? C27 N4 Pd2 122.3(7) . . ? C40 N5 C44 123.1(6) . . ? C40 N5 C37 119.1(6) . . ? C44 N5 C37 117.7(6) . . ? C52 N6 C53 121.0(6) . . ? C52 N6 Pd1 118.6(5) . . ? C53 N6 Pd1 120.4(4) . . ? C54 N7 Pd1 109.2(6) . . ? C55 N8 Pd1 110.8(5) . . ? C56 N9 Pd2 100.0(8) . . ? C57 N10 Pd2 115.9(9) . . ? O11 N11 O12 120.4(5) . . ? O11 N11 C94 121.0(16) . . ? O12 N11 C94 118.5(16) . . ? O14 N12 O13 119.8(5) . . ? O14 N12 C95 134.3(15) . . ? O13 N12 C95 105.5(15) . . ? O16 N13 O15 123.8(15) . . ? O16 N13 C96 116.2(14) . . ? O15 N13 C96 119.8(18) . . ? O18 N14 O17 119(2) . . ? O18 N14 C97 113.3(18) . . ? O17 N14 C97 127.0(18) . . ? C58 O1 C68 118.2(9) . . ? C70 O2 C69 118.4(13) . . ? C71 O3 C72 110.6(11) . . ? C73A O4 C74 116.1(12) . . ? C76 O5 C75 115.9(11) . . ? C81 O6 C86 117.0(13) . . ? C88 O7 C87 112.6(13) . . ? C89 O8 C90 99.8(15) . . ? C92 O9 C91 113.1(10) . . ? C63 O10 C93 118.2(6) . . ? P4 F20 F32 106.1(10) . . ? P6 F32 F20 113.5(8) . . ? F2 P1 F3 89.8(4) . . ? F2 P1 F5 90.5(4) . . ? F3 P1 F5 90.4(3) . . ? F2 P1 F6 89.8(3) . . ? F3 P1 F6 179.4(4) . . ? F5 P1 F6 89.2(3) . . ? F2 P1 F1 91.1(4) . . ? F3 P1 F1 90.2(3) . . ? F5 P1 F1 178.3(4) . . ? F6 P1 F1 90.3(3) . . ? F2 P1 F4 179.2(4) . . ? F3 P1 F4 90.7(4) . . ? F5 P1 F4 88.9(3) . . ? F6 P1 F4 89.7(4) . . ? F1 P1 F4 89.5(3) . . ? F11 P2 F9 178.7(6) . . ? F11 P2 F8 90.9(7) . . ? F9 P2 F8 90.4(7) . . ? F11 P2 F7 91.8(6) . . ? F9 P2 F7 87.9(5) . . ? F8 P2 F7 89.1(5) . . ? F11 P2 F10 90.4(7) . . ? F9 P2 F10 89.9(7) . . ? F8 P2 F10 91.0(5) . . ? F7 P2 F10 177.8(7) . . ? F11 P2 F12 89.9(6) . . ? F9 P2 F12 88.8(6) . . ? F8 P2 F12 179.0(7) . . ? F7 P2 F12 90.4(6) . . ? F10 P2 F12 89.5(6) . . ? F17 P3 F16 92.7(7) . . ? F17 P3 F15 91.1(13) . . ? F16 P3 F15 89.7(8) . . ? F17 P3 F18 177.0(11) . . ? F16 P3 F18 89.5(5) . . ? F15 P3 F18 86.8(8) . . ? F17 P3 F13 97.4(12) . . ? F16 P3 F13 94.1(8) . . ? F15 P3 F13 170.6(10) . . ? F18 P3 F13 84.6(8) . . ? F17 P3 F14 90.0(6) . . ? F16 P3 F14 177.2(6) . . ? F15 P3 F14 89.5(7) . . ? F18 P3 F14 87.8(5) . . ? F13 P3 F14 86.3(5) . . ? F21 P4 F23 97.5(6) . . ? F21 P4 F19 99.5(7) . . ? F23 P4 F19 96.9(8) . . ? F21 P4 F20 89.0(7) . . ? F23 P4 F20 173.4(7) . . ? F19 P4 F20 83.4(10) . . ? F21 P4 F22 80.7(7) . . ? F23 P4 F22 91.5(6) . . ? F19 P4 F22 171.5(9) . . ? F20 P4 F22 88.1(9) . . ? F21 P4 F24 166.6(9) . . ? F23 P4 F24 85.1(6) . . ? F19 P4 F24 93.2(7) . . ? F20 P4 F24 88.3(7) . . ? F22 P4 F24 86.1(8) . . ? F29 P5 F27 99.7(8) . . ? F29 P5 F30 163.9(9) . . ? F27 P5 F30 96.1(8) . . ? F29 P5 F26 90.6(7) . . ? F27 P5 F26 92.4(6) . . ? F30 P5 F26 91.8(5) . . ? F29 P5 F28 89.8(7) . . ? F27 P5 F28 87.6(5) . . ? F30 P5 F28 87.9(5) . . ? F26 P5 F28 179.6(5) . . ? F29 P5 F25 79.8(11) . . ? F27 P5 F25 171.8(7) . . ? F30 P5 F25 84.2(10) . . ? F26 P5 F25 95.8(6) . . ? F28 P5 F25 84.3(6) . . ? F33 P6 F35 175.5(12) . . ? F33 P6 F31 90.2(3) . . ? F35 P6 F31 90.0(3) . . ? F33 P6 F36 93.9(14) . . ? F35 P6 F36 85.3(14) . . ? F31 P6 F36 171.8(10) . . ? F33 P6 F32 88.5(8) . . ? F35 P6 F32 87.0(12) . . ? F31 P6 F32 89.6(3) . . ? F36 P6 F32 83.4(8) . . ? F33 P6 F34 82.3(8) . . ? F35 P6 F34 102.2(12) . . ? F31 P6 F34 89.9(3) . . ? F36 P6 F34 97.6(8) . . ? F32 P6 F34 170.8(9) . . ? F41 P7 F39 95.4(8) . . ? F41 P7 F40 82.9(18) . . ? F39 P7 F40 90.2(7) . . ? F41 P7 F42 90.1(3) . . ? F39 P7 F42 174.5(8) . . ? F40 P7 F42 89.8(3) . . ? F41 P7 F38 98.3(13) . . ? F39 P7 F38 90.2(7) . . ? F40 P7 F38 178.7(16) . . ? F42 P7 F38 89.6(3) . . ? F41 P7 F37 179.2(16) . . ? F39 P7 F37 84.9(7) . . ? F40 P7 F37 97.8(17) . . ? F42 P7 F37 89.6(3) . . ? F38 P7 F37 81.0(11) . . ? N8 Pd1 N1 93.1(2) . . ? N8 Pd1 N6 177.3(3) . . ? N1 Pd1 N6 89.5(2) . . ? N8 Pd1 N7 82.7(2) . . ? N1 Pd1 N7 175.7(2) . . ? N6 Pd1 N7 94.7(2) . . ? N10 Pd2 N4 175.6(4) . . ? N10 Pd2 N3 94.6(4) . . ? N4 Pd2 N3 89.8(3) . . ? N10 Pd2 N9 84.6(4) . . ? N4 Pd2 N9 91.0(3) . . ? N3 Pd2 N9 178.4(3) . . ? O3 C72 C73A 104.8(9) . . ? O4 C73A C72 101.1(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 C1 C2 C3 -1.6(12) . . . . ? C1 C2 C3 C4 2.0(12) . . . . ? C1 C2 C3 C6 178.2(7) . . . . ? C2 C3 C4 C5 -2.6(12) . . . . ? C6 C3 C4 C5 -178.8(8) . . . . ? C3 C4 C5 N1 2.7(12) . . . . ? C2 C3 C6 C7 -108.8(10) . . . . ? C4 C3 C6 C7 67.3(11) . . . . ? C3 C6 C7 C8 75.4(11) . . . . ? C3 C6 C7 C12 -97.8(10) . . . . ? C12 C7 C8 C9 1.4(14) . . . . ? C6 C7 C8 C9 -171.7(8) . . . . ? C7 C8 C9 C10 0.7(13) . . . . ? C8 C9 C10 N2 175.4(7) . . . . ? C8 C9 C10 C11 -1.7(12) . . . . ? C9 C10 C11 C12 0.6(13) . . . . ? N2 C10 C11 C12 -176.4(8) . . . . ? C10 C11 C12 C7 1.5(14) . . . . ? C8 C7 C12 C11 -2.5(14) . . . . ? C6 C7 C12 C11 170.7(8) . . . . ? N2 C13 C14 C15 -1.5(11) . . . . ? N2 C13 C14 C22 177.9(7) . . . . ? C13 C14 C15 C21 179.0(6) . . . . ? C22 C14 C15 C21 -0.4(11) . . . . ? C13 C14 C15 C16 -1.5(10) . . . . ? C22 C14 C15 C16 179.1(7) . . . . ? C21 C15 C16 C17 -178.4(6) . . . . ? C14 C15 C16 C17 2.2(9) . . . . ? C21 C15 C16 C18 1.7(9) . . . . ? C14 C15 C16 C18 -177.7(6) . . . . ? C15 C16 C17 N2 0.2(10) . . . . ? C18 C16 C17 N2 -179.9(6) . . . . ? C17 C16 C18 C19 177.4(7) . . . . ? C15 C16 C18 C19 -2.7(10) . . . . ? C16 C18 C19 C20 2.7(11) . . . . ? C18 C19 C20 C26 178.2(7) . . . . ? C18 C19 C20 C21 -1.7(11) . . . . ? C14 C15 C21 C20 178.6(6) . . . . ? C16 C15 C21 C20 -0.8(10) . . . . ? C14 C15 C21 C24 0.2(10) . . . . ? C16 C15 C21 C24 -179.2(6) . . . . ? C26 C20 C21 C15 -179.2(7) . . . . ? C19 C20 C21 C15 0.7(10) . . . . ? C26 C20 C21 C24 -0.8(10) . . . . ? C19 C20 C21 C24 179.1(7) . . . . ? C13 C14 C22 C23 -177.9(8) . . . . ? C15 C14 C22 C23 1.5(12) . . . . ? C14 C22 C23 C24 -2.6(13) . . . . ? C15 C21 C24 C25 179.5(7) . . . . ? C20 C21 C24 C25 1.1(10) . . . . ? C15 C21 C24 C23 -1.2(11) . . . . ? C20 C21 C24 C23 -179.6(7) . . . . ? C22 C23 C24 C25 -178.3(8) . . . . ? C22 C23 C24 C21 2.4(12) . . . . ? C21 C24 C25 N3 -1.6(12) . . . . ? C23 C24 C25 N3 179.2(8) . . . . ? C21 C20 C26 N3 0.8(12) . . . . ? C19 C20 C26 N3 -179.0(7) . . . . ? N4 C27 C28 C29 1.5(13) . . . . ? C27 C28 C29 C30 -1.4(12) . . . . ? C27 C28 C29 C32 173.2(7) . . . . ? C28 C29 C30 C31 0.5(11) . . . . ? C32 C29 C30 C31 -173.7(7) . . . . ? C29 C30 C31 N4 0.4(13) . . . . ? C30 C29 C32 C34 96.8(10) . . . . ? C28 C29 C32 C34 -77.5(10) . . . . ? C29 C32 C34 C39 -59.0(13) . . . . ? C29 C32 C34 C35 116.0(10) . . . . ? C39 C34 C35 C36 -1.4(15) . . . . ? C32 C34 C35 C36 -176.5(9) . . . . ? C34 C35 C36 C37 1.2(15) . . . . ? C35 C36 C37 C38 -0.7(14) . . . . ? C35 C36 C37 N5 177.4(8) . . . . ? C36 C37 C38 C39 0.4(13) . . . . ? N5 C37 C38 C39 -177.8(7) . . . . ? C35 C34 C39 C38 1.1(15) . . . . ? C32 C34 C39 C38 176.2(9) . . . . ? C37 C38 C39 C34 -0.6(14) . . . . ? N5 C40 C41 C42 0.8(10) . . . . ? N5 C40 C41 C49 -179.7(7) . . . . ? C40 C41 C42 C48 -178.5(6) . . . . ? C49 C41 C42 C48 2.0(9) . . . . ? C40 C41 C42 C43 0.3(9) . . . . ? C49 C41 C42 C43 -179.2(6) . . . . ? C41 C42 C43 C44 -0.8(9) . . . . ? C48 C42 C43 C44 178.1(6) . . . . ? C41 C42 C43 C45 -179.3(6) . . . . ? C48 C42 C43 C45 -0.5(9) . . . . ? C42 C43 C44 N5 0.1(9) . . . . ? C45 C43 C44 N5 178.6(6) . . . . ? C44 C43 C45 C46 -178.6(6) . . . . ? C42 C43 C45 C46 -0.1(10) . . . . ? C43 C45 C46 C47 1.3(10) . . . . ? C45 C46 C47 C53 178.3(6) . . . . ? C45 C46 C47 C48 -1.9(9) . . . . ? C53 C47 C48 C51 0.3(9) . . . . ? C46 C47 C48 C51 -179.5(5) . . . . ? C53 C47 C48 C42 -178.9(5) . . . . ? C46 C47 C48 C42 1.3(8) . . . . ? C41 C42 C48 C51 -0.5(8) . . . . ? C43 C42 C48 C51 -179.3(5) . . . . ? C41 C42 C48 C47 178.7(6) . . . . ? C43 C42 C48 C47 -0.1(8) . . . . ? C40 C41 C49 C50 178.9(7) . . . . ? C42 C41 C49 C50 -1.5(11) . . . . ? C41 C49 C50 C51 -0.4(11) . . . . ? C47 C48 C51 C52 -0.3(8) . . . . ? C42 C48 C51 C52 178.9(6) . . . . ? C47 C48 C51 C50 179.4(6) . . . . ? C42 C48 C51 C50 -1.4(9) . . . . ? C49 C50 C51 C48 1.9(10) . . . . ? C49 C50 C51 C52 -178.5(7) . . . . ? C48 C51 C52 N6 -0.8(9) . . . . ? C50 C51 C52 N6 179.5(6) . . . . ? C48 C47 C53 N6 0.7(9) . . . . ? C46 C47 C53 N6 -179.4(6) . . . . ? N7 C54 C55 N8 -38(2) . . . . ? N9 C56 C57 N10 52.0(18) . . . . ? O1 C58 C59 C60 177.9(8) . . . . ? C67 C58 C59 C60 -0.7(13) . . . . ? C58 C59 C60 C61 0.3(13) . . . . ? C59 C60 C61 C62 0.6(12) . . . . ? C60 C61 C62 C67 -1.0(11) . . . . ? C60 C61 C62 C63 179.7(7) . . . . ? C67 C62 C63 C64 -0.6(10) . . . . ? C61 C62 C63 C64 178.8(7) . . . . ? C67 C62 C63 O10 177.3(6) . . . . ? C61 C62 C63 O10 -3.4(10) . . . . ? O10 C63 C64 C65 -178.4(7) . . . . ? C62 C63 C64 C65 -0.8(10) . . . . ? C63 C64 C65 C66 2.3(11) . . . . ? C64 C65 C66 C67 -2.4(11) . . . . ? C61 C62 C67 C66 -178.9(7) . . . . ? C63 C62 C67 C66 0.4(11) . . . . ? C61 C62 C67 C58 0.5(11) . . . . ? C63 C62 C67 C58 179.9(7) . . . . ? C65 C66 C67 C62 1.0(11) . . . . ? C65 C66 C67 C58 -178.4(7) . . . . ? C59 C58 C67 C62 0.3(12) . . . . ? O1 C58 C67 C62 -178.5(7) . . . . ? C59 C58 C67 C66 179.8(8) . . . . ? O1 C58 C67 C66 1.0(11) . . . . ? O1 C68 C69 O2 -67.8(12) . . . . ? O2 C70 C71 O3 71.6(14) . . . . ? O4 C74 C75 O5 76.8(13) . . . . ? C85 C76 C77 C78 2.8(13) . . . . ? O5 C76 C77 C78 -177.3(9) . . . . ? C76 C77 C78 C79 -3.3(15) . . . . ? C77 C78 C79 C80 1.9(15) . . . . ? C78 C79 C80 C85 0.0(14) . . . . ? C78 C79 C80 C81 178.5(9) . . . . ? C85 C80 C81 C82 -2.6(14) . . . . ? C79 C80 C81 C82 178.8(9) . . . . ? C85 C80 C81 O6 -178.4(8) . . . . ? C79 C80 C81 O6 3.0(14) . . . . ? C80 C81 C82 C83 2.7(14) . . . . ? O6 C81 C82 C83 178.3(9) . . . . ? C81 C82 C83 C84 -0.1(13) . . . . ? C82 C83 C84 C85 -2.3(12) . . . . ? C81 C80 C85 C76 -179.0(8) . . . . ? C79 C80 C85 C76 -0.5(13) . . . . ? C81 C80 C85 C84 0.1(12) . . . . ? C79 C80 C85 C84 178.6(8) . . . . ? C77 C76 C85 C80 -1.0(12) . . . . ? O5 C76 C85 C80 179.2(8) . . . . ? C77 C76 C85 C84 179.9(8) . . . . ? O5 C76 C85 C84 0.1(11) . . . . ? C83 C84 C85 C80 2.3(12) . . . . ? C83 C84 C85 C76 -178.6(7) . . . . ? O6 C86 C87 O7 72(2) . . . . ? O7 C88 C89 O8 -72.2(16) . . . . ? O8 C90 C91 O9 -41(3) . . . . ? O9 C92 C93 O10 -72.6(10) . . . . ? C2 C1 N1 C5 1.6(11) . . . . ? C2 C1 N1 Pd1 -179.6(6) . . . . ? C4 C5 N1 C1 -2.1(10) . . . . ? C4 C5 N1 Pd1 179.0(6) . . . . ? C16 C17 N2 C13 -3.4(10) . . . . ? C16 C17 N2 C10 173.9(6) . . . . ? C14 C13 N2 C17 4.1(11) . . . . ? C14 C13 N2 C10 -173.3(7) . . . . ? C9 C10 N2 C17 -135.8(8) . . . . ? C11 C10 N2 C17 41.1(11) . . . . ? C9 C10 N2 C13 41.6(10) . . . . ? C11 C10 N2 C13 -141.4(8) . . . . ? C24 C25 N3 C26 1.6(12) . . . . ? C24 C25 N3 Pd2 -179.6(6) . . . . ? C20 C26 N3 C25 -1.2(12) . . . . ? C20 C26 N3 Pd2 -179.9(6) . . . . ? C30 C31 N4 C27 -0.3(12) . . . . ? C30 C31 N4 Pd2 177.1(6) . . . . ? C28 C27 N4 C31 -0.7(13) . . . . ? C28 C27 N4 Pd2 -178.1(7) . . . . ? C41 C40 N5 C44 -1.5(11) . . . . ? C41 C40 N5 C37 175.8(7) . . . . ? C43 C44 N5 C40 1.0(10) . . . . ? C43 C44 N5 C37 -176.3(6) . . . . ? C38 C37 N5 C40 -50.3(10) . . . . ? C36 C37 N5 C40 131.5(8) . . . . ? C38 C37 N5 C44 127.1(8) . . . . ? C36 C37 N5 C44 -51.1(10) . . . . ? C51 C52 N6 C53 1.9(10) . . . . ? C51 C52 N6 Pd1 -177.0(5) . . . . ? C47 C53 N6 C52 -1.9(10) . . . . ? C47 C53 N6 Pd1 177.0(5) . . . . ? C55 C54 N7 Pd1 29.4(18) . . . . ? C54 C55 N8 Pd1 26.8(16) . . . . ? C57 C56 N9 Pd2 -37.2(17) . . . . ? C56 C57 N10 Pd2 -44.0(14) . . . . ? C59 C58 O1 C68 4.7(13) . . . . ? C67 C58 O1 C68 -176.5(8) . . . . ? C69 C68 O1 C58 177.9(10) . . . . ? C71 C70 O2 C69 166.8(11) . . . . ? C68 C69 O2 C70 103.8(13) . . . . ? C70 C71 O3 C72 -176.2(11) . . . . ? C75 C74 O4 C73A -77.2(15) . . . . ? C85 C76 O5 C75 -179.1(8) . . . . ? C77 C76 O5 C75 1.1(14) . . . . ? C74 C75 O5 C76 170.8(11) . . . . ? C82 C81 O6 C86 -3.5(15) . . . . ? C80 C81 O6 C86 172.5(10) . . . . ? C87 C86 O6 C81 179.0(10) . . . . ? C89 C88 O7 C87 -178.9(17) . . . . ? C86 C87 O7 C88 -179(2) . . . . ? C88 C89 O8 C90 -166.9(12) . . . . ? C91 C90 O8 C89 -66(2) . . . . ? C93 C92 O9 C91 -172.4(9) . . . . ? C90 C91 O9 C92 -172.2(15) . . . . ? C64 C63 O10 C93 -6.1(11) . . . . ? C62 C63 O10 C93 176.2(6) . . . . ? C92 C93 O10 C63 178.6(9) . . . . ? P4 F20 F32 P6 147.3(9) . . . . ? F32 F20 P4 F21 123.0(10) . . . . ? F32 F20 P4 F23 -44(8) . . . . ? F32 F20 P4 F19 -137.3(10) . . . . ? F32 F20 P4 F22 42.3(10) . . . . ? F32 F20 P4 F24 -43.8(10) . . . . ? F20 F32 P6 F33 51.7(12) . . . . ? F20 F32 P6 F35 -128.5(12) . . . . ? F20 F32 P6 F31 -38.5(12) . . . . ? F20 F32 P6 F36 145.9(16) . . . . ? F20 F32 P6 F34 49(3) . . . . ? C55 N8 Pd1 N1 170.1(9) . . . . ? C55 N8 Pd1 N6 -23(6) . . . . ? C55 N8 Pd1 N7 -9.1(9) . . . . ? C1 N1 Pd1 N8 -73.2(6) . . . . ? C5 N1 Pd1 N8 105.6(5) . . . . ? C1 N1 Pd1 N6 107.4(5) . . . . ? C5 N1 Pd1 N6 -73.8(5) . . . . ? C1 N1 Pd1 N7 -62(4) . . . . ? C5 N1 Pd1 N7 116(4) . . . . ? C52 N6 Pd1 N8 -56(6) . . . . ? C53 N6 Pd1 N8 125(6) . . . . ? C52 N6 Pd1 N1 111.0(5) . . . . ? C53 N6 Pd1 N1 -67.8(5) . . . . ? C52 N6 Pd1 N7 -69.7(5) . . . . ? C53 N6 Pd1 N7 111.4(5) . . . . ? C54 N7 Pd1 N8 -10.2(9) . . . . ? C54 N7 Pd1 N1 -21(4) . . . . ? C54 N7 Pd1 N6 169.1(9) . . . . ? C57 N10 Pd2 N4 30(5) . . . . ? C57 N10 Pd2 N3 -157.2(10) . . . . ? C57 N10 Pd2 N9 21.4(10) . . . . ? C31 N4 Pd2 N10 78(5) . . . . ? C27 N4 Pd2 N10 -105(4) . . . . ? C31 N4 Pd2 N3 -95.4(6) . . . . ? C27 N4 Pd2 N3 81.9(7) . . . . ? C31 N4 Pd2 N9 86.0(7) . . . . ? C27 N4 Pd2 N9 -96.7(7) . . . . ? C25 N3 Pd2 N10 60.9(7) . . . . ? C26 N3 Pd2 N10 -120.3(7) . . . . ? C25 N3 Pd2 N4 -119.6(6) . . . . ? C26 N3 Pd2 N4 59.1(6) . . . . ? C25 N3 Pd2 N9 -1(12) . . . . ? C26 N3 Pd2 N9 178(100) . . . . ? C56 N9 Pd2 N10 6.1(8) . . . . ? C56 N9 Pd2 N4 -173.2(8) . . . . ? C56 N9 Pd2 N3 68(12) . . . . ? C71 O3 C72 C73A 172.3(11) . . . . ? C74 O4 C73A C72 -177.2(12) . . . . ? O3 C72 C73A O4 -78.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.162 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.195