# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_kjc1132 _database_code_depnum_ccdc_archive 'CCDC 891175' #TrackingRef '1HPF6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H47 N2 P2, P F6' _chemical_formula_sum 'C47 H47 F6 N2 P3' _chemical_formula_weight 846.78 _chemical_absolute_configuration ad 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.9727(5) _cell_length_b 13.6776(6) _cell_length_c 13.8349(5) _cell_angle_alpha 86.162(2) _cell_angle_beta 75.759(2) _cell_angle_gamma 74.124(2) _cell_volume 2112.19(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10801 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9415 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14999 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14999 _reflns_number_gt 10801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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. Both anion sites show two-fold disorder. Geometric restraints were applied to the PF6- during refinement to stop distortion of the anions. Restraints were also applied in order to maintain similar atomic displacement parameters for atoms in close proximity. ; _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^)+(0.0543P)^2^+1.9829P] 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 0.03(12) _refine_ls_number_reflns 14999 _refine_ls_number_parameters 1179 _refine_ls_number_restraints 606 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2910(6) 0.5416(5) 0.4096(5) 0.0302(14) Uani 1 1 d . . . H1 H 0.2396 0.5344 0.4724 0.036 Uiso 1 1 calc R . . C2 C 0.3353(5) 0.5486(6) 0.2271(4) 0.0539(18) Uani 1 1 d . . . C3 C 0.4080(5) 0.6204(5) 0.2391(4) 0.0508(16) Uani 1 1 d . . . C4 C 0.4795(5) 0.5574(4) 0.3097(4) 0.0408(13) Uani 1 1 d . . . H4 H 0.5475 0.5845 0.3146 0.049 Uiso 1 1 calc R . . C5 C 0.5229(5) 0.4507(5) 0.2652(5) 0.0541(17) Uani 1 1 d . . . H5A H 0.5267 0.3987 0.3186 0.065 Uiso 1 1 calc R . . H5B H 0.6034 0.4402 0.2200 0.065 Uiso 1 1 calc R . . C6 C 0.4308(6) 0.4434(6) 0.2072(5) 0.0649(19) Uani 1 1 d . . . H6A H 0.3946 0.3869 0.2325 0.078 Uiso 1 1 calc R . . H6B H 0.4682 0.4331 0.1350 0.078 Uiso 1 1 calc R . . C7 C 0.2626(8) 0.5789(9) 0.1494(6) 0.082(3) Uani 1 1 d . . . H7A H 0.2234 0.5259 0.1442 0.123 Uiso 1 1 calc R . . H7B H 0.3153 0.5873 0.0847 0.123 Uiso 1 1 calc R . . H7C H 0.2018 0.6432 0.1689 0.123 Uiso 1 1 calc R . . C8 C 0.3319(6) 0.7260(5) 0.2791(5) 0.0572(19) Uani 1 1 d . . . H8A H 0.3835 0.7640 0.2952 0.086 Uiso 1 1 calc R . . H8B H 0.2716 0.7184 0.3393 0.086 Uiso 1 1 calc R . . H8C H 0.2922 0.7629 0.2283 0.086 Uiso 1 1 calc R . . C9 C 0.4956(7) 0.6354(8) 0.1394(5) 0.081(3) Uani 1 1 d . . . H9A H 0.5494 0.6731 0.1520 0.122 Uiso 1 1 calc R . . H9B H 0.4500 0.6737 0.0927 0.122 Uiso 1 1 calc R . . H9C H 0.5425 0.5689 0.1106 0.122 Uiso 1 1 calc R . . C10 C 0.1412(6) 0.5101(6) 0.3323(5) 0.0407(17) Uani 1 1 d . . . H10A H 0.1588 0.4518 0.2872 0.049 Uiso 1 1 calc R . . H10B H 0.0851 0.5679 0.3076 0.049 Uiso 1 1 calc R . . C11 C 0.0805(5) 0.4823(5) 0.4352(5) 0.0340(15) Uani 1 1 d . . . C12 C 0.0085(6) 0.5549(5) 0.5061(5) 0.0295(15) Uani 1 1 d . . . C13 C -0.0493(6) 0.5224(5) 0.5987(5) 0.0342(15) Uani 1 1 d . . . H13 H -0.1014 0.5708 0.6470 0.041 Uiso 1 1 calc R . . C14 C -0.0297(6) 0.4182(6) 0.6194(6) 0.0452(18) Uani 1 1 d . . . H14 H -0.0671 0.3960 0.6825 0.054 Uiso 1 1 calc R . . C15 C 0.0439(6) 0.3477(5) 0.5481(6) 0.0480(19) Uani 1 1 d . . . H15 H 0.0567 0.2770 0.5620 0.058 Uiso 1 1 calc R . . C16 C 0.0977(6) 0.3798(5) 0.4581(6) 0.0443(18) Uani 1 1 d . . . H16 H 0.1483 0.3309 0.4096 0.053 Uiso 1 1 calc R . . C17 C -0.1662(6) 0.7424(5) 0.5423(5) 0.0341(15) Uani 1 1 d . . . C18 C -0.2534(6) 0.7193(5) 0.5038(6) 0.0494(19) Uani 1 1 d . . . H18 H -0.2293 0.6759 0.4474 0.059 Uiso 1 1 calc R . . C19 C -0.3750(7) 0.7585(6) 0.5459(7) 0.061(2) Uani 1 1 d . . . H19 H -0.4331 0.7406 0.5199 0.073 Uiso 1 1 calc R . . C20 C -0.4090(7) 0.8230(6) 0.6251(7) 0.056(2) Uani 1 1 d . . . H20 H -0.4917 0.8496 0.6547 0.068 Uiso 1 1 calc R . . C21 C -0.3262(7) 0.8499(6) 0.6626(6) 0.0501(19) Uani 1 1 d . . . H21 H -0.3517 0.8956 0.7173 0.060 Uiso 1 1 calc R . . C22 C -0.2046(6) 0.8107(5) 0.6211(5) 0.0424(18) Uani 1 1 d . . . H22 H -0.1477 0.8308 0.6468 0.051 Uiso 1 1 calc R . . C23 C 0.0721(6) 0.7316(5) 0.5521(5) 0.0305(14) Uani 1 1 d . . . C24 C 0.0966(6) 0.6870(5) 0.6406(5) 0.0374(16) Uani 1 1 d . . . H24 H 0.0681 0.6298 0.6661 0.045 Uiso 1 1 calc R . . C25 C 0.1613(7) 0.7241(5) 0.6918(5) 0.0429(18) Uani 1 1 d . . . H25 H 0.1768 0.6925 0.7522 0.052 Uiso 1 1 calc R . . C26 C 0.2039(7) 0.8068(6) 0.6559(6) 0.0465(19) Uani 1 1 d . . . H26 H 0.2488 0.8320 0.6914 0.056 Uiso 1 1 calc R . . C27 C 0.1813(7) 0.8529(6) 0.5684(6) 0.051(2) Uani 1 1 d . . . H27 H 0.2102 0.9101 0.5437 0.061 Uiso 1 1 calc R . . C28 C 0.1159(7) 0.8153(5) 0.5160(5) 0.0423(18) Uani 1 1 d . . . H28 H 0.1011 0.8468 0.4554 0.051 Uiso 1 1 calc R . . C29 C 0.4299(6) 0.5660(5) 0.4999(5) 0.0311(15) Uani 1 1 d . . . H29A H 0.3591 0.5726 0.5565 0.037 Uiso 1 1 calc R . . H29B H 0.4560 0.6291 0.4966 0.037 Uiso 1 1 calc R . . C30 C 0.5293(6) 0.4767(5) 0.5184(5) 0.0329(15) Uani 1 1 d . . . C31 C 0.5090(6) 0.3891(5) 0.5695(4) 0.0303(15) Uani 1 1 d . . . C32 C 0.6066(6) 0.3083(5) 0.5795(5) 0.0331(15) Uani 1 1 d . . . H32 H 0.5931 0.2484 0.6136 0.040 Uiso 1 1 calc R . . C33 C 0.7240(7) 0.3145(5) 0.5402(5) 0.0397(17) Uani 1 1 d . . . H33 H 0.7894 0.2593 0.5479 0.048 Uiso 1 1 calc R . . C34 C 0.7443(6) 0.4014(6) 0.4900(5) 0.0404(17) Uani 1 1 d . . . H34 H 0.8235 0.4064 0.4624 0.048 Uiso 1 1 calc R . . C35 C 0.6456(6) 0.4820(5) 0.4807(5) 0.0351(16) Uani 1 1 d . . . H35 H 0.6593 0.5421 0.4474 0.042 Uiso 1 1 calc R . . C36 C 0.3691(6) 0.2495(5) 0.6624(4) 0.0291(14) Uani 1 1 d . . . C37 C 0.3373(6) 0.1807(5) 0.6122(5) 0.0340(15) Uani 1 1 d . . . H37 H 0.3120 0.1996 0.5521 0.041 Uiso 1 1 calc R . . C38 C 0.3429(6) 0.0826(5) 0.6518(5) 0.0425(17) Uani 1 1 d . . . H38 H 0.3225 0.0349 0.6172 0.051 Uiso 1 1 calc R . . C39 C 0.3772(6) 0.0542(5) 0.7397(5) 0.0399(17) Uani 1 1 d . . . H39 H 0.3797 -0.0123 0.7656 0.048 Uiso 1 1 calc R . . C40 C 0.4080(6) 0.1225(5) 0.7896(5) 0.0378(16) Uani 1 1 d . . . H40 H 0.4321 0.1032 0.8502 0.045 Uiso 1 1 calc R . . C41 C 0.4040(6) 0.2200(5) 0.7518(5) 0.0388(17) Uani 1 1 d . . . H41 H 0.4252 0.2669 0.7869 0.047 Uiso 1 1 calc R . . C42 C 0.2990(6) 0.4503(4) 0.7309(5) 0.0303(15) Uani 1 1 d . . . C43 C 0.1788(7) 0.4612(5) 0.7786(5) 0.0409(17) Uani 1 1 d . . . H43 H 0.1311 0.4325 0.7493 0.049 Uiso 1 1 calc R . . C44 C 0.1285(7) 0.5134(5) 0.8680(5) 0.0453(19) Uani 1 1 d . . . H44 H 0.0466 0.5207 0.8995 0.054 Uiso 1 1 calc R . . C45 C 0.1983(8) 0.5552(5) 0.9117(5) 0.048(2) Uani 1 1 d . . . H45 H 0.1646 0.5903 0.9734 0.058 Uiso 1 1 calc R . . C46 C 0.3171(7) 0.5451(5) 0.8644(5) 0.0439(19) Uani 1 1 d . . . H46 H 0.3650 0.5741 0.8932 0.053 Uiso 1 1 calc R . . C47 C 0.3664(7) 0.4923(5) 0.7744(5) 0.0381(16) Uani 1 1 d . . . H47 H 0.4482 0.4854 0.7426 0.046 Uiso 1 1 calc R . . C48 C -0.1997(5) 0.0833(5) 1.1478(4) 0.0272(14) Uani 1 1 d . . . H48 H -0.1599 0.1122 1.0897 0.033 Uiso 1 1 calc R . . C49 C -0.2162(5) 0.0232(4) 1.3179(4) 0.0379(13) Uani 1 1 d . . . C50 C -0.3518(5) 0.0630(4) 1.3266(4) 0.0393(13) Uani 1 1 d . . . C51 C -0.3605(5) 0.0108(4) 1.2348(4) 0.0366(12) Uani 1 1 d . . . H51 H -0.4451 0.0164 1.2331 0.044 Uiso 1 1 calc R . . C52 C -0.2886(5) -0.0994(5) 1.2431(4) 0.0475(15) Uani 1 1 d . . . H52A H -0.2543 -0.1316 1.1766 0.057 Uiso 1 1 calc R . . H52B H -0.3391 -0.1399 1.2854 0.057 Uiso 1 1 calc R . . C53 C -0.1890(5) -0.0898(5) 1.2920(5) 0.0459(15) Uani 1 1 d . . . H53A H -0.1890 -0.1320 1.3530 0.055 Uiso 1 1 calc R . . H53B H -0.1097 -0.1125 1.2451 0.055 Uiso 1 1 calc R . . C54 C -0.1742(7) 0.0406(6) 1.4089(5) 0.0489(19) Uani 1 1 d . . . H54A H -0.0876 0.0115 1.3971 0.073 Uiso 1 1 calc R . . H54B H -0.2145 0.0078 1.4671 0.073 Uiso 1 1 calc R . . H54C H -0.1936 0.1137 1.4213 0.073 Uiso 1 1 calc R . . C55 C -0.4232(7) 0.0221(6) 1.4209(5) 0.0533(18) Uani 1 1 d . . . H55A H -0.4223 0.0581 1.4795 0.080 Uiso 1 1 calc R . . H55B H -0.3868 -0.0507 1.4275 0.080 Uiso 1 1 calc R . . H55C H -0.5059 0.0328 1.4158 0.080 Uiso 1 1 calc R . . C56 C -0.3991(6) 0.1791(5) 1.3249(4) 0.0466(15) Uani 1 1 d . . . H56A H -0.3871 0.2081 1.3832 0.070 Uiso 1 1 calc R . . H56B H -0.4846 0.1975 1.3264 0.070 Uiso 1 1 calc R . . H56C H -0.3560 0.2059 1.2639 0.070 Uiso 1 1 calc R . . C57 C -0.0470(5) 0.1066(5) 1.2263(5) 0.0314(14) Uani 1 1 d . . . H57A H -0.0685 0.1622 1.2752 0.038 Uiso 1 1 calc R . . H57B H 0.0124 0.0490 1.2478 0.038 Uiso 1 1 calc R . . C58 C 0.0083(6) 0.1422(5) 1.1264(4) 0.0300(14) Uani 1 1 d . . . C59 C 0.0825(6) 0.0726(5) 1.0507(5) 0.0302(15) Uani 1 1 d . . . C60 C 0.1345(6) 0.1114(5) 0.9616(5) 0.0372(16) Uani 1 1 d . . . H60 H 0.1846 0.0653 0.9104 0.045 Uiso 1 1 calc R . . C64 C 0.2611(6) -0.1137(5) 1.0055(5) 0.0374(16) Uani 1 1 d . . . C67 C 0.5026(7) -0.1867(6) 0.9119(6) 0.056(2) Uani 1 1 d . . . H67 H 0.5850 -0.2108 0.8803 0.067 Uiso 1 1 calc R . . C68 C 0.4178(7) -0.2178(6) 0.8800(6) 0.053(2) Uani 1 1 d . . . H68 H 0.4415 -0.2650 0.8266 0.063 Uiso 1 1 calc R . . C69 C 0.2971(6) -0.1804(5) 0.9259(5) 0.0398(17) Uani 1 1 d . . . H69 H 0.2388 -0.2009 0.9023 0.048 Uiso 1 1 calc R . . C70 C 0.0210(6) -0.1045(5) 0.9992(5) 0.0325(15) Uani 1 1 d . . . C71 C -0.0023(6) -0.0581(6) 0.9106(5) 0.0409(17) Uani 1 1 d . . . H71 H 0.0256 -0.0003 0.8866 0.049 Uiso 1 1 calc R . . C72 C -0.0656(6) -0.0954(6) 0.8576(5) 0.0437(18) Uani 1 1 d . . . H72 H -0.0819 -0.0626 0.7980 0.052 Uiso 1 1 calc R . . C73 C -0.1055(7) -0.1806(6) 0.8914(6) 0.049(2) Uani 1 1 d . . . H73 H -0.1481 -0.2069 0.8547 0.059 Uiso 1 1 calc R . . C74 C -0.0825(7) -0.2265(6) 0.9787(6) 0.052(2) Uani 1 1 d . . . H74 H -0.1103 -0.2845 1.0025 0.062 Uiso 1 1 calc R . . C75 C -0.0198(6) -0.1895(5) 1.0316(5) 0.0392(17) Uani 1 1 d . . . H75 H -0.0042 -0.2225 1.0913 0.047 Uiso 1 1 calc R . . C76 C -0.3290(6) 0.0573(5) 1.0473(5) 0.0320(15) Uani 1 1 d . . . H76A H -0.3503 -0.0065 1.0405 0.038 Uiso 1 1 calc R . . H76B H -0.2587 0.0593 0.9924 0.038 Uiso 1 1 calc R . . C77 C -0.4327(6) 0.1466(5) 1.0359(4) 0.0275(14) Uani 1 1 d . . . C78 C -0.4124(6) 0.2351(5) 0.9820(4) 0.0288(14) Uani 1 1 d . . . C79 C -0.5124(6) 0.3115(5) 0.9712(5) 0.0355(16) Uani 1 1 d . . . H79 H -0.5014 0.3711 0.9351 0.043 Uiso 1 1 calc R . . C80 C -0.6274(6) 0.3035(5) 1.0113(5) 0.0361(16) Uani 1 1 d . . . H80 H -0.6936 0.3571 1.0018 0.043 Uiso 1 1 calc R . . C81 C -0.6467(6) 0.2187(5) 1.0648(5) 0.0369(16) Uani 1 1 d . . . H81 H -0.7258 0.2141 1.0934 0.044 Uiso 1 1 calc R . . C82 C -0.5501(6) 0.1406(5) 1.0763(5) 0.0369(16) Uani 1 1 d . . . H82 H -0.5633 0.0815 1.1122 0.044 Uiso 1 1 calc R . . C83 C -0.2031(6) 0.1760(5) 0.8205(5) 0.0325(15) Uani 1 1 d . . . C84 C -0.2715(6) 0.1323(5) 0.7754(5) 0.0333(15) Uani 1 1 d . . . H84 H -0.3529 0.1372 0.8069 0.040 Uiso 1 1 calc R . . C85 C -0.2197(7) 0.0818(5) 0.6848(5) 0.0441(19) Uani 1 1 d . . . H85 H -0.2667 0.0535 0.6542 0.053 Uiso 1 1 calc R . . C86 C -0.1020(7) 0.0722(6) 0.6389(5) 0.0459(19) Uani 1 1 d . . . H86 H -0.0675 0.0361 0.5778 0.055 Uiso 1 1 calc R . . C87 C -0.0337(7) 0.1146(5) 0.6809(5) 0.0427(18) Uani 1 1 d . . . H87 H 0.0476 0.1085 0.6484 0.051 Uiso 1 1 calc R . . C88 C -0.0836(6) 0.1664(5) 0.7711(5) 0.0332(15) Uani 1 1 d . . . H88 H -0.0358 0.1958 0.7996 0.040 Uiso 1 1 calc R . . C89 C -0.2784(6) 0.3769(5) 0.8912(5) 0.0310(15) Uani 1 1 d . . . C90 C -0.2528(6) 0.4472(5) 0.9434(5) 0.0384(17) Uani 1 1 d . . . H90 H -0.2300 0.4275 1.0044 0.046 Uiso 1 1 calc R . . C91 C -0.2595(6) 0.5457(5) 0.9092(5) 0.0419(17) Uani 1 1 d . . . H91 H -0.2414 0.5930 0.9463 0.050 Uiso 1 1 calc R . . C92 C -0.2923(6) 0.5739(5) 0.8217(5) 0.0423(18) Uani 1 1 d . . . H92 H -0.2980 0.6416 0.7984 0.051 Uiso 1 1 calc R . . C93 C -0.3179(6) 0.5053(5) 0.7656(5) 0.0402(17) Uani 1 1 d . . . H93 H -0.3391 0.5252 0.7039 0.048 Uiso 1 1 calc R . . C94 C -0.3118(6) 0.4076(5) 0.8016(5) 0.0338(15) Uani 1 1 d . . . H94 H -0.3305 0.3606 0.7648 0.041 Uiso 1 1 calc R . . N1 N 0.2535(5) 0.5379(4) 0.3271(4) 0.0354(13) Uani 1 1 d . . . N2 N 0.3964(5) 0.5549(4) 0.4076(4) 0.0309(12) Uani 1 1 d . . . N3 N -0.1568(4) 0.0733(4) 1.2267(4) 0.0307(12) Uani 1 1 d . . . N4 N -0.2949(4) 0.0555(4) 1.1443(3) 0.0277(11) Uani 1 1 d . . . C61 C 0.1166(6) 0.2149(5) 0.9438(6) 0.0412(17) Uani 1 1 d . . . H61 H 0.1543 0.2390 0.8817 0.049 Uiso 1 1 calc R . . C62 C 0.0433(6) 0.2821(5) 1.0174(6) 0.0433(18) Uani 1 1 d . . . H62 H 0.0282 0.3532 1.0058 0.052 Uiso 1 1 calc R . . C63 C -0.0085(6) 0.2457(5) 1.1086(5) 0.0367(16) Uani 1 1 d . . . H63 H -0.0564 0.2925 1.1599 0.044 Uiso 1 1 calc R . . C65 C 0.3473(7) -0.0839(6) 1.0370(7) 0.060(2) Uani 1 1 d . . . H65 H 0.3245 -0.0381 1.0914 0.072 Uiso 1 1 calc R . . C66 C 0.4654(7) -0.1197(6) 0.9906(8) 0.072(3) Uani 1 1 d . . . H66 H 0.5234 -0.0979 1.0133 0.086 Uiso 1 1 calc R . . P1 P -0.01146(14) 0.69092(12) 0.47468(11) 0.0309(4) Uani 1 1 d . . . P2 P 0.35360(14) 0.37853(11) 0.61235(11) 0.0307(4) Uani 1 1 d . . . P3 P 0.10616(14) -0.06457(12) 1.07606(12) 0.0324(4) Uani 1 1 d . . . P4 P -0.25841(14) 0.24594(12) 0.93802(11) 0.0302(4) Uani 1 1 d . . . P5 P -0.1293(5) 0.5514(4) 1.2038(4) 0.0325(12) Uani 0.538(6) 1 d PDU A 1 F1 F -0.2553(7) 0.6331(6) 1.2336(8) 0.067(3) Uani 0.538(6) 1 d PDU A 1 F2 F -0.1313(9) 0.5573(8) 1.0902(5) 0.072(2) Uani 0.538(6) 1 d PDU A 1 F3 F -0.0604(9) 0.6381(7) 1.1872(7) 0.050(3) Uani 0.538(6) 1 d PDU A 1 F4 F -0.0053(6) 0.4693(6) 1.1771(7) 0.057(2) Uani 0.538(6) 1 d PDU A 1 F5 F -0.1228(7) 0.5431(6) 1.3186(4) 0.0400(19) Uani 0.538(6) 1 d PDU A 1 F6 F -0.1978(8) 0.4640(6) 1.2218(7) 0.053(2) Uani 0.538(6) 1 d PDU A 1 P5A P -0.1481(6) 0.5678(5) 1.2011(5) 0.0470(19) Uani 0.462(6) 1 d PDU A 2 F1A F -0.2627(8) 0.6144(7) 1.2892(6) 0.064(3) Uani 0.462(6) 1 d PDU A 2 F2A F -0.2149(8) 0.6382(7) 1.1263(6) 0.065(2) Uani 0.462(6) 1 d PDU A 2 F3A F -0.0942(9) 0.6575(7) 1.2199(8) 0.053(3) Uani 0.462(6) 1 d PDU A 2 F4A F -0.0363(8) 0.5240(8) 1.1138(7) 0.087(3) Uani 0.462(6) 1 d PDU A 2 F5A F -0.0855(8) 0.4969(7) 1.2794(8) 0.070(3) Uani 0.462(6) 1 d PDU A 2 F6A F -0.2062(9) 0.4804(7) 1.1833(8) 0.059(3) Uani 0.462(6) 1 d PDU A 2 P6 P 0.2287(9) 0.0763(7) 1.3468(7) 0.0339(18) Uani 0.488(11) 1 d PU B 1 F7 F 0.2096(9) 0.0959(8) 1.2374(7) 0.041(2) Uani 0.488(11) 1 d PU B 1 F8 F 0.2921(13) 0.1686(11) 1.3349(14) 0.050(3) Uani 0.488(11) 1 d PU B 1 F9 F 0.3552(8) -0.0016(8) 1.2988(10) 0.057(3) Uani 0.488(11) 1 d PU B 1 F10 F 0.2556(11) 0.0517(10) 1.4532(8) 0.064(3) Uani 0.488(11) 1 d PU B 1 F11 F 0.1639(12) -0.0132(10) 1.3550(11) 0.044(3) Uani 0.488(11) 1 d PU B 1 F12 F 0.1014(9) 0.1550(9) 1.3892(9) 0.059(3) Uani 0.488(11) 1 d PU B 1 P6A P 0.2249(8) 0.0770(7) 1.3520(7) 0.041(2) Uani 0.512(11) 1 d PDU B 2 F7A F 0.1164(9) 0.1728(6) 1.3424(8) 0.053(2) Uani 0.512(11) 1 d PDU B 2 F8A F 0.3141(12) 0.1463(10) 1.3273(12) 0.061(4) Uani 0.512(11) 1 d PDU B 2 F9A F 0.2490(11) 0.0557(9) 1.2358(6) 0.072(3) Uani 0.512(11) 1 d PDU B 2 F10A F 0.3300(7) -0.0174(6) 1.3641(10) 0.065(3) Uani 0.512(11) 1 d PDU B 2 F11A F 0.1319(10) 0.0087(8) 1.3782(9) 0.046(3) Uani 0.512(11) 1 d PDU B 2 F12A F 0.1969(9) 0.1021(8) 1.4685(5) 0.057(2) Uani 0.512(11) 1 d PDU B 2 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 0.029(4) 0.028(4) 0.032(3) 0.002(3) -0.009(3) -0.004(3) C2 0.037(3) 0.092(5) 0.027(3) -0.004(3) -0.004(3) -0.010(4) C3 0.040(3) 0.074(5) 0.033(3) 0.012(3) -0.006(3) -0.011(3) C4 0.033(3) 0.053(4) 0.036(3) 0.001(3) -0.003(2) -0.014(3) C5 0.037(3) 0.061(4) 0.057(4) -0.014(3) -0.007(3) -0.002(3) C6 0.042(4) 0.092(5) 0.053(4) -0.032(4) 0.000(3) -0.009(4) C7 0.050(5) 0.164(10) 0.033(4) 0.005(5) -0.014(4) -0.028(6) C8 0.056(5) 0.046(4) 0.052(4) 0.019(3) 0.002(3) -0.001(3) C9 0.052(5) 0.153(9) 0.036(4) 0.029(5) -0.004(4) -0.036(5) C10 0.034(4) 0.046(4) 0.042(4) -0.012(3) -0.014(3) -0.003(3) C11 0.021(3) 0.033(4) 0.049(4) -0.005(3) -0.011(3) -0.007(3) C12 0.028(3) 0.027(4) 0.036(4) 0.003(3) -0.015(3) -0.006(3) C13 0.033(3) 0.029(4) 0.039(4) 0.005(3) -0.003(3) -0.013(3) C14 0.040(4) 0.044(4) 0.056(4) 0.019(3) -0.015(3) -0.019(3) C15 0.042(4) 0.025(4) 0.085(6) 0.007(4) -0.019(4) -0.020(3) C16 0.035(4) 0.030(4) 0.071(5) -0.007(3) -0.017(4) -0.008(3) C17 0.039(4) 0.023(3) 0.037(4) 0.005(3) -0.006(3) -0.007(3) C18 0.038(4) 0.029(4) 0.080(5) -0.006(3) -0.010(4) -0.008(3) C19 0.029(4) 0.040(4) 0.108(6) -0.015(4) -0.002(4) -0.008(3) C20 0.037(4) 0.031(4) 0.084(5) 0.004(4) 0.009(4) -0.002(3) C21 0.052(5) 0.039(4) 0.044(4) -0.005(3) 0.006(4) -0.002(4) C22 0.041(4) 0.035(4) 0.043(4) -0.001(3) 0.001(3) -0.005(3) C23 0.033(4) 0.023(3) 0.031(3) 0.000(3) 0.001(3) -0.007(3) C24 0.046(4) 0.025(4) 0.039(4) 0.008(3) -0.008(3) -0.010(3) C25 0.057(5) 0.034(4) 0.036(4) 0.003(3) -0.010(4) -0.010(4) C26 0.051(5) 0.041(5) 0.052(5) -0.005(4) -0.018(4) -0.011(4) C27 0.071(6) 0.039(4) 0.053(5) 0.009(4) -0.018(4) -0.030(4) C28 0.053(5) 0.033(4) 0.040(4) -0.003(3) -0.012(4) -0.010(3) C29 0.036(4) 0.028(4) 0.028(3) -0.003(3) -0.003(3) -0.010(3) C30 0.045(4) 0.036(4) 0.027(3) 0.000(3) -0.011(3) -0.024(3) C31 0.034(4) 0.041(4) 0.022(3) 0.000(3) -0.013(3) -0.015(3) C32 0.030(4) 0.039(4) 0.028(3) 0.007(3) -0.008(3) -0.007(3) C33 0.045(4) 0.037(4) 0.041(4) 0.006(3) -0.018(4) -0.010(3) C34 0.031(4) 0.061(5) 0.038(4) 0.005(3) -0.016(3) -0.020(3) C35 0.043(4) 0.035(4) 0.030(3) 0.006(3) -0.003(3) -0.020(3) C36 0.034(4) 0.027(4) 0.026(3) 0.003(3) -0.003(3) -0.013(3) C37 0.036(4) 0.029(4) 0.035(4) 0.004(3) -0.008(3) -0.006(3) C38 0.046(4) 0.034(4) 0.047(4) -0.010(3) -0.004(3) -0.014(3) C39 0.040(4) 0.038(4) 0.035(3) 0.012(3) 0.000(3) -0.012(3) C40 0.041(4) 0.025(4) 0.040(4) 0.010(3) -0.008(3) -0.003(3) C41 0.044(4) 0.046(4) 0.031(4) 0.001(3) -0.016(3) -0.013(3) C42 0.038(4) 0.022(3) 0.033(4) 0.010(3) -0.014(3) -0.008(3) C43 0.048(4) 0.034(4) 0.040(4) 0.008(3) -0.012(4) -0.011(3) C44 0.040(4) 0.041(4) 0.042(4) 0.007(3) -0.002(4) 0.001(4) C45 0.067(6) 0.037(4) 0.027(4) 0.005(3) -0.012(4) 0.007(4) C46 0.061(5) 0.030(4) 0.042(4) -0.004(3) -0.025(4) -0.004(4) C47 0.045(4) 0.034(4) 0.037(4) 0.004(3) -0.014(3) -0.010(3) C48 0.029(3) 0.027(3) 0.022(3) 0.000(2) -0.004(3) -0.004(3) C49 0.030(3) 0.053(4) 0.027(3) 0.009(3) -0.005(2) -0.007(3) C50 0.032(3) 0.051(4) 0.031(3) 0.000(3) -0.004(2) -0.009(3) C51 0.037(3) 0.043(3) 0.031(3) 0.008(2) -0.007(2) -0.014(3) C52 0.055(4) 0.047(3) 0.042(3) 0.007(3) -0.010(3) -0.020(3) C53 0.044(4) 0.043(3) 0.044(3) 0.017(3) -0.009(3) -0.008(3) C54 0.041(4) 0.083(5) 0.027(3) 0.010(3) -0.014(3) -0.021(4) C55 0.043(4) 0.083(5) 0.029(3) 0.012(3) -0.006(3) -0.014(3) C56 0.037(3) 0.053(4) 0.039(3) -0.011(3) -0.006(3) 0.005(3) C57 0.026(3) 0.039(3) 0.031(3) -0.004(3) -0.008(3) -0.010(3) C58 0.029(3) 0.035(4) 0.027(3) -0.002(3) -0.009(3) -0.008(3) C59 0.025(3) 0.025(3) 0.040(4) 0.006(3) -0.007(3) -0.007(3) C60 0.032(3) 0.028(4) 0.047(4) -0.004(3) -0.009(3) -0.001(3) C64 0.033(4) 0.025(4) 0.048(4) 0.002(3) -0.004(3) -0.002(3) C67 0.036(4) 0.039(4) 0.078(5) -0.005(4) 0.009(4) -0.007(3) C68 0.049(5) 0.042(5) 0.052(4) -0.001(3) 0.006(4) -0.004(4) C69 0.045(4) 0.035(4) 0.036(4) 0.005(3) -0.010(3) -0.007(3) C70 0.029(4) 0.031(4) 0.034(4) 0.001(3) -0.007(3) -0.005(3) C71 0.042(4) 0.037(4) 0.042(4) 0.005(3) -0.012(4) -0.009(3) C72 0.043(4) 0.045(5) 0.047(4) 0.006(4) -0.024(4) -0.007(4) C73 0.056(5) 0.050(5) 0.051(5) -0.006(4) -0.017(4) -0.022(4) C74 0.066(5) 0.040(5) 0.054(5) 0.001(4) -0.014(4) -0.023(4) C75 0.048(4) 0.038(4) 0.033(4) 0.011(3) -0.007(3) -0.018(3) C76 0.036(4) 0.039(4) 0.030(3) 0.007(3) -0.018(3) -0.016(3) C77 0.031(3) 0.029(3) 0.022(3) 0.000(3) -0.009(3) -0.003(3) C78 0.036(4) 0.029(4) 0.023(3) 0.000(3) -0.010(3) -0.009(3) C79 0.044(4) 0.036(4) 0.033(4) 0.001(3) -0.014(3) -0.017(3) C80 0.028(3) 0.046(4) 0.036(4) -0.001(3) -0.015(3) -0.006(3) C81 0.033(4) 0.040(4) 0.037(4) 0.003(3) -0.009(3) -0.008(3) C82 0.039(4) 0.047(4) 0.035(4) 0.005(3) -0.020(3) -0.018(3) C83 0.036(4) 0.031(4) 0.028(3) 0.002(3) -0.006(3) -0.006(3) C84 0.033(4) 0.033(4) 0.032(4) 0.000(3) -0.010(3) -0.005(3) C85 0.057(5) 0.040(5) 0.038(4) 0.004(3) -0.024(4) -0.007(4) C86 0.058(5) 0.041(4) 0.030(4) -0.003(3) -0.014(4) 0.004(4) C87 0.049(5) 0.031(4) 0.038(4) 0.010(3) -0.005(4) -0.003(3) C88 0.035(4) 0.029(4) 0.036(4) 0.007(3) -0.010(3) -0.008(3) C89 0.027(3) 0.035(4) 0.032(3) 0.001(3) -0.007(3) -0.010(3) C90 0.035(4) 0.048(5) 0.032(4) -0.004(3) -0.004(3) -0.013(3) C91 0.045(4) 0.036(4) 0.044(4) -0.010(3) -0.007(3) -0.009(3) C92 0.043(4) 0.018(3) 0.053(4) -0.009(3) 0.006(3) 0.000(3) C93 0.037(4) 0.050(5) 0.030(4) 0.000(3) -0.002(3) -0.012(3) C94 0.043(4) 0.028(4) 0.032(3) 0.003(3) -0.006(3) -0.016(3) N1 0.028(3) 0.049(3) 0.028(3) -0.006(2) -0.007(2) -0.005(2) N2 0.027(3) 0.035(3) 0.028(3) 0.004(2) -0.003(2) -0.008(2) N3 0.026(3) 0.035(3) 0.030(3) -0.003(2) -0.006(2) -0.007(2) N4 0.029(3) 0.032(3) 0.024(2) 0.0016(19) -0.010(2) -0.008(2) C61 0.036(4) 0.039(4) 0.054(4) 0.008(3) -0.015(3) -0.016(3) C62 0.035(4) 0.025(4) 0.068(5) 0.008(3) -0.021(4) -0.001(3) C63 0.027(3) 0.032(4) 0.049(4) -0.013(3) -0.005(3) -0.003(3) C65 0.033(4) 0.055(5) 0.087(6) -0.038(4) -0.002(4) -0.005(4) C66 0.049(5) 0.049(5) 0.123(8) -0.029(5) -0.016(5) -0.019(4) P1 0.0323(9) 0.0273(9) 0.0305(9) 0.0038(7) -0.0055(8) -0.0062(7) P2 0.0364(10) 0.0315(10) 0.0278(9) 0.0041(7) -0.0109(8) -0.0129(8) P3 0.0325(10) 0.0284(9) 0.0344(9) 0.0032(7) -0.0061(8) -0.0073(8) P4 0.0311(9) 0.0354(10) 0.0281(9) 0.0044(7) -0.0115(8) -0.0128(8) P5 0.035(2) 0.034(2) 0.036(2) 0.0062(17) -0.0159(17) -0.0163(18) F1 0.053(4) 0.055(4) 0.096(6) -0.007(4) -0.039(4) 0.003(4) F2 0.099(5) 0.094(5) 0.044(4) 0.015(4) -0.039(4) -0.045(4) F3 0.063(5) 0.055(5) 0.045(5) 0.015(4) -0.018(4) -0.037(4) F4 0.041(4) 0.058(5) 0.078(5) -0.028(4) -0.015(4) -0.014(3) F5 0.043(4) 0.051(4) 0.022(3) -0.011(3) 0.005(3) -0.016(3) F6 0.058(5) 0.053(5) 0.059(5) 0.006(4) -0.017(4) -0.034(4) P5A 0.049(3) 0.051(3) 0.046(3) 0.005(2) -0.013(2) -0.022(2) F1A 0.069(5) 0.074(5) 0.038(4) -0.009(4) 0.019(4) -0.030(4) F2A 0.061(5) 0.082(5) 0.060(4) 0.032(4) -0.023(4) -0.030(4) F3A 0.050(5) 0.053(5) 0.059(6) -0.005(4) 0.003(4) -0.029(4) F4A 0.061(5) 0.090(5) 0.092(5) -0.025(5) 0.017(5) -0.013(4) F5A 0.061(5) 0.077(5) 0.086(6) 0.030(4) -0.034(4) -0.033(4) F6A 0.059(5) 0.054(5) 0.078(6) -0.003(4) -0.022(4) -0.029(4) P6 0.038(3) 0.038(3) 0.034(3) -0.004(3) -0.012(3) -0.019(3) F7 0.037(4) 0.047(5) 0.045(4) 0.017(4) -0.023(4) -0.011(4) F8 0.041(5) 0.038(5) 0.073(6) -0.015(4) -0.007(4) -0.016(4) F9 0.038(4) 0.050(5) 0.084(6) -0.014(4) -0.015(4) -0.007(4) F10 0.080(6) 0.083(6) 0.048(4) 0.013(4) -0.032(4) -0.041(4) F11 0.052(5) 0.036(5) 0.054(6) 0.005(4) -0.015(4) -0.025(4) F12 0.043(4) 0.062(5) 0.062(5) -0.015(4) 0.018(4) -0.019(4) P6A 0.041(3) 0.042(3) 0.042(3) 0.005(3) -0.006(3) -0.017(3) F7A 0.056(5) 0.042(4) 0.069(5) 0.019(4) -0.034(4) -0.010(3) F8A 0.058(6) 0.056(6) 0.078(6) 0.005(5) -0.014(5) -0.032(5) F9A 0.084(6) 0.077(6) 0.052(4) -0.008(4) -0.002(4) -0.023(5) F10A 0.037(4) 0.046(4) 0.105(6) -0.008(5) -0.017(4) 0.002(3) F11A 0.051(5) 0.044(5) 0.048(5) 0.005(4) -0.015(4) -0.021(4) F12A 0.073(5) 0.067(5) 0.037(3) -0.017(3) -0.019(4) -0.020(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 C1 N2 1.316(8) . ? C1 N1 1.334(7) . ? C1 H1 0.9500 . ? C2 N1 1.510(8) . ? C2 C7 1.513(10) . ? C2 C3 1.519(9) . ? C2 C6 1.566(9) . ? C3 C4 1.525(8) . ? C3 C8 1.537(9) . ? C3 C9 1.553(9) . ? C4 N2 1.475(7) . ? C4 C5 1.525(8) . ? C4 H4 1.0000 . ? C5 C6 1.541(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.479(8) . ? C10 C11 1.506(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.387(9) . ? C11 C12 1.392(9) . ? C12 C13 1.405(9) . ? C12 P1 1.845(7) . ? C13 C14 1.401(9) . ? C13 H13 0.9500 . ? C14 C15 1.384(10) . ? C14 H14 0.9500 . ? C15 C16 1.359(11) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.388(9) . ? C17 C18 1.397(9) . ? C17 P1 1.823(7) . ? C18 C19 1.394(10) . ? C18 H18 0.9500 . ? C19 C20 1.362(11) . ? C19 H19 0.9500 . ? C20 C21 1.366(11) . ? C20 H20 0.9500 . ? C21 C22 1.393(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.391(8) . ? C23 C28 1.399(9) . ? C23 P1 1.836(7) . ? C24 C25 1.376(9) . ? C24 H24 0.9500 . ? C25 C26 1.380(10) . ? C25 H25 0.9500 . ? C26 C27 1.380(10) . ? C26 H26 0.9500 . ? C27 C28 1.397(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N2 1.459(8) . ? C29 C30 1.512(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C35 1.382(9) . ? C30 C31 1.399(9) . ? C31 C32 1.400(9) . ? C31 P2 1.851(7) . ? C32 C33 1.400(9) . ? C32 H32 0.9500 . ? C33 C34 1.385(10) . ? C33 H33 0.9500 . ? C34 C35 1.404(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.389(8) . ? C36 C41 1.401(8) . ? C36 P2 1.830(6) . ? C37 C38 1.405(9) . ? C37 H37 0.9500 . ? C38 C39 1.375(9) . ? C38 H38 0.9500 . ? C39 C40 1.374(10) . ? C39 H39 0.9500 . ? C40 C41 1.392(9) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.372(8) . ? C42 C43 1.400(9) . ? C42 P2 1.849(7) . ? C43 C44 1.385(9) . ? C43 H43 0.9500 . ? C44 C45 1.395(10) . ? C44 H44 0.9500 . ? C45 C46 1.385(11) . ? C45 H45 0.9500 . ? C46 C47 1.395(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 N3 1.300(7) . ? C48 N4 1.308(7) . ? C48 H48 0.9500 . ? C49 N3 1.509(7) . ? C49 C54 1.520(8) . ? C49 C53 1.538(8) . ? C49 C50 1.542(7) . ? C50 C56 1.533(8) . ? C50 C55 1.536(9) . ? C50 C51 1.537(7) . ? C51 N4 1.495(7) . ? C51 C52 1.530(8) . ? C51 H51 1.0000 . ? C52 C53 1.546(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.492(9) . ? C57 N3 1.503(8) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C63 1.387(9) . ? C58 C59 1.415(9) . ? C59 C60 1.379(10) . ? C59 P3 1.842(6) . ? C60 C61 1.387(9) . ? C60 H60 0.9500 . ? C64 C65 1.378(9) . ? C64 C69 1.384(9) . ? C64 P3 1.833(7) . ? C67 C68 1.375(11) . ? C67 C66 1.377(11) . ? C67 H67 0.9500 . ? C68 C69 1.393(10) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C75 1.387(9) . ? C70 C71 1.396(9) . ? C70 P3 1.840(7) . ? C71 C72 1.380(9) . ? C71 H71 0.9500 . ? C72 C73 1.388(10) . ? C72 H72 0.9500 . ? C73 C74 1.377(10) . ? C73 H73 0.9500 . ? C74 C75 1.373(9) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 N4 1.493(7) . ? C76 C77 1.516(8) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C82 1.402(9) . ? C77 C78 1.425(8) . ? C78 C79 1.390(9) . ? C78 P4 1.837(7) . ? C79 C80 1.384(9) . ? C79 H79 0.9500 . ? C80 C81 1.376(9) . ? C80 H80 0.9500 . ? C81 C82 1.377(9) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C88 1.400(9) . ? C83 C84 1.410(9) . ? C83 P4 1.824(6) . ? C84 C85 1.390(9) . ? C84 H84 0.9500 . ? C85 C86 1.370(11) . ? C85 H85 0.9500 . ? C86 C87 1.370(10) . ? C86 H86 0.9500 . ? C87 C88 1.392(9) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C90 1.380(9) . ? C89 C94 1.398(8) . ? C89 P4 1.836(7) . ? C90 C91 1.386(10) . ? C90 H90 0.9500 . ? C91 C92 1.364(9) . ? C91 H91 0.9500 . ? C92 C93 1.396(10) . ? C92 H92 0.9500 . ? C93 C94 1.383(9) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? C61 C62 1.378(9) . ? C61 H61 0.9500 . ? C62 C63 1.387(10) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C65 C66 1.367(11) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? P5 F4 1.573(7) . ? P5 F2 1.574(7) . ? P5 F1 1.590(7) . ? P5 F3 1.595(6) . ? P5 F6 1.599(6) . ? P5 F5 1.604(6) . ? P5A F4A 1.572(8) . ? P5A F2A 1.578(7) . ? P5A F5A 1.593(7) . ? P5A F3A 1.596(7) . ? P5A F6A 1.598(7) . ? P5A F1A 1.605(8) . ? P6 F10 1.579(12) . ? P6 F7 1.579(11) . ? P6 F11 1.602(12) . ? P6 F12 1.604(12) . ? P6 F9 1.608(12) . ? P6 F8 1.623(13) . ? P6A F10A 1.570(9) . ? P6A F8A 1.577(9) . ? P6A F9A 1.594(9) . ? P6A F7A 1.597(9) . ? P6A F11A 1.603(9) . ? P6A F12A 1.604(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 122.7(6) . . ? N2 C1 H1 118.7 . . ? N1 C1 H1 118.7 . . ? N1 C2 C7 109.4(5) . . ? N1 C2 C3 108.3(5) . . ? C7 C2 C3 115.7(7) . . ? N1 C2 C6 105.3(5) . . ? C7 C2 C6 114.2(6) . . ? C3 C2 C6 103.2(5) . . ? C2 C3 C4 99.6(5) . . ? C2 C3 C8 114.0(5) . . ? C4 C3 C8 114.4(5) . . ? C2 C3 C9 111.8(6) . . ? C4 C3 C9 109.0(5) . . ? C8 C3 C9 107.9(6) . . ? N2 C4 C3 107.9(4) . . ? N2 C4 C5 108.5(5) . . ? C3 C4 C5 104.2(5) . . ? N2 C4 H4 111.9 . . ? C3 C4 H4 111.9 . . ? C5 C4 H4 111.9 . . ? C4 C5 C6 105.8(5) . . ? C4 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? C6 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C5 C6 C2 103.6(5) . . ? C5 C6 H6A 111.0 . . ? C2 C6 H6A 111.0 . . ? C5 C6 H6B 111.0 . . ? C2 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 114.3(5) . . ? N1 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N1 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C16 C11 C12 119.9(7) . . ? C16 C11 C10 117.5(6) . . ? C12 C11 C10 122.6(6) . . ? C11 C12 C13 118.9(6) . . ? C11 C12 P1 119.2(5) . . ? C13 C12 P1 121.9(5) . . ? C14 C13 C12 119.7(7) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 120.2(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 121.6(7) . . ? C15 C16 H16 119.2 . . ? C11 C16 H16 119.2 . . ? C22 C17 C18 117.5(7) . . ? C22 C17 P1 125.7(5) . . ? C18 C17 P1 116.4(5) . . ? C19 C18 C17 121.7(8) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 118.9(8) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C19 C20 C21 121.0(7) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C22 120.4(7) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 120.4(7) . . ? C17 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C28 118.0(6) . . ? C24 C23 P1 126.6(5) . . ? C28 C23 P1 115.3(5) . . ? C25 C24 C23 121.3(6) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.9(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 119.9(7) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C23 120.5(6) . . ? C27 C28 H28 119.7 . . ? C23 C28 H28 119.7 . . ? N2 C29 C30 112.2(5) . . ? N2 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? N2 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C35 C30 C31 118.9(6) . . ? C35 C30 C29 117.8(6) . . ? C31 C30 C29 123.3(6) . . ? C30 C31 C32 119.4(6) . . ? C30 C31 P2 118.9(5) . . ? C32 C31 P2 121.5(5) . . ? C31 C32 C33 121.0(6) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C34 C33 C32 119.8(6) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 118.7(6) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? C30 C35 C34 122.3(6) . . ? C30 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C37 C36 C41 119.3(6) . . ? C37 C36 P2 117.8(5) . . ? C41 C36 P2 122.8(5) . . ? C36 C37 C38 118.9(6) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C39 C38 C37 121.5(6) . . ? C39 C38 H38 119.3 . . ? C37 C38 H38 119.3 . . ? C40 C39 C38 119.5(6) . . ? C40 C39 H39 120.2 . . ? C38 C39 H39 120.2 . . ? C39 C40 C41 120.2(7) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C36 120.5(6) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? C47 C42 C43 118.7(6) . . ? C47 C42 P2 125.4(5) . . ? C43 C42 P2 115.9(5) . . ? C44 C43 C42 120.8(7) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.8(7) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C46 C45 C44 119.5(7) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 119.9(7) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C42 C47 C46 121.2(7) . . ? C42 C47 H47 119.4 . . ? C46 C47 H47 119.4 . . ? N3 C48 N4 123.4(6) . . ? N3 C48 H48 118.3 . . ? N4 C48 H48 118.3 . . ? N3 C49 C54 111.1(5) . . ? N3 C49 C53 106.6(4) . . ? C54 C49 C53 113.4(5) . . ? N3 C49 C50 106.1(4) . . ? C54 C49 C50 115.4(5) . . ? C53 C49 C50 103.4(4) . . ? C56 C50 C55 108.8(5) . . ? C56 C50 C51 113.4(4) . . ? C55 C50 C51 108.9(5) . . ? C56 C50 C49 115.0(5) . . ? C55 C50 C49 111.2(5) . . ? C51 C50 C49 99.2(4) . . ? N4 C51 C52 107.3(4) . . ? N4 C51 C50 107.6(4) . . ? C52 C51 C50 104.0(4) . . ? N4 C51 H51 112.5 . . ? C52 C51 H51 112.5 . . ? C50 C51 H51 112.5 . . ? C51 C52 C53 103.6(5) . . ? C51 C52 H52A 111.0 . . ? C53 C52 H52A 111.0 . . ? C51 C52 H52B 111.0 . . ? C53 C52 H52B 111.0 . . ? H52A C52 H52B 109.0 . . ? C49 C53 C52 106.5(5) . . ? C49 C53 H53A 110.4 . . ? C52 C53 H53A 110.4 . . ? C49 C53 H53B 110.4 . . ? C52 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C50 C56 H56A 109.5 . . ? C50 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C50 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N3 112.7(5) . . ? C58 C57 H57A 109.0 . . ? N3 C57 H57A 109.0 . . ? C58 C57 H57B 109.0 . . ? N3 C57 H57B 109.0 . . ? H57A C57 H57B 107.8 . . ? C63 C58 C59 119.2(6) . . ? C63 C58 C57 119.4(6) . . ? C59 C58 C57 121.3(6) . . ? C60 C59 C58 118.0(6) . . ? C60 C59 P3 123.2(5) . . ? C58 C59 P3 118.8(5) . . ? C59 C60 C61 122.7(7) . . ? C59 C60 H60 118.7 . . ? C61 C60 H60 118.7 . . ? C65 C64 C69 118.4(7) . . ? C65 C64 P3 116.7(5) . . ? C69 C64 P3 124.8(5) . . ? C68 C67 C66 118.5(7) . . ? C68 C67 H67 120.7 . . ? C66 C67 H67 120.7 . . ? C67 C68 C69 120.1(8) . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C64 C69 C68 120.8(7) . . ? C64 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C75 C70 C71 118.2(6) . . ? C75 C70 P3 116.4(5) . . ? C71 C70 P3 125.4(5) . . ? C72 C71 C70 120.6(7) . . ? C72 C71 H71 119.7 . . ? C70 C71 H71 119.7 . . ? C71 C72 C73 120.2(7) . . ? C71 C72 H72 119.9 . . ? C73 C72 H72 119.9 . . ? C74 C73 C72 119.3(7) . . ? C74 C73 H73 120.3 . . ? C72 C73 H73 120.3 . . ? C75 C74 C73 120.6(7) . . ? C75 C74 H74 119.7 . . ? C73 C74 H74 119.7 . . ? C74 C75 C70 121.0(6) . . ? C74 C75 H75 119.5 . . ? C70 C75 H75 119.5 . . ? N4 C76 C77 114.0(5) . . ? N4 C76 H76A 108.8 . . ? C77 C76 H76A 108.8 . . ? N4 C76 H76B 108.8 . . ? C77 C76 H76B 108.8 . . ? H76A C76 H76B 107.7 . . ? C82 C77 C78 119.6(5) . . ? C82 C77 C76 119.5(6) . . ? C78 C77 C76 120.8(6) . . ? C79 C78 C77 117.2(6) . . ? C79 C78 P4 123.7(5) . . ? C77 C78 P4 119.0(4) . . ? C80 C79 C78 122.1(6) . . ? C80 C79 H79 119.0 . . ? C78 C79 H79 119.0 . . ? C81 C80 C79 120.6(6) . . ? C81 C80 H80 119.7 . . ? C79 C80 H80 119.7 . . ? C80 C81 C82 119.3(7) . . ? C80 C81 H81 120.4 . . ? C82 C81 H81 120.4 . . ? C81 C82 C77 121.2(7) . . ? C81 C82 H82 119.4 . . ? C77 C82 H82 119.4 . . ? C88 C83 C84 117.8(6) . . ? C88 C83 P4 117.0(5) . . ? C84 C83 P4 125.2(5) . . ? C85 C84 C83 119.9(6) . . ? C85 C84 H84 120.0 . . ? C83 C84 H84 120.0 . . ? C86 C85 C84 121.0(7) . . ? C86 C85 H85 119.5 . . ? C84 C85 H85 119.5 . . ? C85 C86 C87 120.3(7) . . ? C85 C86 H86 119.9 . . ? C87 C86 H86 119.9 . . ? C86 C87 C88 120.0(7) . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C87 C88 C83 121.0(6) . . ? C87 C88 H88 119.5 . . ? C83 C88 H88 119.5 . . ? C90 C89 C94 118.0(6) . . ? C90 C89 P4 118.8(5) . . ? C94 C89 P4 123.1(5) . . ? C89 C90 C91 121.8(6) . . ? C89 C90 H90 119.1 . . ? C91 C90 H90 119.1 . . ? C92 C91 C90 119.1(6) . . ? C92 C91 H91 120.5 . . ? C90 C91 H91 120.5 . . ? C91 C92 C93 121.3(7) . . ? C91 C92 H92 119.3 . . ? C93 C92 H92 119.3 . . ? C94 C93 C92 118.6(7) . . ? C94 C93 H93 120.7 . . ? C92 C93 H93 120.7 . . ? C93 C94 C89 121.2(6) . . ? C93 C94 H94 119.4 . . ? C89 C94 H94 119.4 . . ? C1 N1 C10 120.6(5) . . ? C1 N1 C2 118.8(5) . . ? C10 N1 C2 120.0(5) . . ? C1 N2 C29 120.7(5) . . ? C1 N2 C4 118.2(5) . . ? C29 N2 C4 121.1(5) . . ? C48 N3 C57 121.1(5) . . ? C48 N3 C49 118.7(5) . . ? C57 N3 C49 120.1(4) . . ? C48 N4 C76 119.8(5) . . ? C48 N4 C51 119.7(4) . . ? C76 N4 C51 120.2(5) . . ? C62 C61 C60 118.9(7) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? C61 C62 C63 119.8(7) . . ? C61 C62 H62 120.1 . . ? C63 C62 H62 120.1 . . ? C62 C63 C58 121.3(6) . . ? C62 C63 H63 119.3 . . ? C58 C63 H63 119.3 . . ? C66 C65 C64 120.5(7) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C67 121.7(8) . . ? C65 C66 H66 119.2 . . ? C67 C66 H66 119.2 . . ? C17 P1 C23 102.4(3) . . ? C17 P1 C12 100.2(3) . . ? C23 P1 C12 102.8(3) . . ? C36 P2 C42 99.1(3) . . ? C36 P2 C31 104.4(3) . . ? C42 P2 C31 102.6(3) . . ? C64 P3 C70 102.5(3) . . ? C64 P3 C59 100.9(3) . . ? C70 P3 C59 103.7(3) . . ? C83 P4 C89 100.2(3) . . ? C83 P4 C78 103.8(3) . . ? C89 P4 C78 103.3(3) . . ? F4 P5 F2 89.1(5) . . ? F4 P5 F1 178.5(6) . . ? F2 P5 F1 92.2(6) . . ? F4 P5 F3 89.2(5) . . ? F2 P5 F3 89.9(5) . . ? F1 P5 F3 91.5(5) . . ? F4 P5 F6 90.5(5) . . ? F2 P5 F6 90.8(5) . . ? F1 P5 F6 88.7(5) . . ? F3 P5 F6 179.3(6) . . ? F4 P5 F5 89.0(5) . . ? F2 P5 F5 178.1(6) . . ? F1 P5 F5 89.7(5) . . ? F3 P5 F5 89.8(4) . . ? F6 P5 F5 89.5(5) . . ? F4A P5A F2A 91.2(6) . . ? F4A P5A F5A 90.8(6) . . ? F2A P5A F5A 177.8(7) . . ? F4A P5A F3A 91.3(5) . . ? F2A P5A F3A 89.7(6) . . ? F5A P5A F3A 91.2(6) . . ? F4A P5A F6A 90.2(6) . . ? F2A P5A F6A 89.3(5) . . ? F5A P5A F6A 89.8(6) . . ? F3A P5A F6A 178.2(7) . . ? F4A P5A F1A 179.0(7) . . ? F2A P5A F1A 87.9(6) . . ? F5A P5A F1A 90.1(6) . . ? F3A P5A F1A 88.2(5) . . ? F6A P5A F1A 90.3(5) . . ? F10 P6 F7 176.4(9) . . ? F10 P6 F11 92.4(8) . . ? F7 P6 F11 87.6(7) . . ? F10 P6 F12 93.8(8) . . ? F7 P6 F12 89.9(7) . . ? F11 P6 F12 89.6(8) . . ? F10 P6 F9 89.1(7) . . ? F7 P6 F9 87.3(7) . . ? F11 P6 F9 90.3(7) . . ? F12 P6 F9 177.2(9) . . ? F10 P6 F8 89.8(9) . . ? F7 P6 F8 90.3(9) . . ? F11 P6 F8 177.8(10) . . ? F12 P6 F8 89.7(8) . . ? F9 P6 F8 90.3(8) . . ? F10A P6A F8A 90.2(7) . . ? F10A P6A F9A 91.9(6) . . ? F8A P6A F9A 89.3(8) . . ? F10A P6A F7A 178.6(8) . . ? F8A P6A F7A 90.4(7) . . ? F9A P6A F7A 89.4(6) . . ? F10A P6A F11A 90.9(7) . . ? F8A P6A F11A 178.8(8) . . ? F9A P6A F11A 91.3(6) . . ? F7A P6A F11A 88.5(6) . . ? F10A P6A F12A 90.2(6) . . ? F8A P6A F12A 90.6(7) . . ? F9A P6A F12A 178.0(8) . . ? F7A P6A F12A 88.6(6) . . ? F11A P6A F12A 88.8(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.284 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.066 data_kjc1134 _database_code_depnum_ccdc_archive 'CCDC 891176' #TrackingRef 'cmpd2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H47 Cl2 N2 P2 Pd, P1 F6, C1 H1 Cl3' _chemical_formula_sum 'C48 H48 Cl5 F6 N2 P3 Pd' _chemical_formula_weight 1143.44 _chemical_absolute_configuration ad 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.7720(9) _cell_length_b 14.6590(6) _cell_length_c 28.2434(13) _cell_angle_alpha 90.00 _cell_angle_beta 117.031(2) _cell_angle_gamma 90.00 _cell_volume 9873.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9398 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.71 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4640 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8559 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15228 _diffrn_reflns_av_R_equivalents 0.0001 _diffrn_reflns_av_sigmaI/netI 0.1065 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 24.71 _reflns_number_total 15228 _reflns_number_gt 9398 _reflns_threshold_expression >2\s(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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. Two anion sites show two-fold disorder. Geometric restraints were applied to the PF6- during refinement to stop distortion of the anions. Restraints were also applied in order to maintain similar atomic displacement parameters for atoms in close proximity. ; _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^)+(0.0893P)^2^+136.1955P] 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 0.09(6) _refine_ls_number_reflns 15228 _refine_ls_number_parameters 1218 _refine_ls_number_restraints 265 _refine_ls_R_factor_all 0.1530 _refine_ls_R_factor_gt 0.0853 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.027 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 0.2733(6) 0.0838(13) 0.6202(7) 0.028(4) Uani 1 1 d U . . H1 H 0.2757 0.1327 0.5992 0.034 Uiso 1 1 calc R . . C2 C 0.2176(7) -0.0333(12) 0.6385(8) 0.044(5) Uani 1 1 d . . . C3 C 0.2221(6) 0.0034(10) 0.6902(6) 0.041(4) Uani 1 1 d . . . H3A H 0.2058 -0.0401 0.7062 0.049 Uiso 1 1 calc R . . H3B H 0.2023 0.0625 0.6846 0.049 Uiso 1 1 calc R . . C4 C 0.2865(6) 0.0157(12) 0.7270(7) 0.035(4) Uani 1 1 d . . . H4A H 0.2958 0.0809 0.7356 0.042 Uiso 1 1 calc R . . H4B H 0.2984 -0.0188 0.7605 0.042 Uiso 1 1 calc R . . C5 C 0.3157(6) -0.0220(10) 0.6948(6) 0.040(4) Uani 1 1 d . . . H5 H 0.3526 -0.0512 0.7180 0.047 Uiso 1 1 calc R . . C6 C 0.2721(6) -0.0908(10) 0.6585(6) 0.040(4) Uani 1 1 d . . . C7 C 0.1646(8) -0.0865(15) 0.6065(9) 0.067(6) Uani 1 1 d . . . H7A H 0.1330 -0.0565 0.6087 0.100 Uiso 1 1 calc R . . H7B H 0.1688 -0.1486 0.6206 0.100 Uiso 1 1 calc R . . H7C H 0.1574 -0.0889 0.5692 0.100 Uiso 1 1 calc R . . C8 C 0.2846(7) -0.1223(14) 0.6109(8) 0.069(6) Uani 1 1 d . . . H8A H 0.2761 -0.0721 0.5854 0.097 Uiso 1 1 calc R . . H8B H 0.2612 -0.1751 0.5930 0.097 Uiso 1 1 calc R . . H8C H 0.3242 -0.1390 0.6250 0.097 Uiso 1 1 calc R . . C9 C 0.2735(9) -0.1765(15) 0.6929(9) 0.069(7) Uani 1 1 d . . . H9A H 0.3125 -0.1942 0.7157 0.103 Uiso 1 1 calc R . . H9B H 0.2536 -0.2274 0.6693 0.103 Uiso 1 1 calc R . . H9C H 0.2552 -0.1613 0.7151 0.103 Uiso 1 1 calc R . . C10 C 0.1738(6) 0.1050(11) 0.5758(7) 0.026(4) Uani 1 1 d . . . H10A H 0.1398 0.0714 0.5712 0.031 Uiso 1 1 calc R . . H10B H 0.1761 0.1604 0.5968 0.031 Uiso 1 1 calc R . . C11 C 0.1648(7) 0.1348(13) 0.5236(8) 0.034(5) Uani 1 1 d . . . C12 C 0.1602(8) 0.2273(12) 0.5061(8) 0.035(5) Uani 1 1 d . . . C13 C 0.1478(7) 0.2416(14) 0.4509(8) 0.041(5) Uani 1 1 d . . . H13 H 0.1422 0.3021 0.4373 0.050 Uiso 1 1 calc R . . C14 C 0.1442(10) 0.1759(15) 0.4203(9) 0.068(7) Uani 1 1 d . . . H14 H 0.1351 0.1892 0.3843 0.082 Uiso 1 1 calc R . . C15 C 0.1529(8) 0.0854(13) 0.4366(7) 0.047(5) Uani 1 1 d . . . H15 H 0.1513 0.0384 0.4128 0.056 Uiso 1 1 calc R . . C16 C 0.1638(7) 0.0651(12) 0.4880(8) 0.041(5) Uani 1 1 d . . . H16 H 0.1707 0.0036 0.4999 0.049 Uiso 1 1 calc R . . C17 C 0.1294(7) 0.3238(13) 0.5809(7) 0.034(5) Uani 1 1 d . . . C18 C 0.0806(7) 0.2684(15) 0.5589(9) 0.051(6) Uani 1 1 d . . . H18 H 0.0722 0.2279 0.5300 0.061 Uiso 1 1 calc R . . C19 C 0.0451(9) 0.2792(17) 0.5843(9) 0.060(7) Uani 1 1 d . . . H19 H 0.0133 0.2410 0.5744 0.072 Uiso 1 1 calc R . . C20 C 0.0569(10) 0.344(2) 0.6224(9) 0.079(9) Uani 1 1 d . . . H20 H 0.0312 0.3520 0.6367 0.095 Uiso 1 1 calc R . . C21 C 0.1040(9) 0.3978(18) 0.6414(9) 0.063(6) Uani 1 1 d . . . H21 H 0.1118 0.4408 0.6691 0.075 Uiso 1 1 calc R . . C22 C 0.1382(7) 0.3871(14) 0.6192(7) 0.042(5) Uani 1 1 d . . . H22 H 0.1702 0.4254 0.6306 0.051 Uiso 1 1 calc R . . C23 C 0.1642(8) 0.4239(15) 0.5139(8) 0.044(5) Uani 1 1 d . . . C24 C 0.1075(9) 0.4422(15) 0.4763(9) 0.058(6) Uani 1 1 d . . . H24 H 0.0795 0.3971 0.4692 0.069 Uiso 1 1 calc R . . C25 C 0.0926(9) 0.5272(17) 0.4494(9) 0.068(7) Uani 1 1 d . . . H25 H 0.0546 0.5411 0.4259 0.081 Uiso 1 1 calc R . . C26 C 0.1350(9) 0.5890(15) 0.4584(9) 0.057(6) Uani 1 1 d . . . H26 H 0.1261 0.6442 0.4385 0.069 Uiso 1 1 calc R . . C27 C 0.1886(7) 0.5733(12) 0.4944(7) 0.031(4) Uani 1 1 d U . . H27 H 0.2165 0.6182 0.5007 0.038 Uiso 1 1 calc R . . C28 C 0.2031(8) 0.4912(13) 0.5226(7) 0.038(5) Uani 1 1 d . . . H28 H 0.2408 0.4817 0.5484 0.045 Uiso 1 1 calc R . . C29 C 0.3751(7) 0.0983(12) 0.6724(8) 0.041(5) Uani 1 1 d . . . H29A H 0.3688 0.1402 0.6427 0.049 Uiso 1 1 calc R . . H29B H 0.4042 0.0534 0.6760 0.049 Uiso 1 1 calc R . . C30 C 0.3932(9) 0.1527(13) 0.7254(10) 0.049(6) Uani 1 1 d . . . C31 C 0.3945(7) 0.2474(11) 0.7305(8) 0.030(5) Uani 1 1 d . . . C32 C 0.4134(7) 0.2879(13) 0.7791(7) 0.038(5) Uani 1 1 d . . . H32 H 0.4118 0.3524 0.7810 0.046 Uiso 1 1 calc R . . C33 C 0.4345(7) 0.2384(14) 0.8253(8) 0.046(5) Uani 1 1 d . . . H33 H 0.4470 0.2678 0.8587 0.055 Uiso 1 1 calc R . . C34 C 0.4372(8) 0.1461(13) 0.8221(8) 0.040(5) Uani 1 1 d U . . H34 H 0.4527 0.1115 0.8540 0.048 Uiso 1 1 calc R . . C35 C 0.4179(7) 0.1000(15) 0.7731(8) 0.042(5) Uani 1 1 d U . . H35 H 0.4212 0.0357 0.7719 0.051 Uiso 1 1 calc R . . C36 C 0.3825(8) 0.4337(15) 0.6892(9) 0.052(6) Uani 1 1 d . . . C37 C 0.3446(9) 0.4834(15) 0.7016(10) 0.060(7) Uani 1 1 d . . . H37 H 0.3116 0.4532 0.6979 0.073 Uiso 1 1 calc R . . C38 C 0.3523(9) 0.5718(14) 0.7185(9) 0.060(7) Uani 1 1 d . . . H38 H 0.3263 0.6011 0.7278 0.072 Uiso 1 1 calc R . . C39 C 0.3978(9) 0.6165(13) 0.7217(8) 0.047(6) Uani 1 1 d . . . H39 H 0.4021 0.6797 0.7299 0.057 Uiso 1 1 calc R . . C40 C 0.4364(8) 0.5728(14) 0.7135(8) 0.047(6) Uani 1 1 d . . . H40 H 0.4687 0.6059 0.7179 0.056 Uiso 1 1 calc R . . C41 C 0.4326(6) 0.4826(11) 0.6989(7) 0.026(4) Uani 1 1 d U . . H41 H 0.4625 0.4535 0.6954 0.031 Uiso 1 1 calc R . . C42 C 0.4222(8) 0.2992(15) 0.6453(8) 0.043(5) Uani 1 1 d . . . C43 C 0.4163(8) 0.3443(13) 0.5973(8) 0.044(5) Uani 1 1 d U . . H43 H 0.3866 0.3863 0.5793 0.053 Uiso 1 1 calc R . . C44 C 0.4539(7) 0.3259(13) 0.5785(8) 0.044(5) Uani 1 1 d . . . H44 H 0.4508 0.3583 0.5481 0.053 Uiso 1 1 calc R . . C45 C 0.4940(8) 0.2655(14) 0.6002(8) 0.046(5) Uani 1 1 d U . . H45 H 0.5182 0.2529 0.5847 0.056 Uiso 1 1 calc R . . C46 C 0.5015(8) 0.2182(14) 0.6476(8) 0.050(6) Uani 1 1 d . . . H46 H 0.5322 0.1775 0.6643 0.060 Uiso 1 1 calc R . . C47 C 0.4655(6) 0.2304(13) 0.6690(8) 0.040(5) Uani 1 1 d . . . H47 H 0.4686 0.1951 0.6985 0.048 Uiso 1 1 calc R . . C48 C 0.2238(9) 0.1205(13) 0.8754(7) 0.040(5) Uani 1 1 d . . . H48 H 0.2238 0.0585 0.8851 0.048 Uiso 1 1 calc R . . C49 C 0.2725(7) 0.2563(11) 0.8711(8) 0.043(5) Uani 1 1 d . . . C50 C 0.2502(8) 0.3173(10) 0.9032(7) 0.050(4) Uani 1 1 d . . . H50A H 0.2630 0.2920 0.9394 0.060 Uiso 1 1 calc R . . H50B H 0.2653 0.3800 0.9066 0.060 Uiso 1 1 calc R . . C51 C 0.1888(8) 0.3198(14) 0.8755(8) 0.060(6) Uani 1 1 d . . . H51A H 0.1751 0.3822 0.8628 0.072 Uiso 1 1 calc R . . H51B H 0.1728 0.2990 0.8991 0.072 Uiso 1 1 calc R . . C52 C 0.1732(8) 0.2527(11) 0.8278(7) 0.056(5) Uani 1 1 d . . . H52 H 0.1361 0.2667 0.7969 0.068 Uiso 1 1 calc R . . C53 C 0.2222(8) 0.2603(10) 0.8145(7) 0.053(5) Uani 1 1 d . . . C54 C 0.3305(8) 0.2815(13) 0.8807(10) 0.068(7) Uani 1 1 d . . . H54A H 0.3429 0.2397 0.8610 0.103 Uiso 1 1 calc R . . H54B H 0.3561 0.2772 0.9188 0.103 Uiso 1 1 calc R . . H54C H 0.3305 0.3441 0.8685 0.103 Uiso 1 1 calc R . . C55 C 0.2277(10) 0.1908(14) 0.7777(9) 0.071(7) Uani 1 1 d . . . H55A H 0.2227 0.1294 0.7886 0.107 Uiso 1 1 calc R . . H55B H 0.2650 0.1956 0.7795 0.107 Uiso 1 1 calc R . . H55C H 0.1991 0.2023 0.7412 0.107 Uiso 1 1 calc R . . C56 C 0.2217(9) 0.3591(13) 0.7938(10) 0.064(6) Uani 1 1 d . . . H56A H 0.2441 0.3609 0.7744 0.096 Uiso 1 1 calc R . . H56B H 0.2377 0.4012 0.8240 0.096 Uiso 1 1 calc R . . H56C H 0.1831 0.3772 0.7701 0.096 Uiso 1 1 calc R . . C57 C 0.3201(7) 0.0975(14) 0.9150(7) 0.039(5) Uani 1 1 d U . . H57A H 0.3538 0.1262 0.9156 0.046 Uiso 1 1 calc R . . H57B H 0.3117 0.0409 0.8936 0.046 Uiso 1 1 calc R . . C58 C 0.3301(8) 0.0751(12) 0.9741(8) 0.039(5) Uani 1 1 d . . . C59 C 0.3408(8) -0.0164(14) 0.9910(8) 0.040(5) Uani 1 1 d U . . C60 C 0.3565(10) -0.0414(14) 1.0421(8) 0.062(7) Uani 1 1 d . . . H60 H 0.3615 -0.1036 1.0528 0.074 Uiso 1 1 calc R . . C61 C 0.3655(9) 0.0344(17) 1.0808(9) 0.075(7) Uani 1 1 d . . . H61 H 0.3768 0.0213 1.1172 0.090 Uiso 1 1 calc R . . C62 C 0.3571(10) 0.1236(18) 1.0628(11) 0.080(7) Uani 1 1 d U . . H62 H 0.3614 0.1730 1.0861 0.095 Uiso 1 1 calc R . . C63 C 0.3428(10) 0.1379(16) 1.0114(9) 0.067(7) Uani 1 1 d . . . H63 H 0.3417 0.1996 1.0006 0.080 Uiso 1 1 calc R . . C64 C 0.3422(7) -0.2210(11) 0.9829(8) 0.035(5) Uani 1 1 d . . . C65 C 0.3984(8) -0.2398(14) 1.0175(8) 0.048(5) Uani 1 1 d U . . H65 H 0.4270 -0.1981 1.0208 0.058 Uiso 1 1 calc R . . C66 C 0.4114(10) -0.3165(16) 1.0455(10) 0.065(7) Uani 1 1 d . . . H66 H 0.4495 -0.3262 1.0704 0.078 Uiso 1 1 calc R . . C67 C 0.3725(10) -0.3832(16) 1.0405(9) 0.059(7) Uani 1 1 d . . . H67 H 0.3832 -0.4403 1.0583 0.070 Uiso 1 1 calc R . . C68 C 0.3169(11) -0.3605(15) 1.0077(11) 0.076(8) Uani 1 1 d . . . H68 H 0.2888 -0.4025 1.0052 0.091 Uiso 1 1 calc R . . C69 C 0.3003(8) -0.2829(13) 0.9793(9) 0.046(6) Uani 1 1 d . . . H69 H 0.2617 -0.2703 0.9575 0.055 Uiso 1 1 calc R . . C70 C 0.3713(8) -0.1173(15) 0.9163(9) 0.052(6) Uani 1 1 d . . . C71 C 0.3601(9) -0.1784(16) 0.8732(10) 0.065(7) Uani 1 1 d . . . H71 H 0.3268 -0.2138 0.8576 0.079 Uiso 1 1 calc R . . C72 C 0.4024(8) -0.1835(18) 0.8548(9) 0.064(6) Uani 1 1 d . . . H72 H 0.3974 -0.2253 0.8273 0.077 Uiso 1 1 calc R . . C73 C 0.4489(8) -0.1306(15) 0.8757(9) 0.057(6) Uani 1 1 d . . . H73 H 0.4751 -0.1340 0.8617 0.068 Uiso 1 1 calc R . . C74 C 0.4587(8) -0.0709(15) 0.9176(10) 0.057(6) Uani 1 1 d . . . H74 H 0.4922 -0.0360 0.9335 0.069 Uiso 1 1 calc R . . C75 C 0.4190(8) -0.0637(14) 0.9355(8) 0.047(5) Uani 1 1 d U . . H75 H 0.4245 -0.0199 0.9622 0.057 Uiso 1 1 calc R . . C76 C 0.1245(8) 0.1098(14) 0.8267(8) 0.057(6) Uani 1 1 d . . . H76A H 0.0963 0.1564 0.8234 0.069 Uiso 1 1 calc R . . H76B H 0.1263 0.0659 0.8541 0.069 Uiso 1 1 calc R . . C77 C 0.1011(7) 0.0591(12) 0.7751(7) 0.023(4) Uani 1 1 d U . . C78 C 0.1035(7) -0.0364(14) 0.7744(7) 0.034(5) Uani 1 1 d . . . C79 C 0.0841(7) -0.0809(14) 0.7230(8) 0.045(6) Uani 1 1 d . . . H79 H 0.0837 -0.1456 0.7207 0.054 Uiso 1 1 calc R . . C80 C 0.0662(8) -0.0279(15) 0.6769(9) 0.051(6) Uani 1 1 d . . . H80 H 0.0546 -0.0566 0.6434 0.062 Uiso 1 1 calc R . . C81 C 0.0652(8) 0.0699(17) 0.6802(10) 0.059(6) Uani 1 1 d . . . H81 H 0.0526 0.1073 0.6494 0.071 Uiso 1 1 calc R . . C82 C 0.0832(9) 0.1061(15) 0.7292(9) 0.052(6) Uani 1 1 d . . . H82 H 0.0831 0.1708 0.7315 0.062 Uiso 1 1 calc R . . C83 C 0.0775(7) -0.0902(12) 0.8580(7) 0.029(4) Uani 1 1 d U . . C84 C 0.0314(9) -0.0340(12) 0.8330(8) 0.049(6) Uani 1 1 d . . . H84 H 0.0243 -0.0109 0.7990 0.059 Uiso 1 1 calc R . . C85 C -0.0051(8) -0.0082(17) 0.8525(8) 0.053(6) Uani 1 1 d . . . H85 H -0.0337 0.0358 0.8350 0.063 Uiso 1 1 calc R . . C86 C 0.0017(9) -0.0485(18) 0.8973(12) 0.072(8) Uani 1 1 d . . . H86 H -0.0232 -0.0340 0.9117 0.086 Uiso 1 1 calc R . . C87 C 0.0451(11) -0.112(2) 0.9241(10) 0.076(10) Uani 1 1 d . . . H87 H 0.0489 -0.1404 0.9558 0.115 Uiso 1 1 calc R . . C88 C 0.0836(9) -0.1341(13) 0.9031(8) 0.048(6) Uani 1 1 d . . . H88 H 0.1125 -0.1779 0.9200 0.058 Uiso 1 1 calc R . . C89 C 0.1162(7) -0.2316(11) 0.8072(7) 0.027(4) Uani 1 1 d U . . C90 C 0.1561(8) -0.2739(14) 0.7967(8) 0.042(5) Uani 1 1 d . . . H90 H 0.1881 -0.2415 0.7996 0.051 Uiso 1 1 calc R . . C91 C 0.1484(9) -0.3653(16) 0.7815(9) 0.059(6) Uani 1 1 d U . . H91 H 0.1764 -0.3943 0.7751 0.071 Uiso 1 1 calc R . . C92 C 0.1037(8) -0.4150(16) 0.7755(8) 0.049(6) Uani 1 1 d U . . H92 H 0.0986 -0.4758 0.7625 0.059 Uiso 1 1 calc R . . C93 C 0.0624(8) -0.3708(15) 0.7901(7) 0.044(5) Uani 1 1 d . . . H93 H 0.0310 -0.4027 0.7890 0.053 Uiso 1 1 calc R . . C94 C 0.0729(8) -0.2793(15) 0.8055(8) 0.053(6) Uani 1 1 d . . . H94 H 0.0476 -0.2491 0.8153 0.063 Uiso 1 1 calc R . . N1 N 0.2239(6) 0.0458(9) 0.6094(6) 0.036(4) Uani 1 1 d . . . N2 N 0.3207(6) 0.0502(10) 0.6626(5) 0.033(4) Uani 1 1 d . . . N3 N 0.2729(6) 0.1595(10) 0.8927(6) 0.031(4) Uani 1 1 d . . . N4 N 0.1775(8) 0.1549(10) 0.8478(7) 0.042(4) Uani 1 1 d . . . P1 P 0.17983(19) 0.3205(3) 0.5529(2) 0.0301(12) Uani 1 1 d . . . P2 P 0.37100(19) 0.3146(4) 0.6697(2) 0.0328(13) Uani 1 1 d . . . P3 P 0.3225(2) -0.1138(4) 0.9441(2) 0.0347(12) Uani 1 1 d . . . P4 P 0.1283(2) -0.1140(4) 0.83227(19) 0.0337(13) Uani 1 1 d . . . Cl1 Cl 0.28660(18) 0.3105(4) 0.53499(18) 0.0387(12) Uani 1 1 d . . . Cl2 Cl 0.25951(18) 0.2791(4) 0.6832(2) 0.0438(14) Uani 1 1 d . . . Cl3 Cl 0.2382(2) -0.0844(4) 0.81486(19) 0.0478(14) Uani 1 1 d . . . Cl4 Cl 0.21558(19) -0.1025(4) 0.96496(19) 0.0468(13) Uani 1 1 d . . . Pd1 Pd 0.27453(6) 0.30815(7) 0.61046(6) 0.0311(4) Uani 1 1 d . . . Pd2 Pd 0.22531(6) -0.10689(7) 0.88847(6) 0.0340(4) Uani 1 1 d . . . P5 P -0.0039(3) 0.3517(5) 0.7464(3) 0.0480(10) Uani 1 1 d . . . F1 F 0.0230(6) 0.4097(11) 0.7978(6) 0.103(6) Uani 1 1 d . . . F2 F 0.0558(5) 0.3572(9) 0.7445(5) 0.070(4) Uani 1 1 d . . . F3 F -0.0273(5) 0.2890(9) 0.6944(5) 0.071(4) Uani 1 1 d . . . F4 F -0.0628(5) 0.3533(8) 0.7464(6) 0.076(4) Uani 1 1 d . . . F5 F 0.0122(5) 0.2621(8) 0.7795(6) 0.074(4) Uani 1 1 d . . . F6 F -0.0217(5) 0.4421(9) 0.7095(6) 0.077(4) Uani 1 1 d . . . P6 P 0.0000 0.0100(5) 0.5000 0.051(2) Uani 1 2 d SD . . F7 F -0.0539(3) 0.0104(6) 0.5092(4) 0.063(3) Uani 1 1 d DU A . F8 F 0.0000 -0.0960(6) 0.5000 0.094(8) Uani 0.64(2) 2 d SPDU A . F9 F 0.0362(4) 0.0101(8) 0.5620(3) 0.090(7) Uani 0.64(2) 1 d PDU . . F10 F 0.0000 0.1162(7) 0.5000 0.098(9) Uani 0.64(2) 2 d SPDU A . F8A F -0.0277(6) -0.0649(10) 0.4570(2) 0.073(8) Uani 0.36(2) 1 d PDU A 2 F9A F -0.0269(9) 0.0863(11) 0.4575(8) 0.126(11) Uani 0.36(2) 1 d PDU A 2 P7 P 0.5000 0.1977(5) 1.0000 0.045(2) Uani 1 2 d SD . 2 F11 F 0.5000 0.3036(7) 1.0000 0.095(11) Uani 0.389(17) 2 d SPDU B 2 F12 F 0.5000 0.0903(7) 1.0000 0.059(9) Uani 0.389(17) 2 d SPDU B 2 F13 F 0.5408(5) 0.1963(7) 0.9744(5) 0.124(5) Uani 1 1 d DU C 2 F14 F 0.5506(6) 0.1968(9) 1.0565(3) 0.119(8) Uani 0.389(17) 1 d PDU B 2 F11A F 0.5374(4) 0.2802(7) 1.0376(3) 0.086(6) Uani 0.611(17) 1 d PDU B 2 F14A F 0.5428(6) 0.1324(9) 1.0457(5) 0.096(6) Uani 0.611(17) 1 d PDU B 2 C95 C 0.1084(5) 0.6113(8) 0.5723(4) 0.085(6) Uani 1 1 d DU D 2 H95 H 0.1330 0.5723 0.5626 0.102 Uiso 1 1 calc R D 2 Cl5 Cl 0.1413(3) 0.6377(5) 0.6411(3) 0.116(3) Uani 1 1 d D D 2 Cl6 Cl 0.0944(4) 0.7171(4) 0.5390(3) 0.128(3) Uani 1 1 d D D 2 Cl7 Cl 0.0414(4) 0.5603(7) 0.5520(5) 0.262(7) Uani 1 1 d D D 2 C96 C 0.3491(5) 0.5830(10) 0.9005(5) 0.085(6) Uani 1 1 d DU E 2 H96 H 0.3646 0.6438 0.9166 0.102 Uiso 1 1 calc R E 2 Cl8 Cl 0.3612(4) 0.5649(8) 0.8448(4) 0.174(4) Uani 1 1 d D E 2 Cl9 Cl 0.2759(3) 0.5827(5) 0.8778(3) 0.151(3) Uani 1 1 d D E 2 Cl10 Cl 0.3848(4) 0.4969(8) 0.9465(4) 0.187(5) Uani 1 1 d D E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(7) 0.035(8) 0.032(8) -0.007(7) 0.017(6) 0.010(6) C2 0.041(9) 0.035(9) 0.062(13) 0.006(9) 0.028(9) 0.007(8) C3 0.035(8) 0.044(9) 0.049(11) 0.009(8) 0.024(8) 0.006(7) C4 0.036(8) 0.034(9) 0.045(12) 0.011(8) 0.027(8) 0.022(7) C5 0.034(8) 0.040(9) 0.050(11) 0.011(8) 0.023(8) -0.005(7) C6 0.046(9) 0.030(9) 0.037(10) 0.015(7) 0.014(8) 0.004(7) C7 0.068(14) 0.045(13) 0.069(15) -0.008(10) 0.016(12) -0.021(10) C8 0.053(12) 0.056(12) 0.093(17) -0.020(11) 0.014(13) 0.028(11) C9 0.057(12) 0.058(14) 0.083(16) 0.031(12) 0.024(12) 0.003(10) C10 0.030(8) 0.020(8) 0.035(10) -0.006(7) 0.021(8) -0.004(6) C11 0.014(8) 0.041(12) 0.033(12) -0.015(9) 0.000(8) -0.002(8) C12 0.049(10) 0.026(9) 0.031(11) 0.006(8) 0.020(9) -0.008(8) C13 0.040(10) 0.036(11) 0.043(13) 0.006(10) 0.013(10) 0.007(8) C14 0.129(19) 0.047(13) 0.047(14) -0.023(11) 0.057(14) -0.053(13) C15 0.084(13) 0.034(10) 0.015(8) -0.006(7) 0.005(8) -0.019(9) C16 0.027(9) 0.022(10) 0.045(14) -0.001(9) -0.009(9) 0.002(7) C17 0.039(10) 0.050(13) 0.016(10) 0.011(9) 0.015(9) 0.005(10) C18 0.029(9) 0.061(12) 0.070(15) 0.015(11) 0.028(10) 0.006(9) C19 0.053(13) 0.079(17) 0.075(18) 0.019(14) 0.052(14) 0.005(12) C20 0.079(17) 0.14(2) 0.047(15) 0.021(15) 0.051(14) 0.033(17) C21 0.073(14) 0.068(14) 0.061(15) 0.006(12) 0.043(13) 0.004(12) C22 0.041(10) 0.042(11) 0.027(10) -0.011(9) 0.000(8) -0.001(9) C23 0.045(12) 0.068(14) 0.018(11) -0.009(10) 0.013(10) -0.001(10) C24 0.067(14) 0.048(12) 0.063(15) 0.007(10) 0.035(12) -0.009(10) C25 0.057(14) 0.069(16) 0.054(16) 0.023(13) 0.006(12) 0.036(13) C26 0.080(16) 0.044(13) 0.052(15) 0.007(11) 0.034(13) -0.010(12) C27 0.037(7) 0.025(7) 0.030(8) 0.016(6) 0.014(6) -0.002(6) C28 0.046(11) 0.035(11) 0.032(12) 0.013(9) 0.018(10) 0.008(9) C29 0.041(11) 0.034(11) 0.065(15) -0.030(10) 0.038(11) -0.005(9) C30 0.047(11) 0.030(10) 0.084(16) 0.006(10) 0.042(11) 0.004(8) C31 0.043(10) 0.017(8) 0.054(14) 0.003(8) 0.044(11) 0.005(7) C32 0.046(11) 0.039(12) 0.023(11) 0.020(9) 0.010(9) 0.012(9) C33 0.039(11) 0.058(14) 0.027(13) -0.007(11) 0.002(10) 0.003(10) C34 0.054(9) 0.032(8) 0.031(9) 0.007(6) 0.016(7) -0.001(6) C35 0.043(8) 0.043(9) 0.035(9) 0.005(7) 0.013(7) 0.003(7) C36 0.045(11) 0.059(13) 0.050(14) -0.023(11) 0.021(11) -0.001(10) C37 0.066(14) 0.036(12) 0.09(2) -0.003(13) 0.050(15) 0.000(11) C38 0.073(14) 0.032(10) 0.096(18) -0.012(10) 0.056(13) 0.013(10) C39 0.056(12) 0.028(10) 0.042(12) -0.018(9) 0.008(10) -0.015(9) C40 0.048(12) 0.033(12) 0.062(16) 0.003(11) 0.028(12) -0.014(10) C41 0.018(7) 0.024(8) 0.032(8) 0.005(6) 0.008(6) -0.012(6) C42 0.054(11) 0.051(11) 0.028(10) 0.005(9) 0.023(9) 0.003(10) C43 0.046(8) 0.036(8) 0.042(9) -0.007(7) 0.014(7) -0.008(7) C44 0.044(10) 0.051(12) 0.052(13) 0.019(10) 0.034(10) 0.013(9) C45 0.045(8) 0.053(9) 0.046(9) -0.001(7) 0.026(7) -0.001(7) C46 0.053(12) 0.034(11) 0.062(16) 0.009(11) 0.024(12) 0.012(9) C47 0.019(8) 0.054(13) 0.059(14) -0.004(11) 0.027(10) -0.006(8) C48 0.076(15) 0.018(9) 0.020(10) 0.010(8) 0.018(11) -0.005(9) C49 0.040(10) 0.028(9) 0.062(13) 0.005(9) 0.023(10) -0.009(8) C50 0.090(13) 0.018(8) 0.054(11) 0.007(7) 0.043(11) 0.002(9) C51 0.075(14) 0.052(11) 0.073(14) 0.009(10) 0.051(12) 0.028(10) C52 0.071(12) 0.050(11) 0.055(13) 0.005(9) 0.035(10) 0.006(9) C53 0.081(13) 0.027(9) 0.053(13) -0.002(8) 0.033(11) 0.010(9) C54 0.055(12) 0.031(12) 0.14(2) 0.030(12) 0.058(14) 0.008(9) C55 0.14(2) 0.046(12) 0.048(14) -0.002(11) 0.060(15) -0.019(13) C56 0.062(12) 0.036(11) 0.091(17) 0.028(11) 0.032(12) 0.006(9) C57 0.044(8) 0.039(8) 0.023(8) -0.003(6) 0.006(6) -0.013(7) C58 0.054(12) 0.017(9) 0.048(14) 0.000(9) 0.024(11) -0.012(8) C59 0.047(8) 0.036(8) 0.034(9) -0.004(7) 0.015(7) -0.011(7) C60 0.125(19) 0.038(12) 0.028(12) -0.012(9) 0.040(13) -0.032(12) C61 0.091(16) 0.063(16) 0.031(13) 0.014(12) -0.008(11) 0.004(12) C62 0.091(11) 0.060(10) 0.078(11) -0.010(8) 0.030(8) -0.013(8) C63 0.112(19) 0.053(14) 0.033(14) 0.003(12) 0.031(14) -0.034(13) C64 0.039(10) 0.016(9) 0.045(13) 0.015(8) 0.015(10) 0.005(7) C65 0.040(8) 0.041(8) 0.043(9) 0.005(7) 0.002(7) 0.002(7) C66 0.064(14) 0.060(15) 0.069(17) 0.007(13) 0.029(13) -0.011(12) C67 0.087(16) 0.056(14) 0.056(15) 0.025(12) 0.053(14) 0.039(13) C68 0.101(19) 0.040(13) 0.13(2) 0.001(14) 0.084(18) -0.003(12) C69 0.058(13) 0.018(10) 0.073(16) 0.001(10) 0.039(12) 0.000(9) C70 0.041(12) 0.033(12) 0.083(18) 0.034(13) 0.030(13) 0.017(11) C71 0.071(14) 0.057(14) 0.11(2) 0.014(14) 0.081(15) 0.016(12) C72 0.051(12) 0.088(17) 0.063(15) -0.004(13) 0.034(12) 0.003(12) C73 0.036(11) 0.058(13) 0.091(18) 0.031(13) 0.042(12) 0.008(9) C74 0.034(11) 0.047(13) 0.074(18) 0.008(13) 0.009(12) -0.001(10) C75 0.057(9) 0.035(8) 0.042(9) 0.013(7) 0.016(7) 0.000(7) C76 0.058(14) 0.037(12) 0.051(15) 0.031(11) 0.002(12) 0.007(10) C77 0.021(7) 0.025(7) 0.015(7) -0.006(6) 0.002(6) 0.000(6) C78 0.020(9) 0.058(13) 0.011(9) -0.005(9) -0.006(7) -0.003(8) C79 0.029(10) 0.057(13) 0.059(15) -0.030(12) 0.029(11) -0.032(9) C80 0.065(14) 0.060(15) 0.041(14) -0.004(12) 0.035(12) -0.029(11) C81 0.037(10) 0.076(16) 0.054(15) 0.014(12) 0.012(10) -0.018(10) C82 0.066(13) 0.032(10) 0.058(15) 0.009(10) 0.029(12) 0.014(9) C83 0.029(7) 0.024(8) 0.030(8) -0.007(6) 0.011(6) -0.007(6) C84 0.085(15) 0.023(10) 0.039(13) 0.008(9) 0.026(12) -0.011(10) C85 0.038(11) 0.090(17) 0.047(15) -0.008(13) 0.034(11) -0.013(11) C86 0.049(13) 0.072(16) 0.091(2) -0.017(14) 0.043(15) -0.010(11) C87 0.100(2) 0.100(2) 0.065(18) -0.028(18) 0.070(18) -0.019(2) C88 0.084(14) 0.026(10) 0.039(12) 0.004(8) 0.033(11) -0.008(9) C89 0.034(8) 0.025(7) 0.021(8) 0.007(6) 0.012(6) -0.015(6) C90 0.051(12) 0.042(12) 0.044(13) -0.004(10) 0.031(11) -0.014(10) C91 0.059(9) 0.066(11) 0.057(10) 0.007(8) 0.031(8) -0.011(8) C92 0.048(9) 0.053(9) 0.038(9) 0.004(8) 0.012(7) 0.000(8) C93 0.043(12) 0.050(14) 0.023(11) -0.004(10) 0.002(10) 0.004(10) C94 0.054(12) 0.058(13) 0.029(11) -0.008(10) 0.003(10) 0.026(10) N1 0.047(9) 0.013(7) 0.052(11) 0.014(7) 0.026(9) -0.002(7) N2 0.034(8) 0.037(8) 0.016(8) 0.012(6) -0.001(6) -0.001(6) N3 0.032(8) 0.039(10) 0.023(9) -0.013(7) 0.013(7) -0.005(8) N4 0.075(12) 0.017(8) 0.051(11) -0.008(7) 0.044(10) -0.016(8) P1 0.036(3) 0.028(3) 0.028(3) 0.000(2) 0.015(2) 0.000(2) P2 0.036(3) 0.029(3) 0.039(3) -0.002(3) 0.022(3) -0.006(2) P3 0.044(3) 0.029(3) 0.030(3) 0.003(3) 0.016(3) -0.010(2) P4 0.043(3) 0.033(3) 0.021(3) 0.001(3) 0.011(3) 0.001(3) Cl1 0.044(3) 0.046(3) 0.033(3) 0.002(3) 0.023(2) 0.004(2) Cl2 0.035(3) 0.058(3) 0.042(3) 0.008(3) 0.022(3) 0.000(2) Cl3 0.053(3) 0.064(4) 0.025(3) 0.009(3) 0.016(3) -0.009(3) Cl4 0.055(3) 0.054(3) 0.028(3) -0.001(3) 0.017(3) 0.008(3) Pd1 0.0360(8) 0.0304(9) 0.0285(10) -0.0016(8) 0.0159(8) -0.0049(7) Pd2 0.0432(9) 0.0288(9) 0.0296(10) 0.0039(8) 0.0163(8) -0.0019(7) P5 0.050(2) 0.0303(16) 0.071(3) -0.0069(18) 0.034(2) 0.0005(16) F1 0.121(11) 0.098(12) 0.119(13) -0.064(10) 0.080(10) -0.063(10) F2 0.061(7) 0.085(9) 0.075(9) -0.001(7) 0.041(7) 0.012(6) F3 0.098(9) 0.062(8) 0.053(8) -0.016(6) 0.034(7) -0.020(7) F4 0.062(7) 0.044(7) 0.140(13) -0.005(7) 0.061(8) -0.006(6) F5 0.072(8) 0.043(7) 0.088(10) 0.008(6) 0.018(7) 0.005(6) F6 0.084(8) 0.051(7) 0.110(11) 0.028(7) 0.057(8) 0.017(6) P6 0.076(6) 0.039(5) 0.038(6) 0.000 0.025(5) 0.000 F7 0.067(5) 0.074(6) 0.064(6) 0.006(5) 0.045(5) 0.021(5) F8 0.109(11) 0.085(11) 0.110(11) 0.000 0.071(8) 0.000 F9 0.080(9) 0.127(11) 0.065(9) 0.018(7) 0.034(7) 0.047(7) F10 0.098(12) 0.074(12) 0.117(13) 0.000 0.043(9) 0.000 F8A 0.046(10) 0.084(11) 0.080(12) -0.045(8) 0.021(8) 0.001(8) F9A 0.129(14) 0.123(14) 0.128(14) 0.021(9) 0.060(9) 0.013(9) P7 0.046(4) 0.040(5) 0.053(6) 0.000 0.025(4) 0.000 F11 0.104(13) 0.093(13) 0.107(13) 0.000 0.066(9) 0.000 F12 0.059(11) 0.035(11) 0.083(12) 0.000 0.032(8) 0.000 F13 0.156(9) 0.118(9) 0.144(9) 0.000(7) 0.110(8) 0.003(7) F14 0.113(10) 0.122(11) 0.107(10) -0.004(8) 0.037(8) -0.017(8) F11A 0.081(8) 0.097(9) 0.081(9) -0.028(7) 0.037(7) -0.019(7) F14A 0.096(8) 0.078(9) 0.110(9) 0.042(7) 0.043(7) 0.031(7) C95 0.095(10) 0.071(9) 0.092(10) 0.011(8) 0.045(8) -0.001(8) Cl5 0.160(7) 0.094(5) 0.114(6) -0.005(4) 0.081(6) -0.019(5) Cl6 0.207(8) 0.052(3) 0.171(8) 0.007(4) 0.126(7) 0.002(4) Cl7 0.208(12) 0.300(16) 0.286(16) -0.088(13) 0.121(11) 0.024(11) C96 0.094(10) 0.070(9) 0.090(10) 0.001(8) 0.041(8) 0.011(8) Cl8 0.182(9) 0.199(10) 0.153(9) 0.015(8) 0.087(8) 0.054(8) Cl9 0.141(6) 0.135(6) 0.173(8) -0.059(6) 0.068(6) -0.015(5) Cl10 0.260(12) 0.176(10) 0.154(9) -0.013(8) 0.118(9) 0.034(9) _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 1.34(2) . ? C1 N2 1.38(2) . ? C1 H1 0.9500 . ? C2 N1 1.48(2) . ? C2 C7 1.51(2) . ? C2 C3 1.51(2) . ? C2 C6 1.55(2) . ? C3 C4 1.57(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.54(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N2 1.441(19) . ? C5 C6 1.53(2) . ? C5 H5 1.0000 . ? C6 C9 1.58(2) . ? C6 C8 1.59(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.45(2) . ? C10 N1 1.52(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.43(2) . ? C11 C12 1.43(3) . ? C12 C13 1.46(3) . ? C12 P1 1.804(19) . ? C13 C14 1.27(3) . ? C13 H13 0.9500 . ? C14 C15 1.39(3) . ? C14 H14 0.9500 . ? C15 C16 1.38(2) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.36(2) . ? C17 C18 1.42(2) . ? C17 P1 1.850(16) . ? C18 C19 1.44(2) . ? C18 H18 0.9500 . ? C19 C20 1.36(3) . ? C19 H19 0.9500 . ? C20 C21 1.37(3) . ? C20 H20 0.9500 . ? C21 C22 1.33(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.37(3) . ? C23 C24 1.43(3) . ? C23 P1 1.81(2) . ? C24 C25 1.42(3) . ? C24 H24 0.9500 . ? C25 C26 1.38(3) . ? C25 H25 0.9500 . ? C26 C27 1.35(3) . ? C26 H26 0.9500 . ? C27 C28 1.40(2) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 N2 1.52(2) . ? C29 C30 1.57(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.40(2) . ? C30 C35 1.43(3) . ? C31 C32 1.36(2) . ? C31 P2 1.826(19) . ? C32 C33 1.37(2) . ? C32 H32 0.9500 . ? C33 C34 1.36(3) . ? C33 H33 0.9500 . ? C34 C35 1.41(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.42(3) . ? C36 C41 1.43(2) . ? C36 P2 1.81(2) . ? C37 C38 1.36(3) . ? C37 H37 0.9500 . ? C38 C39 1.35(3) . ? C38 H38 0.9500 . ? C39 C40 1.32(3) . ? C39 H39 0.9500 . ? C40 C41 1.38(3) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C47 1.45(3) . ? C42 C43 1.45(3) . ? C42 P2 1.807(17) . ? C43 C44 1.36(2) . ? C43 H43 0.9500 . ? C44 C45 1.31(2) . ? C44 H44 0.9500 . ? C45 C46 1.44(3) . ? C45 H45 0.9500 . ? C46 C47 1.36(2) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 N4 1.23(2) . ? C48 N3 1.31(2) . ? C48 H48 0.9500 . ? C49 C54 1.50(2) . ? C49 C53 1.55(3) . ? C49 N3 1.54(2) . ? C49 C50 1.57(2) . ? C50 C51 1.47(2) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.57(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.52(2) . ? C52 N4 1.53(2) . ? C52 H52 1.0000 . ? C53 C55 1.51(2) . ? C53 C56 1.56(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N3 1.45(2) . ? C57 C58 1.60(3) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C63 1.32(3) . ? C58 C59 1.41(3) . ? C59 C60 1.36(3) . ? C59 P3 1.85(2) . ? C60 C61 1.50(3) . ? C60 H60 0.9500 . ? C61 C62 1.38(3) . ? C61 H61 0.9500 . ? C62 C63 1.34(3) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C65 1.40(2) . ? C64 C69 1.41(2) . ? C64 P3 1.849(17) . ? C65 C66 1.33(3) . ? C65 H65 0.9500 . ? C66 C67 1.39(3) . ? C66 H66 0.9500 . ? C67 C68 1.39(3) . ? C67 H67 0.9500 . ? C68 C69 1.35(3) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C75 1.38(3) . ? C70 C71 1.43(3) . ? C70 P3 1.806(19) . ? C71 C72 1.45(2) . ? C71 H71 0.9500 . ? C72 C73 1.35(3) . ? C72 H72 0.9500 . ? C73 C74 1.40(3) . ? C73 H73 0.9500 . ? C74 C75 1.37(3) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 N4 1.43(2) . ? C76 C77 1.49(3) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C82 1.35(3) . ? C77 C78 1.40(2) . ? C78 C79 1.46(2) . ? C78 P4 1.849(19) . ? C79 C80 1.40(3) . ? C79 H79 0.9500 . ? C80 C81 1.44(3) . ? C80 H80 0.9500 . ? C81 C82 1.35(3) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C88 1.37(2) . ? C83 C84 1.38(2) . ? C83 P4 1.845(16) . ? C84 C85 1.38(2) . ? C84 H84 0.9500 . ? C85 C86 1.33(3) . ? C85 H85 0.9500 . ? C86 C87 1.41(4) . ? C86 H86 0.9500 . ? C87 C88 1.44(3) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C94 1.33(3) . ? C89 C90 1.38(2) . ? C89 P4 1.835(18) . ? C90 C91 1.39(3) . ? C90 H90 0.9500 . ? C91 C92 1.34(3) . ? C91 H91 0.9500 . ? C92 C93 1.49(3) . ? C92 H92 0.9500 . ? C93 C94 1.40(3) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? P1 Pd1 2.315(5) . ? P2 Pd1 2.356(5) . ? P3 Pd2 2.352(5) . ? P4 Pd2 2.351(5) . ? Cl1 Pd1 2.297(4) . ? Cl2 Pd1 2.306(5) . ? Cl3 Pd2 2.280(5) . ? Cl4 Pd2 2.292(5) . ? P5 F1 1.550(15) . ? P5 F5 1.556(14) . ? P5 F4 1.577(12) . ? P5 F3 1.599(14) . ? P5 F6 1.618(14) . ? P5 F2 1.623(12) . ? P6 F8A 1.554(9) . ? P6 F8A 1.554(9) 2_556 ? P6 F8 1.554(8) . ? P6 F10 1.556(9) . ? P6 F9A 1.558(10) 2_556 ? P6 F9 1.569(7) 2_556 ? P6 F7 1.578(6) . ? P6 F7 1.578(6) 2_556 ? P7 F11 1.552(9) . ? P7 F14 1.554(8) 2_657 ? P7 F14 1.554(8) . ? P7 F13 1.560(6) 2_657 ? P7 F13 1.560(6) . ? P7 F12 1.575(9) . ? P7 F14A 1.597(9) 2_657 ? P7 F14A 1.597(9) . ? P7 F11A 1.621(8) . ? P7 F11A 1.621(8) 2_657 ? C95 Cl6 1.764(9) . ? C95 Cl5 1.772(9) . ? C95 Cl7 1.780(9) . ? C95 H95 1.0000 . ? C96 Cl10 1.751(9) . ? C96 Cl8 1.763(9) . ? C96 Cl9 1.763(9) . ? C96 H96 1.0000 . ? 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 N2 118.3(17) . . ? N1 C1 H1 120.9 . . ? N2 C1 H1 120.9 . . ? N1 C2 C7 112.8(17) . . ? N1 C2 C3 106.3(13) . . ? C7 C2 C3 113.9(14) . . ? N1 C2 C6 107.6(12) . . ? C7 C2 C6 114.2(15) . . ? C3 C2 C6 101.1(14) . . ? C2 C3 C4 105.2(11) . . ? C2 C3 H3A 110.7 . . ? C4 C3 H3A 110.7 . . ? C2 C3 H3B 110.7 . . ? C4 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C5 C4 C3 105.5(13) . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? C5 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.8 . . ? N2 C5 C6 108.8(13) . . ? N2 C5 C4 109.1(13) . . ? C6 C5 C4 101.2(12) . . ? N2 C5 H5 112.3 . . ? C6 C5 H5 112.4 . . ? C4 C5 H5 112.4 . . ? C5 C6 C2 100.9(13) . . ? C5 C6 C9 108.3(14) . . ? C2 C6 C9 114.3(13) . . ? C5 C6 C8 111.6(12) . . ? C2 C6 C8 111.9(13) . . ? C9 C6 C8 109.5(15) . . ? C2 C7 H7A 109.4 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.4 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N1 119.9(13) . . ? C11 C10 H10A 107.3 . . ? N1 C10 H10A 107.4 . . ? C11 C10 H10B 107.4 . . ? N1 C10 H10B 107.3 . . ? H10A C10 H10B 106.9 . . ? C16 C11 C12 117.8(17) . . ? C16 C11 C10 116.3(17) . . ? C12 C11 C10 125.8(17) . . ? C11 C12 C13 116.6(17) . . ? C11 C12 P1 121.0(15) . . ? C13 C12 P1 121.6(14) . . ? C14 C13 C12 122.1(19) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 123(2) . . ? C13 C14 H14 118.4 . . ? C15 C14 H14 118.3 . . ? C16 C15 C14 118.7(18) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.7 . . ? C15 C16 C11 121.0(17) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.4 . . ? C22 C17 C18 122.0(16) . . ? C22 C17 P1 117.4(14) . . ? C18 C17 P1 120.3(14) . . ? C17 C18 C19 114(2) . . ? C17 C18 H18 123.0 . . ? C19 C18 H18 123.1 . . ? C20 C19 C18 120(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 123.5(19) . . ? C19 C20 H20 118.3 . . ? C21 C20 H20 118.3 . . ? C22 C21 C20 117(2) . . ? C22 C21 H21 121.6 . . ? C20 C21 H21 121.6 . . ? C21 C22 C17 123(2) . . ? C21 C22 H22 118.4 . . ? C17 C22 H22 118.5 . . ? C28 C23 C24 117.4(19) . . ? C28 C23 P1 123.1(15) . . ? C24 C23 P1 119.0(16) . . ? C25 C24 C23 121(2) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 118(2) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C27 C26 C25 122(2) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 120.1(18) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 120.0 . . ? C23 C28 C27 121.7(18) . . ? C23 C28 H28 119.2 . . ? C27 C28 H28 119.1 . . ? N2 C29 C30 105.4(12) . . ? N2 C29 H29A 110.7 . . ? C30 C29 H29A 110.6 . . ? N2 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C31 C30 C35 117(2) . . ? C31 C30 C29 126(2) . . ? C35 C30 C29 115.9(17) . . ? C32 C31 C30 121.1(19) . . ? C32 C31 P2 121.6(13) . . ? C30 C31 P2 117.3(17) . . ? C33 C32 C31 122.1(19) . . ? C33 C32 H32 118.9 . . ? C31 C32 H32 119.0 . . ? C34 C33 C32 118(2) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C33 C34 C35 122(2) . . ? C33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C30 C35 C34 118.2(19) . . ? C30 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C37 C36 C41 114.2(19) . . ? C37 C36 P2 121.8(16) . . ? C41 C36 P2 123.7(14) . . ? C38 C37 C36 124(2) . . ? C38 C37 H37 117.9 . . ? C36 C37 H37 117.8 . . ? C39 C38 C37 118.2(18) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C40 C39 C38 120.5(18) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 124.2(18) . . ? C39 C40 H40 117.9 . . ? C41 C40 H40 117.9 . . ? C40 C41 C36 118.2(17) . . ? C40 C41 H41 120.9 . . ? C36 C41 H41 120.9 . . ? C47 C42 C43 118.3(16) . . ? C47 C42 P2 119.7(13) . . ? C43 C42 P2 121.3(15) . . ? C44 C43 C42 119.2(18) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C45 C44 C43 123.0(19) . . ? C45 C44 H44 118.5 . . ? C43 C44 H44 118.5 . . ? C44 C45 C46 120.1(17) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 121.5(18) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C42 117.6(18) . . ? C46 C47 H47 121.2 . . ? C42 C47 H47 121.2 . . ? N4 C48 N3 127.6(18) . . ? N4 C48 H48 116.2 . . ? N3 C48 H48 116.3 . . ? C54 C49 C53 121.4(17) . . ? C54 C49 N3 109.6(14) . . ? C53 C49 N3 106.7(13) . . ? C54 C49 C50 113.0(16) . . ? C53 C49 C50 101.1(13) . . ? N3 C49 C50 103.4(12) . . ? C51 C50 C49 109.5(15) . . ? C51 C50 H50A 109.8 . . ? C49 C50 H50A 109.8 . . ? C51 C50 H50B 109.7 . . ? C49 C50 H50B 109.8 . . ? H50A C50 H50B 108.2 . . ? C50 C51 C52 103.9(13) . . ? C50 C51 H51A 111.0 . . ? C52 C51 H51A 111.0 . . ? C50 C51 H51B 111.0 . . ? C52 C51 H51B 110.9 . . ? H51A C51 H51B 109.0 . . ? C53 C52 N4 103.3(13) . . ? C53 C52 C51 104.1(14) . . ? N4 C52 C51 108.9(15) . . ? C53 C52 H52 113.2 . . ? N4 C52 H52 113.3 . . ? C51 C52 H52 113.2 . . ? C55 C53 C52 119.0(16) . . ? C55 C53 C49 111.8(15) . . ? C52 C53 C49 100.8(14) . . ? C55 C53 C56 110.8(16) . . ? C52 C53 C56 107.4(14) . . ? C49 C53 C56 106.0(15) . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.4 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.4 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N3 C57 C58 106.4(14) . . ? N3 C57 H57A 110.4 . . ? C58 C57 H57A 110.5 . . ? N3 C57 H57B 110.5 . . ? C58 C57 H57B 110.4 . . ? H57A C57 H57B 108.6 . . ? C63 C58 C59 117(2) . . ? C63 C58 C57 123.3(16) . . ? C59 C58 C57 117.3(18) . . ? C60 C59 C58 122(2) . . ? C60 C59 P3 113.9(16) . . ? C58 C59 P3 123.0(17) . . ? C59 C60 C61 116(2) . . ? C59 C60 H60 121.8 . . ? C61 C60 H60 121.8 . . ? C62 C61 C60 119(2) . . ? C62 C61 H61 120.4 . . ? C60 C61 H61 120.4 . . ? C63 C62 C61 118(2) . . ? C63 C62 H62 121.2 . . ? C61 C62 H62 121.1 . . ? C58 C63 C62 127(2) . . ? C58 C63 H63 116.7 . . ? C62 C63 H63 116.6 . . ? C65 C64 C69 119.4(16) . . ? C65 C64 P3 120.5(14) . . ? C69 C64 P3 120.0(14) . . ? C66 C65 C64 119(2) . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? C65 C66 C67 124(2) . . ? C65 C66 H66 118.1 . . ? C67 C66 H66 118.1 . . ? C68 C67 C66 115(2) . . ? C68 C67 H67 122.4 . . ? C66 C67 H67 122.4 . . ? C69 C68 C67 124(2) . . ? C69 C68 H68 117.9 . . ? C67 C68 H68 117.9 . . ? C68 C69 C64 118(2) . . ? C68 C69 H69 121.2 . . ? C64 C69 H69 121.1 . . ? C75 C70 C71 119.3(18) . . ? C75 C70 P3 122.4(19) . . ? C71 C70 P3 118.3(15) . . ? C70 C71 C72 116(2) . . ? C70 C71 H71 121.8 . . ? C72 C71 H71 121.9 . . ? C73 C72 C71 122(2) . . ? C73 C72 H72 119.0 . . ? C71 C72 H72 119.0 . . ? C72 C73 C74 120.5(18) . . ? C72 C73 H73 119.8 . . ? C74 C73 H73 119.7 . . ? C75 C74 C73 118.9(19) . . ? C75 C74 H74 120.6 . . ? C73 C74 H74 120.6 . . ? C74 C75 C70 123(2) . . ? C74 C75 H75 118.5 . . ? C70 C75 H75 118.6 . . ? N4 C76 C77 122.3(17) . . ? N4 C76 H76A 106.8 . . ? C77 C76 H76A 106.7 . . ? N4 C76 H76B 106.7 . . ? C77 C76 H76B 106.8 . . ? H76A C76 H76B 106.6 . . ? C82 C77 C78 119.6(18) . . ? C82 C77 C76 119.4(17) . . ? C78 C77 C76 120.5(16) . . ? C77 C78 C79 117.7(17) . . ? C77 C78 P4 127.0(14) . . ? C79 C78 P4 115.3(15) . . ? C80 C79 C78 119.7(19) . . ? C80 C79 H79 120.2 . . ? C78 C79 H79 120.1 . . ? C79 C80 C81 120(2) . . ? C79 C80 H80 119.9 . . ? C81 C80 H80 119.9 . . ? C82 C81 C80 117(2) . . ? C82 C81 H81 121.6 . . ? C80 C81 H81 121.7 . . ? C81 C82 C77 126(2) . . ? C81 C82 H82 116.9 . . ? C77 C82 H82 116.9 . . ? C88 C83 C84 117.4(17) . . ? C88 C83 P4 118.6(15) . . ? C84 C83 P4 123.9(15) . . ? C85 C84 C83 126.1(19) . . ? C85 C84 H84 117.0 . . ? C83 C84 H84 116.9 . . ? C86 C85 C84 116(2) . . ? C86 C85 H85 121.8 . . ? C84 C85 H85 121.8 . . ? C85 C86 C87 122(2) . . ? C85 C86 H86 119.1 . . ? C87 C86 H86 119.1 . . ? C86 C87 C88 120(2) . . ? C86 C87 H87 120.1 . . ? C88 C87 H87 120.1 . . ? C83 C88 C87 118(2) . . ? C83 C88 H88 120.9 . . ? C87 C88 H88 120.9 . . ? C94 C89 C90 120.0(17) . . ? C94 C89 P4 120.3(14) . . ? C90 C89 P4 119.2(13) . . ? C91 C90 C89 118.5(18) . . ? C91 C90 H90 120.8 . . ? C89 C90 H90 120.8 . . ? C92 C91 C90 124(2) . . ? C92 C91 H91 117.9 . . ? C90 C91 H91 118.0 . . ? C91 C92 C93 117(2) . . ? C91 C92 H92 121.4 . . ? C93 C92 H92 121.3 . . ? C94 C93 C92 115.6(19) . . ? C94 C93 H93 122.2 . . ? C92 C93 H93 122.2 . . ? C89 C94 C93 124.3(18) . . ? C89 C94 H94 117.9 . . ? C93 C94 H94 117.9 . . ? C1 N1 C2 123.5(16) . . ? C1 N1 C10 114.1(13) . . ? C2 N1 C10 120.3(13) . . ? C1 N2 C5 119.8(14) . . ? C1 N2 C29 114.7(14) . . ? C5 N2 C29 125.5(14) . . ? C48 N3 C57 114.8(16) . . ? C48 N3 C49 115.4(15) . . ? C57 N3 C49 126.7(14) . . ? C48 N4 C76 126.7(17) . . ? C48 N4 C52 120.3(16) . . ? C76 N4 C52 112.7(17) . . ? C12 P1 C23 106.2(9) . . ? C12 P1 C17 107.8(9) . . ? C23 P1 C17 103.1(8) . . ? C12 P1 Pd1 108.4(6) . . ? C23 P1 Pd1 111.8(7) . . ? C17 P1 Pd1 118.8(6) . . ? C42 P2 C36 100.5(10) . . ? C42 P2 C31 107.1(8) . . ? C36 P2 C31 107.2(9) . . ? C42 P2 Pd1 120.1(7) . . ? C36 P2 Pd1 103.6(7) . . ? C31 P2 Pd1 116.4(6) . . ? C70 P3 C64 99.5(9) . . ? C70 P3 C59 108.8(10) . . ? C64 P3 C59 108.7(9) . . ? C70 P3 Pd2 120.7(7) . . ? C64 P3 Pd2 111.3(6) . . ? C59 P3 Pd2 107.3(7) . . ? C89 P4 C83 107.3(8) . . ? C89 P4 C78 107.9(8) . . ? C83 P4 C78 101.5(8) . . ? C89 P4 Pd2 104.4(6) . . ? C83 P4 Pd2 120.8(6) . . ? C78 P4 Pd2 114.4(6) . . ? Cl1 Pd1 Cl2 170.0(2) . . ? Cl1 Pd1 P1 85.30(16) . . ? Cl2 Pd1 P1 93.52(16) . . ? Cl1 Pd1 P2 94.98(16) . . ? Cl2 Pd1 P2 87.36(17) . . ? P1 Pd1 P2 173.2(2) . . ? Cl3 Pd2 Cl4 169.9(2) . . ? Cl3 Pd2 P4 88.23(17) . . ? Cl4 Pd2 P4 94.23(17) . . ? Cl3 Pd2 P3 92.06(17) . . ? Cl4 Pd2 P3 86.34(17) . . ? P4 Pd2 P3 175.0(2) . . ? F1 P5 F5 90.9(9) . . ? F1 P5 F4 91.7(8) . . ? F5 P5 F4 90.9(8) . . ? F1 P5 F3 175.9(11) . . ? F5 P5 F3 87.4(8) . . ? F4 P5 F3 92.0(8) . . ? F1 P5 F6 91.6(9) . . ? F5 P5 F6 177.5(11) . . ? F4 P5 F6 89.1(8) . . ? F3 P5 F6 90.1(8) . . ? F1 P5 F2 87.6(8) . . ? F5 P5 F2 93.2(8) . . ? F4 P5 F2 175.9(10) . . ? F3 P5 F2 88.8(7) . . ? F6 P5 F2 86.9(7) . . ? F8A P6 F8A 90.1(8) . 2_556 ? F8A P6 F8 45.0(4) . . ? F8A P6 F8 45.0(4) 2_556 . ? F8A P6 F10 135.0(4) . . ? F8A P6 F10 135.0(4) 2_556 . ? F8 P6 F10 180.000(3) . . ? F8A P6 F9A 178.9(12) . 2_556 ? F8A P6 F9A 90.9(7) 2_556 2_556 ? F8 P6 F9A 135.9(9) . 2_556 ? F10 P6 F9A 44.1(9) . 2_556 ? F8A P6 F9 45.1(5) . 2_556 ? F8A P6 F9 135.0(6) 2_556 2_556 ? F8 P6 F9 90.0(4) . 2_556 ? F10 P6 F9 90.0(4) . 2_556 ? F9A P6 F9 134.0(10) 2_556 2_556 ? F8A P6 F7 89.1(6) . . ? F8A P6 F7 91.2(7) 2_556 . ? F8 P6 F7 90.2(3) . . ? F10 P6 F7 89.8(3) . . ? F9A P6 F7 90.4(8) 2_556 . ? F9 P6 F7 92.1(5) 2_556 . ? F8A P6 F7 91.2(7) . 2_556 ? F8A P6 F7 89.1(6) 2_556 2_556 ? F8 P6 F7 90.2(3) . 2_556 ? F10 P6 F7 89.8(3) . 2_556 ? F9A P6 F7 89.2(6) 2_556 2_556 ? F9 P6 F7 87.9(5) 2_556 2_556 ? F7 P6 F7 179.6(7) . 2_556 ? F11 P7 F14 90.5(4) . 2_657 ? F11 P7 F14 90.5(5) . . ? F14 P7 F14 179.1(9) 2_657 . ? F11 P7 F13 90.7(4) . 2_657 ? F14 P7 F13 90.5(6) 2_657 2_657 ? F14 P7 F13 89.5(6) . 2_657 ? F11 P7 F13 90.7(4) . . ? F14 P7 F13 89.5(6) 2_657 . ? F14 P7 F13 90.5(6) . . ? F13 P7 F13 178.5(7) 2_657 . ? F11 P7 F12 180.000(8) . . ? F14 P7 F12 89.5(5) 2_657 . ? F14 P7 F12 89.5(5) . . ? F13 P7 F12 89.3(4) 2_657 . ? F13 P7 F12 89.3(4) . . ? F11 P7 F14A 126.8(6) . 2_657 ? F14 P7 F14A 36.4(7) 2_657 2_657 ? F14 P7 F14A 142.6(8) . 2_657 ? F13 P7 F14A 88.2(5) 2_657 2_657 ? F13 P7 F14A 90.9(6) . 2_657 ? F12 P7 F14A 53.2(6) . 2_657 ? F11 P7 F14A 126.8(6) . . ? F14 P7 F14A 142.6(8) 2_657 . ? F14 P7 F14A 36.4(7) . . ? F13 P7 F14A 90.9(6) 2_657 . ? F13 P7 F14A 88.2(5) . . ? F12 P7 F14A 53.2(6) . . ? F14A P7 F14A 106.3(12) 2_657 . ? F11 P7 F11A 41.8(3) . . ? F14 P7 F11A 132.0(6) 2_657 . ? F14 P7 F11A 48.9(5) . . ? F13 P7 F11A 93.4(7) 2_657 . ? F13 P7 F11A 87.6(5) . . ? F12 P7 F11A 138.2(3) . . ? F14A P7 F11A 168.4(8) 2_657 . ? F14A P7 F11A 85.1(5) . . ? F11 P7 F11A 41.8(3) . 2_657 ? F14 P7 F11A 48.9(5) 2_657 2_657 ? F14 P7 F11A 132.0(6) . 2_657 ? F13 P7 F11A 87.6(5) 2_657 2_657 ? F13 P7 F11A 93.4(7) . 2_657 ? F12 P7 F11A 138.2(3) . 2_657 ? F14A P7 F11A 85.1(5) 2_657 2_657 ? F14A P7 F11A 168.4(9) . 2_657 ? F11A P7 F11A 83.5(6) . 2_657 ? Cl6 C95 Cl5 105.7(7) . . ? Cl6 C95 Cl7 104.9(7) . . ? Cl5 C95 Cl7 111.8(7) . . ? Cl6 C95 H95 111.3 . . ? Cl5 C95 H95 111.4 . . ? Cl7 C95 H95 111.4 . . ? Cl10 C96 Cl8 107.1(7) . . ? Cl10 C96 Cl9 114.2(8) . . ? Cl8 C96 Cl9 107.3(7) . . ? Cl10 C96 H96 109.4 . . ? Cl8 C96 H96 109.4 . . ? Cl9 C96 H96 109.4 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.346 _refine_diff_density_min -0.911 _refine_diff_density_rms 0.120 data_kjc1135 _database_code_depnum_ccdc_archive 'CCDC 891177' #TrackingRef 'cmpd3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H53 Cl2 F6 N4 P3 Pt' _chemical_formula_weight 1194.87 _chemical_absolute_configuration ad 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' Pt Pt -1.7033 8.3905 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.9538(5) _cell_length_b 14.4075(4) _cell_length_c 29.2856(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.809(2) _cell_angle_gamma 90.00 _cell_volume 5032.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11357 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 37.54 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 3.052 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4613 _exptl_absorpt_correction_T_max 0.8877 _exptl_absorpt_process_details Denzo/scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19515 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1757 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.54 _reflns_number_total 19515 _reflns_number_gt 11357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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. Geometric restraints were applied to the acetinitrrile solvent molecules as well as to and the atomic displacement parameters to stop distortion. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+83.4269P] 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 0.049(14) _refine_ls_number_reflns 19515 _refine_ls_number_parameters 1217 _refine_ls_number_restraints 173 _refine_ls_R_factor_all 0.1889 _refine_ls_R_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1947 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4286(15) 0.2799(10) 0.1262(6) 0.032(4) Uani 1 1 d . . . H1 H 0.4294 0.3418 0.1150 0.039 Uiso 1 1 calc R . . C2 C 0.5142(18) 0.1358(16) 0.1454(8) 0.064(6) Uani 1 1 d U . . C3 C 0.4615(15) 0.0826(12) 0.1002(7) 0.051(6) Uani 1 1 d . . . H3A H 0.4813 0.1155 0.0721 0.062 Uiso 1 1 calc R . . H3B H 0.4901 0.0182 0.0991 0.062 Uiso 1 1 calc R . . C4 C 0.336(2) 0.0829(15) 0.1038(9) 0.078(8) Uani 1 1 d . . . H4A H 0.3080 0.0191 0.1079 0.094 Uiso 1 1 calc R . . H4B H 0.2977 0.1102 0.0760 0.094 Uiso 1 1 calc R . . C5 C 0.318(2) 0.1435(18) 0.1467(8) 0.081(7) Uani 1 1 d . . . H5 H 0.2460 0.1294 0.1611 0.097 Uiso 1 1 calc R . . C6 C 0.4168(18) 0.1274(13) 0.1769(7) 0.061(6) Uani 1 1 d . . . C7 C 0.6201(19) 0.1019(17) 0.1593(9) 0.084(8) Uani 1 1 d . . . H7A H 0.6545 0.1421 0.1833 0.126 Uiso 1 1 calc R . . H7B H 0.6671 0.1012 0.1331 0.126 Uiso 1 1 calc R . . H7C H 0.6132 0.0388 0.1712 0.126 Uiso 1 1 calc R . . C8 C 0.419(2) 0.0253(18) 0.1933(9) 0.095(8) Uani 1 1 d U . . H8A H 0.3455 -0.0031 0.1862 0.143 Uiso 1 1 calc R . . H8B H 0.4370 0.0233 0.2265 0.143 Uiso 1 1 calc R . . H8C H 0.4762 -0.0091 0.1777 0.143 Uiso 1 1 calc R . . C9 C 0.4299(19) 0.1913(16) 0.2183(7) 0.064(6) Uani 1 1 d . . . H9A H 0.4002 0.2529 0.2100 0.097 Uiso 1 1 calc R . . H9B H 0.5095 0.1966 0.2284 0.097 Uiso 1 1 calc R . . H9C H 0.3885 0.1657 0.2432 0.097 Uiso 1 1 calc R . . C10 C 0.6240(14) 0.2974(16) 0.1256(7) 0.055(6) Uani 1 1 d . . . H10A H 0.6911 0.2679 0.1410 0.066 Uiso 1 1 calc R . . H10B H 0.6137 0.3583 0.1403 0.066 Uiso 1 1 calc R . . C11 C 0.6453(15) 0.3131(13) 0.0766(7) 0.043(5) Uani 1 1 d . . . C12 C 0.6395(14) 0.4015(14) 0.0560(6) 0.039(5) Uani 1 1 d . . . C13 C 0.6551(13) 0.4056(11) 0.0091(6) 0.032(4) Uani 1 1 d . . . H13 H 0.6514 0.4648 -0.0052 0.039 Uiso 1 1 calc R . . C14 C 0.6760(15) 0.3277(14) -0.0183(7) 0.050(5) Uani 1 1 d . . . H14 H 0.6818 0.3335 -0.0504 0.060 Uiso 1 1 calc R . . C15 C 0.6877(15) 0.2422(13) 0.0035(8) 0.051(6) Uani 1 1 d . . . H15 H 0.7092 0.1886 -0.0126 0.061 Uiso 1 1 calc R . . C16 C 0.6675(13) 0.2377(12) 0.0489(8) 0.042(5) Uani 1 1 d . . . H16 H 0.6685 0.1779 0.0626 0.051 Uiso 1 1 calc R . . C17 C 0.7083(12) 0.5220(13) 0.1334(6) 0.040(4) Uani 1 1 d . . . C18 C 0.7954(16) 0.4604(14) 0.1417(7) 0.054(6) Uani 1 1 d . . . H18 H 0.8036 0.4079 0.1226 0.065 Uiso 1 1 calc R . . C19 C 0.8716(16) 0.4778(14) 0.1793(7) 0.050(5) Uani 1 1 d U . . H19 H 0.9324 0.4362 0.1856 0.060 Uiso 1 1 calc R . . C20 C 0.8606(17) 0.5534(16) 0.2073(8) 0.065(6) Uani 1 1 d . . . H20 H 0.9158 0.5661 0.2314 0.077 Uiso 1 1 calc R . . C21 C 0.7673(17) 0.6113(16) 0.2000(8) 0.070(7) Uani 1 1 d . . . H21 H 0.7516 0.6583 0.2214 0.085 Uiso 1 1 calc R . . C22 C 0.6986(14) 0.5985(11) 0.1608(6) 0.035(4) Uani 1 1 d . . . H22 H 0.6431 0.6437 0.1525 0.042 Uiso 1 1 calc R . . C23 C 0.6587(13) 0.6003(10) 0.0483(6) 0.026(4) Uani 1 1 d . . . C24 C 0.7686(13) 0.6066(12) 0.0371(7) 0.046(5) Uani 1 1 d . . . H24 H 0.8192 0.5584 0.0466 0.055 Uiso 1 1 calc R . . C25 C 0.8076(16) 0.6796(15) 0.0128(7) 0.052(6) Uani 1 1 d . . . H25 H 0.8838 0.6806 0.0054 0.062 Uiso 1 1 calc R . . C26 C 0.7383(16) 0.7508(12) -0.0009(6) 0.042(5) Uani 1 1 d U . . H26 H 0.7663 0.8029 -0.0163 0.050 Uiso 1 1 calc R . . C27 C 0.6276(16) 0.7458(12) 0.0081(6) 0.041(5) Uani 1 1 d . . . H27 H 0.5785 0.7949 -0.0014 0.049 Uiso 1 1 calc R . . C28 C 0.5853(15) 0.6686(10) 0.0313(6) 0.036(5) Uani 1 1 d . . . H28 H 0.5073 0.6636 0.0353 0.043 Uiso 1 1 calc R . . C29 C 0.2270(17) 0.2948(15) 0.1272(7) 0.057(6) Uani 1 1 d . . . H29A H 0.1648 0.2498 0.1223 0.068 Uiso 1 1 calc R . . H29B H 0.2292 0.3324 0.0989 0.068 Uiso 1 1 calc R . . C30 C 0.2001(13) 0.3598(14) 0.1667(6) 0.039(5) Uani 1 1 d . . . C31 C 0.1975(13) 0.4527(12) 0.1606(6) 0.033(4) Uani 1 1 d U . . C32 C 0.1735(13) 0.5051(14) 0.1992(7) 0.043(4) Uani 1 1 d . . . H32 H 0.1735 0.5708 0.1963 0.052 Uiso 1 1 calc R . . C33 C 0.1502(15) 0.4689(17) 0.2402(8) 0.055(6) Uani 1 1 d . . . H33 H 0.1363 0.5071 0.2657 0.065 Uiso 1 1 calc R . . C34 C 0.1481(15) 0.3765(19) 0.2428(6) 0.057(6) Uani 1 1 d . . . H34 H 0.1288 0.3483 0.2705 0.069 Uiso 1 1 calc R . . C35 C 0.1740(15) 0.3181(14) 0.2049(6) 0.046(5) Uani 1 1 d . . . H35 H 0.1725 0.2523 0.2073 0.055 Uiso 1 1 calc R . . C36 C 0.1175(17) 0.4675(15) 0.0645(8) 0.058(6) Uani 1 1 d U . . C37 C 0.1177(16) 0.5012(15) 0.0232(7) 0.056(5) Uani 1 1 d U . . H37 H 0.1700 0.5486 0.0171 0.067 Uiso 1 1 calc R . . C38 C 0.041(2) 0.4687(16) -0.0139(9) 0.074(7) Uani 1 1 d U . . H38 H 0.0464 0.4894 -0.0444 0.088 Uiso 1 1 calc R . . C39 C -0.0378(15) 0.4092(18) -0.0033(7) 0.065(7) Uani 1 1 d . . . H39 H -0.0942 0.3909 -0.0259 0.078 Uiso 1 1 calc R . . C40 C -0.0380(16) 0.3722(14) 0.0421(8) 0.057(6) Uani 1 1 d . . . H40 H -0.0895 0.3252 0.0494 0.069 Uiso 1 1 calc R . . C41 C 0.0400(16) 0.4075(13) 0.0751(7) 0.049(5) Uani 1 1 d U . . H41 H 0.0373 0.3877 0.1059 0.059 Uiso 1 1 calc R . . C42 C 0.1792(15) 0.6363(14) 0.1168(7) 0.050(5) Uani 1 1 d . . . C43 C 0.2558(17) 0.7033(15) 0.1225(7) 0.049(5) Uani 1 1 d . . . H43 H 0.3332 0.6889 0.1214 0.059 Uiso 1 1 calc R . . C44 C 0.224(2) 0.7911(18) 0.1298(9) 0.074(7) Uani 1 1 d . . . H44 H 0.2801 0.8370 0.1350 0.089 Uiso 1 1 calc R . . C45 C 0.115(2) 0.8177(18) 0.1300(9) 0.074(7) Uani 1 1 d U . . H45 H 0.0947 0.8803 0.1355 0.089 Uiso 1 1 calc R . . C46 C 0.036(2) 0.7507(14) 0.1221(10) 0.100(10) Uani 1 1 d D . . H46 H -0.0410 0.7668 0.1210 0.121 Uiso 1 1 calc R . . C47 C 0.0669(18) 0.6580(13) 0.1153(8) 0.068(7) Uani 1 1 d D . . H47 H 0.0115 0.6113 0.1098 0.082 Uiso 1 1 calc R . . C48 C 0.5570(14) 0.3586(13) 0.3817(8) 0.055(6) Uani 1 1 d . . . H48 H 0.5630 0.3103 0.4039 0.067 Uiso 1 1 calc R . . C49 C 0.4435(14) 0.4756(12) 0.3361(7) 0.041(5) Uani 1 1 d . . . C50 C 0.4475(15) 0.4358(13) 0.2903(6) 0.044(5) Uani 1 1 d . . . H50A H 0.4144 0.4798 0.2673 0.052 Uiso 1 1 calc R . . H50B H 0.4033 0.3777 0.2883 0.052 Uiso 1 1 calc R . . C51 C 0.5735(17) 0.4150(17) 0.2804(8) 0.069(7) Uani 1 1 d . . . H51A H 0.5875 0.3475 0.2775 0.083 Uiso 1 1 calc R . . H51B H 0.5954 0.4471 0.2525 0.083 Uiso 1 1 calc R . . C52 C 0.6348(15) 0.4559(12) 0.3244(6) 0.042(5) Uani 1 1 d . . . H52 H 0.7093 0.4822 0.3176 0.050 Uiso 1 1 calc R . . C53 C 0.5568(15) 0.5333(11) 0.3429(6) 0.041(5) Uani 1 1 d . . . C54 C 0.3432(16) 0.5348(15) 0.3440(8) 0.069(7) Uani 1 1 d . . . H54A H 0.3301 0.5783 0.3185 0.104 Uiso 1 1 calc R . . H54B H 0.3569 0.5697 0.3726 0.104 Uiso 1 1 calc R . . H54C H 0.2772 0.4952 0.3462 0.104 Uiso 1 1 calc R . . C55 C 0.5561(17) 0.6130(11) 0.3062(8) 0.058(6) Uani 1 1 d . . . H55A H 0.5027 0.6612 0.3140 0.088 Uiso 1 1 calc R . . H55B H 0.5340 0.5875 0.2760 0.088 Uiso 1 1 calc R . . H55C H 0.6313 0.6400 0.3059 0.088 Uiso 1 1 calc R . . C56 C 0.5904(17) 0.5717(14) 0.3898(7) 0.062(6) Uani 1 1 d . . . H56A H 0.6428 0.6234 0.3869 0.093 Uiso 1 1 calc R . . H56B H 0.6266 0.5228 0.4088 0.093 Uiso 1 1 calc R . . H56C H 0.5235 0.5939 0.4041 0.093 Uiso 1 1 calc R . . C57 C 0.3581(14) 0.3409(10) 0.3802(7) 0.042(5) Uani 1 1 d . . . H57A H 0.3630 0.2802 0.3647 0.051 Uiso 1 1 calc R . . H57B H 0.2901 0.3731 0.3671 0.051 Uiso 1 1 calc R . . C58 C 0.3475(13) 0.3248(11) 0.4326(6) 0.036(4) Uani 1 1 d U . . C59 C 0.3447(13) 0.2338(11) 0.4518(6) 0.032(4) Uani 1 1 d U . . C60 C 0.3339(14) 0.2241(13) 0.4988(7) 0.048(5) Uani 1 1 d . . . H60 H 0.3372 0.1643 0.5125 0.058 Uiso 1 1 calc R . . C61 C 0.3186(14) 0.3005(14) 0.5247(7) 0.046(5) Uani 1 1 d . . . H61 H 0.3067 0.2942 0.5563 0.055 Uiso 1 1 calc R . . C62 C 0.3203(16) 0.3846(14) 0.5057(8) 0.050(5) Uani 1 1 d . . . H62 H 0.3144 0.4370 0.5251 0.060 Uiso 1 1 calc R . . C63 C 0.3302(13) 0.4003(13) 0.4595(7) 0.041(5) Uani 1 1 d . . . H63 H 0.3251 0.4611 0.4471 0.050 Uiso 1 1 calc R . . C64 C 0.2729(13) 0.1198(14) 0.3698(6) 0.038(4) Uani 1 1 d . . . C65 C 0.1805(13) 0.1744(11) 0.3632(6) 0.031(4) Uani 1 1 d . . . H65 H 0.1669 0.2211 0.3851 0.037 Uiso 1 1 calc R . . C66 C 0.1052(14) 0.1632(13) 0.3251(7) 0.045(5) Uani 1 1 d . . . H66 H 0.0448 0.2054 0.3194 0.054 Uiso 1 1 calc R . . C67 C 0.1200(17) 0.0896(16) 0.2958(8) 0.061(6) Uani 1 1 d . . . H67 H 0.0661 0.0788 0.2710 0.073 Uiso 1 1 calc R . . C68 C 0.2105(18) 0.0323(15) 0.3018(7) 0.057(6) Uani 1 1 d . . . H68 H 0.2221 -0.0149 0.2800 0.069 Uiso 1 1 calc R . . C69 C 0.2868(17) 0.0428(15) 0.3401(7) 0.056(6) Uani 1 1 d . . . H69 H 0.3462 -0.0003 0.3460 0.067 Uiso 1 1 calc R . . C70 C 0.3289(17) 0.0275(10) 0.4536(7) 0.047(5) Uani 1 1 d . . . C71 C 0.4045(14) -0.0471(11) 0.4627(6) 0.031(4) Uani 1 1 d U . . H71 H 0.4777 -0.0439 0.4520 0.037 Uiso 1 1 calc R . . C72 C 0.3731(19) -0.1245(15) 0.4868(8) 0.064(6) Uani 1 1 d . . . H72 H 0.4258 -0.1725 0.4941 0.076 Uiso 1 1 calc R . . C73 C 0.2637(19) -0.1313(17) 0.5003(8) 0.066(7) Uani 1 1 d . . . H73 H 0.2402 -0.1840 0.5167 0.079 Uiso 1 1 calc R . . C74 C 0.1862(17) -0.0555(14) 0.4886(7) 0.052(5) Uani 1 1 d . . . H74 H 0.1101 -0.0603 0.4959 0.062 Uiso 1 1 calc R . . C75 C 0.2224(13) 0.0241(15) 0.4668(6) 0.047(5) Uani 1 1 d . . . H75 H 0.1732 0.0752 0.4613 0.057 Uiso 1 1 calc R . . C76 C 0.7549(13) 0.3357(12) 0.3743(6) 0.033(4) Uani 1 1 d . . . H76A H 0.8146 0.3817 0.3821 0.039 Uiso 1 1 calc R . . H76B H 0.7453 0.2971 0.4017 0.039 Uiso 1 1 calc R . . C77 C 0.7900(16) 0.2752(15) 0.3364(8) 0.055(6) Uani 1 1 d . . . C78 C 0.7911(15) 0.1762(14) 0.3401(7) 0.048(5) Uani 1 1 d . . . C79 C 0.8161(12) 0.1198(14) 0.3015(6) 0.039(4) Uani 1 1 d . . . H79 H 0.8150 0.0540 0.3037 0.047 Uiso 1 1 calc R . . C80 C 0.8417(14) 0.1625(13) 0.2612(7) 0.045(5) Uani 1 1 d U . . H80 H 0.8552 0.1246 0.2356 0.054 Uiso 1 1 calc R . . C81 C 0.8487(15) 0.2613(13) 0.2564(7) 0.050(5) Uani 1 1 d U . . H81 H 0.8693 0.2904 0.2291 0.060 Uiso 1 1 calc R . . C82 C 0.8237(15) 0.3093(13) 0.2935(8) 0.049(6) Uani 1 1 d . . . H82 H 0.8291 0.3749 0.2910 0.059 Uiso 1 1 calc R . . C83 C 0.8658(13) 0.1523(12) 0.4343(6) 0.038(4) Uani 1 1 d U . . C84 C 0.8707(15) 0.1111(12) 0.4772(6) 0.044(5) Uani 1 1 d U . . H84 H 0.8162 0.0654 0.4831 0.052 Uiso 1 1 calc R . . C85 C 0.9474(16) 0.1320(17) 0.5107(6) 0.059(5) Uani 1 1 d . . . H85 H 0.9545 0.0983 0.5387 0.071 Uiso 1 1 calc R . . C86 C 1.0189(17) 0.2095(19) 0.5016(8) 0.075(8) Uani 1 1 d . . . H86 H 1.0686 0.2311 0.5260 0.090 Uiso 1 1 calc R . . C87 C 1.0204(18) 0.2529(17) 0.4614(8) 0.063(6) Uani 1 1 d . . . H87 H 1.0740 0.3001 0.4570 0.076 Uiso 1 1 calc R . . C88 C 0.9436(15) 0.2287(15) 0.4268(7) 0.054(6) Uani 1 1 d . . . H88 H 0.9408 0.2607 0.3984 0.065 Uiso 1 1 calc R . . C89 C 0.7861(15) -0.0002(14) 0.3834(6) 0.045(5) Uani 1 1 d . . . C90 C 0.6996(15) -0.0608(14) 0.3630(6) 0.045(5) Uani 1 1 d . . . H90 H 0.6265 -0.0369 0.3557 0.054 Uiso 1 1 calc R . . C91 C 0.722(2) -0.1535(13) 0.3541(7) 0.057(6) Uani 1 1 d . . . H91 H 0.6631 -0.1935 0.3434 0.068 Uiso 1 1 calc R . . C92 C 0.824(3) -0.1862(19) 0.3602(8) 0.076(8) Uani 1 1 d . . . H92 H 0.8381 -0.2481 0.3510 0.091 Uiso 1 1 calc R . . C93 C 0.913(2) -0.1337(17) 0.3796(10) 0.079(8) Uani 1 1 d . . . H93 H 0.9845 -0.1614 0.3857 0.095 Uiso 1 1 calc R . . C94 C 0.8959(18) -0.0390(16) 0.3900(7) 0.063(6) Uani 1 1 d . . . H94 H 0.9571 -0.0015 0.4013 0.075 Uiso 1 1 calc R . . C95 C 0.339(4) 0.784(3) 0.2471(16) 0.152(15) Uani 1 1 d U . . C96 C 0.449(2) 0.782(2) 0.2317(12) 0.144(15) Uani 1 1 d D . . H96A H 0.4750 0.7179 0.2306 0.216 Uiso 1 1 calc R . . H96B H 0.4996 0.8179 0.2528 0.216 Uiso 1 1 calc R . . H96C H 0.4485 0.8097 0.2011 0.216 Uiso 1 1 calc R . . C97 C 0.352(3) 0.798(2) 0.3727(12) 0.080(10) Uani 1 1 d . . . C98 C 0.236(2) 0.775(2) 0.3835(13) 0.110(13) Uani 1 1 d . . . H98A H 0.1828 0.8120 0.3638 0.165 Uiso 1 1 calc R . . H98B H 0.2255 0.7901 0.4156 0.165 Uiso 1 1 calc R . . H98C H 0.2213 0.7091 0.3782 0.165 Uiso 1 1 calc R . . C99 C 0.8425(17) 0.869(2) 0.2356(11) 0.101(10) Uani 1 1 d DU . . C100 C 0.9618(18) 0.858(3) 0.2468(13) 0.154(15) Uani 1 1 d DU . . H10C H 0.9896 0.9117 0.2648 0.232 Uiso 1 1 calc R . . H10D H 1.0011 0.8546 0.2185 0.232 Uiso 1 1 calc R . . H10E H 0.9753 0.8012 0.2646 0.232 Uiso 1 1 calc R . . C101 C 0.608(3) 0.8429(19) 0.1136(9) 0.074(9) Uani 1 1 d . . . C102 C 0.722(2) 0.871(3) 0.1054(13) 0.123(15) Uani 1 1 d . . . H10F H 0.7238 0.8983 0.0747 0.184 Uiso 1 1 calc R . . H10G H 0.7721 0.8174 0.1079 0.184 Uiso 1 1 calc R . . H10H H 0.7479 0.9179 0.1283 0.184 Uiso 1 1 calc R . . N1 N 0.5261(14) 0.2392(9) 0.1329(6) 0.049(4) Uani 1 1 d . . . N2 N 0.3289(14) 0.2446(10) 0.1333(6) 0.054(5) Uani 1 1 d . . . N3 N 0.4596(12) 0.3977(11) 0.3715(6) 0.048(4) Uani 1 1 d . . . N4 N 0.6472(12) 0.3859(12) 0.3615(5) 0.048(4) Uani 1 1 d . . . N5 N 0.247(3) 0.797(4) 0.259(2) 0.28(3) Uani 1 1 d DU . . N6 N 0.437(3) 0.8105(16) 0.3638(12) 0.108(11) Uani 1 1 d . . . N7 N 0.7471(17) 0.879(3) 0.2307(13) 0.164(14) Uani 1 1 d DU . . N8 N 0.521(2) 0.8227(18) 0.1234(10) 0.102(10) Uani 1 1 d . . . F1 F 0.0143(14) 0.1801(12) 0.0992(6) 0.109(6) Uani 1 1 d U . . F2 F 0.0220(19) 0.0334(16) 0.1197(8) 0.152(8) Uani 1 1 d U . . F3 F 0.0343(11) 0.1408(12) 0.1753(4) 0.096(5) Uani 1 1 d . . . F4 F -0.1385(12) 0.0893(11) 0.0917(6) 0.086(5) Uani 1 1 d . . . F5 F -0.1224(15) 0.1969(10) 0.1483(6) 0.113(6) Uani 1 1 d . . . F6 F -0.111(2) 0.0448(18) 0.1628(10) 0.222(16) Uani 1 1 d . . . F7 F 0.1182(11) 0.5363(11) 0.3934(6) 0.092(6) Uani 1 1 d . . . F8 F -0.0616(13) 0.5061(14) 0.3985(6) 0.111(5) Uani 1 1 d U . . F9 F -0.0164(12) 0.6427(12) 0.3835(5) 0.094(5) Uani 1 1 d U . . F10 F -0.0987(19) 0.5505(16) 0.3292(8) 0.165(9) Uani 1 1 d U . . F11 F 0.0728(13) 0.5958(10) 0.3239(5) 0.080(5) Uani 1 1 d . . . F12 F 0.0403(19) 0.4470(15) 0.3434(8) 0.145(8) Uani 1 1 d U . . P1 P 0.6087(4) 0.5093(5) 0.08365(18) 0.0283(11) Uani 1 1 d . . . P2 P 0.2251(4) 0.5141(6) 0.1073(2) 0.0379(13) Uani 1 1 d . . . P3 P 0.7545(4) 0.1190(5) 0.39172(19) 0.0386(14) Uani 1 1 d . . . P4 P 0.3772(4) 0.1266(5) 0.4198(2) 0.0346(13) Uani 1 1 d . . . P5 P -0.0515(5) 0.1096(5) 0.1334(2) 0.0581(18) Uani 1 1 d . . . P6 P 0.0077(6) 0.5431(7) 0.3623(3) 0.095(4) Uani 1 1 d . . . Cl1 Cl 0.3882(3) 0.4966(3) 0.01669(15) 0.0365(10) Uani 1 1 d . . . Cl2 Cl 0.4498(4) 0.5192(4) 0.17283(16) 0.0531(13) Uani 1 1 d . . . Cl3 Cl 0.5263(4) 0.1432(4) 0.32849(15) 0.0503(13) Uani 1 1 d . . . Cl4 Cl 0.6007(3) 0.1307(3) 0.48481(14) 0.0397(10) Uani 1 1 d . . . Pt1 Pt 0.41718(5) 0.51126(6) 0.09473(2) 0.03357(19) Uani 1 1 d . . . Pt2 Pt 0.56588(5) 0.12986(6) 0.40651(2) 0.0368(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.066(13) 0.008(8) 0.022(10) -0.004(7) 0.003(9) 0.005(8) C2 0.066(9) 0.064(9) 0.063(10) 0.007(8) 0.008(8) 0.014(8) C3 0.048(12) 0.038(10) 0.072(17) -0.033(10) 0.039(12) -0.016(8) C4 0.11(2) 0.052(14) 0.069(19) -0.015(12) 0.009(16) -0.031(13) C5 0.075(16) 0.10(2) 0.065(17) -0.009(16) -0.019(13) 0.018(15) C6 0.100(16) 0.040(11) 0.038(12) 0.015(10) -0.032(11) -0.035(12) C7 0.080(18) 0.093(19) 0.074(19) -0.031(14) -0.027(14) -0.011(14) C8 0.099(11) 0.093(11) 0.093(12) 0.001(9) -0.002(9) -0.007(9) C9 0.082(17) 0.092(17) 0.018(12) -0.012(11) -0.003(11) 0.003(13) C10 0.019(10) 0.113(18) 0.033(13) -0.002(12) -0.009(9) 0.025(10) C11 0.036(11) 0.051(12) 0.039(13) -0.004(10) -0.009(9) -0.005(9) C12 0.023(10) 0.064(13) 0.028(12) -0.009(10) -0.005(8) 0.001(9) C13 0.029(9) 0.031(9) 0.036(12) -0.013(8) -0.006(8) 0.003(7) C14 0.045(12) 0.068(15) 0.036(13) -0.009(11) 0.004(10) 0.000(10) C15 0.034(11) 0.034(11) 0.088(19) -0.018(11) 0.031(12) -0.004(8) C16 0.020(10) 0.032(10) 0.075(17) 0.008(10) 0.007(10) 0.000(7) C17 0.017(8) 0.045(11) 0.057(13) -0.011(10) -0.003(8) 0.003(8) C18 0.048(13) 0.064(13) 0.050(15) -0.013(11) 0.002(11) -0.003(10) C19 0.037(8) 0.060(9) 0.052(9) -0.001(7) 0.001(7) 0.004(7) C20 0.036(12) 0.094(17) 0.060(16) -0.010(13) -0.023(11) 0.000(11) C21 0.058(14) 0.081(16) 0.065(16) -0.009(13) -0.052(12) 0.000(12) C22 0.029(10) 0.040(10) 0.036(12) -0.006(8) 0.007(8) -0.002(7) C23 0.019(9) 0.036(10) 0.023(10) 0.001(7) -0.010(7) -0.015(7) C24 0.022(10) 0.050(12) 0.066(15) 0.026(10) 0.006(9) 0.018(8) C25 0.035(12) 0.079(15) 0.043(14) -0.010(11) 0.015(10) -0.017(10) C26 0.049(8) 0.037(8) 0.039(8) 0.005(7) 0.001(7) 0.002(7) C27 0.061(13) 0.040(11) 0.021(11) 0.003(8) -0.004(9) 0.011(9) C28 0.046(11) 0.009(8) 0.052(13) -0.005(8) 0.001(10) -0.006(7) C29 0.055(14) 0.080(15) 0.038(14) -0.025(11) 0.025(11) -0.023(12) C30 0.018(9) 0.078(14) 0.021(11) 0.000(9) -0.011(8) -0.016(8) C31 0.026(7) 0.041(8) 0.031(8) -0.006(7) -0.001(6) -0.015(6) C32 0.028(9) 0.046(10) 0.054(13) 0.009(11) -0.006(8) 0.004(9) C33 0.027(11) 0.084(16) 0.053(16) -0.004(12) 0.005(10) -0.005(10) C34 0.032(11) 0.13(2) 0.013(11) -0.005(12) -0.004(8) 0.001(12) C35 0.051(13) 0.063(13) 0.026(12) 0.002(10) 0.015(10) -0.011(10) C36 0.046(9) 0.076(9) 0.051(10) -0.004(8) 0.000(8) -0.001(7) C37 0.050(8) 0.066(9) 0.052(9) 0.000(8) 0.006(7) -0.006(8) C38 0.064(10) 0.086(10) 0.071(11) 0.011(8) 0.001(8) 0.001(8) C39 0.024(11) 0.14(2) 0.029(13) -0.002(13) 0.000(9) -0.003(12) C40 0.053(13) 0.064(14) 0.056(16) -0.026(12) 0.008(11) -0.029(10) C41 0.048(8) 0.058(9) 0.042(9) 0.004(7) -0.002(7) 0.000(7) C42 0.043(11) 0.058(12) 0.048(13) -0.002(11) 0.004(9) -0.020(11) C43 0.046(13) 0.067(14) 0.034(13) -0.007(10) 0.013(10) 0.017(11) C44 0.059(16) 0.089(19) 0.08(2) -0.020(15) 0.020(14) -0.025(14) C45 0.077(10) 0.075(10) 0.070(11) 0.011(8) 0.003(8) 0.016(8) C46 0.079(19) 0.09(2) 0.13(3) 0.064(19) 0.002(18) 0.028(16) C47 0.047(14) 0.060(15) 0.10(2) 0.006(13) -0.008(13) 0.015(10) C48 0.023(11) 0.052(12) 0.093(19) 0.014(12) 0.017(11) -0.005(9) C49 0.026(10) 0.046(11) 0.051(14) -0.016(9) 0.011(9) 0.009(8) C50 0.045(12) 0.066(13) 0.019(11) 0.000(9) -0.002(9) 0.005(9) C51 0.039(13) 0.101(19) 0.064(18) 0.003(14) -0.017(12) -0.010(12) C52 0.043(11) 0.048(11) 0.034(12) 0.029(9) -0.002(9) -0.007(9) C53 0.047(11) 0.045(12) 0.032(12) 0.003(8) 0.001(9) -0.017(8) C54 0.051(13) 0.079(17) 0.077(18) 0.036(13) 0.005(12) 0.021(11) C55 0.078(15) 0.018(10) 0.079(17) 0.017(10) -0.001(12) -0.003(9) C56 0.058(14) 0.067(14) 0.059(16) 0.021(12) -0.005(12) -0.044(11) C57 0.037(11) 0.012(8) 0.076(16) -0.005(9) -0.016(10) -0.001(7) C58 0.026(7) 0.043(8) 0.040(8) -0.001(7) -0.002(7) 0.005(6) C59 0.029(7) 0.026(7) 0.040(8) -0.001(6) 0.002(7) 0.002(6) C60 0.035(11) 0.050(12) 0.061(16) 0.028(11) 0.013(10) 0.014(9) C61 0.034(11) 0.054(13) 0.050(14) -0.010(11) 0.006(10) 0.021(9) C62 0.043(12) 0.045(12) 0.060(16) -0.021(11) -0.003(11) 0.005(9) C63 0.021(10) 0.054(12) 0.049(14) -0.021(10) -0.002(9) -0.007(8) C64 0.028(9) 0.067(12) 0.019(10) 0.015(10) 0.002(7) -0.015(9) C65 0.024(9) 0.051(10) 0.017(10) 0.003(8) -0.012(7) 0.007(7) C66 0.017(10) 0.058(12) 0.059(15) -0.003(11) -0.012(9) -0.012(8) C67 0.036(13) 0.083(16) 0.061(17) -0.004(13) -0.012(11) -0.009(11) C68 0.058(14) 0.076(16) 0.037(13) -0.023(11) 0.005(11) -0.027(12) C69 0.048(13) 0.081(16) 0.043(14) 0.001(11) 0.029(11) -0.001(10) C70 0.074(14) 0.013(10) 0.054(14) -0.004(8) 0.011(11) -0.012(8) C71 0.034(7) 0.035(7) 0.022(8) -0.004(6) -0.006(6) -0.002(6) C72 0.067(16) 0.059(14) 0.066(17) -0.010(12) 0.014(13) -0.002(11) C73 0.070(17) 0.082(17) 0.048(16) -0.007(12) 0.025(13) -0.007(13) C74 0.046(13) 0.067(14) 0.044(14) -0.011(11) 0.013(11) -0.020(11) C75 0.023(9) 0.069(14) 0.051(13) -0.005(11) 0.010(9) -0.004(10) C76 0.016(9) 0.050(11) 0.032(11) 0.016(8) -0.008(8) 0.007(7) C77 0.039(12) 0.074(15) 0.057(16) 0.003(12) 0.027(11) -0.007(10) C78 0.025(11) 0.074(14) 0.042(14) 0.020(11) -0.011(9) 0.002(9) C79 0.032(9) 0.067(12) 0.018(10) -0.001(10) 0.000(7) 0.007(9) C80 0.033(8) 0.058(9) 0.042(9) 0.000(7) -0.004(7) 0.003(6) C81 0.047(8) 0.057(9) 0.045(9) 0.007(7) 0.004(7) -0.006(7) C82 0.033(11) 0.039(11) 0.072(17) -0.008(11) -0.030(11) 0.001(8) C83 0.030(7) 0.057(8) 0.025(8) 0.001(7) -0.006(6) -0.003(6) C84 0.051(8) 0.047(8) 0.033(8) 0.013(7) -0.003(7) 0.001(7) C85 0.057(13) 0.103(17) 0.019(11) 0.002(12) 0.011(9) -0.006(14) C86 0.032(13) 0.15(2) 0.045(16) -0.025(16) -0.017(11) 0.013(13) C87 0.051(14) 0.093(17) 0.048(16) 0.012(13) 0.027(12) 0.009(12) C88 0.027(11) 0.104(17) 0.031(13) -0.012(11) -0.004(9) -0.010(11) C89 0.041(11) 0.063(13) 0.030(11) 0.003(10) 0.011(9) 0.016(10) C90 0.023(10) 0.081(15) 0.030(12) 0.003(10) -0.016(9) -0.012(9) C91 0.10(2) 0.034(12) 0.031(13) -0.019(9) -0.003(12) -0.001(12) C92 0.10(2) 0.082(18) 0.045(17) 0.013(14) 0.032(16) 0.030(18) C93 0.066(17) 0.064(16) 0.11(2) -0.009(15) 0.012(16) 0.041(13) C94 0.049(14) 0.092(17) 0.046(15) 0.022(12) -0.001(11) 0.013(12) C95 0.151(17) 0.156(17) 0.150(17) 0.003(10) 0.006(10) 0.003(10) C96 0.15(4) 0.14(3) 0.13(3) 0.08(3) -0.03(3) 0.01(3) C97 0.09(2) 0.058(17) 0.09(3) -0.035(17) -0.017(19) 0.006(16) C98 0.07(2) 0.11(2) 0.16(3) -0.07(2) 0.05(2) -0.009(17) C99 0.113(13) 0.101(12) 0.090(13) 0.001(9) 0.009(9) -0.002(9) C100 0.154(17) 0.158(17) 0.152(17) -0.004(10) 0.016(10) -0.008(10) C101 0.10(2) 0.078(19) 0.047(18) 0.012(13) 0.042(17) 0.021(16) C102 0.042(16) 0.21(4) 0.12(3) -0.09(3) 0.008(17) 0.004(19) N1 0.075(12) 0.022(8) 0.050(11) 0.002(7) 0.018(9) 0.015(8) N2 0.059(12) 0.029(9) 0.076(14) 0.017(8) 0.023(10) -0.007(8) N3 0.035(10) 0.059(10) 0.049(12) 0.009(9) 0.001(8) 0.008(8) N4 0.036(9) 0.081(12) 0.028(10) -0.014(9) 0.011(8) -0.011(8) N5 0.28(3) 0.28(3) 0.28(3) 0.000(10) 0.017(10) -0.001(10) N6 0.12(2) 0.051(14) 0.16(3) -0.017(16) 0.06(2) -0.009(15) N7 0.168(16) 0.164(16) 0.161(16) 0.001(10) 0.011(10) 0.003(10) N8 0.084(17) 0.11(2) 0.12(2) -0.008(16) 0.061(17) 0.001(14) F1 0.107(9) 0.121(9) 0.098(9) 0.002(7) 0.002(7) -0.030(7) F2 0.171(11) 0.145(12) 0.136(11) -0.024(9) -0.018(8) 0.049(9) F3 0.097(10) 0.128(12) 0.056(9) -0.044(9) -0.047(7) 0.018(10) F4 0.066(9) 0.101(12) 0.090(13) -0.035(9) -0.017(8) 0.021(7) F5 0.137(15) 0.068(9) 0.132(16) -0.038(9) 0.000(12) 0.034(9) F6 0.21(2) 0.21(3) 0.23(3) 0.10(2) -0.11(2) -0.15(2) F7 0.061(9) 0.099(13) 0.117(15) -0.029(11) 0.017(9) 0.005(8) F8 0.110(8) 0.134(9) 0.090(9) -0.013(8) 0.020(7) -0.025(8) F9 0.098(7) 0.108(8) 0.074(8) -0.017(7) -0.017(6) 0.041(7) F10 0.158(11) 0.185(12) 0.151(12) -0.012(9) -0.011(9) -0.032(9) F11 0.116(12) 0.076(9) 0.052(10) -0.022(7) 0.026(9) -0.002(8) F12 0.166(11) 0.136(10) 0.135(11) -0.030(8) 0.017(9) -0.014(8) P1 0.029(2) 0.029(3) 0.026(3) 0.006(3) -0.006(2) 0.007(3) P2 0.025(2) 0.051(3) 0.036(3) 0.006(4) -0.004(2) -0.013(3) P3 0.028(3) 0.068(4) 0.020(3) 0.007(3) 0.000(2) 0.001(3) P4 0.031(3) 0.042(3) 0.030(3) 0.001(3) 0.002(2) 0.001(3) P5 0.056(4) 0.077(5) 0.041(4) -0.012(3) 0.000(3) 0.002(3) P6 0.060(5) 0.144(8) 0.085(6) -0.078(6) 0.022(4) -0.050(5) Cl1 0.039(2) 0.039(3) 0.030(3) 0.0003(19) -0.0074(19) 0.0070(19) Cl2 0.037(2) 0.089(4) 0.033(3) 0.020(3) -0.004(2) -0.015(3) Cl3 0.035(2) 0.088(4) 0.026(3) 0.016(3) -0.0102(19) -0.001(3) Cl4 0.035(2) 0.057(3) 0.026(2) -0.002(2) 0.0014(18) 0.000(2) Pt1 0.0325(4) 0.0356(3) 0.0316(4) 0.0035(4) -0.0058(3) -0.0023(4) Pt2 0.0285(3) 0.0508(4) 0.0304(4) 0.0068(4) -0.0023(3) 0.0030(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 C1 N1 1.31(2) . ? C1 N2 1.32(2) . ? C2 C7 1.39(3) . ? C2 C6 1.54(3) . ? C2 N1 1.54(3) . ? C2 C3 1.62(3) . ? C3 C4 1.51(3) . ? C4 C5 1.56(3) . ? C5 C6 1.45(3) . ? C5 N2 1.52(3) . ? C6 C9 1.52(3) . ? C6 C8 1.55(3) . ? C10 N1 1.47(2) . ? C10 C11 1.49(3) . ? C11 C16 1.39(3) . ? C11 C12 1.41(3) . ? C12 C13 1.40(2) . ? C12 P1 1.80(2) . ? C13 C14 1.41(2) . ? C14 C15 1.39(3) . ? C15 C16 1.37(3) . ? C17 C22 1.37(2) . ? C17 C18 1.38(2) . ? C17 P1 1.830(18) . ? C18 C19 1.40(3) . ? C19 C20 1.37(3) . ? C20 C21 1.40(3) . ? C21 C22 1.38(2) . ? C23 C24 1.38(2) . ? C23 C28 1.39(2) . ? C23 P1 1.797(16) . ? C24 C25 1.37(2) . ? C25 C26 1.36(3) . ? C26 C27 1.37(2) . ? C27 C28 1.41(2) . ? C29 N2 1.42(2) . ? C29 C30 1.54(2) . ? C30 C35 1.33(2) . ? C30 C31 1.35(2) . ? C31 C32 1.40(2) . ? C31 P2 1.844(19) . ? C32 C33 1.36(3) . ? C33 C34 1.33(3) . ? C34 C35 1.44(3) . ? C36 C37 1.30(3) . ? C36 C41 1.32(3) . ? C36 P2 1.86(2) . ? C37 C38 1.45(3) . ? C38 C39 1.32(3) . ? C39 C40 1.43(3) . ? C40 C41 1.39(3) . ? C42 C43 1.33(3) . ? C42 C47 1.38(3) . ? C42 P2 1.87(2) . ? C43 C44 1.34(3) . ? C44 C45 1.36(3) . ? C45 C46 1.36(3) . ? C46 C47 1.402(10) . ? C48 N3 1.31(2) . ? C48 N4 1.32(2) . ? C49 C50 1.46(2) . ? C49 C54 1.50(2) . ? C49 N3 1.53(2) . ? C49 C53 1.59(2) . ? C50 C51 1.58(3) . ? C51 C52 1.55(3) . ? C52 N4 1.48(2) . ? C52 C53 1.57(2) . ? C53 C56 1.51(3) . ? C53 C55 1.57(2) . ? C57 N3 1.50(2) . ? C57 C58 1.56(3) . ? C58 C63 1.37(2) . ? C58 C59 1.43(2) . ? C59 C60 1.40(3) . ? C59 P4 1.861(16) . ? C60 C61 1.36(3) . ? C61 C62 1.33(3) . ? C62 C63 1.38(3) . ? C64 C65 1.36(2) . ? C64 C69 1.42(3) . ? C64 P4 1.862(16) . ? C65 C66 1.40(2) . ? C66 C67 1.38(3) . ? C67 C68 1.36(3) . ? C68 C69 1.41(3) . ? C70 C75 1.36(2) . ? C70 C71 1.42(2) . ? C70 P4 1.851(17) . ? C71 C72 1.38(3) . ? C72 C73 1.40(3) . ? C73 C74 1.46(3) . ? C74 C75 1.39(3) . ? C76 C77 1.49(3) . ? C76 N4 1.50(2) . ? C77 C78 1.43(3) . ? C77 C82 1.43(3) . ? C78 C79 1.44(3) . ? C78 P3 1.801(19) . ? C79 C80 1.38(2) . ? C80 C81 1.43(2) . ? C81 C82 1.34(3) . ? C83 C84 1.39(2) . ? C83 C88 1.47(3) . ? C83 P3 1.825(17) . ? C84 C85 1.33(3) . ? C85 C86 1.44(3) . ? C86 C87 1.33(3) . ? C87 C88 1.37(3) . ? C89 C94 1.43(2) . ? C89 C90 1.45(3) . ? C89 P3 1.780(19) . ? C90 C91 1.39(3) . ? C91 C92 1.31(3) . ? C92 C93 1.39(3) . ? C93 C94 1.42(3) . ? C95 N5 1.19(4) . ? C95 C96 1.42(4) . ? C97 N6 1.08(3) . ? C97 C98 1.48(4) . ? C99 N7 1.1500(11) . ? C99 C100 1.4500(11) . ? C101 N8 1.14(3) . ? C101 C102 1.46(4) . ? F1 P5 1.660(17) . ? F2 P5 1.48(2) . ? F3 P5 1.610(13) . ? F4 P5 1.579(17) . ? F5 P5 1.595(15) . ? F6 P5 1.49(2) . ? F7 P6 1.558(19) . ? F8 P6 1.486(17) . ? F9 P6 1.598(18) . ? F10 P6 1.55(2) . ? F11 P6 1.601(16) . ? F12 P6 1.55(2) . ? P1 Pt1 2.334(4) . ? P2 Pt1 2.349(5) . ? P3 Pt2 2.329(5) . ? P4 Pt2 2.315(4) . ? Cl1 Pt1 2.298(4) . ? Cl2 Pt1 2.297(5) . ? Cl3 Pt2 2.310(5) . ? Cl4 Pt2 2.303(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 127.4(15) . . ? C7 C2 C6 120(2) . . ? C7 C2 N1 108.1(19) . . ? C6 C2 N1 107.7(16) . . ? C7 C2 C3 111.7(18) . . ? C6 C2 C3 100.7(16) . . ? N1 C2 C3 107.4(17) . . ? C4 C3 C2 106.0(15) . . ? C3 C4 C5 104.8(18) . . ? C6 C5 N2 103.2(19) . . ? C6 C5 C4 104(2) . . ? N2 C5 C4 108(2) . . ? C5 C6 C9 115(2) . . ? C5 C6 C2 104.0(18) . . ? C9 C6 C2 112.9(17) . . ? C5 C6 C8 109.8(18) . . ? C9 C6 C8 109.2(18) . . ? C2 C6 C8 105.2(19) . . ? N1 C10 C11 114.6(16) . . ? C16 C11 C12 117.6(18) . . ? C16 C11 C10 119.6(18) . . ? C12 C11 C10 122.8(18) . . ? C13 C12 C11 116.8(17) . . ? C13 C12 P1 116.7(14) . . ? C11 C12 P1 126.5(15) . . ? C12 C13 C14 124.4(17) . . ? C15 C14 C13 117.3(19) . . ? C16 C15 C14 118.1(17) . . ? C15 C16 C11 125.5(18) . . ? C22 C17 C18 120.5(17) . . ? C22 C17 P1 118.0(13) . . ? C18 C17 P1 121.3(15) . . ? C17 C18 C19 117.8(18) . . ? C20 C19 C18 121.8(19) . . ? C19 C20 C21 119(2) . . ? C22 C21 C20 118(2) . . ? C17 C22 C21 121.7(18) . . ? C24 C23 C28 117.3(15) . . ? C24 C23 P1 122.9(13) . . ? C28 C23 P1 119.8(12) . . ? C25 C24 C23 122.5(16) . . ? C26 C25 C24 120.6(16) . . ? C25 C26 C27 118.8(17) . . ? C26 C27 C28 121.0(17) . . ? C23 C28 C27 119.4(16) . . ? N2 C29 C30 115.8(18) . . ? C35 C30 C31 123.7(18) . . ? C35 C30 C29 115.6(18) . . ? C31 C30 C29 120.6(17) . . ? C30 C31 C32 115.6(17) . . ? C30 C31 P2 125.7(14) . . ? C32 C31 P2 118.7(14) . . ? C33 C32 C31 124.8(19) . . ? C34 C33 C32 116(2) . . ? C33 C34 C35 122(2) . . ? C30 C35 C34 117.3(19) . . ? C37 C36 C41 120(2) . . ? C37 C36 P2 116.5(17) . . ? C41 C36 P2 123.0(18) . . ? C36 C37 C38 122(2) . . ? C39 C38 C37 117(2) . . ? C38 C39 C40 120(2) . . ? C41 C40 C39 117.8(19) . . ? C36 C41 C40 122(2) . . ? C43 C42 C47 120(2) . . ? C43 C42 P2 119.6(15) . . ? C47 C42 P2 120.3(14) . . ? C42 C43 C44 120(2) . . ? C43 C44 C45 124(2) . . ? C44 C45 C46 117(2) . . ? C45 C46 C47 121(2) . . ? C42 C47 C46 118(2) . . ? N3 C48 N4 120.5(19) . . ? C50 C49 C54 116.1(18) . . ? C50 C49 N3 108.9(14) . . ? C54 C49 N3 112.1(15) . . ? C50 C49 C53 104.0(14) . . ? C54 C49 C53 111.4(15) . . ? N3 C49 C53 103.3(14) . . ? C49 C50 C51 109.5(16) . . ? C52 C51 C50 100.2(17) . . ? N4 C52 C51 111.6(16) . . ? N4 C52 C53 105.1(14) . . ? C51 C52 C53 107.3(15) . . ? C56 C53 C55 110.1(15) . . ? C56 C53 C52 116.5(17) . . ? C55 C53 C52 104.9(14) . . ? C56 C53 C49 118.6(15) . . ? C55 C53 C49 109.3(15) . . ? C52 C53 C49 96.0(13) . . ? N3 C57 C58 111.5(14) . . ? C63 C58 C59 119.6(18) . . ? C63 C58 C57 118.2(16) . . ? C59 C58 C57 121.9(15) . . ? C60 C59 C58 119.1(16) . . ? C60 C59 P4 116.6(13) . . ? C58 C59 P4 123.6(14) . . ? C61 C60 C59 119.6(17) . . ? C62 C61 C60 120(2) . . ? C61 C62 C63 124.2(19) . . ? C58 C63 C62 117.4(19) . . ? C65 C64 C69 119.4(17) . . ? C65 C64 P4 125.1(14) . . ? C69 C64 P4 114.9(15) . . ? C64 C65 C66 121.3(17) . . ? C67 C66 C65 118.9(18) . . ? C68 C67 C66 121(2) . . ? C67 C68 C69 120(2) . . ? C68 C69 C64 118.3(19) . . ? C75 C70 C71 121.1(16) . . ? C75 C70 P4 120.9(15) . . ? C71 C70 P4 117.9(14) . . ? C72 C71 C70 121.0(17) . . ? C71 C72 C73 119(2) . . ? C72 C73 C74 118(2) . . ? C75 C74 C73 120.8(18) . . ? C70 C75 C74 119.2(18) . . ? C77 C76 N4 112.0(15) . . ? C78 C77 C82 114.0(18) . . ? C78 C77 C76 121.8(18) . . ? C82 C77 C76 124.1(18) . . ? C77 C78 C79 120.3(18) . . ? C77 C78 P3 121.2(16) . . ? C79 C78 P3 118.4(15) . . ? C80 C79 C78 119.3(19) . . ? C79 C80 C81 122.8(19) . . ? C82 C81 C80 114.6(19) . . ? C81 C82 C77 128.7(19) . . ? C84 C83 C88 117.8(17) . . ? C84 C83 P3 119.5(13) . . ? C88 C83 P3 122.4(14) . . ? C85 C84 C83 123.8(18) . . ? C84 C85 C86 115(2) . . ? C87 C86 C85 125(2) . . ? C86 C87 C88 119(2) . . ? C87 C88 C83 119(2) . . ? C94 C89 C90 116.4(19) . . ? C94 C89 P3 124.1(16) . . ? C90 C89 P3 119.0(14) . . ? C91 C90 C89 120.8(18) . . ? C92 C91 C90 121(2) . . ? C91 C92 C93 123(2) . . ? C92 C93 C94 120(2) . . ? C93 C94 C89 119(2) . . ? N5 C95 C96 172(6) . . ? N6 C97 C98 177(3) . . ? N7 C99 C100 174(4) . . ? N8 C101 C102 175(3) . . ? C1 N1 C10 115.8(14) . . ? C1 N1 C2 111.9(15) . . ? C10 N1 C2 132.3(16) . . ? C1 N2 C29 124.0(15) . . ? C1 N2 C5 120.4(16) . . ? C29 N2 C5 115.6(16) . . ? C48 N3 C57 116.3(15) . . ? C48 N3 C49 122.7(15) . . ? C57 N3 C49 116.6(14) . . ? C48 N4 C52 119.0(17) . . ? C48 N4 C76 117.1(17) . . ? C52 N4 C76 123.5(13) . . ? C23 P1 C12 106.6(8) . . ? C23 P1 C17 99.4(8) . . ? C12 P1 C17 107.6(8) . . ? C23 P1 Pt1 116.0(6) . . ? C12 P1 Pt1 107.7(6) . . ? C17 P1 Pt1 118.7(6) . . ? C31 P2 C36 104.0(9) . . ? C31 P2 C42 104.8(9) . . ? C36 P2 C42 104.1(9) . . ? C31 P2 Pt1 110.9(6) . . ? C36 P2 Pt1 121.8(7) . . ? C42 P2 Pt1 109.8(6) . . ? C89 P3 C78 105.1(9) . . ? C89 P3 C83 101.2(8) . . ? C78 P3 C83 104.3(8) . . ? C89 P3 Pt2 107.9(6) . . ? C78 P3 Pt2 114.7(6) . . ? C83 P3 Pt2 121.7(5) . . ? C70 P4 C59 106.8(7) . . ? C70 P4 C64 99.4(8) . . ? C59 P4 C64 106.8(8) . . ? C70 P4 Pt2 116.6(6) . . ? C59 P4 Pt2 107.8(5) . . ? C64 P4 Pt2 118.6(5) . . ? F2 P5 F6 90.5(16) . . ? F2 P5 F4 91.5(11) . . ? F6 P5 F4 90.8(11) . . ? F2 P5 F5 175.5(13) . . ? F6 P5 F5 92.9(15) . . ? F4 P5 F5 91.3(9) . . ? F2 P5 F3 93.1(11) . . ? F6 P5 F3 92.3(12) . . ? F4 P5 F3 174.4(10) . . ? F5 P5 F3 83.9(9) . . ? F2 P5 F1 88.7(12) . . ? F6 P5 F1 178.4(14) . . ? F4 P5 F1 87.7(10) . . ? F5 P5 F1 87.9(10) . . ? F3 P5 F1 89.2(9) . . ? F8 P6 F10 89.9(11) . . ? F8 P6 F12 95.7(12) . . ? F10 P6 F12 93.1(13) . . ? F8 P6 F7 92.9(11) . . ? F10 P6 F7 177.2(12) . . ? F12 P6 F7 86.0(12) . . ? F8 P6 F9 85.5(10) . . ? F10 P6 F9 91.1(12) . . ? F12 P6 F9 175.6(13) . . ? F7 P6 F9 89.8(8) . . ? F8 P6 F11 172.2(12) . . ? F10 P6 F11 86.9(12) . . ? F12 P6 F11 91.6(10) . . ? F7 P6 F11 90.5(9) . . ? F9 P6 F11 87.4(9) . . ? Cl2 Pt1 Cl1 177.34(19) . . ? Cl2 Pt1 P1 92.06(17) . . ? Cl1 Pt1 P1 86.85(17) . . ? Cl2 Pt1 P2 86.91(18) . . ? Cl1 Pt1 P2 94.19(18) . . ? P1 Pt1 P2 178.9(2) . . ? Cl4 Pt2 Cl3 174.73(19) . . ? Cl4 Pt2 P4 86.93(15) . . ? Cl3 Pt2 P4 91.73(15) . . ? Cl4 Pt2 P3 94.15(14) . . ? Cl3 Pt2 P3 87.63(14) . . ? P4 Pt2 P3 174.9(3) . . ? _diffrn_measured_fraction_theta_max 0.95 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.95 _refine_diff_density_max 1.514 _refine_diff_density_min -1.057 _refine_diff_density_rms 0.174 data_kjc1139 _database_code_depnum_ccdc_archive 'CCDC 891178' #TrackingRef 'cmpd6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H94 I4 N4 P4 Pd2, 0.27(I), 1.73(P F6) ' _chemical_formula_sum 'C94 H94 F10.40 I4.27 N4 P5.73 Pd2' _chemical_formula_weight 2409.12 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 27.8377(9) _cell_length_b 19.8686(12) _cell_length_c 21.6459(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11972.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8498 _cell_measurement_theta_min 1.19 _cell_measurement_theta_max 20.82 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4735 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6567 _exptl_absorpt_correction_T_max 0.7494 _exptl_absorpt_process_details Denzo/Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31434 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.1194 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 20.82 _reflns_number_total 12167 _reflns_number_gt 8498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement DENZO/SCALEPACK _computing_data_reduction DENZO/SCALEPACK _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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. Difference Fourrier sythesis showed large spaces occupied by diffuse electron density, interpretted as disordered solvent, and hence SQUEEZE was used. The large asymmetric unit combined with the disordered solvent a re accountable for the weak high angle data which were omitted from the refinement. Geometric restraints were applied to the PF6 counterions during refinement to stop distortion of the anions. ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(5) _refine_ls_number_reflns 12167 _refine_ls_number_parameters 1145 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.1023 _refine_ls_wR_factor_ref 0.2961 _refine_ls_wR_factor_gt 0.2721 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.35094(5) 0.21433(8) 0.23711(9) 0.0344(5) Uani 1 1 d . . 1 Pd2 Pd 0.72593(5) 0.25572(8) 0.26328(9) 0.0327(5) Uani 1 1 d . . 1 C1 C 0.2783(8) 0.2301(11) 0.3556(10) 0.033(6) Uani 1 1 d . . 1 C2 C 0.2500(9) 0.1820(14) 0.3845(12) 0.054(7) Uani 1 1 d . . 1 H2 H 0.2646 0.1447 0.4045 0.065 Uiso 1 1 calc R . 1 C3 C 0.2002(9) 0.1886(13) 0.3842(11) 0.049(7) Uani 1 1 d . . 1 H3 H 0.1808 0.1557 0.4040 0.058 Uiso 1 1 calc R . 1 C4 C 0.1789(10) 0.2432(15) 0.3549(13) 0.061(8) Uani 1 1 d . . 1 H4 H 0.1449 0.2477 0.3547 0.073 Uiso 1 1 calc R . 1 C5 C 0.2073(9) 0.2912(15) 0.3258(12) 0.060(8) Uani 1 1 d . . 1 H5 H 0.1927 0.3285 0.3057 0.072 Uiso 1 1 calc R . 1 C6 C 0.2569(9) 0.2847(14) 0.3261(12) 0.053(7) Uani 1 1 d . . 1 H6 H 0.2763 0.3176 0.3063 0.063 Uiso 1 1 calc R . 1 C7 C 0.3627(6) 0.1488(10) 0.3920(10) 0.023(5) Uani 1 1 d . . 1 C8 C 0.3898(7) 0.0966(13) 0.3676(11) 0.039(6) Uani 1 1 d . . 1 H8 H 0.3960 0.0948 0.3244 0.046 Uiso 1 1 calc R . 1 C9 C 0.4080(7) 0.0467(12) 0.4065(11) 0.034(6) Uani 1 1 d . . 1 H9 H 0.4266 0.0110 0.3899 0.041 Uiso 1 1 calc R . 1 C10 C 0.3990(9) 0.0495(14) 0.4693(13) 0.052(8) Uani 1 1 d . . 1 H10 H 0.4114 0.0155 0.4958 0.063 Uiso 1 1 calc R . 1 C11 C 0.3718(8) 0.1017(12) 0.4940(11) 0.039(6) Uani 1 1 d . . 1 H11 H 0.3655 0.1034 0.5371 0.047 Uiso 1 1 calc R . 1 C12 C 0.3540(9) 0.1514(14) 0.4552(12) 0.047(7) Uani 1 1 d . . 1 H12 H 0.3357 0.1874 0.4719 0.057 Uiso 1 1 calc R . 1 C13 C 0.3684(8) 0.2942(13) 0.3861(11) 0.047(7) Uani 1 1 d . . 1 C14 C 0.4171(7) 0.3088(10) 0.3840(9) 0.023(5) Uani 1 1 d . . 1 C15 C 0.4354(9) 0.3627(12) 0.4173(11) 0.044(6) Uani 1 1 d . . 1 H15 H 0.4688 0.3725 0.4157 0.053 Uiso 1 1 calc R . 1 C16 C 0.4052(9) 0.4022(14) 0.4530(12) 0.055(7) Uani 1 1 d . . 1 H16 H 0.4179 0.4388 0.4760 0.065 Uiso 1 1 calc R . 1 C17 C 0.3563(9) 0.3882(13) 0.4551(11) 0.047(7) Uani 1 1 d . . 1 H17 H 0.3355 0.4155 0.4792 0.057 Uiso 1 1 calc R . 1 C18 C 0.3379(7) 0.3341(12) 0.4218(10) 0.035(6) Uani 1 1 d . . 1 H18 H 0.3045 0.3244 0.4234 0.042 Uiso 1 1 calc R . 1 C19 C 0.4531(7) 0.2678(11) 0.3469(10) 0.037(6) Uani 1 1 d . . 1 H19A H 0.4370 0.2278 0.3292 0.045 Uiso 1 1 calc R . 1 H19B H 0.4657 0.2953 0.3124 0.045 Uiso 1 1 calc R . 1 C20 C 0.5402(7) 0.2740(10) 0.3753(9) 0.022(5) Uani 1 1 d . . 1 H20 H 0.5446 0.3038 0.3414 0.026 Uiso 1 1 calc R . 1 C21 C 0.5703(8) 0.2047(13) 0.4560(11) 0.042(7) Uani 1 1 d . . 1 C22 C 0.5646(9) 0.1326(14) 0.4222(14) 0.063(8) Uani 1 1 d . . 1 H22A H 0.5847 0.1307 0.3845 0.076 Uiso 1 1 calc R . 1 H22B H 0.5744 0.0957 0.4502 0.076 Uiso 1 1 calc R . 1 C23 C 0.5137(7) 0.1269(11) 0.4064(10) 0.029(5) Uani 1 1 d . . 1 H23A H 0.4994 0.0868 0.4264 0.035 Uiso 1 1 calc R . 1 H23B H 0.5095 0.1229 0.3611 0.035 Uiso 1 1 calc R . 1 C24 C 0.4890(9) 0.1947(13) 0.4317(12) 0.049(7) Uani 1 1 d . . 1 H24 H 0.4548 0.1874 0.4444 0.059 Uiso 1 1 calc R . 1 C25 C 0.5213(8) 0.2090(13) 0.4865(11) 0.046(7) Uani 1 1 d . . 1 C26 C 0.6136(7) 0.2063(12) 0.5054(11) 0.045(6) Uani 1 1 d . . 1 H26A H 0.6444 0.2034 0.4837 0.067 Uiso 1 1 calc R . 1 H26B H 0.6104 0.1681 0.5338 0.067 Uiso 1 1 calc R . 1 H26C H 0.6122 0.2484 0.5289 0.067 Uiso 1 1 calc R . 1 C27 C 0.5110(11) 0.1555(18) 0.5402(15) 0.092(10) Uani 1 1 d . . 1 H27A H 0.5319 0.1648 0.5755 0.138 Uiso 1 1 calc R . 1 H27B H 0.5174 0.1100 0.5248 0.138 Uiso 1 1 calc R . 1 H27C H 0.4773 0.1588 0.5531 0.138 Uiso 1 1 calc R . 1 C28 C 0.5104(9) 0.2830(13) 0.5161(12) 0.055(7) Uani 1 1 d . . 1 H28A H 0.5318 0.2908 0.5513 0.083 Uiso 1 1 calc R . 1 H28B H 0.4769 0.2850 0.5301 0.083 Uiso 1 1 calc R . 1 H28C H 0.5159 0.3178 0.4848 0.083 Uiso 1 1 calc R . 1 C29 C 0.6259(7) 0.2689(12) 0.3830(10) 0.036(6) Uani 1 1 d . . 1 H29A H 0.6225 0.2858 0.3402 0.043 Uiso 1 1 calc R . 1 H29B H 0.6436 0.2257 0.3816 0.043 Uiso 1 1 calc R . 1 C30 C 0.6545(8) 0.3213(12) 0.4229(11) 0.041(6) Uani 1 1 d . . 1 C31 C 0.7044(7) 0.3194(10) 0.4198(9) 0.026(5) Uani 1 1 d . . 1 C32 C 0.7315(8) 0.3687(12) 0.4493(10) 0.036(6) Uani 1 1 d . . 1 H32 H 0.7656 0.3674 0.4472 0.044 Uiso 1 1 calc R . 1 C33 C 0.7088(8) 0.4199(12) 0.4816(10) 0.039(6) Uani 1 1 d . . 1 H33 H 0.7273 0.4536 0.5017 0.046 Uiso 1 1 calc R . 1 C34 C 0.6590(9) 0.4220(14) 0.4847(12) 0.053(7) Uani 1 1 d . . 1 H34 H 0.6434 0.4571 0.5069 0.064 Uiso 1 1 calc R . 1 C35 C 0.6319(8) 0.3728(12) 0.4554(10) 0.035(6) Uani 1 1 d . . 1 H35 H 0.5979 0.3743 0.4575 0.041 Uiso 1 1 calc R . 1 C36 C 0.7245(8) 0.1784(12) 0.4145(11) 0.039(6) Uani 1 1 d . . 1 C37 C 0.7047(7) 0.1228(11) 0.3845(10) 0.028(5) Uani 1 1 d . . 1 H37 H 0.6981 0.1247 0.3415 0.034 Uiso 1 1 calc R . 1 C38 C 0.6947(8) 0.0645(13) 0.4175(11) 0.041(6) Uani 1 1 d . . 1 H38 H 0.6814 0.0266 0.3971 0.049 Uiso 1 1 calc R . 1 C39 C 0.7042(8) 0.0618(14) 0.4806(12) 0.048(7) Uani 1 1 d . . 1 H39 H 0.6972 0.0219 0.5031 0.058 Uiso 1 1 calc R . 1 C40 C 0.7237(9) 0.1171(15) 0.5107(14) 0.063(8) Uani 1 1 d . . 1 H40 H 0.7303 0.1151 0.5538 0.076 Uiso 1 1 calc R . 1 C41 C 0.7337(9) 0.1761(15) 0.4772(13) 0.060(8) Uani 1 1 d . . 1 H41 H 0.7467 0.2143 0.4976 0.072 Uiso 1 1 calc R . 1 C42 C 0.8003(9) 0.2708(14) 0.3762(11) 0.047(7) Uani 1 1 d . . 1 C43 C 0.8299(9) 0.2212(14) 0.4005(11) 0.051(7) Uani 1 1 d . . 1 H43 H 0.8163 0.1820 0.4184 0.061 Uiso 1 1 calc R . 1 C44 C 0.8796(10) 0.2288(16) 0.3986(13) 0.066(8) Uani 1 1 d . . 1 H44 H 0.8998 0.1948 0.4153 0.079 Uiso 1 1 calc R . 1 C45 C 0.8995(11) 0.2861(19) 0.3724(15) 0.082(10) Uani 1 1 d . . 1 H45 H 0.9334 0.2913 0.3710 0.099 Uiso 1 1 calc R . 1 C46 C 0.8701(9) 0.3358(15) 0.3481(12) 0.054(7) Uani 1 1 d . . 1 H46 H 0.8839 0.3749 0.3302 0.065 Uiso 1 1 calc R . 1 C47 C 0.8203(10) 0.3283(16) 0.3499(13) 0.068(8) Uani 1 1 d . . 1 H47 H 0.8001 0.3623 0.3333 0.082 Uiso 1 1 calc R . 1 C48 C 0.7968(7) 0.2799(11) 0.1495(10) 0.031(5) Uani 1 1 d . . 1 C49 C 0.8161(9) 0.3346(14) 0.1806(12) 0.055(7) Uani 1 1 d . . 1 H49 H 0.7956 0.3634 0.2037 0.066 Uiso 1 1 calc R . 1 C50 C 0.8649(9) 0.3477(14) 0.1784(12) 0.051(7) Uani 1 1 d . . 1 H50 H 0.8779 0.3851 0.2000 0.061 Uiso 1 1 calc R . 1 C51 C 0.8949(10) 0.3057(15) 0.1442(13) 0.065(8) Uani 1 1 d . . 1 H51 H 0.9284 0.3146 0.1424 0.078 Uiso 1 1 calc R . 1 C52 C 0.8759(8) 0.2509(13) 0.1128(11) 0.040(6) Uani 1 1 d . . 1 H52 H 0.8963 0.2223 0.0894 0.048 Uiso 1 1 calc R . 1 C53 C 0.8268(8) 0.2379(13) 0.1156(11) 0.041(6) Uani 1 1 d . . 1 H53 H 0.8137 0.2003 0.0944 0.049 Uiso 1 1 calc R . 1 C54 C 0.7193(8) 0.1881(13) 0.1083(11) 0.042(7) Uani 1 1 d . . 1 C55 C 0.7233(8) 0.1953(13) 0.0447(11) 0.040(6) Uani 1 1 d . . 1 H55 H 0.7318 0.2376 0.0274 0.048 Uiso 1 1 calc R . 1 C56 C 0.7148(7) 0.1403(13) 0.0066(12) 0.043(6) Uani 1 1 d . . 1 H56 H 0.7175 0.1450 -0.0370 0.051 Uiso 1 1 calc R . 1 C57 C 0.7024(7) 0.0783(12) 0.0321(11) 0.034(6) Uani 1 1 d . . 1 H57 H 0.6965 0.0408 0.0059 0.041 Uiso 1 1 calc R . 1 C58 C 0.6987(8) 0.0713(13) 0.0958(12) 0.045(7) Uani 1 1 d . . 1 H58 H 0.6905 0.0290 0.1133 0.054 Uiso 1 1 calc R . 1 C59 C 0.7071(7) 0.1263(13) 0.1338(12) 0.042(6) Uani 1 1 d . . 1 H59 H 0.7044 0.1216 0.1773 0.051 Uiso 1 1 calc R . 1 C60 C 0.7022(7) 0.3316(11) 0.1150(9) 0.029(5) Uani 1 1 d . . 1 C61 C 0.6524(8) 0.3347(12) 0.1140(11) 0.040(6) Uani 1 1 d . . 1 C62 C 0.6294(10) 0.3849(15) 0.0803(13) 0.063(8) Uani 1 1 d . . 1 H62 H 0.5953 0.3867 0.0794 0.075 Uiso 1 1 calc R . 1 C63 C 0.6560(10) 0.4322(15) 0.0482(13) 0.059(8) Uani 1 1 d . . 1 H63 H 0.6402 0.4667 0.0256 0.071 Uiso 1 1 calc R . 1 C64 C 0.7061(11) 0.4293(17) 0.0490(14) 0.077(9) Uani 1 1 d . . 1 H64 H 0.7244 0.4616 0.0268 0.092 Uiso 1 1 calc R . 1 C65 C 0.7292(11) 0.3787(15) 0.0825(13) 0.064(8) Uani 1 1 d . . 1 H65 H 0.7633 0.3765 0.0832 0.077 Uiso 1 1 calc R . 1 C66 C 0.6186(7) 0.2868(11) 0.1513(10) 0.031(5) Uani 1 1 d . . 1 H66A H 0.6376 0.2495 0.1691 0.037 Uiso 1 1 calc R . 1 H66B H 0.6036 0.3120 0.1858 0.037 Uiso 1 1 calc R . 1 C67 C 0.5327(8) 0.2713(11) 0.1209(11) 0.032(6) Uani 1 1 d . . 1 H67 H 0.5253 0.3000 0.1547 0.038 Uiso 1 1 calc R . 1 C68 C 0.5086(8) 0.1970(13) 0.0464(11) 0.046(7) Uani 1 1 d . . 1 C69 C 0.5222(6) 0.1300(10) 0.0755(10) 0.026(5) Uani 1 1 d . . 1 H69A H 0.5160 0.0923 0.0466 0.031 Uiso 1 1 calc R . 1 H69B H 0.5039 0.1223 0.1140 0.031 Uiso 1 1 calc R . 1 C70 C 0.5799(6) 0.1373(10) 0.0899(9) 0.017(5) Uani 1 1 d . . 1 H70A H 0.5867 0.1354 0.1347 0.021 Uiso 1 1 calc R . 1 H70B H 0.5989 0.1022 0.0683 0.021 Uiso 1 1 calc R . 1 C71 C 0.5897(7) 0.2080(12) 0.0630(10) 0.033(6) Uani 1 1 d . . 1 H71 H 0.6245 0.2112 0.0518 0.040 Uiso 1 1 calc R . 1 C72 C 0.5600(7) 0.2174(13) 0.0049(11) 0.038(6) Uani 1 1 d . . 1 C73 C 0.4664(7) 0.1858(12) -0.0018(11) 0.045(6) Uani 1 1 d . . 1 H73A H 0.4577 0.2290 -0.0206 0.067 Uiso 1 1 calc R . 1 H73B H 0.4384 0.1669 0.0194 0.067 Uiso 1 1 calc R . 1 H73C H 0.4770 0.1546 -0.0341 0.067 Uiso 1 1 calc R . 1 C74 C 0.5710(8) 0.1706(14) -0.0440(12) 0.056(7) Uani 1 1 d . . 1 H74A H 0.5738 0.1252 -0.0268 0.085 Uiso 1 1 calc R . 1 H74B H 0.6013 0.1835 -0.0635 0.085 Uiso 1 1 calc R . 1 H74C H 0.5452 0.1714 -0.0748 0.085 Uiso 1 1 calc R . 1 C75 C 0.5547(8) 0.2894(13) -0.0167(12) 0.055(7) Uani 1 1 d . . 1 H75A H 0.5473 0.3183 0.0187 0.083 Uiso 1 1 calc R . 1 H75B H 0.5286 0.2922 -0.0470 0.083 Uiso 1 1 calc R . 1 H75C H 0.5848 0.3042 -0.0358 0.083 Uiso 1 1 calc R . 1 C76 C 0.4505(7) 0.2516(12) 0.1222(10) 0.031(5) Uani 1 1 d . . 1 H76A H 0.4527 0.2721 0.1638 0.038 Uiso 1 1 calc R . 1 H76B H 0.4381 0.2051 0.1269 0.038 Uiso 1 1 calc R . 1 C77 C 0.4138(10) 0.2954(15) 0.0791(13) 0.065(8) Uani 1 1 d . . 1 C78 C 0.3645(7) 0.2842(12) 0.0830(10) 0.036(6) Uani 1 1 d . . 1 C79 C 0.3329(9) 0.3248(13) 0.0503(11) 0.047(7) Uani 1 1 d . . 1 H79 H 0.2993 0.3171 0.0530 0.056 Uiso 1 1 calc R . 1 C80 C 0.3504(8) 0.3765(11) 0.0136(10) 0.034(6) Uani 1 1 d . . 1 H80 H 0.3287 0.4042 -0.0087 0.041 Uiso 1 1 calc R . 1 C81 C 0.3995(10) 0.3879(15) 0.0096(13) 0.064(8) Uani 1 1 d . . 1 H81 H 0.4115 0.4235 -0.0154 0.076 Uiso 1 1 calc R . 1 C82 C 0.4313(8) 0.3471(11) 0.0424(10) 0.032(6) Uani 1 1 d . . 1 H82 H 0.4649 0.3546 0.0395 0.039 Uiso 1 1 calc R . 1 C83 C 0.3582(8) 0.1412(13) 0.0843(12) 0.044(7) Uani 1 1 d . . 1 C84 C 0.3450(8) 0.1363(13) 0.0228(12) 0.049(7) Uani 1 1 d . . 1 H84 H 0.3244 0.1692 0.0050 0.059 Uiso 1 1 calc R . 1 C85 C 0.3619(7) 0.0830(12) -0.0128(11) 0.039(6) Uani 1 1 d . . 1 H85 H 0.3527 0.0794 -0.0550 0.046 Uiso 1 1 calc R . 1 C86 C 0.3922(7) 0.0350(12) 0.0132(11) 0.037(6) Uani 1 1 d . . 1 H86 H 0.4039 -0.0012 -0.0113 0.044 Uiso 1 1 calc R . 1 C87 C 0.4053(7) 0.0401(12) 0.0751(10) 0.031(6) Uani 1 1 d . . 1 H87 H 0.4258 0.0072 0.0929 0.038 Uiso 1 1 calc R . 1 C88 C 0.3884(7) 0.0932(12) 0.1106(10) 0.032(6) Uani 1 1 d . . 1 H88 H 0.3975 0.0967 0.1528 0.038 Uiso 1 1 calc R . 1 C89 C 0.2737(8) 0.2203(12) 0.1228(10) 0.035(6) Uani 1 1 d . . 1 C90 C 0.2528(9) 0.2736(14) 0.1541(12) 0.053(7) Uani 1 1 d . . 1 H90 H 0.2725 0.3062 0.1740 0.064 Uiso 1 1 calc R . 1 C91 C 0.2029(9) 0.2795(14) 0.1566(12) 0.056(7) Uani 1 1 d . . 1 H91 H 0.1885 0.3158 0.1783 0.067 Uiso 1 1 calc R . 1 C92 C 0.1742(10) 0.2319(15) 0.1272(13) 0.064(8) Uani 1 1 d . . 1 H92 H 0.1402 0.2359 0.1285 0.076 Uiso 1 1 calc R . 1 C93 C 0.1952(9) 0.1784(13) 0.0958(11) 0.048(7) Uani 1 1 d . . 1 H93 H 0.1755 0.1458 0.0760 0.058 Uiso 1 1 calc R . 1 C94 C 0.2451(7) 0.1726(11) 0.0934(9) 0.025(5) Uani 1 1 d . . 1 H94 H 0.2594 0.1362 0.0718 0.030 Uiso 1 1 calc R . 1 N1 N 0.4934(7) 0.2461(11) 0.3876(9) 0.048(5) Uani 1 1 d . . 1 N2 N 0.5772(6) 0.2582(9) 0.4112(8) 0.029(4) Uani 1 1 d . . 1 N3 N 0.5010(7) 0.2497(10) 0.0922(8) 0.033(5) Uani 1 1 d . . 1 N4 N 0.5792(6) 0.2582(9) 0.1093(8) 0.034(5) Uani 1 1 d . . 1 P1 P 0.34310(19) 0.2196(3) 0.3437(3) 0.0390(16) Uani 1 1 d . . 1 P2 P 0.33930(18) 0.2143(3) 0.1305(3) 0.0341(16) Uani 1 1 d . . 1 P3 P 0.73638(18) 0.2549(3) 0.3716(3) 0.0387(16) Uani 1 1 d . . 1 P4 P 0.73292(18) 0.2626(3) 0.1578(3) 0.0349(15) Uani 1 1 d . . 1 I1 I 0.30766(5) 0.09661(8) 0.24038(8) 0.0537(5) Uani 1 1 d . . 1 I2 I 0.37553(6) 0.34004(10) 0.23247(12) 0.0815(7) Uani 1 1 d . . 1 I3 I 0.68763(7) 0.37306(11) 0.26746(12) 0.0908(7) Uani 1 1 d . . 1 I4 I 0.77887(9) 0.15222(15) 0.25983(14) 0.1250(10) Uani 1 1 d . . 1 F1 F 0.6588(10) 0.9693(10) 0.7084(13) 0.131(16) Uani 0.472(11) 1 d PD . 1 F2 F 0.6879(7) 1.0485(14) 0.6490(12) 0.135(16) Uani 0.472(11) 1 d PD . 1 F3 F 0.6511(8) 1.0756(11) 0.7343(9) 0.080(9) Uani 0.472(11) 1 d PD . 1 F4 F 0.6143(10) 1.0885(14) 0.6451(12) 0.126(16) Uani 0.472(11) 1 d PD . 1 F5 F 0.6247(10) 0.9933(16) 0.6191(10) 0.154(19) Uani 0.472(11) 1 d PD . 1 F6 F 0.5884(6) 1.0190(16) 0.7046(13) 0.136(17) Uani 0.472(11) 1 d PD . 1 P5 P 0.6388(5) 1.0317(8) 0.6779(8) 0.092(7) Uani 0.472(11) 1 d PD . 1 P6 P 0.5000 0.0000 0.2436(9) 0.104(6) Uani 0.732(8) 2 d SPD . 1 F7 F 0.4659(9) -0.0307(11) 0.1960(9) 0.152(12) Uani 0.732(8) 1 d PD . 1 F8 F 0.4683(9) -0.0235(11) 0.2967(9) 0.134(11) Uani 0.732(8) 1 d PD . 1 F9 F 0.4743(7) 0.0675(6) 0.2404(12) 0.124(10) Uani 0.732(8) 1 d PD . 1 I5 I 0.4727(3) 0.1324(5) 0.2346(4) 0.088(4) Uani 0.268(7) 1 d P . 2 F14 F 0.4188(6) 0.7978(10) 0.7886(7) 0.127(8) Uani 0.894(11) 1 d PD . 1 F11 F 0.4393(6) 0.8329(9) 0.6959(7) 0.126(8) Uani 0.894(11) 1 d PD . 1 F12 F 0.5053(5) 0.7725(9) 0.7039(7) 0.129(8) Uani 0.894(11) 1 d PD . 1 F13 F 0.4809(7) 0.7464(11) 0.7972(7) 0.133(9) Uani 0.894(11) 1 d PD . 1 F15 F 0.4879(6) 0.8462(9) 0.7747(8) 0.147(9) Uani 0.894(11) 1 d PD . 1 F10 F 0.4357(6) 0.7249(8) 0.7166(8) 0.175(12) Uani 0.894(11) 1 d PD . 1 P7 P 0.4610(4) 0.7873(6) 0.7441(6) 0.170(7) Uani 0.894(11) 1 d PD . 1 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 0.0204(8) 0.0418(10) 0.0408(10) 0.0046(10) 0.0033(8) -0.0019(6) Pd2 0.0175(8) 0.0407(10) 0.0400(10) 0.0029(9) -0.0057(8) -0.0003(6) C1 0.032(13) 0.035(16) 0.033(15) 0.000(12) 0.001(11) 0.000(12) C2 0.052(19) 0.06(2) 0.056(19) 0.001(15) 0.001(13) 0.001(14) C3 0.048(18) 0.049(19) 0.049(17) -0.002(14) -0.001(12) -0.001(13) C4 0.061(18) 0.06(2) 0.06(2) -0.002(17) 0.000(14) 0.002(17) C5 0.06(2) 0.06(2) 0.060(19) -0.001(16) 0.003(13) -0.002(15) C6 0.053(19) 0.051(18) 0.055(18) -0.001(15) 0.001(12) 0.000(14) C7 0.024(12) 0.023(14) 0.023(15) 0.000(10) 0.000(9) 0.000(10) C8 0.039(13) 0.039(17) 0.038(15) 0.000(14) 0.000(11) -0.002(12) C9 0.036(14) 0.032(16) 0.034(17) -0.001(12) 0.000(11) 0.000(11) C10 0.052(17) 0.05(2) 0.05(2) -0.001(15) 0.002(13) 0.000(15) C11 0.038(13) 0.040(16) 0.039(15) 0.000(14) -0.001(11) 0.001(13) C12 0.047(15) 0.046(19) 0.05(2) -0.001(14) 0.001(13) 0.000(13) C13 0.045(18) 0.047(18) 0.048(17) 0.000(14) -0.001(12) 0.000(13) C14 0.024(13) 0.023(14) 0.023(13) 0.001(10) 0.000(9) 0.001(10) C15 0.044(15) 0.042(17) 0.046(16) 0.001(14) -0.001(13) 0.000(13) C16 0.053(19) 0.054(19) 0.057(18) -0.002(15) 0.000(13) 0.000(15) C17 0.049(18) 0.046(18) 0.047(17) -0.001(14) 0.001(12) 0.002(13) C18 0.033(13) 0.036(16) 0.035(15) 0.000(13) 0.000(11) 0.002(12) C19 0.037(14) 0.037(16) 0.039(15) 0.001(12) -0.002(11) -0.001(11) C20 0.021(13) 0.022(14) 0.023(13) 0.000(10) 0.001(10) -0.002(10) C21 0.040(15) 0.047(18) 0.039(16) -0.001(13) 0.000(11) 0.002(12) C22 0.06(2) 0.06(2) 0.06(2) 0.001(16) 0.001(15) 0.001(15) C23 0.029(13) 0.029(14) 0.029(14) -0.001(11) 0.001(9) 0.000(10) C24 0.048(16) 0.049(19) 0.050(17) 0.000(15) 0.002(13) 0.000(13) C25 0.046(15) 0.047(17) 0.045(16) 0.000(14) -0.001(12) -0.001(12) C26 0.046(14) 0.044(16) 0.043(16) 0.000(13) 0.000(11) 0.000(11) C27 0.10(2) 0.09(3) 0.09(3) 0.00(2) -0.001(19) 0.00(2) C28 0.054(16) 0.054(18) 0.057(18) 0.000(15) 0.000(13) 0.000(13) C29 0.036(14) 0.036(16) 0.036(15) -0.001(11) 0.000(11) 0.000(11) C30 0.040(16) 0.040(16) 0.042(16) -0.002(13) 0.001(11) 0.000(12) C31 0.026(14) 0.026(14) 0.026(13) 0.001(10) 0.000(9) 0.000(10) C32 0.035(13) 0.037(16) 0.038(15) -0.002(12) 0.000(11) -0.002(12) C33 0.039(16) 0.038(17) 0.039(15) -0.001(12) 0.000(11) 0.000(12) C34 0.052(19) 0.053(19) 0.054(19) 0.000(15) 0.001(13) -0.001(14) C35 0.033(13) 0.035(15) 0.035(15) 0.001(12) -0.002(11) 0.000(12) C36 0.040(14) 0.041(17) 0.036(17) 0.002(13) -0.001(12) 0.001(12) C37 0.029(12) 0.027(15) 0.029(14) -0.001(12) 0.001(10) -0.001(11) C38 0.039(14) 0.044(18) 0.039(17) -0.001(13) 0.000(12) -0.001(12) C39 0.048(16) 0.045(18) 0.051(19) 0.001(14) 0.001(13) 0.000(13) C40 0.064(17) 0.06(2) 0.06(2) 0.002(18) 0.000(15) 0.002(16) C41 0.058(18) 0.06(2) 0.06(2) -0.001(17) 0.000(14) 0.000(15) C42 0.046(15) 0.049(19) 0.047(17) -0.001(14) 0.000(12) -0.001(14) C43 0.053(18) 0.050(18) 0.051(18) -0.001(15) -0.001(13) 0.000(14) C44 0.06(2) 0.07(2) 0.07(2) 0.000(17) -0.002(15) -0.001(16) C45 0.08(2) 0.08(3) 0.09(3) 0.00(2) -0.002(18) 0.00(2) C46 0.053(18) 0.056(19) 0.052(19) -0.001(15) 0.002(13) -0.002(15) C47 0.07(2) 0.07(2) 0.07(2) 0.001(17) 0.002(15) -0.001(17) C48 0.029(13) 0.031(14) 0.032(14) 0.002(12) -0.001(10) -0.001(11) C49 0.053(18) 0.055(19) 0.056(18) 0.001(15) -0.001(13) 0.000(15) C50 0.048(17) 0.051(18) 0.053(18) 0.001(14) -0.001(12) 0.000(14) C51 0.064(18) 0.06(2) 0.07(2) 0.002(17) -0.002(15) 0.000(17) C52 0.040(16) 0.039(17) 0.041(16) -0.001(13) 0.000(11) 0.000(12) C53 0.039(16) 0.043(17) 0.042(16) 0.000(12) 0.001(11) -0.001(12) C54 0.039(14) 0.043(19) 0.045(18) -0.001(13) -0.001(12) 0.000(12) C55 0.040(14) 0.040(18) 0.041(17) 0.000(13) 0.000(12) -0.001(12) C56 0.041(14) 0.045(18) 0.042(16) 0.000(14) 0.001(11) -0.001(12) C57 0.034(14) 0.033(17) 0.035(17) -0.001(12) -0.001(10) -0.001(11) C58 0.044(15) 0.045(18) 0.046(19) 0.000(14) 0.000(12) -0.001(13) C59 0.041(14) 0.042(18) 0.044(16) 0.000(14) 0.000(11) -0.002(12) C60 0.028(14) 0.029(14) 0.030(14) 0.000(11) 0.000(10) 0.001(11) C61 0.041(16) 0.039(16) 0.039(16) 0.001(13) -0.002(11) -0.001(12) C62 0.061(18) 0.06(2) 0.06(2) 0.001(17) 0.001(15) 0.000(17) C63 0.06(2) 0.06(2) 0.06(2) 0.002(16) 0.000(14) -0.002(15) C64 0.07(3) 0.08(3) 0.08(2) 0.001(19) 0.000(17) -0.001(18) C65 0.064(18) 0.06(2) 0.06(2) 0.001(17) 0.000(16) 0.002(17) C66 0.030(12) 0.032(14) 0.031(14) 0.001(11) 0.000(10) -0.001(10) C67 0.032(16) 0.029(16) 0.034(15) 0.000(11) 0.000(12) 0.000(12) C68 0.044(15) 0.049(19) 0.047(17) 0.002(14) -0.001(12) -0.001(13) C69 0.027(12) 0.025(13) 0.026(13) 0.000(10) 0.000(9) 0.000(10) C70 0.016(10) 0.019(13) 0.016(12) 0.001(9) 0.001(8) 0.000(8) C71 0.031(13) 0.034(15) 0.034(15) 0.000(12) 0.000(10) 0.002(11) C72 0.035(13) 0.039(16) 0.040(16) 0.003(13) -0.001(11) -0.001(11) C73 0.043(14) 0.046(16) 0.044(16) -0.001(13) 0.000(11) 0.000(11) C74 0.056(16) 0.059(19) 0.055(19) -0.003(16) 0.001(13) 0.000(14) C75 0.054(15) 0.06(2) 0.055(18) 0.002(15) 0.000(12) -0.002(13) C76 0.030(13) 0.031(14) 0.032(14) -0.001(11) 0.000(10) 0.001(10) C77 0.06(2) 0.06(2) 0.07(2) 0.001(18) 0.002(15) -0.001(16) C78 0.034(16) 0.036(15) 0.037(15) 0.001(12) 0.000(11) 0.001(12) C79 0.046(15) 0.046(18) 0.048(18) 0.000(15) 0.000(12) -0.002(13) C80 0.033(15) 0.032(15) 0.036(15) -0.001(12) -0.001(11) -0.001(11) C81 0.06(2) 0.06(2) 0.07(2) -0.001(16) -0.001(15) -0.001(15) C82 0.031(12) 0.032(15) 0.033(15) 0.002(12) 0.000(11) 0.000(11) C83 0.042(15) 0.046(18) 0.044(19) 0.000(13) 0.001(13) -0.002(13) C84 0.049(15) 0.050(19) 0.048(19) 0.001(14) -0.001(13) -0.001(13) C85 0.039(14) 0.039(16) 0.039(15) -0.001(13) 0.000(11) -0.002(12) C86 0.037(13) 0.035(16) 0.038(17) -0.001(12) 0.001(11) -0.001(11) C87 0.031(13) 0.031(16) 0.032(16) 0.001(12) 0.001(10) -0.001(11) C88 0.030(13) 0.032(16) 0.034(15) 0.000(13) 0.000(10) 0.001(12) C89 0.035(13) 0.036(16) 0.034(15) 0.001(12) 0.000(11) 0.003(12) C90 0.052(19) 0.05(2) 0.053(18) 0.002(15) 0.000(12) 0.000(14) C91 0.05(2) 0.06(2) 0.056(18) 0.000(15) 0.000(13) 0.000(15) C92 0.059(18) 0.07(2) 0.06(2) 0.002(17) 0.000(15) 0.000(17) C93 0.047(18) 0.048(18) 0.049(17) -0.001(14) 0.000(12) 0.001(13) C94 0.025(13) 0.025(13) 0.024(13) -0.001(10) 0.000(9) -0.002(10) N1 0.049(14) 0.046(14) 0.049(14) 0.000(12) 0.000(10) 0.000(11) N2 0.028(11) 0.030(12) 0.030(11) 0.000(9) -0.001(9) 0.001(9) N3 0.032(11) 0.032(12) 0.034(12) 0.000(10) 0.000(10) 0.000(10) N4 0.032(13) 0.035(13) 0.035(12) 0.000(10) 0.000(8) -0.001(9) P1 0.027(3) 0.047(4) 0.043(4) 0.000(3) 0.004(3) -0.001(3) P2 0.019(3) 0.051(4) 0.032(4) 0.014(3) 0.002(2) 0.000(3) P3 0.016(3) 0.050(4) 0.050(4) 0.004(3) -0.011(3) -0.004(3) P4 0.020(3) 0.037(4) 0.048(4) 0.007(3) -0.001(3) -0.002(3) I1 0.0484(9) 0.0634(11) 0.0493(10) 0.0034(9) 0.0026(8) -0.0117(7) I2 0.0671(12) 0.0819(14) 0.0957(16) 0.0037(14) 0.0080(11) 0.0010(9) I3 0.0767(13) 0.0929(16) 0.1029(17) 0.0084(15) -0.0003(13) 0.0046(10) I4 0.1110(18) 0.150(2) 0.114(2) 0.004(2) -0.0053(17) 0.0045(15) F1 0.13(4) 0.13(4) 0.13(4) 0.00(3) 0.00(3) 0.00(3) F2 0.13(4) 0.14(4) 0.14(4) 0.00(3) 0.00(3) 0.00(3) F3 0.08(2) 0.08(2) 0.08(2) 0.00(2) -0.002(19) 0.001(16) F4 0.12(3) 0.12(4) 0.13(4) 0.00(3) 0.00(3) 0.00(3) F5 0.16(4) 0.15(5) 0.15(5) -0.01(4) -0.01(4) -0.01(4) F6 0.13(4) 0.14(4) 0.13(4) 0.01(3) 0.00(3) 0.00(3) P5 0.092(15) 0.090(17) 0.094(16) 0.001(13) 0.000(12) -0.001(12) P6 0.106(14) 0.105(16) 0.102(17) 0.000 0.000 0.001(12) F7 0.15(3) 0.16(3) 0.15(3) 0.00(2) 0.00(2) 0.00(2) F8 0.14(2) 0.14(3) 0.13(3) 0.01(2) 0.005(19) 0.00(2) F9 0.13(2) 0.13(3) 0.12(3) 0.00(2) 0.001(18) 0.00(2) I5 0.088(6) 0.088(7) 0.087(6) 0.000(6) 0.000(5) 0.001(4) F14 0.124(18) 0.13(2) 0.13(2) 0.003(16) 0.001(16) -0.001(15) F11 0.123(18) 0.13(2) 0.13(2) 0.002(17) -0.001(15) -0.003(16) F12 0.127(18) 0.13(2) 0.13(2) -0.001(17) 0.001(16) 0.003(16) F13 0.131(19) 0.14(2) 0.13(2) 0.003(18) 0.000(16) -0.001(16) F15 0.145(19) 0.15(2) 0.15(2) 0.00(2) -0.003(18) 0.000(17) F10 0.18(3) 0.17(3) 0.18(3) 0.00(2) 0.00(2) 0.00(2) P7 0.166(16) 0.174(17) 0.169(19) 0.001(16) 0.000(14) -0.002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.321(7) . ? Pd1 P2 2.330(6) . ? Pd1 I2 2.592(3) . ? Pd1 I1 2.632(2) . ? Pd2 P4 2.295(6) . ? Pd2 P3 2.362(7) . ? Pd2 I4 2.531(3) . ? Pd2 I3 2.565(2) . ? C1 C2 1.39(3) . ? C1 C6 1.39(3) . ? C1 P1 1.83(2) . ? C2 C3 1.39(3) . ? C2 H2 0.9500 . ? C3 C4 1.39(3) . ? C3 H3 0.9500 . ? C4 C5 1.39(4) . ? C4 H4 0.9500 . ? C5 C6 1.39(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.39(3) . ? C7 C12 1.39(3) . ? C7 P1 1.83(2) . ? C8 C9 1.40(3) . ? C8 H8 0.9500 . ? C9 C10 1.39(3) . ? C9 H9 0.9500 . ? C10 C11 1.39(3) . ? C10 H10 0.9500 . ? C11 C12 1.39(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.39(3) . ? C13 C18 1.40(3) . ? C13 P1 1.88(3) . ? C14 C15 1.39(3) . ? C14 C19 1.52(3) . ? C15 C16 1.39(3) . ? C15 H15 0.9500 . ? C16 C17 1.39(3) . ? C16 H16 0.9500 . ? C17 C18 1.39(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 N1 1.49(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N2 1.33(2) . ? C20 N1 1.44(3) . ? C20 H20 0.9500 . ? C21 N2 1.45(3) . ? C21 C25 1.52(3) . ? C21 C26 1.61(3) . ? C21 C22 1.62(4) . ? C22 C23 1.46(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.61(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 N1 1.40(3) . ? C24 C25 1.52(3) . ? C24 H24 1.0000 . ? C25 C27 1.60(4) . ? C25 C28 1.63(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N2 1.50(3) . ? C29 C30 1.57(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.39(3) . ? C30 C35 1.39(3) . ? C31 C32 1.39(3) . ? C31 P3 1.88(2) . ? C32 C33 1.39(3) . ? C32 H32 0.9500 . ? C33 C34 1.39(3) . ? C33 H33 0.9500 . ? C34 C35 1.39(3) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.38(3) . ? C36 C37 1.40(3) . ? C36 P3 1.81(3) . ? C37 C38 1.39(3) . ? C37 H37 0.9500 . ? C38 C39 1.39(3) . ? C38 H38 0.9500 . ? C39 C40 1.39(4) . ? C39 H39 0.9500 . ? C40 C41 1.41(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.39(3) . ? C42 C47 1.39(4) . ? C42 P3 1.81(2) . ? C43 C44 1.39(3) . ? C43 H43 0.9500 . ? C44 C45 1.39(4) . ? C44 H44 0.9500 . ? C45 C46 1.38(4) . ? C45 H45 0.9500 . ? C46 C47 1.40(4) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.39(3) . ? C48 C53 1.39(3) . ? C48 P4 1.82(2) . ? C49 C50 1.39(3) . ? C49 H49 0.9500 . ? C50 C51 1.39(4) . ? C50 H50 0.9500 . ? C51 C52 1.39(4) . ? C51 H51 0.9500 . ? C52 C53 1.39(3) . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 C55 1.39(3) . ? C54 C59 1.39(3) . ? C54 P4 1.87(3) . ? C55 C56 1.39(3) . ? C55 H55 0.9500 . ? C56 C57 1.39(3) . ? C56 H56 0.9500 . ? C57 C58 1.39(3) . ? C57 H57 0.9500 . ? C58 C59 1.39(3) . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 C65 1.39(3) . ? C60 C61 1.39(3) . ? C60 P4 1.86(2) . ? C61 C62 1.39(3) . ? C61 C66 1.56(3) . ? C62 C63 1.38(4) . ? C62 H62 0.9500 . ? C63 C64 1.40(4) . ? C63 H63 0.9500 . ? C64 C65 1.40(4) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 N4 1.53(3) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 N3 1.16(3) . ? C67 N4 1.35(3) . ? C67 H67 0.9500 . ? C68 N3 1.46(3) . ? C68 C69 1.52(3) . ? C68 C73 1.59(3) . ? C68 C72 1.74(3) . ? C69 C70 1.64(3) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.55(3) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 N4 1.44(3) . ? C71 C72 1.52(3) . ? C71 H71 1.0000 . ? C72 C74 1.44(3) . ? C72 C75 1.51(3) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 N3 1.55(3) . ? C76 C77 1.64(3) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C82 1.39(3) . ? C77 C78 1.39(3) . ? C78 C79 1.39(3) . ? C78 P2 1.87(2) . ? C79 C80 1.39(3) . ? C79 H79 0.9500 . ? C80 C81 1.39(3) . ? C80 H80 0.9500 . ? C81 C82 1.39(3) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.39(3) . ? C83 C88 1.39(3) . ? C83 P2 1.84(3) . ? C84 C85 1.39(3) . ? C84 H84 0.9500 . ? C85 C86 1.39(3) . ? C85 H85 0.9500 . ? C86 C87 1.39(3) . ? C86 H86 0.9500 . ? C87 C88 1.39(3) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? C89 C90 1.39(3) . ? C89 C94 1.39(3) . ? C89 P2 1.84(2) . ? C90 C91 1.40(3) . ? C90 H90 0.9500 . ? C91 C92 1.39(4) . ? C91 H91 0.9500 . ? C92 C93 1.39(4) . ? C92 H92 0.9500 . ? C93 C94 1.39(3) . ? C93 H93 0.9500 . ? C94 H94 0.9500 . ? F1 P5 1.510(10) . ? F2 P5 1.541(9) . ? F3 P5 1.540(9) . ? F4 P5 1.499(10) . ? F5 P5 1.534(9) . ? F6 P5 1.539(9) . ? P6 F9 1.522(10) 2_655 ? P6 F9 1.522(10) . ? P6 F8 1.523(10) . ? P6 F8 1.523(10) 2_655 ? P6 F7 1.529(10) . ? P6 F7 1.529(10) 2_655 ? P6 I5 2.745(9) . ? P6 I5 2.745(9) 2_655 ? F9 I5 1.296(14) . ? F14 P7 1.534(9) . ? F11 P7 1.509(9) . ? F12 P7 1.537(9) . ? F13 P7 1.512(9) . ? F15 P7 1.539(9) . ? F10 P7 1.545(9) . ? 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 P1 Pd1 P2 166.36(18) . . ? P1 Pd1 I2 91.13(18) . . ? P2 Pd1 I2 89.94(18) . . ? P1 Pd1 I1 88.31(17) . . ? P2 Pd1 I1 87.85(17) . . ? I2 Pd1 I1 168.06(8) . . ? P4 Pd2 P3 167.69(17) . . ? P4 Pd2 I4 88.24(17) . . ? P3 Pd2 I4 87.23(17) . . ? P4 Pd2 I3 90.95(17) . . ? P3 Pd2 I3 91.30(18) . . ? I4 Pd2 I3 168.95(9) . . ? C2 C1 C6 120(2) . . ? C2 C1 P1 122.9(19) . . ? C6 C1 P1 116.4(18) . . ? C1 C2 C3 120(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120(3) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 120(2) . . ? C8 C7 P1 121.2(17) . . ? C12 C7 P1 118.6(17) . . ? C7 C8 C9 120(2) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120(2) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120(2) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C7 120(2) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C14 C13 C18 120(2) . . ? C14 C13 P1 121.0(18) . . ? C18 C13 P1 119.3(17) . . ? C13 C14 C15 120(2) . . ? C13 C14 C19 123(2) . . ? C15 C14 C19 116.5(19) . . ? C16 C15 C14 120(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120(3) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120(2) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120(2) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? N1 C19 C14 109.8(17) . . ? N1 C19 H19A 109.7 . . ? C14 C19 H19A 109.7 . . ? N1 C19 H19B 109.7 . . ? C14 C19 H19B 109.7 . . ? H19A C19 H19B 108.2 . . ? N2 C20 N1 120.1(18) . . ? N2 C20 H20 120.0 . . ? N1 C20 H20 120.0 . . ? N2 C21 C25 111.5(19) . . ? N2 C21 C26 109.3(18) . . ? C25 C21 C26 112.5(18) . . ? N2 C21 C22 111.0(19) . . ? C25 C21 C22 99.1(19) . . ? C26 C21 C22 113(2) . . ? C23 C22 C21 106(2) . . ? C23 C22 H22A 110.6 . . ? C21 C22 H22A 110.6 . . ? C23 C22 H22B 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? C22 C23 C24 105.7(19) . . ? C22 C23 H23A 110.6 . . ? C24 C23 H23A 110.6 . . ? C22 C23 H23B 110.6 . . ? C24 C23 H23B 110.6 . . ? H23A C23 H23B 108.7 . . ? N1 C24 C25 110(2) . . ? N1 C24 C23 109.8(19) . . ? C25 C24 C23 99.7(18) . . ? N1 C24 H24 112.2 . . ? C25 C24 H24 112.2 . . ? C23 C24 H24 112.2 . . ? C24 C25 C21 100.6(19) . . ? C24 C25 C27 110(2) . . ? C21 C25 C27 116(2) . . ? C24 C25 C28 111(2) . . ? C21 C25 C28 113(2) . . ? C27 C25 C28 106(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N2 C29 C30 109.2(17) . . ? N2 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? N2 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? C31 C30 C35 120(2) . . ? C31 C30 C29 118(2) . . ? C35 C30 C29 122(2) . . ? C32 C31 C30 120(2) . . ? C32 C31 P3 118.7(15) . . ? C30 C31 P3 121.2(17) . . ? C33 C32 C31 120(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120(2) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C30 120(2) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C41 C36 C37 120(2) . . ? C41 C36 P3 120(2) . . ? C37 C36 P3 119.9(18) . . ? C38 C37 C36 120(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120(2) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120(3) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120(3) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C36 C41 C40 120(3) . . ? C36 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C47 120(2) . . ? C43 C42 P3 119(2) . . ? C47 C42 P3 121(2) . . ? C42 C43 C44 120(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120(3) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C46 C45 C44 120(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 120(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C42 C47 C46 120(3) . . ? C42 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C49 C48 C53 120(2) . . ? C49 C48 P4 118.5(18) . . ? C53 C48 P4 121.7(17) . . ? C50 C49 C48 121(2) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 120(3) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 120(3) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 120(2) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C48 C53 C52 120(2) . . ? C48 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C55 C54 C59 120(2) . . ? C55 C54 P4 118.2(19) . . ? C59 C54 P4 121.5(19) . . ? C54 C55 C56 120(2) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C57 120(2) . . ? C55 C56 H56 119.9 . . ? C57 C56 H56 119.9 . . ? C58 C57 C56 120(2) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C59 C58 C57 120(2) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C58 C59 C54 120(2) . . ? C58 C59 H59 119.9 . . ? C54 C59 H59 119.9 . . ? C65 C60 C61 120(2) . . ? C65 C60 P4 120.0(18) . . ? C61 C60 P4 119.9(18) . . ? C60 C61 C62 120(2) . . ? C60 C61 C66 124(2) . . ? C62 C61 C66 115(2) . . ? C63 C62 C61 120(3) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? C62 C63 C64 120(3) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C65 120(3) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C60 C65 C64 120(3) . . ? C60 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? N4 C66 C61 110.4(17) . . ? N4 C66 H66A 109.6 . . ? C61 C66 H66A 109.6 . . ? N4 C66 H66B 109.6 . . ? C61 C66 H66B 109.6 . . ? H66A C66 H66B 108.1 . . ? N3 C67 N4 124(2) . . ? N3 C67 H67 118.0 . . ? N4 C67 H67 118.0 . . ? N3 C68 C69 112.5(19) . . ? N3 C68 C73 116.1(19) . . ? C69 C68 C73 109.5(19) . . ? N3 C68 C72 107.7(18) . . ? C69 C68 C72 102.3(18) . . ? C73 C68 C72 107.6(17) . . ? C68 C69 C70 104.2(16) . . ? C68 C69 H69A 110.9 . . ? C70 C69 H69A 110.9 . . ? C68 C69 H69B 110.9 . . ? C70 C69 H69B 110.9 . . ? H69A C69 H69B 108.9 . . ? C71 C70 C69 100.4(15) . . ? C71 C70 H70A 111.7 . . ? C69 C70 H70A 111.7 . . ? C71 C70 H70B 111.7 . . ? C69 C70 H70B 111.7 . . ? H70A C70 H70B 109.5 . . ? N4 C71 C72 112.4(19) . . ? N4 C71 C70 109.4(17) . . ? C72 C71 C70 109.1(18) . . ? N4 C71 H71 108.6 . . ? C72 C71 H71 108.6 . . ? C70 C71 H71 108.6 . . ? C74 C72 C75 114(2) . . ? C74 C72 C71 114(2) . . ? C75 C72 C71 115.1(19) . . ? C74 C72 C68 113.9(19) . . ? C75 C72 C68 107.5(18) . . ? C71 C72 C68 89.5(16) . . ? C68 C73 H73A 109.5 . . ? C68 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C68 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N3 C76 C77 109.9(18) . . ? N3 C76 H76A 109.7 . . ? C77 C76 H76A 109.7 . . ? N3 C76 H76B 109.7 . . ? C77 C76 H76B 109.7 . . ? H76A C76 H76B 108.2 . . ? C82 C77 C78 120(2) . . ? C82 C77 C76 120(2) . . ? C78 C77 C76 120(2) . . ? C79 C78 C77 120(2) . . ? C79 C78 P2 118.4(17) . . ? C77 C78 P2 121.6(19) . . ? C80 C79 C78 120(2) . . ? C80 C79 H79 120.0 . . ? C78 C79 H79 120.0 . . ? C79 C80 C81 120(2) . . ? C79 C80 H80 119.9 . . ? C81 C80 H80 119.9 . . ? C80 C81 C82 120(3) . . ? C80 C81 H81 120.1 . . ? C82 C81 H81 120.1 . . ? C77 C82 C81 120(2) . . ? C77 C82 H82 120.0 . . ? C81 C82 H82 120.0 . . ? C84 C83 C88 120(2) . . ? C84 C83 P2 120.1(19) . . ? C88 C83 P2 119.4(19) . . ? C83 C84 C85 120(2) . . ? C83 C84 H84 120.1 . . ? C85 C84 H84 120.1 . . ? C86 C85 C84 120(2) . . ? C86 C85 H85 119.9 . . ? C84 C85 H85 119.9 . . ? C85 C86 C87 120(2) . . ? C85 C86 H86 120.1 . . ? C87 C86 H86 120.1 . . ? C88 C87 C86 120(2) . . ? C88 C87 H87 120.0 . . ? C86 C87 H87 120.0 . . ? C87 C88 C83 120(2) . . ? C87 C88 H88 120.1 . . ? C83 C88 H88 120.1 . . ? C90 C89 C94 120(2) . . ? C90 C89 P2 115.0(18) . . ? C94 C89 P2 124.5(18) . . ? C89 C90 C91 120(3) . . ? C89 C90 H90 120.0 . . ? C91 C90 H90 120.0 . . ? C92 C91 C90 120(3) . . ? C92 C91 H91 120.1 . . ? C90 C91 H91 120.1 . . ? C93 C92 C91 120(3) . . ? C93 C92 H92 119.9 . . ? C91 C92 H92 119.9 . . ? C92 C93 C94 120(2) . . ? C92 C93 H93 120.0 . . ? C94 C93 H93 120.0 . . ? C89 C94 C93 120(2) . . ? C89 C94 H94 120.1 . . ? C93 C94 H94 120.1 . . ? C24 N1 C20 119.1(19) . . ? C24 N1 C19 123.0(19) . . ? C20 N1 C19 117.4(19) . . ? C20 N2 C21 117.5(17) . . ? C20 N2 C29 115.4(17) . . ? C21 N2 C29 119.6(17) . . ? C67 N3 C68 121.3(19) . . ? C67 N3 C76 117(2) . . ? C68 N3 C76 115.8(19) . . ? C67 N4 C71 117.2(18) . . ? C67 N4 C66 120.3(19) . . ? C71 N4 C66 121.6(16) . . ? C1 P1 C7 107.5(10) . . ? C1 P1 C13 102.2(10) . . ? C7 P1 C13 102.5(10) . . ? C1 P1 Pd1 103.7(7) . . ? C7 P1 Pd1 120.2(7) . . ? C13 P1 Pd1 119.0(8) . . ? C89 P2 C83 106.7(11) . . ? C89 P2 C78 106.0(10) . . ? C83 P2 C78 100.4(11) . . ? C89 P2 Pd1 103.2(7) . . ? C83 P2 Pd1 119.9(9) . . ? C78 P2 Pd1 119.5(7) . . ? C42 P3 C36 107.3(12) . . ? C42 P3 C31 108.4(11) . . ? C36 P3 C31 101.6(10) . . ? C42 P3 Pd2 100.1(8) . . ? C36 P3 Pd2 119.5(8) . . ? C31 P3 Pd2 119.3(7) . . ? C48 P4 C60 105.0(10) . . ? C48 P4 C54 107.0(10) . . ? C60 P4 C54 101.8(10) . . ? C48 P4 Pd2 101.1(7) . . ? C60 P4 Pd2 120.0(7) . . ? C54 P4 Pd2 120.5(8) . . ? F4 P5 F1 173.3(12) . . ? F4 P5 F5 82.3(14) . . ? F1 P5 F5 92.8(8) . . ? F4 P5 F6 83.4(13) . . ? F1 P5 F6 92.1(7) . . ? F5 P5 F6 89.8(6) . . ? F4 P5 F3 92.8(8) . . ? F1 P5 F3 92.1(7) . . ? F5 P5 F3 175.1(11) . . ? F6 P5 F3 89.8(6) . . ? F4 P5 F2 92.8(8) . . ? F1 P5 F2 91.7(7) . . ? F5 P5 F2 89.9(6) . . ? F6 P5 F2 176.2(11) . . ? F3 P5 F2 90.1(6) . . ? F9 P6 F9 175(2) 2_655 . ? F9 P6 F8 92.1(15) 2_655 . ? F9 P6 F8 91.8(7) . . ? F9 P6 F8 91.8(7) 2_655 2_655 ? F9 P6 F8 92.1(15) . 2_655 ? F8 P6 F8 82(2) . 2_655 ? F9 P6 F7 84.8(14) 2_655 . ? F9 P6 F7 91.7(7) . . ? F8 P6 F7 91.5(7) . . ? F8 P6 F7 172.5(18) 2_655 . ? F9 P6 F7 91.7(7) 2_655 2_655 ? F9 P6 F7 84.8(14) . 2_655 ? F8 P6 F7 172.5(18) . 2_655 ? F8 P6 F7 91.5(7) 2_655 2_655 ? F7 P6 F7 95(2) . 2_655 ? F9 P6 I5 166.3(10) 2_655 . ? F9 P6 I5 12.1(8) . . ? F8 P6 I5 100.8(9) . . ? F8 P6 I5 85.4(10) 2_655 . ? F7 P6 I5 99.4(10) . . ? F7 P6 I5 75.0(11) 2_655 . ? F9 P6 I5 12.1(8) 2_655 2_655 ? F9 P6 I5 166.3(10) . 2_655 ? F8 P6 I5 85.4(10) . 2_655 ? F8 P6 I5 100.8(9) 2_655 2_655 ? F7 P6 I5 75.0(11) . 2_655 ? F7 P6 I5 99.4(10) 2_655 2_655 ? I5 P6 I5 171.9(9) . 2_655 ? I5 F9 P6 153.7(18) . . ? F9 I5 P6 14.2(9) . . ? F11 P7 F13 174.3(10) . . ? F11 P7 F14 92.6(7) . . ? F13 P7 F14 82.8(11) . . ? F11 P7 F12 92.5(7) . . ? F13 P7 F12 92.0(7) . . ? F14 P7 F12 174.8(10) . . ? F11 P7 F15 92.0(7) . . ? F13 P7 F15 84.5(11) . . ? F14 P7 F15 90.0(6) . . ? F12 P7 F15 90.0(6) . . ? F11 P7 F10 91.8(7) . . ? F13 P7 F10 91.7(7) . . ? F14 P7 F10 90.0(6) . . ? F12 P7 F10 89.7(6) . . ? F15 P7 F10 176.2(10) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 3.294 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.230