# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Ok-Sang Jung' _publ_contact_author_email oksjung@pusan.ac.kr _publ_section_title ; Pseudorotaxane-type n-hydrocarbon container. Metallacyclodimer of ionic palladium(II) complexes containing 1,3-bis(4-pyridyl)tetramethyldisiloxane ; loop_ _publ_author_name 'Ok-Sang Jung' 'Jungmin Ahn' 'Sung Min Kim' 'Tae Hwan Noh' # Attachment '- 825734.cif' data_jm _database_code_depnum_ccdc_archive 'CCDC 825734' #TrackingRef '- 825734.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H84 F12 N8 O14 Pd2 S4 Si4' _chemical_formula_weight 1690.64 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0638(2) _cell_length_b 13.5769(2) _cell_length_c 13.6782(2) _cell_angle_alpha 96.8630(10) _cell_angle_beta 98.9950(10) _cell_angle_gamma 90.9640(10) _cell_volume 1831.51(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2311 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.66 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 866 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8752 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33801 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0913 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9019 _reflns_number_gt 6119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0545P)^2^+0.4172P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9019 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.27083(3) 0.15282(2) 0.20532(2) 0.02383(10) Uani 1 1 d . . . Si1 Si 0.53531(14) 0.61070(9) 0.20465(11) 0.0436(4) Uani 1 1 d . . . Si2 Si 0.82525(13) 0.65609(9) 0.33707(9) 0.0331(3) Uani 1 1 d . . . S1 S 0.15165(12) 0.72580(9) 0.89710(10) 0.0386(3) Uani 1 1 d . . . S2 S 0.35102(12) 0.98715(9) 0.71141(10) 0.0431(3) Uani 1 1 d . . . F1 F 0.2068(4) 0.5654(3) 0.9790(4) 0.141(2) Uani 1 1 d . . . F2 F 0.1051(5) 0.6703(5) 1.0633(4) 0.152(3) Uani 1 1 d . . . F3 F -0.0018(4) 0.5834(4) 0.9339(5) 0.180(3) Uani 1 1 d . . . F4 F 0.1392(4) 1.0134(4) 0.5832(3) 0.1155(16) Uani 1 1 d . . . F5 F 0.2966(5) 0.9344(5) 0.5225(3) 0.154(2) Uani 1 1 d . . . F6 F 0.1739(5) 0.8629(4) 0.6056(4) 0.1309(19) Uani 1 1 d . . . O1 O 0.6742(3) 0.6177(2) 0.2843(2) 0.0396(8) Uani 1 1 d . . . O2 O 0.0429(3) 0.7906(3) 0.9011(3) 0.0573(10) Uani 1 1 d . . . O3 O 0.2794(3) 0.7639(3) 0.9471(3) 0.0624(11) Uani 1 1 d . . . O4 O 0.1502(4) 0.6727(3) 0.8014(3) 0.0839(14) Uani 1 1 d . . . O5 O 0.2682(4) 0.9894(4) 0.7869(3) 0.0852(15) Uani 1 1 d . . . O6 O 0.4497(3) 0.9128(3) 0.7137(3) 0.0532(9) Uani 1 1 d . . . O7 O 0.3985(4) 1.0813(3) 0.6954(4) 0.1052(19) Uani 1 1 d . . . N1 N 0.3545(3) 0.2902(2) 0.2035(3) 0.0278(8) Uani 1 1 d . . . N2 N 0.7656(3) 0.7990(2) 0.6558(3) 0.0273(8) Uani 1 1 d . . . N3 N 0.1836(4) 0.0141(3) 0.2047(3) 0.0328(9) Uani 1 1 d . . . N4 N 0.2991(3) 0.1050(3) 0.0609(3) 0.0314(8) Uani 1 1 d . . . C1 C 0.2738(4) 0.3655(3) 0.1880(3) 0.0356(11) Uani 1 1 d . . . H1 H 0.1791 0.3531 0.1760 0.043 Uiso 1 1 calc R . . C2 C 0.3239(4) 0.4614(3) 0.1889(3) 0.0368(11) Uani 1 1 d . . . H2 H 0.2633 0.5133 0.1781 0.044 Uiso 1 1 calc R . . C3 C 0.4623(4) 0.4825(3) 0.2055(3) 0.0315(10) Uani 1 1 d . . . C4 C 0.5430(4) 0.4031(3) 0.2224(3) 0.0326(10) Uani 1 1 d . . . H4 H 0.6380 0.4134 0.2347 0.039 Uiso 1 1 calc R . . C5 C 0.4885(4) 0.3091(3) 0.2219(3) 0.0317(10) Uani 1 1 d . . . H5 H 0.5470 0.2564 0.2348 0.038 Uiso 1 1 calc R . . C6 C 0.5721(7) 0.6253(5) 0.0800(4) 0.090(2) Uani 1 1 d . . . H6A H 0.6057 0.6933 0.0792 0.134 Uiso 1 1 calc R . . H6B H 0.4897 0.6118 0.0311 0.134 Uiso 1 1 calc R . . H6C H 0.6405 0.5785 0.0631 0.134 Uiso 1 1 calc R . . C7 C 0.4165(7) 0.7025(4) 0.2451(5) 0.0805(15) Uani 1 1 d . . . H7A H 0.4007 0.6932 0.3124 0.121 Uiso 1 1 calc R . . H7B H 0.3311 0.6936 0.1989 0.121 Uiso 1 1 calc R . . H7C H 0.4543 0.7696 0.2456 0.121 Uiso 1 1 calc R . . C8 C 0.9359(5) 0.5499(4) 0.3490(4) 0.0574(15) Uani 1 1 d . . . H8A H 0.9072 0.5092 0.3970 0.086 Uiso 1 1 calc R . . H8B H 1.0290 0.5744 0.3724 0.086 Uiso 1 1 calc R . . H8C H 0.9303 0.5097 0.2839 0.086 Uiso 1 1 calc R . . C9 C 0.8930(5) 0.7491(4) 0.2681(4) 0.0549(15) Uani 1 1 d . . . H9A H 0.9019 0.7182 0.2010 0.082 Uiso 1 1 calc R . . H9B H 0.9815 0.7743 0.3036 0.082 Uiso 1 1 calc R . . H9C H 0.8315 0.8041 0.2631 0.082 Uiso 1 1 calc R . . C10 C 0.8057(4) 0.7159(3) 0.4649(3) 0.0276(9) Uani 1 1 d . . . C11 C 0.6939(5) 0.7716(3) 0.4812(3) 0.0349(10) Uani 1 1 d . . . H11 H 0.6288 0.7829 0.4259 0.042 Uiso 1 1 calc R . . C12 C 0.6762(4) 0.8099(3) 0.5746(3) 0.0311(10) Uani 1 1 d . . . H12 H 0.5976 0.8458 0.5826 0.037 Uiso 1 1 calc R . . C13 C 0.8761(4) 0.7484(3) 0.6430(3) 0.0341(10) Uani 1 1 d . . . H13 H 0.9415 0.7414 0.6996 0.041 Uiso 1 1 calc R . . C14 C 0.8978(4) 0.7063(3) 0.5506(3) 0.0342(10) Uani 1 1 d . . . H14 H 0.9768 0.6701 0.5449 0.041 Uiso 1 1 calc R . . C15 C 0.0452(5) 0.0192(4) 0.2309(5) 0.0665(18) Uani 1 1 d . . . H15A H -0.0043 0.0699 0.1964 0.100 Uiso 1 1 calc R . . H15B H 0.0510 0.0365 0.3032 0.100 Uiso 1 1 calc R . . H15C H -0.0021 -0.0454 0.2105 0.100 Uiso 1 1 calc R . . C16 C 0.2610(5) -0.0448(4) 0.2739(5) 0.0649(18) Uani 1 1 d . . . H16A H 0.2145 -0.1093 0.2712 0.097 Uiso 1 1 calc R . . H16B H 0.2703 -0.0099 0.3418 0.097 Uiso 1 1 calc R . . H16C H 0.3505 -0.0549 0.2555 0.097 Uiso 1 1 calc R . . C17 C 0.1670(7) -0.0308(4) 0.1006(5) 0.0805(15) Uani 1 1 d . . . H17A H 0.1637 -0.1039 0.0989 0.097 Uiso 1 1 calc R . . H17B H 0.0794 -0.0115 0.0656 0.097 Uiso 1 1 calc R . . C18 C 0.2693(6) -0.0040(4) 0.0477(4) 0.0630(18) Uani 1 1 d . . . H18A H 0.2413 -0.0270 -0.0242 0.076 Uiso 1 1 calc R . . H18B H 0.3524 -0.0382 0.0708 0.076 Uiso 1 1 calc R . . C19 C 0.2081(5) 0.1564(4) -0.0103(3) 0.0450(13) Uani 1 1 d . . . H19A H 0.2149 0.1281 -0.0786 0.067 Uiso 1 1 calc R . . H19B H 0.2336 0.2273 -0.0010 0.067 Uiso 1 1 calc R . . H19C H 0.1152 0.1479 0.0015 0.067 Uiso 1 1 calc R . . C20 C 0.4384(4) 0.1211(4) 0.0426(3) 0.0400(11) Uani 1 1 d . . . H20A H 0.4457 0.0930 -0.0256 0.060 Uiso 1 1 calc R . . H20B H 0.5008 0.0885 0.0899 0.060 Uiso 1 1 calc R . . H20C H 0.4609 0.1924 0.0515 0.060 Uiso 1 1 calc R . . C21 C 0.1145(7) 0.6327(6) 0.9717(7) 0.093(3) Uani 1 1 d . . . C22 C 0.2375(7) 0.9463(6) 0.5993(5) 0.0727(19) Uani 1 1 d . . . C23 C 0.4832(8) 0.5521(5) 0.5033(6) 0.095(3) Uani 1 1 d . . . H23A H 0.5199 0.5823 0.4503 0.114 Uiso 1 1 calc R . . H23B H 0.5287 0.5862 0.5683 0.114 Uiso 1 1 calc R . . C24 C 0.3349(8) 0.5711(7) 0.4938(7) 0.115(3) Uani 1 1 d . . . H24A H 0.2894 0.5410 0.4272 0.138 Uiso 1 1 d R B . H24B H 0.2967 0.5381 0.5444 0.138 Uiso 1 1 d R . . H24C H 0.3080 0.6699 0.5059 0.138 Uiso 0.50 1 d PR A 1 C25 C 0.3075(15) 0.6722(14) 0.5056(13) 0.115(6) Uani 0.50 1 d P B 2 H25A H 0.2100 0.6799 0.4992 0.173 Uiso 0.50 1 calc PR B 2 H25B H 0.3426 0.7047 0.4543 0.173 Uiso 0.50 1 calc PR B 2 H25C H 0.3508 0.7026 0.5718 0.173 Uiso 0.50 1 calc PR 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 Pd1 0.02459(17) 0.02193(16) 0.02472(17) 0.00029(12) 0.00540(12) -0.00129(12) Si1 0.0533(8) 0.0240(6) 0.0474(8) 0.0083(6) -0.0123(7) -0.0096(6) Si2 0.0397(7) 0.0286(6) 0.0291(7) -0.0035(5) 0.0048(6) -0.0003(5) S1 0.0331(6) 0.0319(6) 0.0483(8) 0.0003(6) 0.0020(5) 0.0050(5) S2 0.0363(7) 0.0389(7) 0.0519(8) 0.0067(6) -0.0009(6) 0.0043(5) F1 0.093(3) 0.086(3) 0.232(6) 0.091(4) -0.060(4) -0.004(3) F2 0.110(4) 0.262(8) 0.110(4) 0.122(5) 0.024(3) 0.003(4) F3 0.083(3) 0.172(5) 0.279(7) 0.176(5) -0.096(4) -0.080(3) F4 0.072(3) 0.158(5) 0.108(4) 0.046(3) -0.033(2) 0.012(3) F5 0.144(4) 0.278(7) 0.038(2) 0.004(3) 0.023(3) 0.019(4) F6 0.115(3) 0.109(4) 0.145(4) -0.036(3) -0.007(3) -0.057(3) O1 0.0472(19) 0.0320(17) 0.0343(18) -0.0011(14) -0.0049(15) -0.0085(15) O2 0.052(2) 0.062(2) 0.065(3) 0.015(2) 0.0201(19) 0.0284(19) O3 0.042(2) 0.058(2) 0.082(3) 0.005(2) -0.004(2) -0.0094(18) O4 0.097(3) 0.080(3) 0.059(3) -0.026(2) -0.012(2) 0.035(3) O5 0.069(3) 0.133(4) 0.053(3) -0.006(3) 0.019(2) 0.029(3) O6 0.044(2) 0.050(2) 0.072(3) 0.0241(19) 0.0139(19) 0.0196(17) O7 0.068(3) 0.045(3) 0.194(6) 0.042(3) -0.026(3) -0.008(2) N1 0.0253(18) 0.0243(18) 0.034(2) 0.0049(15) 0.0028(15) -0.0012(15) N2 0.0267(18) 0.0270(18) 0.0268(19) 0.0007(15) 0.0021(15) -0.0009(15) N3 0.039(2) 0.0275(19) 0.031(2) 0.0009(16) 0.0068(17) -0.0082(16) N4 0.033(2) 0.031(2) 0.029(2) -0.0024(16) 0.0081(16) -0.0040(16) C1 0.027(2) 0.036(3) 0.042(3) 0.004(2) -0.001(2) 0.000(2) C2 0.037(3) 0.024(2) 0.046(3) 0.002(2) 0.000(2) 0.0045(19) C3 0.042(3) 0.022(2) 0.027(2) 0.0029(18) -0.001(2) -0.0020(19) C4 0.033(2) 0.026(2) 0.039(3) 0.0020(19) 0.004(2) -0.0041(18) C5 0.034(2) 0.025(2) 0.037(3) 0.0071(19) 0.004(2) 0.0025(18) C6 0.114(6) 0.090(5) 0.057(4) 0.038(4) -0.026(4) -0.058(4) C7 0.097(4) 0.040(2) 0.097(4) -0.012(2) 0.011(3) -0.020(2) C8 0.064(4) 0.051(3) 0.050(3) -0.011(3) -0.002(3) 0.022(3) C9 0.065(4) 0.057(3) 0.044(3) 0.000(3) 0.019(3) -0.014(3) C10 0.032(2) 0.024(2) 0.026(2) 0.0018(17) 0.0045(18) -0.0054(18) C11 0.040(3) 0.035(2) 0.027(2) 0.002(2) -0.001(2) 0.001(2) C12 0.029(2) 0.032(2) 0.032(2) 0.0042(19) 0.0033(19) 0.0046(18) C13 0.032(2) 0.041(3) 0.028(2) 0.004(2) -0.0004(19) 0.004(2) C14 0.032(2) 0.038(3) 0.032(2) 0.000(2) 0.007(2) 0.011(2) C15 0.033(3) 0.046(3) 0.124(6) 0.025(4) 0.013(3) -0.007(2) C16 0.048(3) 0.034(3) 0.111(5) 0.027(3) -0.007(3) -0.005(2) C17 0.097(4) 0.040(2) 0.097(4) -0.012(2) 0.011(3) -0.020(2) C18 0.088(4) 0.037(3) 0.069(4) -0.015(3) 0.046(3) -0.023(3) C19 0.040(3) 0.063(3) 0.030(3) -0.002(2) 0.004(2) 0.005(2) C20 0.033(2) 0.050(3) 0.039(3) 0.003(2) 0.012(2) 0.007(2) C21 0.046(4) 0.095(6) 0.138(8) 0.071(6) -0.027(5) -0.020(4) C22 0.065(4) 0.098(6) 0.051(4) 0.007(4) -0.002(3) -0.001(4) C23 0.113(6) 0.097(5) 0.078(5) 0.003(5) 0.032(4) -0.033(6) C24 0.094(6) 0.131(8) 0.123(8) 0.012(6) 0.031(6) -0.019(6) C25 0.079(11) 0.140(17) 0.113(14) -0.045(12) 0.017(9) 0.012(11) _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 N2 2.024(3) 2_666 ? Pd1 N1 2.038(3) . ? Pd1 N3 2.063(3) . ? Pd1 N4 2.068(3) . ? Si1 O1 1.626(3) . ? Si1 C6 1.832(6) . ? Si1 C7 1.839(6) . ? Si1 C3 1.880(4) . ? Si2 O1 1.626(3) . ? Si2 C8 1.843(5) . ? Si2 C9 1.845(5) . ? Si2 C10 1.878(4) . ? S1 O4 1.414(4) . ? S1 O3 1.417(3) . ? S1 O2 1.420(3) . ? S1 C21 1.786(7) . ? S2 O7 1.410(4) . ? S2 O5 1.423(4) . ? S2 O6 1.427(3) . ? S2 C22 1.786(6) . ? F1 C21 1.315(9) . ? F2 C21 1.314(10) . ? F3 C21 1.337(7) . ? F4 C22 1.367(8) . ? F5 C22 1.282(7) . ? F6 C22 1.310(8) . ? N1 C1 1.333(5) . ? N1 C5 1.347(5) . ? N2 C13 1.340(5) . ? N2 C12 1.341(5) . ? N2 Pd1 2.024(3) 2_666 ? N3 C16 1.454(6) . ? N3 C17 1.465(7) . ? N3 C15 1.492(6) . ? N4 C19 1.476(6) . ? N4 C20 1.479(5) . ? N4 C18 1.490(6) . ? C1 C2 1.386(6) . ? C1 H1 0.9500 . ? C2 C3 1.394(6) . ? C2 H2 0.9500 . ? C3 C4 1.380(6) . ? C4 C5 1.379(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 C14 1.397(6) . ? C10 C11 1.398(6) . ? C11 C12 1.360(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.375(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.413(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C23 C23 1.456(14) 2_666 ? C23 C24 1.508(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.399(18) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 H24C 1.3693 . ? C25 H24C 0.0310 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 87.29(13) 2_666 . ? N2 Pd1 N3 93.30(13) 2_666 . ? N1 Pd1 N3 178.92(15) . . ? N2 Pd1 N4 177.39(14) 2_666 . ? N1 Pd1 N4 93.02(13) . . ? N3 Pd1 N4 86.36(13) . . ? O1 Si1 C6 110.1(2) . . ? O1 Si1 C7 110.8(2) . . ? C6 Si1 C7 111.8(3) . . ? O1 Si1 C3 104.96(18) . . ? C6 Si1 C3 109.9(2) . . ? C7 Si1 C3 109.0(2) . . ? O1 Si2 C8 110.2(2) . . ? O1 Si2 C9 110.9(2) . . ? C8 Si2 C9 111.8(3) . . ? O1 Si2 C10 105.05(17) . . ? C8 Si2 C10 109.2(2) . . ? C9 Si2 C10 109.4(2) . . ? O4 S1 O3 115.6(3) . . ? O4 S1 O2 113.0(2) . . ? O3 S1 O2 116.4(2) . . ? O4 S1 C21 103.9(4) . . ? O3 S1 C21 102.1(3) . . ? O2 S1 C21 103.4(3) . . ? O7 S2 O5 114.4(3) . . ? O7 S2 O6 114.5(2) . . ? O5 S2 O6 115.5(3) . . ? O7 S2 C22 103.7(3) . . ? O5 S2 C22 103.6(3) . . ? O6 S2 C22 103.0(3) . . ? Si1 O1 Si2 158.1(2) . . ? C1 N1 C5 118.4(4) . . ? C1 N1 Pd1 118.9(3) . . ? C5 N1 Pd1 122.6(3) . . ? C13 N2 C12 117.9(4) . . ? C13 N2 Pd1 120.5(3) . 2_666 ? C12 N2 Pd1 121.4(3) . 2_666 ? C16 N3 C17 113.7(4) . . ? C16 N3 C15 106.9(4) . . ? C17 N3 C15 105.9(4) . . ? C16 N3 Pd1 113.0(3) . . ? C17 N3 Pd1 104.9(3) . . ? C15 N3 Pd1 112.4(3) . . ? C19 N4 C20 108.1(3) . . ? C19 N4 C18 112.1(4) . . ? C20 N4 C18 107.8(4) . . ? C19 N4 Pd1 110.0(3) . . ? C20 N4 Pd1 114.0(3) . . ? C18 N4 Pd1 104.8(3) . . ? N1 C1 C2 121.9(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 120.8(4) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 115.8(4) . . ? C4 C3 Si1 121.8(3) . . ? C2 C3 Si1 122.4(3) . . ? C5 C4 C3 121.4(4) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 114.9(4) . . ? C14 C10 Si2 123.4(3) . . ? C11 C10 Si2 121.7(3) . . ? C12 C11 C10 121.5(4) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? N2 C12 C11 122.4(4) . . ? N2 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? N2 C13 C14 122.2(4) . . ? N2 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C13 C14 C10 121.1(4) . . ? C13 C14 H14 119.5 . . ? C10 C14 H14 119.5 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N3 114.8(5) . . ? C18 C17 H17A 108.6 . . ? N3 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? N3 C17 H17B 108.6 . . ? H17A C17 H17B 107.5 . . ? C17 C18 N4 112.7(4) . . ? C17 C18 H18A 109.0 . . ? N4 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? N4 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F1 C21 F2 106.4(7) . . ? F1 C21 F3 106.2(7) . . ? F2 C21 F3 107.1(8) . . ? F1 C21 S1 112.8(6) . . ? F2 C21 S1 112.2(6) . . ? F3 C21 S1 111.8(5) . . ? F5 C22 F6 108.4(7) . . ? F5 C22 F4 108.2(6) . . ? F6 C22 F4 105.4(6) . . ? F5 C22 S2 112.6(5) . . ? F6 C22 S2 111.6(5) . . ? F4 C22 S2 110.3(5) . . ? C23 C23 C24 115.0(9) 2_666 . ? C23 C23 H23A 108.5 2_666 . ? C24 C23 H23A 108.5 . . ? C23 C23 H23B 108.5 2_666 . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C25 C24 C23 113.1(10) . . ? C25 C24 H24A 108.7 . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C25 C24 H24C 0.3 . . ? C23 C24 H24C 113.2 . . ? H24A C24 H24C 108.9 . . ? H24B C24 H24C 108.9 . . ? C24 C25 H24C 13.7 . . ? C24 C25 H25A 109.5 . . ? H24C C25 H25A 105.6 . . ? C24 C25 H25B 109.5 . . ? H24C C25 H25B 122.6 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H24C C25 H25C 99.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Si1 O1 Si2 37.4(7) . . . . ? C7 Si1 O1 Si2 -86.9(6) . . . . ? C3 Si1 O1 Si2 155.6(6) . . . . ? C8 Si2 O1 Si1 -126.8(6) . . . . ? C9 Si2 O1 Si1 -2.4(7) . . . . ? C10 Si2 O1 Si1 115.7(6) . . . . ? N2 Pd1 N1 C1 -77.0(3) 2_666 . . . ? N3 Pd1 N1 C1 46(8) . . . . ? N4 Pd1 N1 C1 100.4(3) . . . . ? N2 Pd1 N1 C5 100.0(3) 2_666 . . . ? N3 Pd1 N1 C5 -137(8) . . . . ? N4 Pd1 N1 C5 -82.6(3) . . . . ? N2 Pd1 N3 C16 -69.0(4) 2_666 . . . ? N1 Pd1 N3 C16 168(8) . . . . ? N4 Pd1 N3 C16 113.6(4) . . . . ? N2 Pd1 N3 C17 166.7(4) 2_666 . . . ? N1 Pd1 N3 C17 44(8) . . . . ? N4 Pd1 N3 C17 -10.7(4) . . . . ? N2 Pd1 N3 C15 52.2(4) 2_666 . . . ? N1 Pd1 N3 C15 -70(8) . . . . ? N4 Pd1 N3 C15 -125.2(4) . . . . ? N2 Pd1 N4 C19 27(3) 2_666 . . . ? N1 Pd1 N4 C19 -69.9(3) . . . . ? N3 Pd1 N4 C19 109.2(3) . . . . ? N2 Pd1 N4 C20 148(3) 2_666 . . . ? N1 Pd1 N4 C20 51.7(3) . . . . ? N3 Pd1 N4 C20 -129.2(3) . . . . ? N2 Pd1 N4 C18 -94(3) 2_666 . . . ? N1 Pd1 N4 C18 169.3(3) . . . . ? N3 Pd1 N4 C18 -11.6(3) . . . . ? C5 N1 C1 C2 0.9(6) . . . . ? Pd1 N1 C1 C2 178.0(3) . . . . ? N1 C1 C2 C3 0.5(7) . . . . ? C1 C2 C3 C4 -1.2(6) . . . . ? C1 C2 C3 Si1 178.6(3) . . . . ? O1 Si1 C3 C4 -32.0(4) . . . . ? C6 Si1 C3 C4 86.4(4) . . . . ? C7 Si1 C3 C4 -150.8(4) . . . . ? O1 Si1 C3 C2 148.1(4) . . . . ? C6 Si1 C3 C2 -93.5(4) . . . . ? C7 Si1 C3 C2 29.4(5) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? Si1 C3 C4 C5 -179.3(3) . . . . ? C1 N1 C5 C4 -1.6(6) . . . . ? Pd1 N1 C5 C4 -178.6(3) . . . . ? C3 C4 C5 N1 0.9(7) . . . . ? O1 Si2 C10 C14 140.5(3) . . . . ? C8 Si2 C10 C14 22.3(4) . . . . ? C9 Si2 C10 C14 -100.3(4) . . . . ? O1 Si2 C10 C11 -37.6(4) . . . . ? C8 Si2 C10 C11 -155.8(4) . . . . ? C9 Si2 C10 C11 81.5(4) . . . . ? C14 C10 C11 C12 -2.1(6) . . . . ? Si2 C10 C11 C12 176.2(3) . . . . ? C13 N2 C12 C11 0.2(6) . . . . ? Pd1 N2 C12 C11 -174.9(3) 2_666 . . . ? C10 C11 C12 N2 1.7(7) . . . . ? C12 N2 C13 C14 -1.6(6) . . . . ? Pd1 N2 C13 C14 173.6(3) 2_666 . . . ? N2 C13 C14 C10 1.0(7) . . . . ? C11 C10 C14 C13 0.8(6) . . . . ? Si2 C10 C14 C13 -177.4(3) . . . . ? C16 N3 C17 C18 -89.7(6) . . . . ? C15 N3 C17 C18 153.2(5) . . . . ? Pd1 N3 C17 C18 34.1(6) . . . . ? N3 C17 C18 N4 -48.1(8) . . . . ? C19 N4 C18 C17 -85.5(6) . . . . ? C20 N4 C18 C17 155.7(5) . . . . ? Pd1 N4 C18 C17 33.9(6) . . . . ? O4 S1 C21 F1 63.1(7) . . . . ? O3 S1 C21 F1 -57.5(7) . . . . ? O2 S1 C21 F1 -178.7(6) . . . . ? O4 S1 C21 F2 -176.8(5) . . . . ? O3 S1 C21 F2 62.6(6) . . . . ? O2 S1 C21 F2 -58.6(6) . . . . ? O4 S1 C21 F3 -56.5(8) . . . . ? O3 S1 C21 F3 -177.0(7) . . . . ? O2 S1 C21 F3 61.7(8) . . . . ? O7 S2 C22 F5 63.8(7) . . . . ? O5 S2 C22 F5 -176.4(6) . . . . ? O6 S2 C22 F5 -55.8(6) . . . . ? O7 S2 C22 F6 -173.9(5) . . . . ? O5 S2 C22 F6 -54.2(6) . . . . ? O6 S2 C22 F6 66.5(5) . . . . ? O7 S2 C22 F4 -57.2(5) . . . . ? O5 S2 C22 F4 62.6(5) . . . . ? O6 S2 C22 F4 -176.8(4) . . . . ? C23 C23 C24 C25 177.0(12) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.480 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.111 # Attachment '- 825735.cif' data_mm _database_code_depnum_ccdc_archive 'CCDC 825735' #TrackingRef '- 825735.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H86 F12 N8 O14 Pd2 S4 Si4' _chemical_formula_weight 1704.67 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0994(2) _cell_length_b 13.5934(2) _cell_length_c 13.6673(3) _cell_angle_alpha 96.2680(10) _cell_angle_beta 99.3650(10) _cell_angle_gamma 91.0070(10) _cell_volume 1839.05(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9832 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9000 _exptl_absorpt_correction_T_max 0.9531 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33960 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9111 _reflns_number_gt 8364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0496P)^2^+1.9818P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9111 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.227297(15) 0.848368(11) 0.294776(11) 0.02358(6) Uani 1 1 d . . . Si1 Si 0.32154(7) 0.65443(5) -0.16018(5) 0.03375(14) Uani 1 1 d . . . Si2 Si 0.03450(8) 0.60928(5) -0.29707(6) 0.04318(18) Uani 1 1 d . . . S1 S 0.15097(7) 0.00994(5) 0.78639(5) 0.04159(15) Uani 1 1 d . . . S2 S 0.34907(7) 0.27331(5) 0.60352(5) 0.03977(14) Uani 1 1 d . . . F1 F 0.3631(2) -0.0267(2) 0.9121(2) 0.0902(8) Uani 1 1 d . . . F2 F 0.3383(3) 0.1263(2) 0.8953(2) 0.1004(9) Uani 1 1 d . . . F3 F 0.2133(4) 0.0535(3) 0.97784(19) 0.1262(13) Uani 1 1 d . . . F4 F 0.3984(4) 0.3318(4) 0.4387(3) 0.164(2) Uani 1 1 d . . . F5 F 0.2921(3) 0.4338(2) 0.5207(3) 0.1467(17) Uani 1 1 d . . . F6 F 0.5002(3) 0.4183(3) 0.5711(4) 0.194(3) Uani 1 1 d . . . O1 O 0.1708(2) 0.61720(13) -0.21414(14) 0.0428(4) Uani 1 1 d . . . O3 O 0.0558(2) 0.08706(16) 0.78834(18) 0.0536(5) Uani 1 1 d . . . O4 O 0.2308(3) 0.0098(3) 0.70927(19) 0.0800(9) Uani 1 1 d . . . O5 O 0.1003(3) -0.08501(19) 0.7999(3) 0.0927(11) Uani 1 1 d . . . O6 O 0.3476(3) 0.3243(2) 0.7000(2) 0.0898(10) Uani 1 1 d . . . O7 O 0.2223(2) 0.23537(18) 0.5516(2) 0.0613(6) Uani 1 1 d . . . O8 O 0.4589(2) 0.20911(18) 0.60101(19) 0.0588(6) Uani 1 1 d . . . N1 N 0.26247(19) 0.80004(14) 0.15581(14) 0.0281(4) Uani 1 1 d . . . N2 N -0.14379(19) 0.28893(13) -0.29742(14) 0.0286(4) Uani 1 1 d . . . N3 N 0.3145(2) 0.98688(14) 0.29453(15) 0.0312(4) Uani 1 1 d . . . N4 N 0.2004(2) 0.89609(14) 0.43864(14) 0.0297(4) Uani 1 1 d . . . C1 C 0.3732(2) 0.74956(19) 0.14476(18) 0.0343(5) Uani 1 1 d . . . H1 H 0.4371 0.7432 0.2007 0.041 Uiso 1 1 calc R . . C2 C 0.3947(2) 0.70691(19) 0.05260(18) 0.0353(5) Uani 1 1 d . . . H2 H 0.4722 0.6721 0.0475 0.042 Uiso 1 1 calc R . . C3 C 0.3015(2) 0.71545(16) -0.03304(16) 0.0296(4) Uani 1 1 d . . . C4 C 0.1896(2) 0.77045(18) -0.01943(18) 0.0341(5) Uani 1 1 d . . . H4 H 0.1260 0.7803 -0.0745 0.041 Uiso 1 1 calc R . . C5 C 0.1717(2) 0.81050(17) 0.07432(18) 0.0321(5) Uani 1 1 d . . . H5 H 0.0950 0.8456 0.0814 0.039 Uiso 1 1 calc R . . C6 C 0.4304(4) 0.5471(2) -0.1457(2) 0.0582(9) Uani 1 1 d . . . H6A H 0.3979 0.5057 -0.1015 0.087 Uiso 1 1 calc R . . H6B H 0.5206 0.5702 -0.1185 0.087 Uiso 1 1 calc R . . H6C H 0.4291 0.5098 -0.2097 0.087 Uiso 1 1 calc R . . C7 C 0.3920(4) 0.7460(3) -0.2302(2) 0.0555(8) Uani 1 1 d . . . H7A H 0.4001 0.7153 -0.2956 0.083 Uiso 1 1 calc R . . H7B H 0.4789 0.7695 -0.1953 0.083 Uiso 1 1 calc R . . H7C H 0.3334 0.8006 -0.2362 0.083 Uiso 1 1 calc R . . C8 C 0.0743(5) 0.6251(3) -0.4206(3) 0.0835(15) Uani 1 1 d . . . H8A H 0.1082 0.6915 -0.4207 0.125 Uiso 1 1 calc R . . H8B H -0.0054 0.6129 -0.4697 0.125 Uiso 1 1 calc R . . H8C H 0.1410 0.5791 -0.4362 0.125 Uiso 1 1 calc R . . C9 C -0.0869(4) 0.7014(2) -0.2624(4) 0.0890(16) Uani 1 1 d . . . H9A H -0.1107 0.6899 -0.1992 0.133 Uiso 1 1 calc R . . H9B H -0.1661 0.6953 -0.3125 0.133 Uiso 1 1 calc R . . H9C H -0.0472 0.7668 -0.2573 0.133 Uiso 1 1 calc R . . C10 C -0.0381(3) 0.48061(16) -0.29652(17) 0.0329(5) Uani 1 1 d . . . C11 C 0.0444(2) 0.40134(17) -0.27971(19) 0.0341(5) Uani 1 1 d . . . H11 H 0.1372 0.4118 -0.2679 0.041 Uiso 1 1 calc R . . C12 C -0.0100(2) 0.30706(16) -0.28031(18) 0.0323(5) Uani 1 1 d . . . H12 H 0.0471 0.2551 -0.2686 0.039 Uiso 1 1 calc R . . C13 C -0.2252(3) 0.36404(18) -0.3133(2) 0.0363(5) Uani 1 1 d . . . H13 H -0.3176 0.3516 -0.3249 0.044 Uiso 1 1 calc R . . C14 C -0.1763(3) 0.45969(18) -0.3130(2) 0.0387(5) Uani 1 1 d . . . H14 H -0.2357 0.5104 -0.3238 0.046 Uiso 1 1 calc R . . C15 C 0.2341(3) 1.0465(2) 0.2262(3) 0.0582(9) Uani 1 1 d . A . H15A H 0.1453 1.0513 0.2425 0.087 Uiso 1 1 calc R . . H15B H 0.2289 1.0158 0.1589 0.087 Uiso 1 1 calc R . . H15C H 0.2752 1.1116 0.2322 0.087 Uiso 1 1 calc R . . C16 C 0.4505(3) 0.9821(2) 0.2656(3) 0.0612(9) Uani 1 1 d . A . H16A H 0.4423 0.9574 0.1963 0.092 Uiso 1 1 calc R . . H16B H 0.5042 0.9387 0.3052 0.092 Uiso 1 1 calc R . . H16C H 0.4925 1.0472 0.2767 0.092 Uiso 1 1 calc R . . C17 C 0.3406(4) 1.0295(3) 0.4010(3) 0.0440(8) Uani 0.80 1 d P A 1 H17A H 0.3549 1.1007 0.4054 0.053 Uiso 0.80 1 calc PR A 1 H17B H 0.4210 1.0021 0.4351 0.053 Uiso 0.80 1 calc PR A 1 C18 C 0.2238(5) 1.0062(3) 0.4499(3) 0.0418(9) Uani 0.80 1 d P A 1 H18A H 0.1444 1.0373 0.4189 0.050 Uiso 0.80 1 calc PR A 1 H18B H 0.2421 1.0315 0.5201 0.050 Uiso 0.80 1 calc PR A 1 C17' C 0.2478(12) 1.0512(8) 0.3777(9) 0.030(2) Uiso 0.20 1 d P A 2 H17C H 0.2889 1.1174 0.3923 0.036 Uiso 0.20 1 calc PR A 2 H17D H 0.1521 1.0562 0.3559 0.036 Uiso 0.20 1 calc PR A 2 C18' C 0.2741(17) 0.9968(14) 0.4649(13) 0.037(4) Uiso 0.20 1 d P A 2 H18C H 0.2424 1.0331 0.5212 0.044 Uiso 0.20 1 calc PR A 2 H18D H 0.3697 0.9882 0.4830 0.044 Uiso 0.20 1 calc PR A 2 C19 C 0.2930(3) 0.8450(2) 0.51058(19) 0.0440(6) Uani 1 1 d . A . H19A H 0.2868 0.8723 0.5774 0.066 Uiso 1 1 calc R . . H19B H 0.3834 0.8540 0.4989 0.066 Uiso 1 1 calc R . . H19C H 0.2688 0.7756 0.5021 0.066 Uiso 1 1 calc R . . C20 C 0.0620(3) 0.8790(2) 0.4583(2) 0.0388(5) Uani 1 1 d . A . H20A H 0.0409 0.8092 0.4504 0.058 Uiso 1 1 calc R . . H20B H -0.0005 0.9106 0.4120 0.058 Uiso 1 1 calc R . . H20C H 0.0561 0.9062 0.5253 0.058 Uiso 1 1 calc R . . C21 C -0.2009(6) 0.6758(4) 0.0099(5) 0.1101(19) Uani 1 1 d . . . H21A H -0.1633 0.7021 0.0769 0.165 Uiso 1 1 calc R . . H21B H -0.2969 0.6801 0.0006 0.165 Uiso 1 1 calc R . . H21C H -0.1658 0.7133 -0.0364 0.165 Uiso 1 1 calc R . . C22 C -0.1646(6) 0.5689(4) -0.0081(5) 0.1098(19) Uani 1 1 d . . . H22A H -0.2046 0.5316 0.0369 0.132 Uiso 1 1 calc R . . H22B H -0.2046 0.5432 -0.0757 0.132 Uiso 1 1 calc R . . C23 C -0.0184(5) 0.5506(3) 0.0053(4) 0.0846(13) Uani 1 1 d . . . H23A H 0.0202 0.5846 -0.0428 0.102 Uiso 1 1 calc R . . H23B H 0.0223 0.5805 0.0713 0.102 Uiso 1 1 calc R . . C24 C 0.2720(4) 0.0427(3) 0.8985(3) 0.0597(8) Uani 1 1 d . . . C25 C 0.3870(4) 0.3681(4) 0.5299(5) 0.0967(19) 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 Pd1 0.02501(9) 0.02192(8) 0.02362(9) 0.00023(5) 0.00516(6) -0.00028(6) Si1 0.0422(4) 0.0296(3) 0.0275(3) -0.0036(2) 0.0045(3) 0.0012(3) Si2 0.0547(4) 0.0236(3) 0.0446(4) 0.0048(3) -0.0110(3) -0.0085(3) S1 0.0380(3) 0.0392(3) 0.0452(4) 0.0038(3) 0.0002(3) 0.0051(3) S2 0.0353(3) 0.0335(3) 0.0472(4) -0.0010(2) 0.0001(3) 0.0063(2) F1 0.0679(14) 0.1028(19) 0.0904(18) 0.0230(14) -0.0250(12) 0.0165(13) F2 0.0915(18) 0.0740(16) 0.119(2) -0.0226(15) -0.0049(16) -0.0285(14) F3 0.141(3) 0.200(4) 0.0399(13) 0.0088(17) 0.0235(15) 0.028(3) F4 0.108(3) 0.288(6) 0.122(3) 0.137(4) 0.022(2) 0.002(3) F5 0.099(2) 0.0826(19) 0.242(4) 0.090(2) -0.068(2) -0.0069(16) F6 0.090(2) 0.168(3) 0.308(6) 0.177(4) -0.105(3) -0.084(2) O1 0.0512(11) 0.0348(9) 0.0368(10) -0.0004(7) -0.0056(8) -0.0068(8) O3 0.0476(11) 0.0479(12) 0.0701(15) 0.0196(10) 0.0144(10) 0.0146(9) O4 0.0710(17) 0.122(3) 0.0467(14) -0.0044(14) 0.0167(12) 0.0261(16) O5 0.0624(16) 0.0443(13) 0.161(3) 0.0272(16) -0.0214(18) -0.0066(12) O6 0.101(2) 0.086(2) 0.0665(17) -0.0278(15) -0.0124(15) 0.0423(17) O7 0.0443(12) 0.0579(14) 0.0763(17) 0.0040(12) -0.0027(11) -0.0086(10) O8 0.0536(13) 0.0656(14) 0.0634(14) 0.0159(11) 0.0196(11) 0.0271(11) N1 0.0302(9) 0.0284(9) 0.0251(9) 0.0008(7) 0.0043(7) 0.0006(7) N2 0.0320(9) 0.0239(8) 0.0290(9) 0.0003(7) 0.0040(7) -0.0002(7) N3 0.0342(10) 0.0269(9) 0.0326(10) 0.0026(7) 0.0071(8) -0.0044(7) N4 0.0329(10) 0.0281(9) 0.0286(9) -0.0008(7) 0.0101(7) -0.0019(7) C1 0.0311(11) 0.0432(13) 0.0267(11) -0.0002(9) 0.0015(8) 0.0054(9) C2 0.0306(11) 0.0422(13) 0.0322(12) -0.0017(9) 0.0061(9) 0.0074(9) C3 0.0361(11) 0.0263(10) 0.0251(10) -0.0010(8) 0.0043(8) -0.0020(8) C4 0.0381(12) 0.0333(11) 0.0276(11) 0.0005(9) -0.0027(9) 0.0050(9) C5 0.0316(11) 0.0316(11) 0.0316(12) 0.0014(9) 0.0019(9) 0.0056(9) C6 0.068(2) 0.0502(17) 0.0496(17) -0.0111(13) -0.0008(15) 0.0243(15) C7 0.067(2) 0.0581(18) 0.0448(16) 0.0026(13) 0.0230(14) -0.0110(15) C8 0.108(3) 0.082(3) 0.053(2) 0.0323(19) -0.019(2) -0.050(2) C9 0.072(2) 0.0297(15) 0.145(4) -0.014(2) -0.026(3) 0.0084(15) C10 0.0445(13) 0.0228(10) 0.0290(11) 0.0012(8) 0.0007(9) -0.0023(9) C11 0.0340(12) 0.0273(11) 0.0392(13) 0.0015(9) 0.0029(9) -0.0039(9) C12 0.0319(11) 0.0246(10) 0.0392(13) 0.0014(9) 0.0039(9) 0.0010(8) C13 0.0320(12) 0.0310(11) 0.0441(14) 0.0037(10) 0.0010(10) 0.0004(9) C14 0.0425(13) 0.0256(11) 0.0457(14) 0.0045(9) 0.0004(11) 0.0046(9) C15 0.0479(16) 0.0365(14) 0.088(2) 0.0267(15) -0.0091(15) -0.0059(12) C16 0.0361(15) 0.0422(16) 0.110(3) 0.0204(17) 0.0186(16) -0.0053(12) C17 0.053(2) 0.0378(16) 0.0393(17) -0.0081(13) 0.0114(14) -0.0188(15) C18 0.055(3) 0.0290(17) 0.043(2) -0.0111(14) 0.024(2) -0.0078(18) C19 0.0404(14) 0.0618(17) 0.0292(12) 0.0023(11) 0.0050(10) 0.0084(12) C20 0.0348(12) 0.0478(14) 0.0360(13) 0.0019(10) 0.0144(10) 0.0048(10) C21 0.096(4) 0.103(4) 0.127(5) -0.015(3) 0.025(3) 0.008(3) C22 0.085(3) 0.092(4) 0.146(5) -0.015(3) 0.021(3) -0.007(3) C23 0.091(3) 0.082(3) 0.081(3) -0.008(2) 0.027(2) -0.015(2) C24 0.064(2) 0.067(2) 0.0447(17) 0.0013(15) 0.0015(15) 0.0002(17) C25 0.053(2) 0.095(3) 0.137(5) 0.075(3) -0.036(3) -0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0299(19) . ? Pd1 N2 2.0408(19) 2_565 ? Pd1 N4 2.0646(19) . ? Pd1 N3 2.0653(19) . ? Si1 O1 1.626(2) . ? Si1 C7 1.850(3) . ? Si1 C6 1.850(3) . ? Si1 C3 1.885(2) . ? Si2 O1 1.6286(19) . ? Si2 C8 1.832(4) . ? Si2 C9 1.847(4) . ? Si2 C10 1.886(2) . ? S1 O5 1.422(3) . ? S1 O4 1.427(3) . ? S1 O3 1.435(2) . ? S1 C24 1.806(3) . ? S2 O7 1.418(2) . ? S2 O6 1.424(3) . ? S2 O8 1.426(2) . ? S2 C25 1.791(4) . ? F1 C24 1.337(4) . ? F2 C24 1.317(5) . ? F3 C24 1.314(5) . ? F4 C25 1.313(8) . ? F5 C25 1.322(6) . ? F6 C25 1.330(5) . ? N1 C1 1.343(3) . ? N1 C5 1.344(3) . ? N2 C13 1.336(3) . ? N2 C12 1.347(3) . ? N2 Pd1 2.0408(18) 2_565 ? N3 C15 1.460(3) . ? N3 C17 1.486(4) . ? N3 C16 1.490(4) . ? N3 C17' 1.601(12) . ? N4 C19 1.482(3) . ? N4 C20 1.485(3) . ? N4 C18 1.499(4) . ? N4 C18' 1.525(18) . ? C1 C2 1.380(3) . ? C1 H1 0.9300 . ? C2 C3 1.394(3) . ? C2 H2 0.9300 . ? C3 C4 1.392(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.390(3) . ? C10 C14 1.396(4) . ? C11 C12 1.384(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.382(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.493(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17' C18' 1.46(2) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.509(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.487(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C23 1.429(9) 2_565 ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? 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 Pd1 N2 87.06(8) . 2_565 ? N1 Pd1 N4 177.41(7) . . ? N2 Pd1 N4 93.27(7) 2_565 . ? N1 Pd1 N3 93.51(8) . . ? N2 Pd1 N3 178.88(8) 2_565 . ? N4 Pd1 N3 86.13(8) . . ? O1 Si1 C7 110.87(14) . . ? O1 Si1 C6 110.13(14) . . ? C7 Si1 C6 111.58(18) . . ? O1 Si1 C3 105.20(11) . . ? C7 Si1 C3 109.50(13) . . ? C6 Si1 C3 109.36(13) . . ? O1 Si2 C8 110.51(16) . . ? O1 Si2 C9 111.14(15) . . ? C8 Si2 C9 110.4(3) . . ? O1 Si2 C10 105.02(10) . . ? C8 Si2 C10 110.21(15) . . ? C9 Si2 C10 109.47(16) . . ? O5 S1 O4 114.7(2) . . ? O5 S1 O3 114.76(16) . . ? O4 S1 O3 115.03(16) . . ? O5 S1 C24 103.24(19) . . ? O4 S1 C24 102.94(18) . . ? O3 S1 C24 103.92(16) . . ? O7 S2 O6 115.15(19) . . ? O7 S2 O8 116.57(16) . . ? O6 S2 O8 112.92(16) . . ? O7 S2 C25 102.05(17) . . ? O6 S2 C25 104.4(3) . . ? O8 S2 C25 103.4(2) . . ? Si1 O1 Si2 157.94(14) . . ? C1 N1 C5 118.8(2) . . ? C1 N1 Pd1 119.76(15) . . ? C5 N1 Pd1 121.25(16) . . ? C13 N2 C12 119.0(2) . . ? C13 N2 Pd1 118.61(16) . 2_565 ? C12 N2 Pd1 122.38(15) . 2_565 ? C15 N3 C17 115.6(3) . . ? C15 N3 C16 107.0(2) . . ? C17 N3 C16 104.1(3) . . ? C15 N3 C17' 83.8(5) . . ? C17 N3 C17' 37.6(4) . . ? C16 N3 C17' 135.6(5) . . ? C15 N3 Pd1 112.49(16) . . ? C17 N3 Pd1 104.98(17) . . ? C16 N3 Pd1 112.61(16) . . ? C17' N3 Pd1 101.6(4) . . ? C19 N4 C20 107.6(2) . . ? C19 N4 C18 113.9(3) . . ? C20 N4 C18 106.0(2) . . ? C19 N4 C18' 95.3(6) . . ? C20 N4 C18' 122.2(7) . . ? C18 N4 C18' 20.5(6) . . ? C19 N4 Pd1 109.82(15) . . ? C20 N4 Pd1 114.34(15) . . ? C18 N4 Pd1 105.22(18) . . ? C18' N4 Pd1 105.6(7) . . ? N1 C1 C2 121.8(2) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 120.7(2) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 116.1(2) . . ? C4 C3 Si1 121.17(17) . . ? C2 C3 Si1 122.73(18) . . ? C5 C4 C3 121.0(2) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? N1 C5 C4 121.6(2) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C14 116.5(2) . . ? C11 C10 Si2 121.20(19) . . ? C14 C10 Si2 122.25(18) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? N2 C12 C11 121.4(2) . . ? N2 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? N2 C13 C14 122.0(2) . . ? N2 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C10 120.3(2) . . ? C13 C14 H14 119.8 . . ? C10 C14 H14 119.8 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 109.7(3) . . ? N3 C17 H17A 109.7 . . ? C18 C17 H17A 109.7 . . ? N3 C17 H17B 109.7 . . ? C18 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C17 C18 N4 108.7(3) . . ? C17 C18 H18A 109.9 . . ? N4 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? N4 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C18' C17' N3 104.2(10) . . ? C18' C17' H17C 110.9 . . ? N3 C17' H17C 110.9 . . ? C18' C17' H17D 110.9 . . ? N3 C17' H17D 110.9 . . ? H17C C17' H17D 108.9 . . ? C17' C18' N4 108.1(12) . . ? C17' C18' H18C 110.1 . . ? N4 C18' H18C 110.1 . . ? C17' C18' H18D 110.1 . . ? N4 C18' H18D 110.1 . . ? H18C C18' H18D 108.4 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C21 115.5(5) . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22B 108.4 . . ? C21 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C23 C23 C22 116.5(5) 2_565 . ? C23 C23 H23A 108.2 2_565 . ? C22 C23 H23A 108.2 . . ? C23 C23 H23B 108.2 2_565 . ? C22 C23 H23B 108.2 . . ? H23A C23 H23B 107.3 . . ? F3 C24 F2 107.7(3) . . ? F3 C24 F1 107.6(3) . . ? F2 C24 F1 106.9(3) . . ? F3 C24 S1 111.2(3) . . ? F2 C24 S1 111.8(3) . . ? F1 C24 S1 111.5(2) . . ? F4 C25 F5 106.1(4) . . ? F4 C25 F6 108.5(5) . . ? F5 C25 F6 106.4(4) . . ? F4 C25 S2 112.0(4) . . ? F5 C25 S2 112.2(4) . . ? F6 C25 S2 111.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Si1 O1 Si2 0.7(4) . . . . ? C6 Si1 O1 Si2 -123.3(4) . . . . ? C3 Si1 O1 Si2 119.0(4) . . . . ? C8 Si2 O1 Si1 32.9(4) . . . . ? C9 Si2 O1 Si1 -90.0(4) . . . . ? C10 Si2 O1 Si1 151.7(4) . . . . ? N2 Pd1 N1 C1 -84.36(19) 2_565 . . . ? N4 Pd1 N1 C1 12.9(17) . . . . ? N3 Pd1 N1 C1 94.66(19) . . . . ? N2 Pd1 N1 C5 90.21(18) 2_565 . . . ? N4 Pd1 N1 C5 -172.6(15) . . . . ? N3 Pd1 N1 C5 -90.76(18) . . . . ? N1 Pd1 N3 C15 70.5(2) . . . . ? N2 Pd1 N3 C15 -169(4) 2_565 . . . ? N4 Pd1 N3 C15 -112.1(2) . . . . ? N1 Pd1 N3 C17 -163.0(2) . . . . ? N2 Pd1 N3 C17 -43(4) 2_565 . . . ? N4 Pd1 N3 C17 14.4(2) . . . . ? N1 Pd1 N3 C16 -50.5(2) . . . . ? N2 Pd1 N3 C16 70(4) 2_565 . . . ? N4 Pd1 N3 C16 127.0(2) . . . . ? N1 Pd1 N3 C17' 158.5(4) . . . . ? N2 Pd1 N3 C17' -81(4) 2_565 . . . ? N4 Pd1 N3 C17' -24.1(4) . . . . ? N1 Pd1 N4 C19 -26.7(17) . . . . ? N2 Pd1 N4 C19 70.38(17) 2_565 . . . ? N3 Pd1 N4 C19 -108.67(17) . . . . ? N1 Pd1 N4 C20 -147.8(15) . . . . ? N2 Pd1 N4 C20 -50.73(17) 2_565 . . . ? N3 Pd1 N4 C20 130.22(17) . . . . ? N1 Pd1 N4 C18 96.2(16) . . . . ? N2 Pd1 N4 C18 -166.7(2) 2_565 . . . ? N3 Pd1 N4 C18 14.3(2) . . . . ? N1 Pd1 N4 C18' 74.9(17) . . . . ? N2 Pd1 N4 C18' 172.0(6) 2_565 . . . ? N3 Pd1 N4 C18' -7.0(6) . . . . ? C5 N1 C1 C2 -1.2(4) . . . . ? Pd1 N1 C1 C2 173.49(19) . . . . ? N1 C1 C2 C3 0.4(4) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? C1 C2 C3 Si1 -177.4(2) . . . . ? O1 Si1 C3 C4 -36.5(2) . . . . ? C7 Si1 C3 C4 82.7(2) . . . . ? C6 Si1 C3 C4 -154.8(2) . . . . ? O1 Si1 C3 C2 142.1(2) . . . . ? C7 Si1 C3 C2 -98.7(2) . . . . ? C6 Si1 C3 C2 23.8(3) . . . . ? C2 C3 C4 C5 -2.2(4) . . . . ? Si1 C3 C4 C5 176.50(19) . . . . ? C1 N1 C5 C4 0.3(4) . . . . ? Pd1 N1 C5 C4 -174.34(18) . . . . ? C3 C4 C5 N1 1.5(4) . . . . ? O1 Si2 C10 C11 -34.2(2) . . . . ? C8 Si2 C10 C11 84.8(3) . . . . ? C9 Si2 C10 C11 -153.6(3) . . . . ? O1 Si2 C10 C14 145.9(2) . . . . ? C8 Si2 C10 C14 -95.1(3) . . . . ? C9 Si2 C10 C14 26.5(3) . . . . ? C14 C10 C11 C12 0.4(4) . . . . ? Si2 C10 C11 C12 -179.45(19) . . . . ? C13 N2 C12 C11 -0.5(4) . . . . ? Pd1 N2 C12 C11 -178.17(18) 2_565 . . . ? C10 C11 C12 N2 0.2(4) . . . . ? C12 N2 C13 C14 0.2(4) . . . . ? Pd1 N2 C13 C14 177.9(2) 2_565 . . . ? N2 C13 C14 C10 0.5(4) . . . . ? C11 C10 C14 C13 -0.7(4) . . . . ? Si2 C10 C14 C13 179.1(2) . . . . ? C15 N3 C17 C18 83.0(4) . . . . ? C16 N3 C17 C18 -160.1(3) . . . . ? C17' N3 C17 C18 48.0(7) . . . . ? Pd1 N3 C17 C18 -41.6(3) . . . . ? N3 C17 C18 N4 57.2(5) . . . . ? C19 N4 C18 C17 79.4(4) . . . . ? C20 N4 C18 C17 -162.4(3) . . . . ? C18' N4 C18 C17 53(2) . . . . ? Pd1 N4 C18 C17 -40.9(4) . . . . ? C15 N3 C17' C18' 164.7(10) . . . . ? C17 N3 C17' C18' -46.6(9) . . . . ? C16 N3 C17' C18' -87.4(10) . . . . ? Pd1 N3 C17' C18' 53.0(10) . . . . ? N3 C17' C18' N4 -63.8(12) . . . . ? C19 N4 C18' C17' 153.4(10) . . . . ? C20 N4 C18' C17' -91.9(12) . . . . ? C18 N4 C18' C17' -50.6(17) . . . . ? Pd1 N4 C18' C17' 41.1(12) . . . . ? C21 C22 C23 C23 176.2(6) . . . 2_565 ? O5 S1 C24 F3 -65.0(3) . . . . ? O4 S1 C24 F3 175.3(3) . . . . ? O3 S1 C24 F3 55.1(3) . . . . ? O5 S1 C24 F2 174.6(3) . . . . ? O4 S1 C24 F2 55.0(3) . . . . ? O3 S1 C24 F2 -65.3(3) . . . . ? O5 S1 C24 F1 55.0(3) . . . . ? O4 S1 C24 F1 -64.6(3) . . . . ? O3 S1 C24 F1 175.1(3) . . . . ? O7 S2 C25 F4 -62.8(4) . . . . ? O6 S2 C25 F4 177.0(3) . . . . ? O8 S2 C25 F4 58.6(3) . . . . ? O7 S2 C25 F5 56.4(5) . . . . ? O6 S2 C25 F5 -63.9(4) . . . . ? O8 S2 C25 F5 177.8(4) . . . . ? O7 S2 C25 F6 175.5(5) . . . . ? O6 S2 C25 F6 55.3(5) . . . . ? O8 S2 C25 F6 -63.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.989 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.079 # Attachment '- 825736.cif' data_hh _database_code_depnum_ccdc_archive 'CCDC 825736' #TrackingRef '- 825736.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H88 F12 N8 O14 Pd2 S4 Si4' _chemical_formula_weight 1718.69 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0959(2) _cell_length_b 13.5504(2) _cell_length_c 13.6869(2) _cell_angle_alpha 95.8110(10) _cell_angle_beta 98.5510(10) _cell_angle_gamma 91.1020(10) _cell_volume 1840.97(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3248 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.30 _exptl_crystal_description BLOCK _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9280 _exptl_absorpt_correction_T_max 0.9776 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30932 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.1207 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7974 _reflns_number_gt 4883 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0757P)^2^+8.0007P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7974 _refine_ls_number_parameters 436 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1959 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 6.351 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.2309(3) 0.3495(2) 0.7959(2) 0.0260(11) Uani 1 1 d . . . Si1 Si -0.3143(15) -0.1508(10) 0.6583(10) 0.040(3) Uani 1 1 d . . . Si2 Si -0.030(2) -0.1098(11) 0.7941(14) 0.072(6) Uani 1 1 d . . . S1 S 0.8535(13) 0.4933(10) 0.7145(10) 0.045(3) Uani 1 1 d . . . S2 S 0.3476(13) 0.7727(9) 0.1041(10) 0.045(3) Uani 1 1 d . . . F1 F 0.798(5) 0.448(5) 0.526(3) 0.13(2) Uani 1 1 d . . . F2 F 0.644(4) 0.527(4) 0.589(3) 0.114(16) Uani 1 1 d . . . F3 F 0.672(5) 0.374(4) 0.610(4) 0.115(16) Uani 1 1 d . . . F4 F 0.498(6) 0.916(5) 0.069(7) 0.28(6) Uani 1 1 d . . . F5 F 0.290(6) 0.933(4) 0.022(6) 0.20(4) Uani 1 1 d . . . F6 F 0.395(7) 0.830(9) -0.061(6) 0.23(6) Uani 1 1 d . . . O1 O -0.162(4) -0.118(2) 0.709(2) 0.051(9) Uani 1 1 d . . . O2 O 0.949(3) 0.417(3) 0.716(3) 0.054(10) Uani 1 1 d . . . O3 O 0.903(4) 0.589(3) 0.698(4) 0.095(17) Uani 1 1 d . . . O4 O 0.772(4) 0.496(4) 0.791(3) 0.080(14) Uani 1 1 d . . . O5 O 0.223(3) 0.735(3) 0.054(3) 0.060(11) Uani 1 1 d . . . O6 O 0.456(4) 0.709(3) 0.101(3) 0.062(11) Uani 1 1 d . . . O7 O 0.345(6) 0.824(4) 0.200(4) 0.12(2) Uani 1 1 d . . . N1 N 0.147(4) 0.212(3) 0.799(3) 0.032(8) Uani 1 1 d . . . N2 N -0.265(3) -0.302(3) 0.344(3) 0.030(8) Uani 1 1 d . . . N3 N 0.204(3) 0.396(3) 0.940(3) 0.029(8) Uani 1 1 d . . . N4 N 0.317(4) 0.489(3) 0.795(3) 0.035(9) Uani 1 1 d . . . C1 C 0.014(5) 0.193(3) 0.781(3) 0.035(9) Uani 1 1 d . . . H1 H -0.0436 0.2444 0.7689 0.043 Uiso 1 1 calc R . . C2 C -0.039(5) 0.098(3) 0.780(3) 0.037(11) Uani 1 1 d . . . H2 H -0.1311 0.0876 0.7684 0.045 Uiso 1 1 calc R . . C3 C 0.043(5) 0.019(3) 0.795(3) 0.040(12) Uani 1 1 d . . . C4 C 0.179(6) 0.041(4) 0.814(4) 0.048(13) Uani 1 1 d . . . H4 H 0.2389 -0.0093 0.8259 0.058 Uiso 1 1 calc R . . C5 C 0.229(5) 0.136(3) 0.814(3) 0.038(11) Uani 1 1 d . . . H5 H 0.3210 0.1485 0.8247 0.046 Uiso 1 1 calc R . . C6 C -0.080(13) -0.125(8) 0.915(7) 0.21(7) Uani 1 1 d . . . H6A H -0.1410 -0.0743 0.9311 0.322 Uiso 1 1 calc R . . H6B H -0.0023 -0.1199 0.9653 0.322 Uiso 1 1 calc R . . H6C H -0.1238 -0.1891 0.9128 0.322 Uiso 1 1 calc R . . C7 C 0.095(9) -0.201(5) 0.760(10) 0.20(7) Uani 1 1 d D . . H7A H 0.1032 -0.2001 0.6909 0.298 Uiso 1 1 calc R . . H7B H 0.0653 -0.2667 0.7705 0.298 Uiso 1 1 calc R . . H7C H 0.1799 -0.1847 0.7999 0.298 Uiso 1 1 calc R . . C8 C -0.416(9) -0.041(6) 0.642(6) 0.11(2) Uani 1 1 d . . . H8A H -0.4171 -0.0033 0.7052 0.170 Uiso 1 1 calc R . . H8B H -0.5065 -0.0613 0.6130 0.170 Uiso 1 1 calc R . . H8C H -0.3790 0.0002 0.5987 0.170 Uiso 1 1 calc R . . C9 C -0.389(6) -0.239(5) 0.731(4) 0.064(17) Uani 1 1 d . . . H9A H -0.3307 -0.2938 0.7394 0.096 Uiso 1 1 calc R . . H9B H -0.4745 -0.2629 0.6956 0.096 Uiso 1 1 calc R . . H9C H -0.3992 -0.2061 0.7943 0.096 Uiso 1 1 calc R . . C10 C -0.298(5) -0.215(3) 0.532(3) 0.033(10) Uani 1 1 d . . . C11 C -0.394(5) -0.208(3) 0.448(3) 0.037(11) Uani 1 1 d . . . H11 H -0.4711 -0.1734 0.4548 0.044 Uiso 1 1 calc R . . C12 C -0.375(5) -0.252(3) 0.356(3) 0.037(11) Uani 1 1 d . . . H12 H -0.4409 -0.2473 0.3015 0.044 Uiso 1 1 calc R . . C13 C -0.173(4) -0.311(3) 0.423(3) 0.035(11) Uani 1 1 d . . . H13 H -0.0966 -0.3464 0.4153 0.042 Uiso 1 1 calc R . . C14 C -0.187(5) -0.269(3) 0.516(3) 0.035(11) Uani 1 1 d . . . H14 H -0.1212 -0.2766 0.5694 0.041 Uiso 1 1 calc R . . C15 C 0.065(5) 0.379(4) 0.959(4) 0.042(12) Uani 1 1 d . A . H15A H 0.0567 0.4096 1.0245 0.063 Uiso 1 1 calc R . . H15B H 0.0456 0.3094 0.9553 0.063 Uiso 1 1 calc R . . H15C H 0.0037 0.4083 0.9107 0.063 Uiso 1 1 calc R . . C16 C 0.293(5) 0.344(4) 1.012(3) 0.051(14) Uani 1 1 d . A . H16A H 0.3845 0.3547 1.0019 0.076 Uiso 1 1 calc R . . H16B H 0.2707 0.2742 1.0012 0.076 Uiso 1 1 calc R . . H16C H 0.2830 0.3691 1.0781 0.076 Uiso 1 1 calc R . . C17 C 0.225(18) 0.509(13) 0.945(11) 0.05(4) Uani 0.70 1 d P A 1 H17A H 0.1475 0.5375 0.9087 0.056 Uiso 0.70 1 calc PR A 1 H17B H 0.2359 0.5382 1.0137 0.056 Uiso 0.70 1 calc PR A 1 C18 C 0.344(7) 0.528(5) 0.902(5) 0.035(9) Uani 0.70 1 d P A 1 H18A H 0.4194 0.4954 0.9353 0.043 Uiso 0.70 1 calc PR A 1 H18B H 0.3646 0.5988 0.9083 0.043 Uiso 0.70 1 calc PR A 1 C17' C 0.26(4) 0.49(3) 0.97(2) 0.03(7) Uani 0.30 1 d P A 2 H17C H 0.3475 0.4926 1.0074 0.041 Uiso 0.30 1 calc PR A 2 H17D H 0.2023 0.5289 1.0164 0.041 Uiso 0.30 1 calc PR A 2 C18' C 0.26(2) 0.551(11) 0.878(12) 0.05(5) Uani 0.30 1 d P A 2 H18C H 0.1673 0.5685 0.8537 0.057 Uiso 0.30 1 calc PR A 2 H18D H 0.3112 0.6127 0.8971 0.057 Uiso 0.30 1 calc PR A 2 C19 C 0.453(8) 0.485(7) 0.769(8) 0.14(3) Uani 1 1 d . A . H19A H 0.4943 0.5502 0.7803 0.204 Uiso 1 1 calc R . . H19B H 0.4494 0.4594 0.7010 0.204 Uiso 1 1 calc R . . H19C H 0.5054 0.4418 0.8107 0.204 Uiso 1 1 calc R . . C20 C 0.241(6) 0.547(4) 0.725(5) 0.068(19) Uani 1 1 d . A . H20A H 0.2834 0.6115 0.7290 0.102 Uiso 1 1 calc R . . H20B H 0.1515 0.5537 0.7403 0.102 Uiso 1 1 calc R . . H20C H 0.2372 0.5145 0.6589 0.102 Uiso 1 1 calc R . . C21 C 0.737(7) 0.458(6) 0.604(5) 0.071(18) Uani 1 1 d . . . C22 C 0.385(9) 0.868(7) 0.029(11) 0.15(6) Uani 1 1 d . . . C23 C -0.040(7) 0.046(4) 0.506(6) 0.11(2) Uani 1 1 d D . . H23A H 0.0091 0.0970 0.4800 0.136 Uiso 1 1 calc R . . H23B H -0.0315 0.0640 0.5769 0.136 Uiso 1 1 calc R . . C24 C -0.185(6) 0.059(7) 0.466(8) 0.14(3) Uani 1 1 d D C . H24A H -0.2436 0.0142 0.4925 0.163 Uiso 1 1 calc R . . H24B H -0.2018 0.0504 0.3944 0.163 Uiso 1 1 calc R . . C25 C -0.195(15) 0.165(8) 0.508(12) 0.24(8) Uani 1 1 d D . . H25A H -0.1082 0.1985 0.5160 0.285 Uiso 1 1 d R C . H25B H -0.2203 0.1639 0.5733 0.285 Uiso 1 1 d R . . H25C H -0.2945 0.2270 0.4494 0.285 Uiso 0.50 1 d PRD B 1 C26 C -0.297(17) 0.229(13) 0.455(15) 0.21(7) Uani 0.50 1 d PD C 2 H26A H -0.2696 0.2425 0.3928 0.322 Uiso 0.50 1 calc PR C 2 H26B H -0.3018 0.2904 0.4954 0.322 Uiso 0.50 1 calc PR C 2 H26C H -0.3828 0.1953 0.4420 0.322 Uiso 0.50 1 calc PR C 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 Pd1 0.0285(19) 0.0256(17) 0.0244(17) 0.0025(12) 0.0059(13) 0.0013(12) Si1 0.055(9) 0.032(7) 0.028(7) -0.005(6) 0.001(6) 0.006(6) Si2 0.098(14) 0.025(7) 0.077(12) 0.012(8) -0.045(10) -0.017(8) S1 0.041(7) 0.045(7) 0.047(8) 0.006(6) 0.001(6) 0.007(6) S2 0.042(7) 0.036(7) 0.054(8) 0.001(6) -0.004(6) 0.007(6) F1 0.14(4) 0.22(6) 0.04(2) 0.01(3) 0.02(3) -0.01(4) F2 0.08(3) 0.16(4) 0.10(3) 0.05(3) -0.03(2) 0.02(3) F3 0.11(3) 0.11(4) 0.11(4) -0.03(3) 0.00(3) -0.05(3) F4 0.13(4) 0.22(7) 0.47(12) 0.28(8) -0.17(6) -0.12(5) F5 0.14(5) 0.09(4) 0.33(9) 0.12(5) -0.13(6) -0.02(3) F6 0.12(5) 0.41(15) 0.17(7) 0.21(9) 0.00(5) -0.04(7) O1 0.06(2) 0.038(19) 0.04(2) -0.002(16) -0.012(17) -0.005(17) O2 0.05(2) 0.04(2) 0.07(3) 0.022(19) 0.016(19) 0.018(17) O3 0.07(3) 0.05(3) 0.17(5) 0.03(3) -0.02(3) -0.01(2) O4 0.08(3) 0.12(4) 0.05(3) -0.01(2) 0.02(2) 0.03(3) O5 0.04(2) 0.06(3) 0.07(3) 0.01(2) -0.008(19) -0.004(18) O6 0.05(2) 0.08(3) 0.07(3) 0.03(2) 0.02(2) 0.03(2) O7 0.14(5) 0.10(4) 0.08(3) -0.05(3) -0.04(3) 0.07(4) N1 0.04(2) 0.024(19) 0.03(2) 0.002(16) 0.007(17) 0.004(16) N2 0.03(2) 0.03(2) 0.024(19) 0.001(16) 0.005(16) 0.003(16) N3 0.03(2) 0.029(19) 0.03(2) 0.001(16) 0.010(16) 0.000(16) N4 0.04(2) 0.03(2) 0.04(2) 0.009(18) 0.010(18) -0.003(17) C1 0.04(2) 0.03(2) 0.04(2) 0.000(17) 0.003(18) -0.006(17) C2 0.04(3) 0.03(2) 0.04(3) 0.00(2) 0.00(2) -0.01(2) C3 0.06(3) 0.02(2) 0.03(3) 0.000(19) -0.01(2) 0.00(2) C4 0.06(4) 0.03(3) 0.05(3) 0.00(2) -0.01(3) 0.01(2) C5 0.04(3) 0.03(2) 0.04(3) 0.00(2) 0.00(2) 0.01(2) C6 0.30(14) 0.19(10) 0.12(8) 0.10(7) -0.11(8) -0.18(10) C7 0.13(8) 0.03(4) 0.36(17) -0.05(7) -0.14(9) 0.03(4) C8 0.16(6) 0.10(5) 0.08(4) -0.01(3) 0.02(4) 0.03(4) C9 0.07(4) 0.08(4) 0.04(3) 0.01(3) 0.02(3) 0.00(3) C10 0.04(3) 0.03(2) 0.03(2) 0.001(19) 0.01(2) 0.00(2) C11 0.03(3) 0.05(3) 0.03(2) 0.00(2) 0.01(2) 0.01(2) C12 0.03(3) 0.05(3) 0.03(2) 0.01(2) 0.00(2) 0.01(2) C13 0.03(3) 0.04(3) 0.03(2) 0.01(2) 0.00(2) 0.00(2) C14 0.04(3) 0.03(2) 0.02(2) 0.007(19) -0.01(2) 0.00(2) C15 0.04(3) 0.05(3) 0.04(3) 0.01(2) 0.02(2) 0.01(2) C16 0.05(3) 0.08(4) 0.03(3) 0.00(3) 0.01(2) 0.02(3) C17 0.08(11) 0.03(6) 0.04(9) 0.00(6) 0.02(7) 0.00(6) C18 0.04(2) 0.03(2) 0.04(2) 0.000(17) 0.003(18) -0.006(17) C17' 0.07(19) 0.02(12) 0.01(12) -0.01(10) 0.01(11) 0.01(10) C18' 0.09(15) 0.02(8) 0.03(10) 0.00(7) 0.02(10) 0.01(9) C19 0.09(5) 0.11(5) 0.22(9) 0.07(6) 0.05(5) 0.02(4) C20 0.06(4) 0.05(3) 0.10(5) 0.04(3) -0.02(3) -0.01(3) C21 0.08(5) 0.10(5) 0.04(4) 0.01(4) 0.01(3) 0.00(4) C22 0.06(5) 0.10(7) 0.26(14) 0.11(9) -0.08(8) -0.04(5) C23 0.16(6) 0.10(5) 0.08(4) -0.01(3) 0.02(4) 0.03(4) C24 0.09(5) 0.11(5) 0.22(9) 0.07(6) 0.05(5) 0.02(4) C25 0.27(18) 0.16(13) 0.3(2) 0.06(13) 0.01(15) 0.07(12) C26 0.30(14) 0.19(10) 0.12(8) 0.10(7) -0.11(8) -0.18(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N2 2.03(3) ? ? Pd1 N1 2.03(4) . ? Pd1 N4 2.06(4) . ? Pd1 N3 2.07(3) . ? Si1 O1 1.62(4) . ? Si1 C9 1.84(6) . ? Si1 C8 1.84(8) . ? Si1 C10 1.88(4) . ? Si2 O1 1.63(4) . ? Si2 C6 1.83(11) . ? Si2 C7 1.86(9) . ? Si2 C3 1.87(5) . ? S1 O4 1.42(4) . ? S1 O2 1.43(3) . ? S1 O3 1.43(4) . ? S1 C21 1.79(7) . ? S2 O5 1.40(4) . ? S2 O6 1.41(4) . ? S2 O7 1.42(4) . ? S2 C22 1.80(10) . ? F1 C21 1.31(7) . ? F2 C21 1.34(8) . ? F3 C21 1.32(8) . ? F4 C22 1.32(8) . ? F5 C22 1.32(12) . ? F6 C22 1.30(16) . ? N1 C1 1.34(5) . ? N1 C5 1.35(5) . ? N2 C12 1.34(5) . ? N2 C13 1.34(5) . ? N2 Pd1 2.03(3) 2_556 ? N3 C17' 1.4(4) . ? N3 C16 1.48(6) . ? N3 C15 1.48(5) . ? N3 C17 1.53(19) . ? N4 C20 1.44(6) . ? N4 C19 1.47(8) . ? N4 C18 1.49(8) . ? N4 C18' 1.55(16) . ? C1 C2 1.38(6) . ? C1 H1 0.9300 . ? C2 C3 1.38(6) . ? C2 H2 0.9300 . ? C3 C4 1.39(7) . ? C4 C5 1.37(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9602 . ? C7 H7B 0.9602 . ? C7 H7C 0.9602 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C14 1.38(6) . ? C10 C11 1.39(6) . ? C11 C12 1.38(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.37(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.4(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C17' C18' 1.6(3) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C23 C23 1.498(13) 2_556 ? C23 C24 1.500(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.501(14) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.51(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 1.5092 . ? C26 H25C 0.0802 . ? C26 H26A 0.9763 . ? C26 H26B 0.9676 . ? C26 H26C 0.9661 . ? 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 Pd1 N1 86.8(14) ? . ? N2 Pd1 N4 93.8(14) ? . ? N1 Pd1 N4 179.3(15) . . ? N2 Pd1 N3 177.8(15) ? . ? N1 Pd1 N3 93.4(14) . . ? N4 Pd1 N3 86.0(14) . . ? O1 Si1 C9 111(2) . . ? O1 Si1 C8 111(3) . . ? C9 Si1 C8 112(4) . . ? O1 Si1 C10 105(2) . . ? C9 Si1 C10 109(2) . . ? C8 Si1 C10 109(3) . . ? O1 Si2 C6 110(4) . . ? O1 Si2 C7 110(3) . . ? C6 Si2 C7 113(6) . . ? O1 Si2 C3 106(2) . . ? C6 Si2 C3 110(4) . . ? C7 Si2 C3 109(4) . . ? O4 S1 O2 115(3) . . ? O4 S1 O3 114(3) . . ? O2 S1 O3 115(2) . . ? O4 S1 C21 103(3) . . ? O2 S1 C21 104(3) . . ? O3 S1 C21 103(3) . . ? O5 S2 O6 116(3) . . ? O5 S2 O7 115(3) . . ? O6 S2 O7 113(3) . . ? O5 S2 C22 102(3) . . ? O6 S2 C22 104(4) . . ? O7 S2 C22 105(6) . . ? Si1 O1 Si2 157(3) . . ? C1 N1 C5 118(4) . . ? C1 N1 Pd1 123(3) . . ? C5 N1 Pd1 118(3) . . ? C12 N2 C13 119(4) . . ? C12 N2 Pd1 120(3) . 2_556 ? C13 N2 Pd1 121(3) . 2_556 ? C17' N3 C16 98(10) . . ? C17' N3 C15 114(10) . . ? C16 N3 C15 107(4) . . ? C17' N3 C17 19(10) . . ? C16 N3 C17 117(6) . . ? C15 N3 C17 106(7) . . ? C17' N3 Pd1 112(10) . . ? C16 N3 Pd1 111(3) . . ? C15 N3 Pd1 114(3) . . ? C17 N3 Pd1 102(6) . . ? C20 N4 C19 107(5) . . ? C20 N4 C18 119(5) . . ? C19 N4 C18 101(6) . . ? C20 N4 C18' 88(8) . . ? C19 N4 C18' 131(10) . . ? C18 N4 C18' 36(7) . . ? C20 N4 Pd1 113(3) . . ? C19 N4 Pd1 112(4) . . ? C18 N4 Pd1 104(3) . . ? C18' N4 Pd1 103(7) . . ? N1 C1 C2 122(4) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.3 . . ? C1 C2 C3 122(4) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C2 C3 C4 115(4) . . ? C2 C3 Si2 121(4) . . ? C4 C3 Si2 123(4) . . ? C5 C4 C3 121(4) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? N1 C5 C4 122(5) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? Si2 C6 H6A 109.4 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 111.3 . . ? Si2 C7 H7B 108.1 . . ? H7A C7 H7B 109.4 . . ? Si2 C7 H7C 109.0 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C14 C10 C11 115(4) . . ? C14 C10 Si1 122(3) . . ? C11 C10 Si1 123(3) . . ? C12 C11 C10 121(4) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? N2 C12 C11 121(4) . . ? N2 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? N2 C13 C14 122(4) . . ? N2 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C10 121(4) . . ? C13 C14 H14 119.3 . . ? C10 C14 H14 119.3 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 N3 108(10) . . ? C18 C17 H17A 110.1 . . ? N3 C17 H17A 110.1 . . ? C18 C17 H17B 110.3 . . ? N3 C17 H17B 110.3 . . ? H17A C17 H17B 108.5 . . ? C17 C18 N4 108(8) . . ? C17 C18 H18A 110.1 . . ? N4 C18 H18A 110.2 . . ? C17 C18 H18B 110.1 . . ? N4 C18 H18B 110.1 . . ? H18A C18 H18B 108.5 . . ? N3 C17' C18' 108(10) . . ? N3 C17' H17C 110.1 . . ? C18' C17' H17C 110.0 . . ? N3 C17' H17D 109.9 . . ? C18' C17' H17D 110.0 . . ? H17C C17' H17D 108.4 . . ? N4 C18' C17' 112(10) . . ? N4 C18' H18C 109.1 . . ? C17' C18' H18C 109.2 . . ? N4 C18' H18D 109.2 . . ? C17' C18' H18D 109.2 . . ? H18C C18' H18D 107.9 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.6 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.4 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F1 C21 F3 108(6) . . ? F1 C21 F2 107(6) . . ? F3 C21 F2 107(6) . . ? F1 C21 S1 111(5) . . ? F3 C21 S1 112(5) . . ? F2 C21 S1 112(5) . . ? F6 C22 F4 110(10) . . ? F6 C22 F5 108(9) . . ? F4 C22 F5 108(9) . . ? F6 C22 S2 111(8) . . ? F4 C22 S2 110(7) . . ? F5 C22 S2 111(10) . . ? C23 C23 C24 128(8) 2_556 . ? C23 C23 H23A 105.2 2_556 . ? C24 C23 H23A 105.3 . . ? C23 C23 H23B 105.2 2_556 . ? C24 C23 H23B 105.5 . . ? H23A C23 H23B 106.0 . . ? C23 C24 C25 99(7) . . ? C23 C24 H24A 111.8 . . ? C25 C24 H24A 111.4 . . ? C23 C24 H24B 112.0 . . ? C25 C24 H24B 113.3 . . ? H24A C24 H24B 109.5 . . ? C24 C25 C26 120(10) . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25A 108.1 . . ? C24 C25 H25B 107.2 . . ? C26 C25 H25B 104.7 . . ? H25A C25 H25B 107.1 . . ? C24 C25 H25C 117.3 . . ? C26 C25 H25C 3.0 . . ? H25A C25 H25C 107.7 . . ? H25B C25 H25C 107.7 . . ? C25 C26 H25C 90.3 . . ? C25 C26 H26A 116.3 . . ? C25 C26 H26B 108.3 . . ? H26A C26 H26B 107.3 . . ? C25 C26 H26C 106.4 . . ? H26A C26 H26C 109.7 . . ? H26B C26 H26C 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Si1 O1 Si2 -10(7) . . . . ? C8 Si1 O1 Si2 115(7) . . . . ? C10 Si1 O1 Si2 -127(6) . . . . ? C6 Si2 O1 Si1 -23(8) . . . . ? C7 Si2 O1 Si1 101(8) . . . . ? C3 Si2 O1 Si1 -141(6) . . . . ? N2 Pd1 N1 C1 -99(4) ? . . . ? N4 Pd1 N1 C1 104(100) . . . . ? N3 Pd1 N1 C1 83(4) . . . . ? N2 Pd1 N1 C5 77(3) ? . . . ? N4 Pd1 N1 C5 -79(100) . . . . ? N3 Pd1 N1 C5 -101(3) . . . . ? N2 Pd1 N3 C17' 83(40) ? . . . ? N1 Pd1 N3 C17' 178(15) . . . . ? N4 Pd1 N3 C17' -2(15) . . . . ? N2 Pd1 N3 C16 -25(39) ? . . . ? N1 Pd1 N3 C16 70(3) . . . . ? N4 Pd1 N3 C16 -110(3) . . . . ? N2 Pd1 N3 C15 -145(36) ? . . . ? N1 Pd1 N3 C15 -51(3) . . . . ? N4 Pd1 N3 C15 129(3) . . . . ? N2 Pd1 N3 C17 101(38) ? . . . ? N1 Pd1 N3 C17 -165(7) . . . . ? N4 Pd1 N3 C17 16(7) . . . . ? N2 Pd1 N4 C20 67(4) ? . . . ? N1 Pd1 N4 C20 -136(100) . . . . ? N3 Pd1 N4 C20 -115(4) . . . . ? N2 Pd1 N4 C19 -54(5) ? . . . ? N1 Pd1 N4 C19 103(100) . . . . ? N3 Pd1 N4 C19 124(5) . . . . ? N2 Pd1 N4 C18 -162(4) ? . . . ? N1 Pd1 N4 C18 -6(100) . . . . ? N3 Pd1 N4 C18 16(4) . . . . ? N2 Pd1 N4 C18' 160(8) ? . . . ? N1 Pd1 N4 C18' -43(100) . . . . ? N3 Pd1 N4 C18' -22(8) . . . . ? C5 N1 C1 C2 1(6) . . . . ? Pd1 N1 C1 C2 178(3) . . . . ? N1 C1 C2 C3 -1(7) . . . . ? C1 C2 C3 C4 1(7) . . . . ? C1 C2 C3 Si2 180(4) . . . . ? O1 Si2 C3 C2 36(5) . . . . ? C6 Si2 C3 C2 -82(6) . . . . ? C7 Si2 C3 C2 154(5) . . . . ? O1 Si2 C3 C4 -145(4) . . . . ? C6 Si2 C3 C4 97(6) . . . . ? C7 Si2 C3 C4 -27(6) . . . . ? C2 C3 C4 C5 -1(7) . . . . ? Si2 C3 C4 C5 180(4) . . . . ? C1 N1 C5 C4 -1(7) . . . . ? Pd1 N1 C5 C4 -178(4) . . . . ? C3 C4 C5 N1 1(8) . . . . ? O1 Si1 C10 C14 32(4) . . . . ? C9 Si1 C10 C14 -86(4) . . . . ? C8 Si1 C10 C14 151(5) . . . . ? O1 Si1 C10 C11 -145(4) . . . . ? C9 Si1 C10 C11 96(4) . . . . ? C8 Si1 C10 C11 -27(5) . . . . ? C14 C10 C11 C12 -1(7) . . . . ? Si1 C10 C11 C12 177(4) . . . . ? C13 N2 C12 C11 1(7) . . . . ? Pd1 N2 C12 C11 -172(3) 2_556 . . . ? C10 C11 C12 N2 -1(7) . . . . ? C12 N2 C13 C14 -1(7) . . . . ? Pd1 N2 C13 C14 172(3) 2_556 . . . ? N2 C13 C14 C10 0(7) . . . . ? C11 C10 C14 C13 1(7) . . . . ? Si1 C10 C14 C13 -177(3) . . . . ? C17' N3 C17 C18 77(67) . . . . ? C16 N3 C17 C18 75(10) . . . . ? C15 N3 C17 C18 -165(7) . . . . ? Pd1 N3 C17 C18 -46(9) . . . . ? N3 C17 C18 N4 64(9) . . . . ? C20 N4 C18 C17 80(9) . . . . ? C19 N4 C18 C17 -163(8) . . . . ? C18' N4 C18 C17 47(13) . . . . ? Pd1 N4 C18 C17 -46(8) . . . . ? C16 N3 C17' C18' 142(21) . . . . ? C15 N3 C17' C18' -105(23) . . . . ? C17 N3 C17' C18' -37(48) . . . . ? Pd1 N3 C17' C18' 26(28) . . . . ? C20 N4 C18' C17' 156(22) . . . . ? C19 N4 C18' C17' -94(22) . . . . ? C18 N4 C18' C17' -53(21) . . . . ? Pd1 N4 C18' C17' 43(23) . . . . ? N3 C17' C18' N4 -47(31) . . . . ? O4 S1 C21 F1 -177(5) . . . . ? O2 S1 C21 F1 -56(6) . . . . ? O3 S1 C21 F1 64(6) . . . . ? O4 S1 C21 F3 -56(6) . . . . ? O2 S1 C21 F3 65(5) . . . . ? O3 S1 C21 F3 -175(5) . . . . ? O4 S1 C21 F2 63(5) . . . . ? O2 S1 C21 F2 -176(4) . . . . ? O3 S1 C21 F2 -56(5) . . . . ? O5 S2 C22 F6 -62(8) . . . . ? O6 S2 C22 F6 59(7) . . . . ? O7 S2 C22 F6 178(7) . . . . ? O5 S2 C22 F4 177(10) . . . . ? O6 S2 C22 F4 -62(11) . . . . ? O7 S2 C22 F4 56(11) . . . . ? O5 S2 C22 F5 58(9) . . . . ? O6 S2 C22 F5 179(8) . . . . ? O7 S2 C22 F5 -63(8) . . . . ? C23 C23 C24 C25 179(13) 2_556 . . . ? C23 C24 C25 C26 152(15) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.823 _refine_diff_density_min -1.780 _refine_diff_density_rms 0.138