Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Mark John Sarsfield' 'Madeleine Helliwell' 'Helen Steele' 'Simon J. Teat' _publ_contact_author_name 'Dr Mark John Sarsfield' _publ_contact_author_address ; Department of Chemistry The University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email MARK.J.SARSFIELD@MAN.AC.UK _publ_section_title ; Uranyl Bis-Iminophosphorane Complexes with In and Out-of-Plane Equatorial Coordination ; data_s1286babs _database_code_CSD 209174 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; #------------------------------------------------------------------------------ _publ_section_exptl_refinement ; The structure was solved by direct methods. The asymmetric unit contains 2 molecules and 2 THF solvent molecules. C36 and C37 were disordered over 2 sites each whose occupancies were constrained to sum to 1.0, with isotropic thermal parameters constrained to be equal, and restraints on the bond lengths. The non-H atoms were refined anisotropically, except for the disordered atoms. H atoms bonded were included in calculated positions, except for H1 and H40, which were found by difference Fourier techniques and refined isotropically. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H55 Cl N2 O4 P2 Si2 U' _chemical_formula_weight 1007.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.410(3) _cell_length_b 24.902(4) _cell_length_c 16.987(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.577(3) _cell_angle_gamma 90.00 _cell_volume 8458(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5046 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.38 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4016 _exptl_absorpt_coefficient_mu 4.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.286 _exptl_absorpt_correction_T_max 0.443 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38900 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.41 _reflns_number_total 16867 _reflns_number_gt 13415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0567P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16867 _refine_ls_number_parameters 936 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.123531(7) 0.410604(7) 0.130661(9) 0.01089(6) Uani 1 1 d . . . O1 O 0.18446(13) 0.36130(12) 0.12244(18) 0.0146(7) Uani 1 1 d . . . O2 O 0.05951(14) 0.45942(13) 0.13001(18) 0.0158(7) Uani 1 1 d . . . O5 O 0.30674(13) 0.87323(13) 0.36956(17) 0.0150(7) Uani 1 1 d . . . N1 N 0.15939(17) 0.43201(15) 0.2774(2) 0.0121(8) Uani 1 1 d . . . N2 N 0.02696(16) 0.34651(15) 0.0873(2) 0.0123(8) Uani 1 1 d . . . C1 C 0.0949(2) 0.33930(18) 0.2393(2) 0.0106(9) Uani 1 1 d . . . H1 H 0.124(3) 0.317(3) 0.237(4) 0.05(2) Uiso 1 1 d . . . Cl1 Cl 0.21360(5) 0.48636(5) 0.11594(7) 0.0205(2) Uani 1 1 d . . . P1 P 0.12245(5) 0.38494(5) 0.31523(7) 0.0110(2) Uani 1 1 d . . . P2 P 0.02185(5) 0.32239(5) 0.17320(7) 0.0117(2) Uani 1 1 d . . . Si1 Si 0.18460(6) 0.49353(5) 0.32241(7) 0.0141(3) Uani 1 1 d . . . Si2 Si -0.02292(6) 0.33131(5) -0.00491(7) 0.0154(3) Uani 1 1 d . . . C2 C 0.1782(2) 0.34716(18) 0.3918(3) 0.0136(9) Uani 1 1 d . . . C3 C 0.2432(2) 0.36410(19) 0.4233(3) 0.0176(10) Uani 1 1 d . . . H3 H 0.2585 0.3973 0.4064 0.021 Uiso 1 1 calc R . . C4 C 0.2856(2) 0.3331(2) 0.4789(3) 0.0241(11) Uani 1 1 d . . . H4 H 0.3301 0.3447 0.4992 0.029 Uiso 1 1 calc R . . C5 C 0.2633(2) 0.2853(2) 0.5047(3) 0.0243(11) Uani 1 1 d . . . H5 H 0.2926 0.2641 0.5430 0.029 Uiso 1 1 calc R . . C6 C 0.1990(2) 0.2677(2) 0.4757(3) 0.0242(11) Uani 1 1 d . . . H6 H 0.1836 0.2352 0.4949 0.029 Uiso 1 1 calc R . . C7 C 0.1569(2) 0.29782(18) 0.4186(3) 0.0175(10) Uani 1 1 d . . . H7 H 0.1131 0.2851 0.3971 0.021 Uiso 1 1 calc R . . C8 C 0.0553(2) 0.41070(18) 0.3604(3) 0.0132(9) Uani 1 1 d . . . C9 C 0.0456(2) 0.3951(2) 0.4357(3) 0.0197(10) Uani 1 1 d . . . H9 H 0.0739 0.3688 0.4655 0.024 Uiso 1 1 calc R . . C10 C -0.0058(2) 0.4183(2) 0.4674(3) 0.0221(11) Uani 1 1 d . . . H10 H -0.0120 0.4080 0.5192 0.026 Uiso 1 1 calc R . . C11 C -0.0474(2) 0.4560(2) 0.4242(3) 0.0220(11) Uani 1 1 d . . . H11 H -0.0822 0.4715 0.4462 0.026 Uiso 1 1 calc R . . C12 C -0.0386(2) 0.47135(19) 0.3489(3) 0.0172(10) Uani 1 1 d . . . H12 H -0.0676 0.4971 0.3189 0.021 Uiso 1 1 calc R . . C13 C 0.0129(2) 0.44901(19) 0.3171(3) 0.0155(10) Uani 1 1 d . . . H13 H 0.0192 0.4599 0.2655 0.019 Uiso 1 1 calc R . . C14 C -0.0506(2) 0.34569(18) 0.2086(3) 0.0147(9) Uani 1 1 d . . . C15 C -0.0619(2) 0.33063(19) 0.2845(3) 0.0190(10) Uani 1 1 d . . . H15 H -0.0311 0.3077 0.3181 0.023 Uiso 1 1 calc R . . C16 C -0.1181(2) 0.3494(2) 0.3102(3) 0.0212(11) Uani 1 1 d . . . H16 H -0.1256 0.3395 0.3617 0.025 Uiso 1 1 calc R . . C17 C -0.1639(2) 0.3828(2) 0.2607(3) 0.0265(12) Uani 1 1 d . . . H17 H -0.2031 0.3945 0.2777 0.032 Uiso 1 1 calc R . . C18 C -0.1518(2) 0.3986(2) 0.1869(3) 0.0222(11) Uani 1 1 d . . . H18 H -0.1823 0.4219 0.1537 0.027 Uiso 1 1 calc R . . C19 C -0.0954(2) 0.38072(19) 0.1613(3) 0.0176(10) Uani 1 1 d . . . H19 H -0.0871 0.3924 0.1110 0.021 Uiso 1 1 calc R . . C20 C 0.0190(2) 0.24938(18) 0.1715(3) 0.0155(9) Uani 1 1 d . . . C21 C -0.0297(2) 0.2190(2) 0.1975(3) 0.0252(11) Uani 1 1 d . . . H21 H -0.0653 0.2364 0.2157 0.030 Uiso 1 1 calc R . . C22 C -0.0266(3) 0.1635(2) 0.1971(3) 0.0329(13) Uani 1 1 d . . . H22 H -0.0603 0.1431 0.2148 0.039 Uiso 1 1 calc R . . C23 C 0.0243(3) 0.1377(2) 0.1714(3) 0.0324(13) Uani 1 1 d . . . H23 H 0.0265 0.0996 0.1724 0.039 Uiso 1 1 calc R . . C24 C 0.0728(3) 0.1671(2) 0.1439(3) 0.0293(12) Uani 1 1 d . . . H24 H 0.1079 0.1492 0.1253 0.035 Uiso 1 1 calc R . . C25 C 0.0701(2) 0.22286(19) 0.1435(3) 0.0207(10) Uani 1 1 d . . . H25 H 0.1031 0.2430 0.1242 0.025 Uiso 1 1 calc R . . C26 C 0.1717(2) 0.4966(2) 0.4285(3) 0.0221(11) Uani 1 1 d . . . H26A H 0.1238 0.4989 0.4285 0.033 Uiso 1 1 calc R . . H26B H 0.1944 0.5284 0.4552 0.033 Uiso 1 1 calc R . . H26C H 0.1903 0.4642 0.4574 0.033 Uiso 1 1 calc R . . C27 C 0.2759(2) 0.50475(19) 0.3259(3) 0.0197(10) Uani 1 1 d . . . H27A H 0.3019 0.4771 0.3594 0.030 Uiso 1 1 calc R . . H27B H 0.2887 0.5403 0.3486 0.030 Uiso 1 1 calc R . . H27C H 0.2847 0.5027 0.2713 0.030 Uiso 1 1 calc R . . C28 C 0.1350(2) 0.54950(19) 0.2673(3) 0.0226(11) Uani 1 1 d . . . H28A H 0.1398 0.5492 0.2110 0.034 Uiso 1 1 calc R . . H28B H 0.1512 0.5838 0.2920 0.034 Uiso 1 1 calc R . . H28C H 0.0877 0.5450 0.2698 0.034 Uiso 1 1 calc R . . C29 C -0.0615(2) 0.3927(2) -0.0575(3) 0.0264(12) Uani 1 1 d . . . H29A H -0.0973 0.4055 -0.0316 0.040 Uiso 1 1 calc R . . H29B H -0.0799 0.3842 -0.1139 0.040 Uiso 1 1 calc R . . H29C H -0.0274 0.4208 -0.0546 0.040 Uiso 1 1 calc R . . C30 C -0.0924(2) 0.2835(2) 0.0031(3) 0.0268(12) Uani 1 1 d . . . H30A H -0.0735 0.2483 0.0206 0.040 Uiso 1 1 calc R . . H30B H -0.1224 0.2800 -0.0495 0.040 Uiso 1 1 calc R . . H30C H -0.1175 0.2972 0.0422 0.040 Uiso 1 1 calc R . . C31 C 0.0286(2) 0.2970(2) -0.0684(3) 0.0277(12) Uani 1 1 d . . . H31A H 0.0673 0.3195 -0.0721 0.041 Uiso 1 1 calc R . . H31B H 0.0016 0.2912 -0.1223 0.041 Uiso 1 1 calc R . . H31C H 0.0440 0.2624 -0.0442 0.041 Uiso 1 1 calc R . . C32 C 0.1644(2) 0.4034(2) -0.0562(3) 0.0213(11) Uani 1 1 d . . . H32A H 0.1731 0.3647 -0.0455 0.026 Uiso 1 1 calc R . . H32B H 0.2066 0.4236 -0.0385 0.026 Uiso 1 1 calc R . . C33 C 0.1356(3) 0.4132(2) -0.1455(3) 0.0276(12) Uani 1 1 d . . . H33A H 0.1121 0.3810 -0.1710 0.033 Uiso 1 1 calc R . . H33B H 0.1713 0.4232 -0.1745 0.033 Uiso 1 1 calc R . . C34 C 0.0865(3) 0.4601(2) -0.1448(3) 0.0291(12) Uani 1 1 d . . . H34A H 0.0995 0.4915 -0.1740 0.035 Uiso 1 1 calc R . . H34B H 0.0404 0.4493 -0.1702 0.035 Uiso 1 1 calc R . . C35 C 0.0912(2) 0.47321(19) -0.0566(3) 0.0220(11) Uani 1 1 d . . . H35A H 0.1241 0.5021 -0.0390 0.026 Uiso 1 1 calc R . . H35B H 0.0472 0.4845 -0.0462 0.026 Uiso 1 1 calc R . . U2 U 0.371655(7) 0.919742(7) 0.363093(9) 0.01081(6) Uani 1 1 d . . . O3 O 0.11297(15) 0.42270(12) -0.01549(19) 0.0163(7) Uani 1 1 d . . . O4 O 0.43957(13) 0.96490(12) 0.36649(17) 0.0144(7) Uani 1 1 d . . . O6 O 0.38285(14) 0.93239(13) 0.50847(18) 0.0152(7) Uani 1 1 d . . . N3 N 0.46061(16) 0.84912(15) 0.4038(2) 0.0134(8) Uani 1 1 d . . . N4 N 0.33902(16) 0.94531(14) 0.2167(2) 0.0104(7) Uani 1 1 d . . . C40 C 0.3944(2) 0.84871(19) 0.2514(3) 0.0127(9) Uani 1 1 d . . . H40 H 0.364(2) 0.833(2) 0.254(3) 0.027(16) Uiso 1 1 d . . . Cl2 Cl 0.28583(5) 0.99940(5) 0.37914(7) 0.0182(2) Uani 1 1 d . . . P3 P 0.46373(5) 0.82511(5) 0.31766(7) 0.0114(2) Uani 1 1 d . . . P4 P 0.37163(5) 0.89667(5) 0.17729(7) 0.0112(2) Uani 1 1 d . . . Si3 Si 0.50313(6) 0.82748(5) 0.49755(7) 0.0147(3) Uani 1 1 d . . . Si4 Si 0.31987(6) 1.00965(5) 0.17774(7) 0.0140(3) Uani 1 1 d . . . C41 C 0.31286(19) 0.86437(18) 0.0973(3) 0.0122(9) Uani 1 1 d . . . C42 C 0.2511(2) 0.88697(18) 0.0659(3) 0.0162(10) Uani 1 1 d . . . H42 H 0.2397 0.9206 0.0858 0.019 Uiso 1 1 calc R . . C43 C 0.2058(2) 0.8616(2) 0.0061(3) 0.0210(11) Uani 1 1 d . . . H43 H 0.1635 0.8776 -0.0141 0.025 Uiso 1 1 calc R . . C44 C 0.2221(2) 0.8125(2) -0.0246(3) 0.0220(11) Uani 1 1 d . . . H44 H 0.1915 0.7952 -0.0665 0.026 Uiso 1 1 calc R . . C45 C 0.2834(2) 0.7894(2) 0.0068(3) 0.0221(11) Uani 1 1 d . . . H45 H 0.2949 0.7559 -0.0137 0.027 Uiso 1 1 calc R . . C46 C 0.3281(2) 0.81424(18) 0.0676(3) 0.0170(10) Uani 1 1 d . . . H46 H 0.3695 0.7974 0.0894 0.020 Uiso 1 1 calc R . . C47 C 0.4423(2) 0.91746(18) 0.1343(3) 0.0132(9) Uani 1 1 d . . . C48 C 0.4509(2) 0.9022(2) 0.0588(3) 0.0190(10) Uani 1 1 d . . . H48 H 0.4195 0.8790 0.0266 0.023 Uiso 1 1 calc R . . C49 C 0.5059(2) 0.9211(2) 0.0303(3) 0.0249(12) Uani 1 1 d . . . H49 H 0.5118 0.9107 -0.0216 0.030 Uiso 1 1 calc R . . C50 C 0.5518(2) 0.9546(2) 0.0760(3) 0.0228(11) Uani 1 1 d . . . H50 H 0.5890 0.9673 0.0556 0.027 Uiso 1 1 calc R . . C51 C 0.5439(2) 0.9699(2) 0.1517(3) 0.0187(10) Uani 1 1 d . . . H51 H 0.5759 0.9927 0.1837 0.022 Uiso 1 1 calc R . . C52 C 0.4888(2) 0.95179(19) 0.1811(3) 0.0162(10) Uani 1 1 d . . . H52 H 0.4828 0.9627 0.2328 0.019 Uiso 1 1 calc R . . C53 C 0.5405(2) 0.84146(18) 0.2855(3) 0.0147(9) Uani 1 1 d . . . C54 C 0.5520(2) 0.82599(19) 0.2102(3) 0.0178(10) Uani 1 1 d . . . H54 H 0.5183 0.8074 0.1735 0.021 Uiso 1 1 calc R . . C55 C 0.6125(2) 0.8379(2) 0.1895(3) 0.0235(11) Uani 1 1 d . . . H55 H 0.6206 0.8270 0.1387 0.028 Uiso 1 1 calc R . . C56 C 0.6613(2) 0.8658(2) 0.2426(3) 0.0258(12) Uani 1 1 d . . . H56 H 0.7029 0.8736 0.2281 0.031 Uiso 1 1 calc R . . C57 C 0.6501(2) 0.8821(2) 0.3159(3) 0.0237(11) Uani 1 1 d . . . H57 H 0.6835 0.9016 0.3515 0.028 Uiso 1 1 calc R . . C58 C 0.5894(2) 0.86988(19) 0.3379(3) 0.0195(10) Uani 1 1 d . . . H58 H 0.5815 0.8810 0.3887 0.023 Uiso 1 1 calc R . . C59 C 0.45587(19) 0.75214(18) 0.3184(2) 0.0129(9) Uani 1 1 d . . . C60 C 0.4971(2) 0.71664(19) 0.2873(3) 0.0188(10) Uani 1 1 d . . . H60 H 0.5317 0.7300 0.2627 0.023 Uiso 1 1 calc R . . C61 C 0.4873(2) 0.6615(2) 0.2925(3) 0.0273(12) Uani 1 1 d . . . H61 H 0.5156 0.6374 0.2717 0.033 Uiso 1 1 calc R . . C62 C 0.4369(2) 0.6414(2) 0.3273(3) 0.0244(11) Uani 1 1 d . . . H62 H 0.4305 0.6037 0.3302 0.029 Uiso 1 1 calc R . . C63 C 0.3954(2) 0.6766(2) 0.3582(3) 0.0229(11) Uani 1 1 d . . . H63 H 0.3607 0.6631 0.3824 0.028 Uiso 1 1 calc R . . C64 C 0.4050(2) 0.73151(19) 0.3536(3) 0.0184(10) Uani 1 1 d . . . H64 H 0.3766 0.7554 0.3747 0.022 Uiso 1 1 calc R . . C65 C 0.4424(2) 0.7997(2) 0.5554(3) 0.0265(11) Uani 1 1 d . . . H65A H 0.4059 0.8253 0.5544 0.040 Uiso 1 1 calc R . . H65B H 0.4652 0.7934 0.6112 0.040 Uiso 1 1 calc R . . H65C H 0.4243 0.7657 0.5312 0.040 Uiso 1 1 calc R . . C66 C 0.5497(2) 0.8833(2) 0.5558(3) 0.0240(11) Uani 1 1 d . . . H66A H 0.5858 0.8951 0.5295 0.036 Uiso 1 1 calc R . . H66B H 0.5687 0.8710 0.6104 0.036 Uiso 1 1 calc R . . H66C H 0.5192 0.9134 0.5583 0.036 Uiso 1 1 calc R . . C67 C 0.5640(2) 0.7722(2) 0.4911(3) 0.0256(12) Uani 1 1 d . . . H67A H 0.5396 0.7399 0.4690 0.038 Uiso 1 1 calc R . . H67B H 0.5900 0.7644 0.5449 0.038 Uiso 1 1 calc R . . H67C H 0.5942 0.7834 0.4560 0.038 Uiso 1 1 calc R . . C68 C 0.3380(2) 1.0172(2) 0.0739(3) 0.0226(11) Uani 1 1 d . . . H68A H 0.3865 1.0180 0.0773 0.034 Uiso 1 1 calc R . . H68B H 0.3182 1.0507 0.0498 0.034 Uiso 1 1 calc R . . H68C H 0.3188 0.9868 0.0405 0.034 Uiso 1 1 calc R . . C69 C 0.2290(2) 1.02531(19) 0.1705(3) 0.0207(10) Uani 1 1 d . . . H69A H 0.2022 1.0037 0.1276 0.031 Uiso 1 1 calc R . . H69B H 0.2212 1.0635 0.1583 0.031 Uiso 1 1 calc R . . H69C H 0.2162 1.0169 0.2217 0.031 Uiso 1 1 calc R . . C70 C 0.3723(2) 1.06091(19) 0.2403(3) 0.0218(11) Uani 1 1 d . . . H70A H 0.3642 1.0596 0.2952 0.033 Uiso 1 1 calc R . . H70B H 0.3608 1.0966 0.2175 0.033 Uiso 1 1 calc R . . H70C H 0.4196 1.0536 0.2411 0.033 Uiso 1 1 calc R . . C71 C 0.6761(2) 0.7176(2) 0.2856(3) 0.0298(12) Uani 1 1 d . . . H71A H 0.6692 0.6894 0.3242 0.036 Uiso 1 1 calc R . . H71B H 0.6538 0.7509 0.2981 0.036 Uiso 1 1 calc R . . C72 C 0.7504(2) 0.7274(3) 0.2908(4) 0.0458(17) Uani 1 1 d . . . H72A H 0.7621 0.7652 0.3055 0.055 Uiso 1 1 calc R . . H72B H 0.7775 0.7035 0.3313 0.055 Uiso 1 1 calc R . . C73 C 0.7616(3) 0.7157(4) 0.2126(4) 0.080(3) Uani 1 1 d . . . H73A H 0.8036 0.6950 0.2165 0.096 Uiso 1 1 calc R . . H73B H 0.7657 0.7494 0.1831 0.096 Uiso 1 1 calc R . . C74 C 0.7045(3) 0.6840(3) 0.1697(3) 0.0389(15) Uani 1 1 d . . . H74A H 0.6957 0.6919 0.1114 0.047 Uiso 1 1 calc R . . H74B H 0.7130 0.6451 0.1777 0.047 Uiso 1 1 calc R . . O7 O 0.2454(3) 0.7501(3) 0.1981(4) 0.106(2) Uani 1 1 d . . . C36A C 0.2173(5) 0.7342(4) 0.2711(6) 0.035(2) Uiso 0.644(8) 1 d PD A 1 H36A H 0.2533 0.7294 0.3192 0.042 Uiso 0.644(8) 1 calc PR A 1 H36B H 0.1849 0.7612 0.2828 0.042 Uiso 0.644(8) 1 calc PR A 1 C37A C 0.1841(3) 0.6828(3) 0.2445(5) 0.0126(13) Uiso 0.644(8) 1 d PD A 1 H37A H 0.1729 0.6630 0.2906 0.015 Uiso 0.644(8) 1 calc PR A 1 H37B H 0.1426 0.6889 0.2040 0.015 Uiso 0.644(8) 1 calc PR A 1 C36B C 0.1916(8) 0.7263(6) 0.2422(10) 0.035(2) Uiso 0.356(8) 1 d PD A 2 H36C H 0.1845 0.7514 0.2849 0.042 Uiso 0.356(8) 1 calc PR A 2 H36D H 0.1487 0.7223 0.2035 0.042 Uiso 0.356(8) 1 calc PR A 2 C37B C 0.2111(7) 0.6784(5) 0.2750(8) 0.0126(13) Uiso 0.356(8) 1 d PD A 2 H37C H 0.1734 0.6587 0.2902 0.015 Uiso 0.356(8) 1 calc PR A 2 H37D H 0.2478 0.6820 0.3225 0.015 Uiso 0.356(8) 1 calc PR A 2 C38 C 0.2330(3) 0.6535(3) 0.2099(4) 0.0485(17) Uani 1 1 d . . . H38A H 0.2109 0.6258 0.1719 0.058 Uiso 1 1 calc R A 1 H38B H 0.2664 0.6359 0.2524 0.058 Uiso 1 1 calc R A 1 C39 C 0.2663(3) 0.6961(2) 0.1661(4) 0.0406(15) Uani 1 1 d . A . H39A H 0.2503 0.6935 0.1072 0.049 Uiso 1 1 calc R . . H39B H 0.3156 0.6920 0.1785 0.049 Uiso 1 1 calc R . . O8 O 0.64904(15) 0.70058(15) 0.2045(2) 0.0317(9) Uani 1 1 d . . . C75 C 0.3296(2) 0.91762(19) 0.5491(3) 0.0187(10) Uani 1 1 d . . . H75A H 0.3166 0.8796 0.5385 0.022 Uiso 1 1 calc R . . H75B H 0.2898 0.9406 0.5312 0.022 Uiso 1 1 calc R . . C76 C 0.3588(2) 0.9264(2) 0.6378(3) 0.0211(11) Uani 1 1 d . . . H76A H 0.3799 0.8932 0.6629 0.025 Uiso 1 1 calc R . . H76B H 0.3238 0.9381 0.6668 0.025 Uiso 1 1 calc R . . C77 C 0.4111(2) 0.9708(2) 0.6381(3) 0.0270(12) Uani 1 1 d . . . H77A H 0.3991 1.0035 0.6650 0.032 Uiso 1 1 calc R . . H77B H 0.4560 0.9586 0.6659 0.032 Uiso 1 1 calc R . . C78 C 0.4098(2) 0.98147(19) 0.5497(3) 0.0198(10) Uani 1 1 d . . . H78A H 0.3809 1.0126 0.5305 0.024 Uiso 1 1 calc R . . H78B H 0.4554 0.9887 0.5407 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01285(9) 0.00808(10) 0.01188(10) 0.00090(6) 0.00278(6) -0.00040(6) O1 0.0156(14) 0.0126(18) 0.0154(16) 0.0021(13) 0.0031(12) -0.0001(12) O2 0.0206(15) 0.0110(18) 0.0151(17) -0.0017(13) 0.0017(12) 0.0032(13) O5 0.0165(14) 0.0153(18) 0.0134(16) -0.0035(13) 0.0033(12) -0.0006(13) N1 0.0186(17) 0.009(2) 0.0088(18) 0.0000(15) 0.0026(14) -0.0024(15) N2 0.0139(16) 0.010(2) 0.0124(19) -0.0042(15) 0.0012(14) -0.0024(15) C1 0.016(2) 0.008(2) 0.008(2) -0.0012(17) 0.0040(17) -0.0002(17) Cl1 0.0236(5) 0.0189(7) 0.0191(6) 0.0020(5) 0.0045(4) -0.0091(5) P1 0.0138(5) 0.0079(6) 0.0116(6) 0.0004(4) 0.0029(4) 0.0004(4) P2 0.0124(5) 0.0074(6) 0.0154(6) -0.0008(4) 0.0028(4) -0.0007(4) Si1 0.0166(6) 0.0082(7) 0.0171(7) -0.0019(5) 0.0024(5) -0.0014(5) Si2 0.0175(6) 0.0125(7) 0.0148(7) 0.0001(5) 0.0001(5) -0.0012(5) C2 0.017(2) 0.012(2) 0.011(2) -0.0007(18) 0.0011(17) 0.0004(18) C3 0.020(2) 0.015(3) 0.019(2) -0.0025(19) 0.0052(18) 0.0006(19) C4 0.023(2) 0.033(3) 0.016(3) 0.000(2) 0.0028(19) 0.008(2) C5 0.031(3) 0.022(3) 0.019(3) 0.003(2) 0.002(2) 0.011(2) C6 0.035(3) 0.013(3) 0.024(3) 0.004(2) 0.005(2) 0.005(2) C7 0.020(2) 0.010(2) 0.022(3) 0.0017(19) 0.0025(19) -0.0013(18) C8 0.015(2) 0.010(2) 0.014(2) -0.0044(18) 0.0015(17) -0.0052(17) C9 0.022(2) 0.017(3) 0.019(3) 0.002(2) 0.0019(19) 0.001(2) C10 0.026(2) 0.030(3) 0.011(2) 0.001(2) 0.006(2) -0.001(2) C11 0.019(2) 0.027(3) 0.022(3) -0.007(2) 0.0090(19) 0.005(2) C12 0.016(2) 0.015(3) 0.021(3) -0.005(2) 0.0034(18) 0.0001(18) C13 0.020(2) 0.014(3) 0.013(2) -0.0003(19) 0.0045(18) -0.0011(19) C14 0.014(2) 0.010(2) 0.019(2) -0.0006(19) 0.0028(18) -0.0020(18) C15 0.022(2) 0.016(3) 0.021(3) -0.005(2) 0.0083(19) -0.0080(19) C16 0.025(2) 0.018(3) 0.021(3) -0.003(2) 0.009(2) -0.005(2) C17 0.016(2) 0.032(3) 0.034(3) -0.013(2) 0.009(2) -0.003(2) C18 0.016(2) 0.017(3) 0.032(3) -0.006(2) 0.001(2) 0.0031(19) C19 0.018(2) 0.016(3) 0.019(2) -0.003(2) 0.0025(18) -0.0031(19) C20 0.020(2) 0.007(2) 0.017(2) -0.0009(18) -0.0012(17) -0.0015(18) C21 0.031(3) 0.018(3) 0.028(3) -0.002(2) 0.010(2) -0.007(2) C22 0.054(3) 0.017(3) 0.026(3) 0.002(2) 0.003(3) -0.014(3) C23 0.063(4) 0.007(3) 0.022(3) 0.000(2) -0.004(3) -0.001(3) C24 0.036(3) 0.017(3) 0.030(3) -0.008(2) -0.005(2) 0.011(2) C25 0.025(2) 0.012(3) 0.023(3) -0.005(2) 0.001(2) -0.001(2) C26 0.025(2) 0.019(3) 0.022(3) -0.008(2) 0.004(2) -0.005(2) C27 0.022(2) 0.012(3) 0.024(3) -0.001(2) 0.0010(19) -0.0026(19) C28 0.025(2) 0.010(3) 0.032(3) 0.001(2) 0.005(2) 0.002(2) C29 0.029(3) 0.018(3) 0.028(3) 0.003(2) -0.006(2) 0.002(2) C30 0.026(2) 0.025(3) 0.026(3) -0.003(2) -0.002(2) -0.011(2) C31 0.036(3) 0.025(3) 0.023(3) -0.010(2) 0.007(2) -0.002(2) C32 0.023(2) 0.023(3) 0.020(3) -0.002(2) 0.008(2) 0.001(2) C33 0.032(3) 0.033(3) 0.019(3) -0.004(2) 0.008(2) -0.007(2) C34 0.044(3) 0.024(3) 0.018(3) 0.005(2) 0.003(2) -0.003(2) C35 0.034(3) 0.013(3) 0.019(3) 0.005(2) 0.004(2) -0.001(2) U2 0.01274(8) 0.00862(10) 0.01126(10) -0.00035(6) 0.00283(6) 0.00046(6) O3 0.0222(16) 0.0118(18) 0.0155(17) 0.0003(13) 0.0055(13) 0.0010(13) O4 0.0170(14) 0.0117(18) 0.0135(16) 0.0001(13) 0.0006(12) 0.0021(13) O6 0.0183(15) 0.0150(18) 0.0130(17) -0.0027(13) 0.0049(12) -0.0021(13) N3 0.0128(16) 0.014(2) 0.0135(19) 0.0013(16) 0.0018(14) 0.0022(15) N4 0.0146(16) 0.0048(19) 0.0113(19) 0.0009(14) 0.0012(14) 0.0006(14) C40 0.014(2) 0.011(2) 0.015(2) -0.0017(18) 0.0044(18) -0.0019(18) Cl2 0.0222(5) 0.0150(6) 0.0176(6) -0.0009(5) 0.0045(4) 0.0066(4) P3 0.0130(5) 0.0083(6) 0.0131(6) 0.0004(4) 0.0030(4) 0.0012(4) P4 0.0127(5) 0.0095(6) 0.0114(6) -0.0004(4) 0.0024(4) -0.0007(4) Si3 0.0185(6) 0.0098(7) 0.0144(7) 0.0010(5) 0.0004(5) 0.0017(5) Si4 0.0179(6) 0.0087(7) 0.0153(7) 0.0012(5) 0.0033(5) 0.0010(5) C41 0.016(2) 0.007(2) 0.013(2) 0.0017(17) 0.0031(17) -0.0045(17) C42 0.021(2) 0.010(2) 0.019(2) 0.0003(19) 0.0056(18) -0.0016(18) C43 0.019(2) 0.020(3) 0.022(3) 0.001(2) -0.0008(19) -0.004(2) C44 0.024(2) 0.026(3) 0.016(3) -0.002(2) 0.0036(19) -0.011(2) C45 0.028(2) 0.020(3) 0.020(3) -0.006(2) 0.010(2) -0.008(2) C46 0.022(2) 0.010(3) 0.020(3) -0.0025(19) 0.0065(19) 0.0011(19) C47 0.0121(19) 0.011(2) 0.017(2) 0.0037(18) 0.0022(18) -0.0004(17) C48 0.021(2) 0.021(3) 0.016(2) -0.003(2) 0.0040(19) 0.000(2) C49 0.023(2) 0.037(3) 0.016(3) -0.001(2) 0.008(2) -0.003(2) C50 0.017(2) 0.035(3) 0.019(3) 0.008(2) 0.0073(19) -0.003(2) C51 0.017(2) 0.020(3) 0.018(3) 0.002(2) 0.0005(18) -0.0056(19) C52 0.023(2) 0.013(3) 0.013(2) 0.0019(19) 0.0045(18) -0.0011(19) C53 0.017(2) 0.011(2) 0.017(2) 0.0031(19) 0.0050(18) 0.0040(18) C54 0.020(2) 0.012(3) 0.020(3) 0.001(2) 0.0029(19) 0.0019(19) C55 0.025(2) 0.024(3) 0.025(3) 0.003(2) 0.011(2) 0.007(2) C56 0.017(2) 0.028(3) 0.035(3) 0.009(2) 0.012(2) 0.001(2) C57 0.018(2) 0.024(3) 0.029(3) 0.005(2) 0.005(2) 0.000(2) C58 0.022(2) 0.017(3) 0.020(3) 0.000(2) 0.0049(19) 0.001(2) C59 0.0136(19) 0.010(2) 0.013(2) 0.0004(18) -0.0015(16) 0.0012(17) C60 0.018(2) 0.015(3) 0.021(3) -0.002(2) 0.0011(19) 0.0010(19) C61 0.033(3) 0.015(3) 0.031(3) -0.005(2) 0.002(2) 0.012(2) C62 0.040(3) 0.005(3) 0.023(3) 0.001(2) -0.006(2) -0.001(2) C63 0.030(2) 0.014(3) 0.022(3) 0.004(2) 0.000(2) -0.003(2) C64 0.024(2) 0.013(3) 0.019(3) 0.0004(19) 0.0050(19) -0.0036(19) C65 0.035(3) 0.021(3) 0.022(3) 0.006(2) 0.003(2) 0.003(2) C66 0.026(2) 0.021(3) 0.021(3) -0.004(2) -0.004(2) 0.000(2) C67 0.028(2) 0.021(3) 0.023(3) -0.002(2) -0.006(2) 0.011(2) C68 0.028(2) 0.016(3) 0.022(3) 0.010(2) 0.003(2) 0.005(2) C69 0.024(2) 0.015(3) 0.022(3) 0.002(2) 0.004(2) 0.004(2) C70 0.029(2) 0.009(3) 0.027(3) 0.000(2) 0.005(2) -0.001(2) C71 0.026(2) 0.022(3) 0.039(3) -0.004(2) 0.000(2) -0.002(2) C72 0.028(3) 0.036(4) 0.069(5) -0.017(3) -0.001(3) -0.005(3) C73 0.042(4) 0.170(10) 0.030(4) -0.014(5) 0.010(3) -0.041(5) C74 0.039(3) 0.047(4) 0.031(3) 0.010(3) 0.007(3) -0.008(3) O7 0.159(6) 0.069(5) 0.110(5) 0.014(4) 0.074(5) 0.002(4) C38 0.059(4) 0.034(4) 0.058(4) 0.004(3) 0.023(3) -0.006(3) C39 0.040(3) 0.035(4) 0.052(4) 0.012(3) 0.021(3) 0.011(3) O8 0.0265(17) 0.031(2) 0.033(2) 0.0004(17) -0.0047(15) -0.0017(16) C75 0.020(2) 0.019(3) 0.019(3) 0.0006(19) 0.008(2) 0.0010(19) C76 0.032(2) 0.019(3) 0.013(2) 0.001(2) 0.005(2) 0.003(2) C77 0.038(3) 0.027(3) 0.016(3) -0.004(2) 0.007(2) 0.001(2) C78 0.027(2) 0.013(3) 0.018(3) -0.0040(19) -0.0008(19) -0.002(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 U1 O1 1.773(3) . ? U1 O2 1.783(3) . ? U1 O3 2.467(3) . ? U1 N1 2.510(3) . ? U1 N2 2.528(3) . ? U1 Cl1 2.6806(11) . ? U1 C1 2.707(4) . ? U1 P2 3.2027(12) . ? U1 P1 3.2042(12) . ? N1 P1 1.597(4) . ? N1 Si1 1.743(4) . ? N2 P2 1.601(4) . ? N2 Si2 1.730(4) . ? C1 P1 1.727(4) . ? C1 P2 1.729(4) . ? C1 H1 0.80(6) . ? P1 C2 1.810(4) . ? P1 C8 1.817(4) . ? P2 C14 1.800(4) . ? P2 C20 1.819(5) . ? Si1 C28 1.862(5) . ? Si1 C27 1.873(4) . ? Si1 C26 1.875(5) . ? Si2 C31 1.857(5) . ? Si2 C29 1.864(5) . ? Si2 C30 1.877(5) . ? C2 C3 1.392(6) . ? C2 C7 1.409(6) . ? C3 C4 1.382(6) . ? C3 H3 0.9500 . ? C4 C5 1.378(7) . ? C4 H4 0.9500 . ? C5 C6 1.377(6) . ? C5 H5 0.9500 . ? C6 C7 1.381(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.387(6) . ? C8 C13 1.395(6) . ? C9 C10 1.397(6) . ? C9 H9 0.9500 . ? C10 C11 1.374(7) . ? C10 H10 0.9500 . ? C11 C12 1.380(6) . ? C11 H11 0.9500 . ? C12 C13 1.391(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.396(6) . ? C14 C15 1.406(6) . ? C15 C16 1.389(6) . ? C15 H15 0.9500 . ? C16 C17 1.399(7) . ? C16 H16 0.9500 . ? C17 C18 1.383(7) . ? C17 H17 0.9500 . ? C18 C19 1.384(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.389(6) . ? C20 C25 1.396(6) . ? C21 C22 1.384(7) . ? C21 H21 0.9500 . ? C22 C23 1.366(7) . ? C22 H22 0.9500 . ? C23 C24 1.386(7) . ? C23 H23 0.9500 . ? C24 C25 1.389(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? 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 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 O3 1.449(5) . ? C32 C33 1.532(7) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.540(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.518(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O3 1.464(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? U2 O4 1.777(3) . ? O5 U2 1.780(3) . ? U2 O6 2.454(3) . ? U2 N3 2.523(3) . ? U2 N4 2.524(3) . ? U2 Cl2 2.6962(11) . ? U2 C40 2.702(4) . ? U2 P3 3.2035(12) . ? O6 C75 1.447(5) . ? O6 C78 1.461(5) . ? N3 P3 1.594(4) . ? N3 Si3 1.739(4) . ? N4 P4 1.593(4) . ? N4 Si4 1.748(4) . ? C40 P3 1.725(4) . ? C40 P4 1.729(5) . ? C40 H40 0.74(5) . ? P3 C53 1.807(4) . ? P3 C59 1.824(5) . ? P4 C41 1.811(4) . ? P4 C47 1.818(4) . ? Si3 C66 1.855(5) . ? Si3 C65 1.862(5) . ? Si3 C67 1.872(5) . ? Si4 C70 1.856(5) . ? Si4 C69 1.874(4) . ? Si4 C68 1.883(5) . ? C41 C42 1.386(6) . ? C41 C46 1.405(6) . ? C42 C43 1.381(6) . ? C42 H42 0.9500 . ? C43 C44 1.396(7) . ? C43 H43 0.9500 . ? C44 C45 1.384(6) . ? C44 H44 0.9500 . ? C45 C46 1.379(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.382(6) . ? C47 C52 1.401(6) . ? C48 C49 1.390(6) . ? C48 H48 0.9500 . ? C49 C50 1.373(7) . ? C49 H49 0.9500 . ? C50 C51 1.381(6) . ? C50 H50 0.9500 . ? C51 C52 1.394(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.389(6) . ? C53 C54 1.400(6) . ? C54 C55 1.382(6) . ? C54 H54 0.9500 . ? C55 C56 1.388(7) . ? C55 H55 0.9500 . ? C56 C57 1.372(7) . ? C56 H56 0.9500 . ? C57 C58 1.397(6) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.396(6) . ? C59 C64 1.396(6) . ? C60 C61 1.392(7) . ? C60 H60 0.9500 . ? C61 C62 1.380(7) . ? C61 H61 0.9500 . ? C62 C63 1.393(6) . ? C62 H62 0.9500 . ? C63 C64 1.385(7) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 O8 1.441(6) . ? C71 C72 1.522(6) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.424(8) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.473(8) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O8 1.438(6) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O7 C36A 1.518(10) . ? O7 C39 1.542(8) . ? O7 C36B 1.564(16) . ? C36A C37A 1.476(10) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A C38 1.453(8) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C36B C37B 1.342(14) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B C38 1.417(13) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38 C39 1.532(7) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C75 C76 1.520(6) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.536(7) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.519(6) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? 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 O1 U1 O2 175.12(13) . . ? O1 U1 O3 85.77(12) . . ? O2 U1 O3 89.69(12) . . ? O1 U1 N1 98.97(12) . . ? O2 U1 N1 85.91(12) . . ? O3 U1 N1 157.30(11) . . ? O1 U1 N2 93.32(12) . . ? O2 U1 N2 84.33(12) . . ? O3 U1 N2 83.01(11) . . ? N1 U1 N2 118.58(11) . . ? O1 U1 Cl1 88.57(10) . . ? O2 U1 Cl1 92.01(10) . . ? O3 U1 Cl1 75.12(7) . . ? N1 U1 Cl1 82.78(8) . . ? N2 U1 Cl1 157.86(8) . . ? O1 U1 C1 81.38(13) . . ? O2 U1 C1 101.15(13) . . ? O3 U1 C1 141.14(12) . . ? N1 U1 C1 61.47(12) . . ? N2 U1 C1 61.47(12) . . ? Cl1 U1 C1 140.43(9) . . ? O1 U1 P2 92.25(10) . . ? O2 U1 P2 87.81(10) . . ? O3 U1 P2 112.40(7) . . ? N1 U1 P2 89.70(8) . . ? N2 U1 P2 29.56(8) . . ? Cl1 U1 P2 172.47(3) . . ? C1 U1 P2 32.68(9) . . ? O1 U1 P1 94.69(10) . . ? O2 U1 P1 89.60(10) . . ? O3 U1 P1 173.08(7) . . ? N1 U1 P1 29.38(8) . . ? N2 U1 P1 90.06(8) . . ? Cl1 U1 P1 111.79(3) . . ? C1 U1 P1 32.61(9) . . ? P2 U1 P1 60.69(3) . . ? P1 N1 Si1 126.1(2) . . ? P1 N1 U1 100.19(17) . . ? Si1 N1 U1 128.61(19) . . ? P2 N2 Si2 127.5(2) . . ? P2 N2 U1 99.26(16) . . ? Si2 N2 U1 133.20(19) . . ? P1 C1 P2 139.0(3) . . ? P1 C1 U1 89.72(18) . . ? P2 C1 U1 89.61(17) . . ? P1 C1 H1 110(4) . . ? P2 C1 H1 111(4) . . ? U1 C1 H1 99(4) . . ? N1 P1 C1 106.9(2) . . ? N1 P1 C2 113.04(19) . . ? C1 P1 C2 105.0(2) . . ? N1 P1 C8 111.6(2) . . ? C1 P1 C8 112.8(2) . . ? C2 P1 C8 107.4(2) . . ? N1 P1 U1 50.43(13) . . ? C1 P1 U1 57.67(14) . . ? C2 P1 U1 132.84(14) . . ? C8 P1 U1 119.80(15) . . ? N2 P2 C1 107.15(19) . . ? N2 P2 C14 113.1(2) . . ? C1 P2 C14 111.3(2) . . ? N2 P2 C20 111.6(2) . . ? C1 P2 C20 105.9(2) . . ? C14 P2 C20 107.5(2) . . ? N2 P2 U1 51.18(12) . . ? C1 P2 U1 57.71(14) . . ? C14 P2 U1 117.84(15) . . ? C20 P2 U1 134.62(14) . . ? N1 Si1 C28 110.7(2) . . ? N1 Si1 C27 110.42(19) . . ? C28 Si1 C27 110.0(2) . . ? N1 Si1 C26 111.9(2) . . ? C28 Si1 C26 106.6(2) . . ? C27 Si1 C26 107.1(2) . . ? N2 Si2 C31 109.12(19) . . ? N2 Si2 C29 111.7(2) . . ? C31 Si2 C29 109.4(2) . . ? N2 Si2 C30 112.9(2) . . ? C31 Si2 C30 105.9(2) . . ? C29 Si2 C30 107.7(2) . . ? C3 C2 C7 118.2(4) . . ? C3 C2 P1 122.1(4) . . ? C7 C2 P1 119.7(3) . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.5(5) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 120.8(4) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C9 C8 C13 119.4(4) . . ? C9 C8 P1 123.3(3) . . ? C13 C8 P1 117.3(3) . . ? C8 C9 C10 119.7(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 C8 120.3(4) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C19 C14 C15 119.0(4) . . ? C19 C14 P2 119.8(3) . . ? C15 C14 P2 121.1(3) . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.3(5) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C14 120.7(4) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C21 C20 C25 118.8(4) . . ? C21 C20 P2 124.2(4) . . ? C25 C20 P2 117.0(3) . . ? C22 C21 C20 120.4(5) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.6(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C20 120.2(5) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 C33 104.4(4) . . ? O3 C32 H32A 110.9 . . ? C33 C32 H32A 110.9 . . ? O3 C32 H32B 110.9 . . ? C33 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? C32 C33 C34 103.6(4) . . ? C32 C33 H33A 111.0 . . ? C34 C33 H33A 111.0 . . ? C32 C33 H33B 111.0 . . ? C34 C33 H33B 111.0 . . ? H33A C33 H33B 109.0 . . ? C35 C34 C33 105.0(4) . . ? C35 C34 H34A 110.8 . . ? C33 C34 H34A 110.8 . . ? C35 C34 H34B 110.8 . . ? C33 C34 H34B 110.8 . . ? H34A C34 H34B 108.8 . . ? O3 C35 C34 103.8(4) . . ? O3 C35 H35A 111.0 . . ? C34 C35 H35A 111.0 . . ? O3 C35 H35B 111.0 . . ? C34 C35 H35B 111.0 . . ? H35A C35 H35B 109.0 . . ? O4 U2 O5 174.53(13) . . ? O4 U2 O6 88.38(12) . . ? O5 U2 O6 86.65(12) . . ? O4 U2 N3 85.33(12) . . ? O5 U2 N3 91.89(13) . . ? O6 U2 N3 84.08(11) . . ? O4 U2 N4 85.54(12) . . ? O5 U2 N4 99.93(12) . . ? O6 U2 N4 155.79(11) . . ? N3 U2 N4 118.64(11) . . ? O4 U2 Cl2 92.84(10) . . ? O5 U2 Cl2 88.04(10) . . ? O6 U2 Cl2 74.64(7) . . ? N3 U2 Cl2 158.68(8) . . ? N4 U2 Cl2 82.28(8) . . ? O4 U2 C40 101.21(13) . . ? O5 U2 C40 81.50(13) . . ? O6 U2 C40 142.79(12) . . ? N3 U2 C40 61.36(12) . . ? N4 U2 C40 61.41(12) . . ? Cl2 U2 C40 139.41(10) . . ? O4 U2 P3 88.96(10) . . ? O5 U2 P3 90.92(10) . . ? O6 U2 P3 113.34(7) . . ? N3 U2 P3 29.38(8) . . ? N4 U2 P3 89.99(8) . . ? Cl2 U2 P3 171.89(3) . . ? C40 U2 P3 32.59(9) . . ? C32 O3 C35 103.7(3) . . ? C32 O3 U1 121.0(3) . . ? C35 O3 U1 122.8(3) . . ? C75 O6 C78 103.3(3) . . ? C75 O6 U2 121.3(3) . . ? C78 O6 U2 122.7(3) . . ? P3 N3 Si3 128.3(2) . . ? P3 N3 U2 99.71(16) . . ? Si3 N3 U2 131.82(18) . . ? P4 N4 Si4 128.2(2) . . ? P4 N4 U2 99.93(16) . . ? Si4 N4 U2 126.81(18) . . ? P3 C40 P4 140.8(3) . . ? P3 C40 U2 89.91(18) . . ? P4 C40 U2 90.00(18) . . ? P3 C40 H40 111(4) . . ? P4 C40 H40 108(4) . . ? U2 C40 H40 93(4) . . ? N3 P3 C40 107.0(2) . . ? N3 P3 C53 113.0(2) . . ? C40 P3 C53 111.9(2) . . ? N3 P3 C59 110.3(2) . . ? C40 P3 C59 106.4(2) . . ? C53 P3 C59 108.0(2) . . ? N3 P3 U2 50.91(13) . . ? C40 P3 U2 57.50(15) . . ? C53 P3 U2 119.57(15) . . ? C59 P3 U2 132.41(13) . . ? N4 P4 C40 107.1(2) . . ? N4 P4 C41 112.54(19) . . ? C40 P4 C41 106.3(2) . . ? N4 P4 C47 112.6(2) . . ? C40 P4 C47 111.7(2) . . ? C41 P4 C47 106.5(2) . . ? N3 Si3 C66 111.4(2) . . ? N3 Si3 C65 109.62(19) . . ? C66 Si3 C65 108.7(2) . . ? N3 Si3 C67 112.9(2) . . ? C66 Si3 C67 107.9(2) . . ? C65 Si3 C67 106.1(2) . . ? N4 Si4 C70 110.8(2) . . ? N4 Si4 C69 111.02(19) . . ? C70 Si4 C69 110.1(2) . . ? N4 Si4 C68 112.0(2) . . ? C70 Si4 C68 105.5(2) . . ? C69 Si4 C68 107.2(2) . . ? C42 C41 C46 118.2(4) . . ? C42 C41 P4 121.5(3) . . ? C46 C41 P4 120.2(3) . . ? C43 C42 C41 121.4(4) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 119.0(4) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C46 C45 C44 120.9(5) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C41 120.4(4) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C48 C47 C52 119.8(4) . . ? C48 C47 P4 123.7(3) . . ? C52 C47 P4 116.6(3) . . ? C47 C48 C49 119.5(4) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 121.0(5) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 120.0(4) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C52 119.8(4) . . ? C50 C51 H51 120.1 . . ? C52 C51 H51 120.1 . . ? C51 C52 C47 119.8(4) . . ? C51 C52 H52 120.1 . . ? C47 C52 H52 120.1 . . ? C58 C53 C54 119.7(4) . . ? C58 C53 P3 118.4(3) . . ? C54 C53 P3 121.9(3) . . ? C55 C54 C53 119.6(4) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 120.2(5) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C57 C56 C55 120.6(4) . . ? C57 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C56 C57 C58 119.8(5) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C53 C58 C57 120.0(4) . . ? C53 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C60 C59 C64 119.1(4) . . ? C60 C59 P3 124.6(3) . . ? C64 C59 P3 116.3(3) . . ? C61 C60 C59 119.7(4) . . ? C61 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C62 C61 C60 121.0(5) . . ? C62 C61 H61 119.5 . . ? C60 C61 H61 119.5 . . ? C61 C62 C63 119.6(5) . . ? C61 C62 H62 120.2 . . ? C63 C62 H62 120.2 . . ? C64 C63 C62 119.8(4) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C59 120.9(4) . . ? C63 C64 H64 119.6 . . ? C59 C64 H64 119.6 . . ? Si3 C65 H65A 109.5 . . ? Si3 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? Si3 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si3 C66 H66A 109.5 . . ? Si3 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? Si3 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? Si3 C67 H67A 109.5 . . ? Si3 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? Si3 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? Si4 C68 H68A 109.5 . . ? Si4 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? Si4 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? Si4 C69 H69A 109.5 . . ? Si4 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? Si4 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? Si4 C70 H70A 109.5 . . ? Si4 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? Si4 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O8 C71 C72 106.8(4) . . ? O8 C71 H71A 110.4 . . ? C72 C71 H71A 110.4 . . ? O8 C71 H71B 110.4 . . ? C72 C71 H71B 110.4 . . ? H71A C71 H71B 108.6 . . ? C73 C72 C71 104.9(5) . . ? C73 C72 H72A 110.8 . . ? C71 C72 H72A 110.8 . . ? C73 C72 H72B 110.8 . . ? C71 C72 H72B 110.8 . . ? H72A C72 H72B 108.8 . . ? C72 C73 C74 108.2(5) . . ? C72 C73 H73A 110.1 . . ? C74 C73 H73A 110.1 . . ? C72 C73 H73B 110.1 . . ? C74 C73 H73B 110.1 . . ? H73A C73 H73B 108.4 . . ? O8 C74 C73 104.7(5) . . ? O8 C74 H74A 110.8 . . ? C73 C74 H74A 110.8 . . ? O8 C74 H74B 110.8 . . ? C73 C74 H74B 110.8 . . ? H74A C74 H74B 108.9 . . ? C36A O7 C39 103.8(5) . . ? C36A O7 C36B 25.1(6) . . ? C39 O7 C36B 96.4(7) . . ? C37A C36A O7 101.6(7) . . ? C37A C36A H36A 111.5 . . ? O7 C36A H36A 111.5 . . ? C37A C36A H36B 111.5 . . ? O7 C36A H36B 111.5 . . ? H36A C36A H36B 109.3 . . ? C38 C37A C36A 104.5(6) . . ? C38 C37A H37A 110.9 . . ? C36A C37A H37A 110.9 . . ? C38 C37A H37B 110.9 . . ? C36A C37A H37B 110.9 . . ? H37A C37A H37B 108.9 . . ? C37B C36B O7 110.9(11) . . ? C37B C36B H36C 109.5 . . ? O7 C36B H36C 109.5 . . ? C37B C36B H36D 109.5 . . ? O7 C36B H36D 109.5 . . ? H36C C36B H36D 108.0 . . ? C36B C37B C38 100.3(11) . . ? C36B C37B H37C 111.7 . . ? C38 C37B H37C 111.7 . . ? C36B C37B H37D 111.7 . . ? C38 C37B H37D 111.7 . . ? H37C C37B H37D 109.5 . . ? C37B C38 C37A 27.5(5) . . ? C37B C38 C39 108.4(7) . . ? C37A C38 C39 104.9(5) . . ? C37B C38 H38A 129.8 . . ? C37A C38 H38A 110.8 . . ? C39 C38 H38A 110.8 . . ? C37B C38 H38B 84.5 . . ? C37A C38 H38B 110.8 . . ? C39 C38 H38B 110.8 . . ? H38A C38 H38B 108.9 . . ? C38 C39 O7 104.5(4) . . ? C38 C39 H39A 110.9 . . ? O7 C39 H39A 110.9 . . ? C38 C39 H39B 110.9 . . ? O7 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? C74 O8 C71 107.2(4) . . ? O6 C75 C76 104.7(4) . . ? O6 C75 H75A 110.8 . . ? C76 C75 H75A 110.8 . . ? O6 C75 H75B 110.8 . . ? C76 C75 H75B 110.8 . . ? H75A C75 H75B 108.9 . . ? C75 C76 C77 103.9(4) . . ? C75 C76 H76A 111.0 . . ? C77 C76 H76A 111.0 . . ? C75 C76 H76B 111.0 . . ? C77 C76 H76B 111.0 . . ? H76A C76 H76B 109.0 . . ? C78 C77 C76 104.4(4) . . ? C78 C77 H77A 110.9 . . ? C76 C77 H77A 110.9 . . ? C78 C77 H77B 110.9 . . ? C76 C77 H77B 110.9 . . ? H77A C77 H77B 108.9 . . ? O6 C78 C77 104.9(4) . . ? O6 C78 H78A 110.8 . . ? C77 C78 H78A 110.8 . . ? O6 C78 H78B 110.8 . . ? C77 C78 H78B 110.8 . . ? H78A C78 H78B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 U1 N1 P1 -83.58(18) . . . . ? O2 U1 N1 P1 96.48(18) . . . . ? O3 U1 N1 P1 175.82(19) . . . . ? N2 U1 N1 P1 15.2(2) . . . . ? Cl1 U1 N1 P1 -170.97(16) . . . . ? C1 U1 N1 P1 -8.56(15) . . . . ? P2 U1 N1 P1 8.65(15) . . . . ? O1 U1 N1 Si1 120.9(2) . . . . ? O2 U1 N1 Si1 -59.1(2) . . . . ? O3 U1 N1 Si1 20.3(4) . . . . ? N2 U1 N1 Si1 -140.3(2) . . . . ? Cl1 U1 N1 Si1 33.5(2) . . . . ? C1 U1 N1 Si1 -164.1(3) . . . . ? P2 U1 N1 Si1 -146.9(2) . . . . ? P1 U1 N1 Si1 -155.6(3) . . . . ? O1 U1 N2 P2 88.70(17) . . . . ? O2 U1 N2 P2 -95.59(17) . . . . ? O3 U1 N2 P2 174.02(17) . . . . ? N1 U1 N2 P2 -13.4(2) . . . . ? Cl1 U1 N2 P2 -176.92(10) . . . . ? C1 U1 N2 P2 10.38(15) . . . . ? P1 U1 N2 P2 -6.00(14) . . . . ? O1 U1 N2 Si2 -92.5(3) . . . . ? O2 U1 N2 Si2 83.2(3) . . . . ? O3 U1 N2 Si2 -7.2(2) . . . . ? N1 U1 N2 Si2 165.4(2) . . . . ? Cl1 U1 N2 Si2 1.9(4) . . . . ? C1 U1 N2 Si2 -170.8(3) . . . . ? P2 U1 N2 Si2 178.8(4) . . . . ? P1 U1 N2 Si2 172.8(2) . . . . ? O1 U1 C1 P1 112.97(18) . . . . ? O2 U1 C1 P1 -71.26(18) . . . . ? O3 U1 C1 P1 -174.91(12) . . . . ? N1 U1 C1 P1 7.79(13) . . . . ? N2 U1 C1 P1 -148.4(2) . . . . ? Cl1 U1 C1 P1 35.9(2) . . . . ? P2 U1 C1 P1 -139.0(3) . . . . ? O1 U1 C1 P2 -108.05(18) . . . . ? O2 U1 C1 P2 67.71(18) . . . . ? O3 U1 C1 P2 -35.9(3) . . . . ? N1 U1 C1 P2 146.8(2) . . . . ? N2 U1 C1 P2 -9.47(13) . . . . ? Cl1 U1 C1 P2 174.83(7) . . . . ? P1 U1 C1 P2 139.0(3) . . . . ? Si1 N1 P1 C1 168.8(3) . . . . ? U1 N1 P1 C1 12.4(2) . . . . ? Si1 N1 P1 C2 -76.2(3) . . . . ? U1 N1 P1 C2 127.38(18) . . . . ? Si1 N1 P1 C8 44.9(3) . . . . ? U1 N1 P1 C8 -111.48(18) . . . . ? Si1 N1 P1 U1 156.4(3) . . . . ? P2 C1 P1 N1 -100.4(4) . . . . ? U1 C1 P1 N1 -11.28(19) . . . . ? P2 C1 P1 C2 139.3(4) . . . . ? U1 C1 P1 C2 -131.60(16) . . . . ? P2 C1 P1 C8 22.7(5) . . . . ? U1 C1 P1 C8 111.82(18) . . . . ? P2 C1 P1 U1 -89.1(4) . . . . ? O1 U1 P1 N1 99.98(19) . . . . ? O2 U1 P1 N1 -82.35(19) . . . . ? O3 U1 P1 N1 -166.5(6) . . . . ? N2 U1 P1 N1 -166.68(18) . . . . ? Cl1 U1 P1 N1 9.65(17) . . . . ? C1 U1 P1 N1 166.0(2) . . . . ? P2 U1 P1 N1 -170.07(17) . . . . ? O1 U1 P1 C1 -65.97(19) . . . . ? O2 U1 P1 C1 111.7(2) . . . . ? O3 U1 P1 C1 27.5(6) . . . . ? N1 U1 P1 C1 -166.0(2) . . . . ? N2 U1 P1 C1 27.37(19) . . . . ? Cl1 U1 P1 C1 -156.30(17) . . . . ? P2 U1 P1 C1 23.98(17) . . . . ? O1 U1 P1 C2 14.2(2) . . . . ? O2 U1 P1 C2 -168.1(2) . . . . ? O3 U1 P1 C2 107.7(6) . . . . ? N1 U1 P1 C2 -85.8(3) . . . . ? N2 U1 P1 C2 107.6(2) . . . . ? Cl1 U1 P1 C2 -76.1(2) . . . . ? C1 U1 P1 C2 80.2(3) . . . . ? P2 U1 P1 C2 104.2(2) . . . . ? O1 U1 P1 C8 -165.58(18) . . . . ? O2 U1 P1 C8 12.08(19) . . . . ? O3 U1 P1 C8 -72.1(6) . . . . ? N1 U1 P1 C8 94.4(2) . . . . ? N2 U1 P1 C8 -72.24(18) . . . . ? Cl1 U1 P1 C8 104.09(16) . . . . ? C1 U1 P1 C8 -99.6(2) . . . . ? P2 U1 P1 C8 -75.63(16) . . . . ? Si2 N2 P2 C1 166.1(3) . . . . ? U1 N2 P2 C1 -15.0(2) . . . . ? Si2 N2 P2 C14 -70.9(3) . . . . ? U1 N2 P2 C14 108.00(18) . . . . ? Si2 N2 P2 C20 50.5(3) . . . . ? U1 N2 P2 C20 -130.60(16) . . . . ? Si2 N2 P2 U1 -178.9(3) . . . . ? P1 C1 P2 N2 103.0(4) . . . . ? U1 C1 P2 N2 13.8(2) . . . . ? P1 C1 P2 C14 -21.1(5) . . . . ? U1 C1 P2 C14 -110.26(18) . . . . ? P1 C1 P2 C20 -137.7(4) . . . . ? U1 C1 P2 C20 133.13(17) . . . . ? P1 C1 P2 U1 89.1(4) . . . . ? O1 U1 P2 N2 -92.77(19) . . . . ? O2 U1 P2 N2 82.34(19) . . . . ? O3 U1 P2 N2 -6.42(18) . . . . ? N1 U1 P2 N2 168.26(18) . . . . ? Cl1 U1 P2 N2 171.1(3) . . . . ? C1 U1 P2 N2 -163.0(2) . . . . ? P1 U1 P2 N2 173.12(17) . . . . ? O1 U1 P2 C1 70.2(2) . . . . ? O2 U1 P2 C1 -114.7(2) . . . . ? O3 U1 P2 C1 156.53(19) . . . . ? N1 U1 P2 C1 -28.79(19) . . . . ? N2 U1 P2 C1 163.0(2) . . . . ? Cl1 U1 P2 C1 -26.0(3) . . . . ? P1 U1 P2 C1 -23.93(18) . . . . ? O1 U1 P2 C14 168.98(19) . . . . ? O2 U1 P2 C14 -15.91(19) . . . . ? O3 U1 P2 C14 -104.67(18) . . . . ? N1 U1 P2 C14 70.01(18) . . . . ? N2 U1 P2 C14 -98.2(2) . . . . ? Cl1 U1 P2 C14 72.8(3) . . . . ? C1 U1 P2 C14 98.8(2) . . . . ? P1 U1 P2 C14 74.87(17) . . . . ? O1 U1 P2 C20 -10.2(2) . . . . ? O2 U1 P2 C20 164.9(2) . . . . ? O3 U1 P2 C20 76.2(2) . . . . ? N1 U1 P2 C20 -109.2(2) . . . . ? N2 U1 P2 C20 82.6(3) . . . . ? Cl1 U1 P2 C20 -106.3(3) . . . . ? C1 U1 P2 C20 -80.4(3) . . . . ? P1 U1 P2 C20 -104.3(2) . . . . ? P1 N1 Si1 C28 -112.6(3) . . . . ? U1 N1 Si1 C28 37.1(3) . . . . ? P1 N1 Si1 C27 125.4(3) . . . . ? U1 N1 Si1 C27 -84.9(3) . . . . ? P1 N1 Si1 C26 6.2(3) . . . . ? U1 N1 Si1 C26 155.9(2) . . . . ? P2 N2 Si2 C31 -114.0(3) . . . . ? U1 N2 Si2 C31 67.5(3) . . . . ? P2 N2 Si2 C29 124.9(3) . . . . ? U1 N2 Si2 C29 -53.6(3) . . . . ? P2 N2 Si2 C30 3.4(4) . . . . ? U1 N2 Si2 C30 -175.1(2) . . . . ? N1 P1 C2 C3 10.7(4) . . . . ? C1 P1 C2 C3 126.9(4) . . . . ? C8 P1 C2 C3 -112.8(4) . . . . ? U1 P1 C2 C3 67.4(4) . . . . ? N1 P1 C2 C7 -166.5(3) . . . . ? C1 P1 C2 C7 -50.3(4) . . . . ? C8 P1 C2 C7 70.0(4) . . . . ? U1 P1 C2 C7 -109.8(3) . . . . ? C7 C2 C3 C4 0.4(6) . . . . ? P1 C2 C3 C4 -176.8(4) . . . . ? C2 C3 C4 C5 -1.1(7) . . . . ? C3 C4 C5 C6 0.1(7) . . . . ? C4 C5 C6 C7 1.6(7) . . . . ? C5 C6 C7 C2 -2.4(7) . . . . ? C3 C2 C7 C6 1.4(7) . . . . ? P1 C2 C7 C6 178.7(4) . . . . ? N1 P1 C8 C9 -134.0(4) . . . . ? C1 P1 C8 C9 105.5(4) . . . . ? C2 P1 C8 C9 -9.6(4) . . . . ? U1 P1 C8 C9 170.2(3) . . . . ? N1 P1 C8 C13 44.4(4) . . . . ? C1 P1 C8 C13 -76.1(4) . . . . ? C2 P1 C8 C13 168.8(3) . . . . ? U1 P1 C8 C13 -11.4(4) . . . . ? C13 C8 C9 C10 -0.7(7) . . . . ? P1 C8 C9 C10 177.7(4) . . . . ? C8 C9 C10 C11 0.8(7) . . . . ? C9 C10 C11 C12 -0.1(7) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C11 C12 C13 C8 0.7(7) . . . . ? C9 C8 C13 C12 0.0(6) . . . . ? P1 C8 C13 C12 -178.5(3) . . . . ? N2 P2 C14 C19 0.7(4) . . . . ? C1 P2 C14 C19 121.4(4) . . . . ? C20 P2 C14 C19 -123.0(4) . . . . ? U1 P2 C14 C19 57.6(4) . . . . ? N2 P2 C14 C15 -177.2(3) . . . . ? C1 P2 C14 C15 -56.5(4) . . . . ? C20 P2 C14 C15 59.1(4) . . . . ? U1 P2 C14 C15 -120.3(3) . . . . ? C19 C14 C15 C16 1.9(7) . . . . ? P2 C14 C15 C16 179.8(3) . . . . ? C14 C15 C16 C17 0.6(7) . . . . ? C15 C16 C17 C18 -2.2(7) . . . . ? C16 C17 C18 C19 1.3(7) . . . . ? C17 C18 C19 C14 1.2(7) . . . . ? C15 C14 C19 C18 -2.8(7) . . . . ? P2 C14 C19 C18 179.3(4) . . . . ? N2 P2 C20 C21 -127.6(4) . . . . ? C1 P2 C20 C21 116.1(4) . . . . ? C14 P2 C20 C21 -3.0(5) . . . . ? U1 P2 C20 C21 176.2(3) . . . . ? N2 P2 C20 C25 53.7(4) . . . . ? C1 P2 C20 C25 -62.6(4) . . . . ? C14 P2 C20 C25 178.3(3) . . . . ? U1 P2 C20 C25 -2.5(5) . . . . ? C25 C20 C21 C22 1.2(7) . . . . ? P2 C20 C21 C22 -177.5(4) . . . . ? C20 C21 C22 C23 0.2(8) . . . . ? C21 C22 C23 C24 -1.3(8) . . . . ? C22 C23 C24 C25 0.9(8) . . . . ? C23 C24 C25 C20 0.6(7) . . . . ? C21 C20 C25 C24 -1.6(7) . . . . ? P2 C20 C25 C24 177.1(4) . . . . ? O3 C32 C33 C34 25.8(5) . . . . ? C32 C33 C34 C35 0.1(5) . . . . ? C33 C34 C35 O3 -25.7(5) . . . . ? C33 C32 O3 C35 -43.0(4) . . . . ? C33 C32 O3 U1 174.2(3) . . . . ? C34 C35 O3 C32 42.9(4) . . . . ? C34 C35 O3 U1 -175.2(3) . . . . ? O1 U1 O3 C32 -17.5(3) . . . . ? O2 U1 O3 C32 164.3(3) . . . . ? N1 U1 O3 C32 85.7(4) . . . . ? N2 U1 O3 C32 -111.4(3) . . . . ? Cl1 U1 O3 C32 72.1(3) . . . . ? C1 U1 O3 C32 -88.2(3) . . . . ? P2 U1 O3 C32 -108.2(3) . . . . ? P1 U1 O3 C32 -111.6(6) . . . . ? O1 U1 O3 C35 -153.2(3) . . . . ? O2 U1 O3 C35 28.6(3) . . . . ? N1 U1 O3 C35 -50.0(4) . . . . ? N2 U1 O3 C35 112.9(3) . . . . ? Cl1 U1 O3 C35 -63.6(3) . . . . ? C1 U1 O3 C35 136.1(3) . . . . ? P2 U1 O3 C35 116.1(3) . . . . ? P1 U1 O3 C35 112.8(6) . . . . ? O4 U2 O6 C75 162.9(3) . . . . ? O5 U2 O6 C75 -19.4(3) . . . . ? N3 U2 O6 C75 -111.7(3) . . . . ? N4 U2 O6 C75 87.5(4) . . . . ? Cl2 U2 O6 C75 69.5(3) . . . . ? C40 U2 O6 C75 -90.6(3) . . . . ? P3 U2 O6 C75 -109.0(3) . . . . ? O4 U2 O6 C78 27.5(3) . . . . ? O5 U2 O6 C78 -154.8(3) . . . . ? N3 U2 O6 C78 112.9(3) . . . . ? N4 U2 O6 C78 -47.9(4) . . . . ? Cl2 U2 O6 C78 -65.9(3) . . . . ? C40 U2 O6 C78 134.0(3) . . . . ? P3 U2 O6 C78 115.6(3) . . . . ? O4 U2 N3 P3 -96.21(17) . . . . ? O5 U2 N3 P3 88.51(17) . . . . ? O6 U2 N3 P3 174.95(17) . . . . ? N4 U2 N3 P3 -13.9(2) . . . . ? Cl2 U2 N3 P3 177.97(10) . . . . ? C40 U2 N3 P3 9.27(15) . . . . ? O4 U2 N3 Si3 88.3(3) . . . . ? O5 U2 N3 Si3 -87.0(2) . . . . ? O6 U2 N3 Si3 -0.5(2) . . . . ? N4 U2 N3 Si3 170.6(2) . . . . ? Cl2 U2 N3 Si3 2.5(4) . . . . ? C40 U2 N3 Si3 -166.2(3) . . . . ? P3 U2 N3 Si3 -175.5(4) . . . . ? O4 U2 N4 P4 96.97(17) . . . . ? O5 U2 N4 P4 -82.92(17) . . . . ? O6 U2 N4 P4 172.92(17) . . . . ? N3 U2 N4 P4 14.8(2) . . . . ? Cl2 U2 N4 P4 -169.55(15) . . . . ? C40 U2 N4 P4 -8.37(14) . . . . ? P3 U2 N4 P4 8.01(14) . . . . ? O4 U2 N4 Si4 -59.3(2) . . . . ? O5 U2 N4 Si4 120.8(2) . . . . ? O6 U2 N4 Si4 16.7(4) . . . . ? N3 U2 N4 Si4 -141.49(19) . . . . ? Cl2 U2 N4 Si4 34.19(18) . . . . ? C40 U2 N4 Si4 -164.6(3) . . . . ? P3 U2 N4 Si4 -148.25(19) . . . . ? O4 U2 C40 P3 69.86(19) . . . . ? O5 U2 C40 P3 -105.31(19) . . . . ? O6 U2 C40 P3 -32.4(3) . . . . ? N3 U2 C40 P3 -8.44(14) . . . . ? N4 U2 C40 P3 148.4(2) . . . . ? Cl2 U2 C40 P3 177.85(7) . . . . ? O4 U2 C40 P4 -70.98(18) . . . . ? O5 U2 C40 P4 113.85(18) . . . . ? O6 U2 C40 P4 -173.29(12) . . . . ? N3 U2 C40 P4 -149.3(2) . . . . ? N4 U2 C40 P4 7.59(13) . . . . ? Cl2 U2 C40 P4 37.0(2) . . . . ? P3 U2 C40 P4 -140.8(3) . . . . ? Si3 N3 P3 C40 162.3(3) . . . . ? U2 N3 P3 C40 -13.4(2) . . . . ? Si3 N3 P3 C53 -74.0(3) . . . . ? U2 N3 P3 C53 110.27(18) . . . . ? Si3 N3 P3 C59 47.0(3) . . . . ? U2 N3 P3 C59 -128.73(16) . . . . ? Si3 N3 P3 U2 175.7(3) . . . . ? P4 C40 P3 N3 102.2(4) . . . . ? U2 C40 P3 N3 12.3(2) . . . . ? P4 C40 P3 C53 -22.1(5) . . . . ? U2 C40 P3 C53 -111.97(19) . . . . ? P4 C40 P3 C59 -139.8(4) . . . . ? U2 C40 P3 C59 130.26(16) . . . . ? P4 C40 P3 U2 89.9(4) . . . . ? O4 U2 P3 N3 82.31(19) . . . . ? O5 U2 P3 N3 -92.22(19) . . . . ? O6 U2 P3 N3 -5.48(18) . . . . ? N4 U2 P3 N3 167.85(18) . . . . ? Cl2 U2 P3 N3 -174.8(3) . . . . ? C40 U2 P3 N3 -164.8(2) . . . . ? O4 U2 P3 C40 -112.9(2) . . . . ? O5 U2 P3 C40 72.6(2) . . . . ? O6 U2 P3 C40 159.31(19) . . . . ? N3 U2 P3 C40 164.8(2) . . . . ? N4 U2 P3 C40 -27.4(2) . . . . ? Cl2 U2 P3 C40 -10.0(3) . . . . ? O4 U2 P3 C53 -14.40(19) . . . . ? O5 U2 P3 C53 171.07(19) . . . . ? O6 U2 P3 C53 -102.18(18) . . . . ? N3 U2 P3 C53 -96.7(2) . . . . ? N4 U2 P3 C53 71.14(18) . . . . ? Cl2 U2 P3 C53 88.5(3) . . . . ? C40 U2 P3 C53 98.5(2) . . . . ? O4 U2 P3 C59 164.5(2) . . . . ? O5 U2 P3 C59 -10.0(2) . . . . ? O6 U2 P3 C59 76.7(2) . . . . ? N3 U2 P3 C59 82.2(2) . . . . ? N4 U2 P3 C59 -109.9(2) . . . . ? Cl2 U2 P3 C59 -92.5(3) . . . . ? C40 U2 P3 C59 -82.6(3) . . . . ? Si4 N4 P4 C40 167.8(3) . . . . ? U2 N4 P4 C40 12.1(2) . . . . ? Si4 N4 P4 C41 -75.8(3) . . . . ? U2 N4 P4 C41 128.43(17) . . . . ? Si4 N4 P4 C47 44.6(3) . . . . ? U2 N4 P4 C47 -111.15(18) . . . . ? P3 C40 P4 N4 -100.9(4) . . . . ? U2 C40 P4 N4 -11.08(19) . . . . ? P3 C40 P4 C41 138.6(4) . . . . ? U2 C40 P4 C41 -131.55(16) . . . . ? P3 C40 P4 C47 22.8(5) . . . . ? U2 C40 P4 C47 112.66(19) . . . . ? P3 N3 Si3 C66 126.5(3) . . . . ? U2 N3 Si3 C66 -59.2(3) . . . . ? P3 N3 Si3 C65 -113.2(3) . . . . ? U2 N3 Si3 C65 61.2(3) . . . . ? P3 N3 Si3 C67 4.9(4) . . . . ? U2 N3 Si3 C67 179.2(2) . . . . ? P4 N4 Si4 C70 -114.3(3) . . . . ? U2 N4 Si4 C70 35.4(3) . . . . ? P4 N4 Si4 C69 123.1(3) . . . . ? U2 N4 Si4 C69 -87.3(2) . . . . ? P4 N4 Si4 C68 3.3(3) . . . . ? U2 N4 Si4 C68 152.9(2) . . . . ? N4 P4 C41 C42 11.3(4) . . . . ? C40 P4 C41 C42 128.1(4) . . . . ? C47 P4 C41 C42 -112.6(4) . . . . ? N4 P4 C41 C46 -166.3(3) . . . . ? C40 P4 C41 C46 -49.4(4) . . . . ? C47 P4 C41 C46 69.8(4) . . . . ? C46 C41 C42 C43 -0.9(6) . . . . ? P4 C41 C42 C43 -178.5(3) . . . . ? C41 C42 C43 C44 -0.8(7) . . . . ? C42 C43 C44 C45 1.4(7) . . . . ? C43 C44 C45 C46 -0.1(7) . . . . ? C44 C45 C46 C41 -1.7(7) . . . . ? C42 C41 C46 C45 2.2(6) . . . . ? P4 C41 C46 C45 179.8(3) . . . . ? N4 P4 C47 C48 -133.3(4) . . . . ? C40 P4 C47 C48 106.1(4) . . . . ? C41 P4 C47 C48 -9.5(4) . . . . ? N4 P4 C47 C52 45.2(4) . . . . ? C40 P4 C47 C52 -75.4(4) . . . . ? C41 P4 C47 C52 169.0(3) . . . . ? C52 C47 C48 C49 0.1(7) . . . . ? P4 C47 C48 C49 178.6(4) . . . . ? C47 C48 C49 C50 0.1(8) . . . . ? C48 C49 C50 C51 0.2(8) . . . . ? C49 C50 C51 C52 -0.8(7) . . . . ? C50 C51 C52 C47 1.0(7) . . . . ? C48 C47 C52 C51 -0.7(7) . . . . ? P4 C47 C52 C51 -179.3(3) . . . . ? N3 P3 C53 C58 3.1(4) . . . . ? C40 P3 C53 C58 124.0(4) . . . . ? C59 P3 C53 C58 -119.2(4) . . . . ? U2 P3 C53 C58 59.9(4) . . . . ? N3 P3 C53 C54 -177.4(4) . . . . ? C40 P3 C53 C54 -56.5(4) . . . . ? C59 P3 C53 C54 60.3(4) . . . . ? U2 P3 C53 C54 -120.6(4) . . . . ? C58 C53 C54 C55 1.7(7) . . . . ? P3 C53 C54 C55 -177.9(4) . . . . ? C53 C54 C55 C56 -0.9(7) . . . . ? C54 C55 C56 C57 -0.4(8) . . . . ? C55 C56 C57 C58 1.0(8) . . . . ? C54 C53 C58 C57 -1.2(7) . . . . ? P3 C53 C58 C57 178.4(4) . . . . ? C56 C57 C58 C53 -0.2(7) . . . . ? N3 P3 C59 C60 -133.0(4) . . . . ? C40 P3 C59 C60 111.3(4) . . . . ? C53 P3 C59 C60 -9.1(4) . . . . ? U2 P3 C59 C60 171.9(3) . . . . ? N3 P3 C59 C64 46.4(4) . . . . ? C40 P3 C59 C64 -69.4(4) . . . . ? C53 P3 C59 C64 170.3(3) . . . . ? U2 P3 C59 C64 -8.7(4) . . . . ? C64 C59 C60 C61 -0.5(6) . . . . ? P3 C59 C60 C61 178.8(3) . . . . ? C59 C60 C61 C62 0.6(7) . . . . ? C60 C61 C62 C63 -0.4(7) . . . . ? C61 C62 C63 C64 0.1(7) . . . . ? C62 C63 C64 C59 -0.1(7) . . . . ? C60 C59 C64 C63 0.3(6) . . . . ? P3 C59 C64 C63 -179.1(3) . . . . ? O8 C71 C72 C73 0.2(7) . . . . ? C71 C72 C73 C74 -17.3(9) . . . . ? C72 C73 C74 O8 28.3(8) . . . . ? C39 O7 C36A C37A -36.1(8) . . . . ? C36B O7 C36A C37A 39.1(14) . . . . ? O7 C36A C37A C38 46.5(9) . . . . ? C36A O7 C36B C37B -72.8(16) . . . . ? C39 O7 C36B C37B 36.3(16) . . . . ? O7 C36B C37B C38 -46.3(17) . . . . ? C36B C37B C38 C37A -50.4(12) . . . . ? C36B C37B C38 C39 36.4(14) . . . . ? C36A C37A C38 C37B 63.5(12) . . . . ? C36A C37A C38 C39 -38.0(8) . . . . ? C37B C38 C39 O7 -14.3(9) . . . . ? C37A C38 C39 O7 14.2(7) . . . . ? C36A O7 C39 C38 13.6(7) . . . . ? C36B O7 C39 C38 -10.7(9) . . . . ? C73 C74 O8 C71 -27.7(6) . . . . ? C72 C71 O8 C74 17.4(6) . . . . ? C78 O6 C75 C76 -42.9(4) . . . . ? U2 O6 C75 C76 174.5(3) . . . . ? O6 C75 C76 C77 27.8(5) . . . . ? C75 C76 C77 C78 -2.8(5) . . . . ? C75 O6 C78 C77 41.0(4) . . . . ? U2 O6 C78 C77 -177.0(3) . . . . ? C76 C77 C78 O6 -22.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.004 _refine_diff_density_min -2.016 _refine_diff_density_rms 0.181 #===END data_s1347abs _database_code_CSD 209175 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H46 Cl N3 O3 P2 Si2 U' _chemical_formula_weight 936.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' U U -9.6767 9.6646 '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 10.9989(10) _cell_length_b 12.5950(12) _cell_length_c 16.0980(15) _cell_angle_alpha 73.384(2) _cell_angle_beta 74.307(2) _cell_angle_gamma 64.5490(10) _cell_volume 1901.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 4.523 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15229 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 26.41 _reflns_number_total 7674 _reflns_number_gt 7119 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.0828P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7674 _refine_ls_number_parameters 599 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.202665(12) 0.666332(10) 0.248017(7) 0.01208(4) Uani 1 1 d . . . O1 O 0.2432(2) 0.7255(2) 0.13445(14) 0.0169(5) Uani 1 1 d . . . O2 O 0.1736(2) 0.5949(2) 0.35929(14) 0.0162(5) Uani 1 1 d . . . O3 O 0.4028(2) 0.4765(2) 0.23219(14) 0.0170(5) Uani 1 1 d . . . N1 N 0.0816(3) 0.5623(2) 0.20401(17) 0.0141(6) Uani 1 1 d . . . N2 N -0.0477(3) 0.7500(2) 0.26257(17) 0.0131(5) Uani 1 1 d . . . N3 N 0.0624(3) 0.8775(2) 0.27777(17) 0.0144(6) Uani 1 1 d . . . P1 P -0.07016(8) 0.65110(7) 0.23138(5) 0.01226(16) Uani 1 1 d . . . P2 P -0.08401(8) 0.87506(7) 0.28729(5) 0.01220(16) Uani 1 1 d . . . Si1 Si 0.10724(10) 0.97063(8) 0.31401(6) 0.01473(18) Uani 1 1 d . . . Si2 Si 0.14342(9) 0.45729(8) 0.13804(6) 0.01430(18) Uani 1 1 d . . . C1 C -0.1710(3) 0.7265(3) 0.1443(2) 0.0146(7) Uani 1 1 d . . . C2 C -0.1243(4) 0.8026(3) 0.0733(2) 0.0187(7) Uani 1 1 d . . . C3 C -0.2013(4) 0.8690(3) 0.0074(2) 0.0227(8) Uani 1 1 d . . . C4 C -0.3242(4) 0.8614(3) 0.0107(2) 0.0229(8) Uani 1 1 d . . . C5 C -0.3710(4) 0.7875(3) 0.0805(2) 0.0223(8) Uani 1 1 d . . . C6 C -0.2948(4) 0.7197(3) 0.1467(2) 0.0180(7) Uani 1 1 d . . . C7 C -0.1673(3) 0.5820(3) 0.3212(2) 0.0154(7) Uani 1 1 d . . . C8 C -0.1122(4) 0.4603(3) 0.3545(2) 0.0232(8) Uani 1 1 d . . . C9 C -0.1815(4) 0.4073(4) 0.4278(2) 0.0298(9) Uani 1 1 d . . . C10 C -0.3079(4) 0.4761(4) 0.4683(2) 0.0245(8) Uani 1 1 d . . . C11 C -0.3648(4) 0.5976(3) 0.4355(2) 0.0237(8) Uani 1 1 d . . . C12 C -0.2953(4) 0.6507(3) 0.3626(2) 0.0196(7) Uani 1 1 d . . . C13 C -0.1811(3) 0.8763(3) 0.3977(2) 0.0157(7) Uani 1 1 d . . . C14 C -0.1436(4) 0.7697(3) 0.4597(2) 0.0200(7) Uani 1 1 d . . . C15 C -0.2095(4) 0.7674(4) 0.5463(2) 0.0254(8) Uani 1 1 d . . . C16 C -0.3109(4) 0.8695(4) 0.5719(2) 0.0241(8) Uani 1 1 d . . . C17 C -0.3484(4) 0.9763(3) 0.5113(2) 0.0241(8) Uani 1 1 d . . . C18 C -0.2844(4) 0.9791(3) 0.4243(2) 0.0185(7) Uani 1 1 d . . . C19 C -0.1930(3) 0.9930(3) 0.2136(2) 0.0143(7) Uani 1 1 d . . . C20 C -0.1394(4) 1.0640(3) 0.1441(2) 0.0198(7) Uani 1 1 d . . . C21 C -0.2177(4) 1.1428(3) 0.0805(2) 0.0247(8) Uani 1 1 d . . . C22 C -0.3481(4) 1.1503(3) 0.0866(2) 0.0255(8) Uani 1 1 d . . . C23 C -0.4023(4) 1.0793(3) 0.1555(2) 0.0227(8) Uani 1 1 d . . . C24 C -0.3249(4) 1.0012(3) 0.2190(2) 0.0187(7) Uani 1 1 d . . . C25 C 0.2604(4) 0.3115(3) 0.1926(3) 0.0224(8) Uani 1 1 d . . . C26 C 0.2402(4) 0.5102(4) 0.0318(2) 0.0235(8) Uani 1 1 d . . . C27 C 0.0044(4) 0.4269(4) 0.1165(3) 0.0217(8) Uani 1 1 d . . . C28 C -0.0346(4) 1.1202(3) 0.3198(3) 0.0235(8) Uani 1 1 d . . . C29 C 0.2516(4) 1.0016(4) 0.2346(3) 0.0239(8) Uani 1 1 d . . . C30 C 0.1499(4) 0.9006(4) 0.4260(2) 0.0226(8) Uani 1 1 d . . . C31 C 0.4490(4) 0.3944(3) 0.3129(2) 0.0232(8) Uani 1 1 d . . . C32 C 0.5950(4) 0.3164(4) 0.2839(3) 0.0261(8) Uani 1 1 d . . . C33 C 0.6434(4) 0.4018(4) 0.2089(3) 0.0258(8) Uani 1 1 d . . . C34 C 0.5215(4) 0.4710(3) 0.1635(2) 0.0218(8) Uani 1 1 d . . . Cl1 Cl 0.40729(8) 0.69498(8) 0.28610(6) 0.02225(18) Uani 1 1 d . . . H2 H -0.046(4) 0.812(3) 0.075(2) 0.010(8) Uiso 1 1 d . . . H3 H -0.166(4) 0.923(4) -0.041(3) 0.036(12) Uiso 1 1 d . . . H4 H -0.380(4) 0.911(3) -0.032(2) 0.018(9) Uiso 1 1 d . . . H5 H -0.457(4) 0.788(3) 0.083(2) 0.018(9) Uiso 1 1 d . . . H6 H -0.320(3) 0.676(3) 0.188(2) 0.005(8) Uiso 1 1 d . . . H8 H -0.034(4) 0.416(3) 0.330(2) 0.024(10) Uiso 1 1 d . . . H9 H -0.137(4) 0.324(3) 0.447(2) 0.024(10) Uiso 1 1 d . . . H10 H -0.353(4) 0.445(4) 0.511(3) 0.035(12) Uiso 1 1 d . . . H11 H -0.455(4) 0.647(3) 0.464(2) 0.020(9) Uiso 1 1 d . . . H12 H -0.331(4) 0.729(4) 0.340(2) 0.024(10) Uiso 1 1 d . . . H14 H -0.078(4) 0.703(3) 0.444(2) 0.018(9) Uiso 1 1 d . . . H15 H -0.186(4) 0.707(4) 0.580(3) 0.035(13) Uiso 1 1 d . . . H16 H -0.349(4) 0.874(3) 0.624(2) 0.019(10) Uiso 1 1 d . . . H17 H -0.417(4) 1.044(3) 0.530(2) 0.026(11) Uiso 1 1 d . . . H18 H -0.311(4) 1.047(3) 0.386(2) 0.019(10) Uiso 1 1 d . . . H20 H -0.050(4) 1.058(3) 0.142(2) 0.018(9) Uiso 1 1 d . . . H21 H -0.183(4) 1.182(4) 0.037(3) 0.035(12) Uiso 1 1 d . . . H22 H -0.392(4) 1.197(3) 0.047(2) 0.025(11) Uiso 1 1 d . . . H23 H -0.476(4) 1.083(3) 0.157(2) 0.018(10) Uiso 1 1 d . . . H24 H -0.357(4) 0.961(3) 0.261(2) 0.013(9) Uiso 1 1 d . . . H25A H 0.220(4) 0.275(4) 0.252(3) 0.034(12) Uiso 1 1 d . . . H26A H 0.179(4) 0.583(4) 0.000(3) 0.032(11) Uiso 1 1 d . . . H27A H -0.062(4) 0.492(4) 0.089(3) 0.030(11) Uiso 1 1 d . . . H28A H -0.102(4) 1.118(3) 0.358(3) 0.024(11) Uiso 1 1 d . . . H29A H 0.222(5) 1.065(4) 0.189(3) 0.054(15) Uiso 1 1 d . . . H30A H 0.084(5) 0.886(4) 0.462(3) 0.038(13) Uiso 1 1 d . . . H31A H 0.441(4) 0.443(4) 0.351(3) 0.034(11) Uiso 1 1 d . . . H32A H 0.603(4) 0.252(3) 0.263(2) 0.024(10) Uiso 1 1 d . . . H33A H 0.720(4) 0.359(3) 0.172(3) 0.028(11) Uiso 1 1 d . . . H34A H 0.515(4) 0.549(4) 0.138(2) 0.023(10) Uiso 1 1 d . . . H25B H 0.294(4) 0.253(4) 0.159(3) 0.039(12) Uiso 1 1 d . . . H26B H 0.305(4) 0.533(3) 0.041(2) 0.027(11) Uiso 1 1 d . . . H27B H -0.037(4) 0.397(3) 0.166(3) 0.018(10) Uiso 1 1 d . . . H28B H -0.072(4) 1.159(4) 0.263(3) 0.039(12) Uiso 1 1 d . . . H29B H 0.312(6) 1.025(5) 0.252(4) 0.081(19) Uiso 1 1 d . . . H30B H 0.231(4) 0.823(4) 0.425(3) 0.036(12) Uiso 1 1 d . . . H31B H 0.393(4) 0.357(4) 0.330(3) 0.030(11) Uiso 1 1 d . . . H32B H 0.639(4) 0.296(3) 0.329(3) 0.022(10) Uiso 1 1 d . . . H33B H 0.655(4) 0.458(4) 0.229(3) 0.040(13) Uiso 1 1 d . . . H34B H 0.522(4) 0.431(3) 0.126(2) 0.020(10) Uiso 1 1 d . . . H25C H 0.335(4) 0.307(3) 0.210(2) 0.021(10) Uiso 1 1 d . . . H26C H 0.277(5) 0.453(4) 0.000(3) 0.042(13) Uiso 1 1 d . . . H27C H 0.048(4) 0.367(3) 0.080(2) 0.023(10) Uiso 1 1 d . . . H28C H 0.003(4) 1.163(4) 0.330(2) 0.027(11) Uiso 1 1 d . . . H29C H 0.305(6) 0.940(5) 0.205(3) 0.068(17) Uiso 1 1 d . . . H30C H 0.167(4) 0.950(4) 0.448(2) 0.026(11) Uiso 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 U1 0.01124(7) 0.01364(7) 0.01180(7) -0.00111(4) -0.00307(4) -0.00538(5) O1 0.0159(12) 0.0197(12) 0.0141(11) -0.0022(9) 0.0000(9) -0.0081(10) O2 0.0128(12) 0.0194(12) 0.0157(11) -0.0001(9) -0.0043(9) -0.0065(10) O3 0.0138(12) 0.0181(12) 0.0156(12) -0.0004(9) -0.0020(9) -0.0049(10) N1 0.0136(14) 0.0135(13) 0.0163(14) -0.0021(11) -0.0053(11) -0.0051(11) N2 0.0093(13) 0.0139(13) 0.0170(14) -0.0046(11) -0.0031(11) -0.0037(11) N3 0.0148(14) 0.0137(13) 0.0148(14) -0.0033(11) -0.0038(11) -0.0047(11) P1 0.0117(4) 0.0130(4) 0.0131(4) -0.0014(3) -0.0035(3) -0.0057(3) P2 0.0125(4) 0.0114(4) 0.0127(4) -0.0016(3) -0.0030(3) -0.0044(3) Si1 0.0181(5) 0.0153(4) 0.0135(4) -0.0012(3) -0.0035(4) -0.0094(4) Si2 0.0150(5) 0.0147(4) 0.0144(4) -0.0039(3) -0.0024(4) -0.0061(4) C1 0.0147(17) 0.0174(16) 0.0146(16) -0.0065(13) -0.0037(13) -0.0059(13) C2 0.0164(18) 0.0239(18) 0.0180(17) -0.0044(14) -0.0029(14) -0.0093(15) C3 0.028(2) 0.029(2) 0.0119(17) 0.0005(15) -0.0029(15) -0.0146(17) C4 0.022(2) 0.0256(19) 0.0186(18) -0.0053(15) -0.0089(15) -0.0035(16) C5 0.0159(18) 0.029(2) 0.0253(19) -0.0054(15) -0.0065(15) -0.0096(16) C6 0.0180(18) 0.0236(19) 0.0148(17) -0.0016(15) -0.0045(14) -0.0106(15) C7 0.0174(17) 0.0198(17) 0.0138(16) -0.0009(13) -0.0054(13) -0.0114(14) C8 0.021(2) 0.0225(19) 0.0194(18) -0.0022(15) 0.0002(15) -0.0058(16) C9 0.038(2) 0.020(2) 0.023(2) 0.0067(16) -0.0040(17) -0.0115(18) C10 0.028(2) 0.037(2) 0.0144(18) 0.0015(16) -0.0004(15) -0.0231(18) C11 0.021(2) 0.035(2) 0.0194(18) -0.0062(16) -0.0014(15) -0.0142(17) C12 0.0195(18) 0.0182(18) 0.0205(18) 0.0013(14) -0.0027(14) -0.0102(15) C13 0.0171(17) 0.0194(17) 0.0139(16) -0.0034(13) -0.0019(13) -0.0104(14) C14 0.0176(18) 0.0218(19) 0.0181(18) -0.0030(14) -0.0019(14) -0.0063(15) C15 0.024(2) 0.033(2) 0.0162(18) 0.0051(16) -0.0041(15) -0.0137(17) C16 0.023(2) 0.043(2) 0.0103(17) -0.0067(16) 0.0028(15) -0.0188(18) C17 0.022(2) 0.030(2) 0.025(2) -0.0131(16) -0.0014(16) -0.0110(17) C18 0.0188(18) 0.0198(18) 0.0188(18) -0.0026(15) -0.0045(14) -0.0090(15) C19 0.0178(17) 0.0097(15) 0.0130(16) -0.0022(12) -0.0039(13) -0.0023(13) C20 0.022(2) 0.0189(18) 0.0192(18) -0.0024(14) -0.0055(15) -0.0086(15) C21 0.034(2) 0.0214(19) 0.0161(18) 0.0032(15) -0.0064(16) -0.0113(17) C22 0.032(2) 0.0186(18) 0.0200(19) -0.0008(15) -0.0115(17) -0.0025(16) C23 0.0162(19) 0.0241(19) 0.028(2) -0.0080(15) -0.0096(16) -0.0023(15) C24 0.0178(18) 0.0154(17) 0.0206(18) -0.0029(14) -0.0038(15) -0.0043(14) C25 0.023(2) 0.0168(18) 0.029(2) -0.0071(16) -0.0098(17) -0.0035(15) C26 0.027(2) 0.031(2) 0.0182(18) -0.0092(16) 0.0003(16) -0.0167(18) C27 0.022(2) 0.024(2) 0.023(2) -0.0093(16) -0.0036(16) -0.0092(17) C28 0.025(2) 0.0218(19) 0.027(2) -0.0049(16) -0.0043(18) -0.0117(17) C29 0.027(2) 0.027(2) 0.0210(19) -0.0008(16) -0.0005(16) -0.0183(18) C30 0.027(2) 0.024(2) 0.0196(19) 0.0007(15) -0.0078(16) -0.0127(17) C31 0.023(2) 0.0194(19) 0.0215(19) 0.0037(15) -0.0070(15) -0.0064(16) C32 0.024(2) 0.023(2) 0.027(2) 0.0004(16) -0.0084(17) -0.0067(16) C33 0.0167(19) 0.024(2) 0.032(2) -0.0059(17) -0.0017(16) -0.0046(16) C34 0.0168(18) 0.0218(19) 0.0197(18) -0.0023(15) 0.0019(14) -0.0049(15) Cl1 0.0155(4) 0.0258(4) 0.0300(5) -0.0072(4) -0.0060(3) -0.0097(3) _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 U1 O2 1.771(2) . ? U1 O1 1.778(2) . ? U1 N2 2.459(3) . ? U1 O3 2.480(2) . ? U1 N3 2.547(3) . ? U1 N1 2.556(3) . ? U1 Cl1 2.6724(8) . ? U1 P2 3.1624(8) . ? U1 P1 3.1737(9) . ? O3 C34 1.456(4) . ? O3 C31 1.467(4) . ? N1 P1 1.584(3) . ? N1 Si2 1.726(3) . ? N2 P2 1.591(3) . ? N2 P1 1.598(3) . ? N3 P2 1.589(3) . ? N3 Si1 1.733(3) . ? P1 C7 1.799(3) . ? P1 C1 1.809(3) . ? P2 C13 1.810(3) . ? P2 C19 1.811(3) . ? Si1 C30 1.855(4) . ? Si1 C29 1.859(4) . ? Si1 C28 1.867(4) . ? Si2 C25 1.859(4) . ? Si2 C27 1.863(4) . ? Si2 C26 1.865(4) . ? C1 C6 1.390(5) . ? C1 C2 1.402(4) . ? C2 C3 1.383(5) . ? C3 C4 1.382(5) . ? C4 C5 1.377(5) . ? C5 C6 1.384(5) . ? C7 C8 1.382(5) . ? C7 C12 1.396(5) . ? C8 C9 1.385(5) . ? C9 C10 1.381(6) . ? C10 C11 1.380(5) . ? C11 C12 1.384(5) . ? C13 C18 1.393(5) . ? C13 C14 1.396(5) . ? C14 C15 1.384(5) . ? C15 C16 1.374(6) . ? C16 C17 1.387(5) . ? C17 C18 1.384(5) . ? C19 C20 1.388(5) . ? C19 C24 1.389(5) . ? C20 C21 1.391(5) . ? C21 C22 1.375(6) . ? C22 C23 1.384(5) . ? C23 C24 1.383(5) . ? C31 C32 1.504(5) . ? C32 C33 1.516(5) . ? C33 C34 1.501(5) . ? 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 O2 U1 O1 174.87(10) . . ? O2 U1 N2 84.77(9) . . ? O1 U1 N2 98.70(10) . . ? O2 U1 O3 84.79(9) . . ? O1 U1 O3 90.15(9) . . ? N2 U1 O3 140.75(8) . . ? O2 U1 N3 94.59(9) . . ? O1 U1 N3 90.43(9) . . ? N2 U1 N3 59.42(8) . . ? O3 U1 N3 159.28(8) . . ? O2 U1 N1 90.52(9) . . ? O1 U1 N1 88.05(9) . . ? N2 U1 N1 59.29(8) . . ? O3 U1 N1 83.10(8) . . ? N3 U1 N1 117.62(8) . . ? O2 U1 Cl1 87.60(7) . . ? O1 U1 Cl1 91.88(8) . . ? N2 U1 Cl1 142.11(6) . . ? O3 U1 Cl1 74.89(6) . . ? N3 U1 Cl1 84.39(6) . . ? N1 U1 Cl1 157.99(6) . . ? O2 U1 P2 87.60(7) . . ? O1 U1 P2 97.28(7) . . ? N2 U1 P2 29.64(6) . . ? O3 U1 P2 168.74(5) . . ? N3 U1 P2 29.90(6) . . ? N1 U1 P2 88.69(6) . . ? Cl1 U1 P2 113.12(2) . . ? O2 U1 P1 86.13(7) . . ? O1 U1 P1 95.02(7) . . ? N2 U1 P1 29.65(6) . . ? O3 U1 P1 111.86(6) . . ? N3 U1 P1 88.71(6) . . ? N1 U1 P1 29.68(6) . . ? Cl1 U1 P1 170.28(2) . . ? P2 U1 P1 59.21(2) . . ? C34 O3 C31 108.8(3) . . ? C34 O3 U1 122.3(2) . . ? C31 O3 U1 117.59(19) . . ? P1 N1 Si2 129.86(17) . . ? P1 N1 U1 97.30(12) . . ? Si2 N1 U1 130.60(14) . . ? P2 N2 P1 157.98(19) . . ? P2 N2 U1 100.49(12) . . ? P1 N2 U1 100.78(12) . . ? P2 N3 Si1 129.39(17) . . ? P2 N3 U1 97.02(12) . . ? Si1 N3 U1 130.19(14) . . ? N1 P1 N2 102.49(14) . . ? N1 P1 C7 113.38(15) . . ? N2 P1 C7 109.18(14) . . ? N1 P1 C1 115.95(14) . . ? N2 P1 C1 108.02(14) . . ? C7 P1 C1 107.48(15) . . ? N1 P1 U1 53.02(10) . . ? N2 P1 U1 49.56(9) . . ? C7 P1 U1 122.75(11) . . ? C1 P1 U1 128.97(11) . . ? N3 P2 N2 102.67(14) . . ? N3 P2 C13 113.80(14) . . ? N2 P2 C13 108.83(15) . . ? N3 P2 C19 115.39(15) . . ? N2 P2 C19 108.47(14) . . ? C13 P2 C19 107.37(15) . . ? N3 P2 U1 53.07(10) . . ? N2 P2 U1 49.87(10) . . ? C13 P2 U1 120.97(11) . . ? C19 P2 U1 130.92(11) . . ? N3 Si1 C30 109.46(16) . . ? N3 Si1 C29 109.85(16) . . ? C30 Si1 C29 112.01(19) . . ? N3 Si1 C28 112.11(16) . . ? C30 Si1 C28 107.74(19) . . ? C29 Si1 C28 105.64(19) . . ? N1 Si2 C25 110.43(15) . . ? N1 Si2 C27 112.21(15) . . ? C25 Si2 C27 106.29(18) . . ? N1 Si2 C26 109.47(16) . . ? C25 Si2 C26 108.60(19) . . ? C27 Si2 C26 109.74(18) . . ? C6 C1 C2 118.9(3) . . ? C6 C1 P1 124.1(3) . . ? C2 C1 P1 116.9(2) . . ? C3 C2 C1 119.9(3) . . ? C4 C3 C2 120.7(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 120.3(3) . . ? C5 C6 C1 120.6(3) . . ? C8 C7 C12 118.6(3) . . ? C8 C7 P1 120.3(3) . . ? C12 C7 P1 121.0(3) . . ? C7 C8 C9 121.0(4) . . ? C10 C9 C8 119.9(4) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 120.2(4) . . ? C11 C12 C7 120.4(3) . . ? C18 C13 C14 119.2(3) . . ? C18 C13 P2 123.3(3) . . ? C14 C13 P2 117.4(3) . . ? C15 C14 C13 119.8(3) . . ? C16 C15 C14 120.6(4) . . ? C15 C16 C17 120.3(3) . . ? C18 C17 C16 119.5(4) . . ? C17 C18 C13 120.6(3) . . ? C20 C19 C24 119.5(3) . . ? C20 C19 P2 120.0(3) . . ? C24 C19 P2 119.8(3) . . ? C19 C20 C21 119.9(3) . . ? C22 C21 C20 120.0(4) . . ? C21 C22 C23 120.4(4) . . ? C24 C23 C22 119.7(4) . . ? C23 C24 C19 120.4(3) . . ? O3 C31 C32 105.0(3) . . ? C31 C32 C33 102.2(3) . . ? C34 C33 C32 102.5(3) . . ? O3 C34 C33 105.7(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.643 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.111 #===END data_ms164 _database_code_CSD 209176 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.50 H77 Cl3 N6 O4 P4 Si4 U2' _chemical_formula_weight 1770.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.295(2) _cell_length_b 12.479(2) _cell_length_c 14.211(3) _cell_angle_alpha 107.595(3) _cell_angle_beta 93.089(3) _cell_angle_gamma 103.350(3) _cell_volume 1841.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 865 _exptl_absorpt_coefficient_mu 4.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7990 _exptl_absorpt_correction_T_max 0.9545 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69380 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8211 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.39 _reflns_number_total 5977 _reflns_number_gt 4509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1273P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5977 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1848 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.38023(4) 0.48669(4) 0.61846(3) 0.0425(2) Uani 1 1 d . . . Si1 Si 0.4261(4) 0.8135(4) 0.7825(3) 0.0613(10) Uani 1 1 d . . . Si2 Si 0.2579(3) 0.1450(3) 0.5514(3) 0.0488(8) Uani 1 1 d . . . Cl1 Cl 0.5318(3) 0.6467(3) 0.5464(3) 0.0600(9) Uani 1 1 d . . . O1 O 0.5020(8) 0.4874(9) 0.7009(7) 0.056(2) Uani 1 1 d . . . O2 O 0.2613(8) 0.4866(8) 0.5333(7) 0.053(2) Uani 1 1 d . . . N1 N 0.3462(10) 0.6715(10) 0.7463(9) 0.054(3) Uani 1 1 d . . . N2 N 0.2306(10) 0.4677(11) 0.7341(9) 0.058(3) Uani 1 1 d . . . N3 N 0.2628(9) 0.2894(9) 0.6217(8) 0.047(2) Uani 1 1 d . . . P1 P 0.2390(3) 0.6016(3) 0.7911(3) 0.0519(8) Uani 1 1 d . . . P2 P 0.1766(3) 0.3303(3) 0.7003(3) 0.0492(8) Uani 1 1 d . . . C1 C 0.5872(19) 0.825(2) 0.8171(15) 0.103(7) Uani 1 1 d . . . H1A H 0.5934 0.7733 0.8566 0.155 Uiso 1 1 calc R . . H1B H 0.6290 0.9051 0.8567 0.155 Uiso 1 1 calc R . . H1C H 0.6260 0.8011 0.7568 0.155 Uiso 1 1 calc R . . C2 C 0.412(2) 0.8824(16) 0.6838(14) 0.091(6) Uani 1 1 d . . . H2A H 0.4439 0.8412 0.6245 0.137 Uiso 1 1 calc R . . H2B H 0.4590 0.9642 0.7087 0.137 Uiso 1 1 calc R . . H2C H 0.3253 0.8779 0.6664 0.137 Uiso 1 1 calc R . . C3 C 0.367(3) 0.8968(19) 0.8946(15) 0.118(8) Uani 1 1 d . . . H3A H 0.2796 0.8902 0.8779 0.177 Uiso 1 1 calc R . . H3B H 0.4128 0.9789 0.9159 0.177 Uiso 1 1 calc R . . H3C H 0.3771 0.8649 0.9487 0.177 Uiso 1 1 calc R . . C4 C 0.0880(8) 0.6247(11) 0.7661(8) 0.068(4) Uani 1 1 d G . . C5 C 0.0730(10) 0.6828(11) 0.6986(9) 0.091(6) Uani 1 1 d G . . H5 H 0.1424 0.7186 0.6738 0.109 Uiso 1 1 calc R . . C6 C -0.0436(12) 0.6884(14) 0.6676(9) 0.106(7) Uani 1 1 d G . . H6 H -0.0538 0.7281 0.6215 0.127 Uiso 1 1 calc R . . C7 C -0.1451(9) 0.6360(14) 0.7039(10) 0.125(10) Uani 1 1 d G . . H7 H -0.2248 0.6398 0.6827 0.150 Uiso 1 1 calc R . . C8 C -0.1301(8) 0.5779(12) 0.7714(10) 0.096(7) Uani 1 1 d G . . H8 H -0.1995 0.5420 0.7962 0.115 Uiso 1 1 calc R . . C9 C -0.0135(10) 0.5722(11) 0.8024(9) 0.094(6) Uani 1 1 d G . . H9 H -0.0032 0.5325 0.8485 0.113 Uiso 1 1 calc R . . C10 C 0.2686(9) 0.6294(10) 0.9228(6) 0.062(4) Uani 1 1 d G . . C11 C 0.2121(10) 0.6988(12) 0.9920(7) 0.095(7) Uani 1 1 d G . . H11 H 0.1558 0.7352 0.9704 0.114 Uiso 1 1 calc R . . C12 C 0.2380(12) 0.7148(14) 1.0928(7) 0.125(10) Uani 1 1 d G . . H12 H 0.1994 0.7623 1.1401 0.150 Uiso 1 1 calc R . . C13 C 0.3204(12) 0.6615(14) 1.1244(6) 0.106(7) Uani 1 1 d G . . H13 H 0.3381 0.6725 1.1933 0.127 Uiso 1 1 calc R . . C14 C 0.3769(11) 0.5921(12) 1.0552(9) 0.100(7) Uani 1 1 d G . . H14 H 0.4332 0.5557 1.0768 0.120 Uiso 1 1 calc R . . C15 C 0.3510(10) 0.5761(10) 0.9544(8) 0.081(5) Uani 1 1 d G . . H15 H 0.3896 0.5286 0.9071 0.097 Uiso 1 1 calc R . . C16 C 0.0159(6) 0.2940(9) 0.6541(7) 0.055(3) Uani 1 1 d G . . C17 C -0.0164(8) 0.3525(9) 0.5917(8) 0.071(4) Uani 1 1 d G . . H17 H 0.0453 0.4062 0.5741 0.086 Uiso 1 1 calc R . . C18 C -0.1389(9) 0.3323(11) 0.5551(8) 0.078(5) Uani 1 1 d G . . H18 H -0.1610 0.3723 0.5124 0.093 Uiso 1 1 calc R . . C19 C -0.2291(6) 0.2536(11) 0.5808(9) 0.085(5) Uani 1 1 d G . . H19 H -0.3129 0.2398 0.5558 0.102 Uiso 1 1 calc R . . C20 C -0.1968(7) 0.1951(9) 0.6432(9) 0.073(5) Uani 1 1 d G . . H20 H -0.2585 0.1414 0.6609 0.088 Uiso 1 1 calc R . . C21 C -0.0743(8) 0.2153(9) 0.6799(7) 0.064(4) Uani 1 1 d G . . H21 H -0.0522 0.1753 0.7225 0.077 Uiso 1 1 calc R . . C22 C 0.1887(9) 0.2891(11) 0.8108(6) 0.056(3) Uani 1 1 d G . . C23 C 0.1116(9) 0.3158(13) 0.8825(8) 0.093(6) Uani 1 1 d G . . H23 H 0.0441 0.3448 0.8690 0.112 Uiso 1 1 calc R . . C24 C 0.1332(13) 0.3001(17) 0.9740(8) 0.129(10) Uani 1 1 d G . . H24 H 0.0805 0.3183 1.0230 0.155 Uiso 1 1 calc R . . C25 C 0.2319(13) 0.2577(17) 0.9939(8) 0.135(10) Uani 1 1 d G . . H25 H 0.2467 0.2469 1.0564 0.162 Uiso 1 1 calc R . . C26 C 0.3090(11) 0.2310(15) 0.9222(10) 0.116(8) Uani 1 1 d G . . H26 H 0.3765 0.2020 0.9357 0.139 Uiso 1 1 calc R . . C27 C 0.2874(10) 0.2467(12) 0.8307(8) 0.089(6) Uani 1 1 d G . . H27 H 0.3401 0.2285 0.7817 0.107 Uiso 1 1 calc R . . C28 C 0.1506(13) 0.0371(14) 0.5939(14) 0.067(4) Uani 1 1 d . . . H28A H 0.1799 0.0456 0.6626 0.101 Uiso 1 1 calc R . . H28B H 0.1467 -0.0418 0.5506 0.101 Uiso 1 1 calc R . . H28C H 0.0686 0.0506 0.5908 0.101 Uiso 1 1 calc R . . C29 C 0.4147(13) 0.1236(14) 0.5663(13) 0.065(4) Uani 1 1 d . . . H29A H 0.4733 0.1827 0.5479 0.097 Uiso 1 1 calc R . . H29B H 0.4153 0.0459 0.5231 0.097 Uiso 1 1 calc R . . H29C H 0.4381 0.1310 0.6359 0.097 Uiso 1 1 calc R . . C30 C 0.2046(15) 0.1145(14) 0.4180(13) 0.073(4) Uani 1 1 d . . . H30A H 0.1171 0.1117 0.4095 0.109 Uiso 1 1 calc R . . H30B H 0.2170 0.0395 0.3787 0.109 Uiso 1 1 calc R . . H30C H 0.2515 0.1762 0.3951 0.109 Uiso 1 1 calc R . . Cl1S Cl 0.123(2) 0.953(2) 0.1122(16) 0.097(6) Uiso 0.25 1 d P . . Cl2S Cl 0.025(4) 0.936(3) -0.077(3) 0.164(12) Uiso 0.25 1 d P . . C1S C 0.099(6) 0.980(6) 0.048(5) 0.066(15) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.0394(3) 0.0362(3) 0.0602(3) 0.0239(2) 0.01589(19) 0.01236(19) Si1 0.069(3) 0.049(3) 0.059(2) 0.0120(19) 0.0054(19) 0.010(2) Si2 0.0386(18) 0.038(2) 0.076(2) 0.0276(18) 0.0131(16) 0.0085(15) Cl1 0.073(2) 0.0338(18) 0.078(2) 0.0208(16) 0.0373(18) 0.0127(16) O1 0.052(5) 0.062(6) 0.060(5) 0.024(5) 0.017(4) 0.017(5) O2 0.049(5) 0.050(6) 0.063(5) 0.020(5) 0.013(4) 0.015(4) N1 0.043(6) 0.048(7) 0.070(7) 0.016(6) 0.012(5) 0.013(5) N2 0.042(6) 0.058(8) 0.081(8) 0.028(6) 0.016(5) 0.016(5) N3 0.038(5) 0.038(6) 0.070(7) 0.025(5) 0.014(5) 0.006(4) P1 0.0464(19) 0.054(2) 0.061(2) 0.0200(18) 0.0124(15) 0.0220(17) P2 0.0377(17) 0.050(2) 0.068(2) 0.0298(18) 0.0153(15) 0.0113(15) C1 0.089(14) 0.124(19) 0.081(12) 0.027(13) -0.015(10) 0.011(13) C2 0.137(17) 0.055(11) 0.092(13) 0.030(10) 0.013(12) 0.039(11) C3 0.18(2) 0.071(14) 0.081(13) -0.003(11) 0.051(14) 0.013(14) C4 0.062(9) 0.070(11) 0.075(10) 0.017(8) 0.024(8) 0.027(8) C5 0.084(12) 0.136(18) 0.092(12) 0.066(13) 0.024(10) 0.060(13) C6 0.097(15) 0.15(2) 0.109(15) 0.055(15) 0.027(12) 0.073(15) C7 0.098(16) 0.22(3) 0.084(13) 0.053(17) 0.013(11) 0.100(19) C8 0.057(10) 0.111(17) 0.102(14) -0.001(12) 0.019(9) 0.035(11) C9 0.086(13) 0.116(17) 0.102(13) 0.034(12) 0.035(10) 0.063(12) C10 0.044(7) 0.061(10) 0.078(10) 0.021(8) 0.014(7) 0.009(7) C11 0.086(13) 0.15(2) 0.071(11) 0.038(12) 0.028(9) 0.069(14) C12 0.088(14) 0.23(3) 0.054(10) 0.031(14) 0.021(9) 0.063(17) C13 0.071(12) 0.18(2) 0.079(12) 0.055(14) 0.007(9) 0.033(14) C14 0.101(15) 0.101(17) 0.094(14) 0.019(12) -0.022(12) 0.042(13) C15 0.070(11) 0.097(14) 0.080(11) 0.026(10) -0.003(8) 0.035(10) C16 0.045(7) 0.059(9) 0.068(8) 0.027(7) 0.019(6) 0.015(6) C17 0.054(9) 0.074(12) 0.099(12) 0.043(10) 0.008(8) 0.023(8) C18 0.056(9) 0.101(15) 0.089(11) 0.041(11) 0.000(8) 0.032(10) C19 0.045(9) 0.100(15) 0.101(13) 0.021(11) 0.002(8) 0.017(9) C20 0.042(8) 0.071(11) 0.092(12) 0.014(9) 0.019(8) 0.003(7) C21 0.061(9) 0.056(10) 0.081(10) 0.030(8) 0.025(7) 0.013(7) C22 0.049(8) 0.054(9) 0.073(9) 0.029(7) 0.018(6) 0.014(6) C23 0.056(9) 0.16(2) 0.089(12) 0.075(13) 0.032(8) 0.033(11) C24 0.105(16) 0.24(3) 0.100(15) 0.102(19) 0.052(12) 0.087(19) C25 0.104(17) 0.24(3) 0.127(18) 0.11(2) 0.050(14) 0.08(2) C26 0.099(15) 0.16(2) 0.126(18) 0.081(17) 0.015(13) 0.048(15) C27 0.063(10) 0.118(17) 0.107(14) 0.061(13) 0.003(9) 0.030(10) C28 0.054(8) 0.051(9) 0.103(12) 0.036(9) 0.023(8) 0.007(7) C29 0.054(8) 0.059(10) 0.104(11) 0.047(9) 0.033(8) 0.025(7) C30 0.067(10) 0.049(10) 0.092(11) 0.025(9) 0.007(8) -0.007(7) _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 U1 O1 1.755(9) . ? U1 O2 1.759(9) . ? U1 N2 2.442(11) . ? U1 N3 2.528(10) . ? U1 N1 2.593(11) . ? U1 Cl1 2.795(3) . ? U1 Cl1 2.812(3) 2_666 ? U1 P1 3.158(3) . ? U1 P2 3.169(3) . ? Si1 N1 1.697(12) . ? Si1 C1 1.82(2) . ? Si1 C3 1.871(19) . ? Si1 C2 1.872(18) . ? Si2 N3 1.763(11) . ? Si2 C30 1.855(18) . ? Si2 C28 1.860(14) . ? Si2 C29 1.862(13) . ? Cl1 U1 2.812(3) 2_666 ? N1 P1 1.600(12) . ? N2 P2 1.591(13) . ? N2 P1 1.599(13) . ? N3 P2 1.568(10) . ? P1 C10 1.796(8) . ? P1 C4 1.828(8) . ? P2 C16 1.801(7) . ? P2 C22 1.802(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C6 C7 1.3900 . ? C6 H6 0.9500 . ? C7 C8 1.3900 . ? C7 H7 0.9500 . ? C8 C9 1.3900 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C19 H19 0.9500 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? Cl1S C1S 1.10(6) . ? Cl2S C1S 1.78(7) . ? Cl2S C1S 1.92(7) 2_575 ? Cl2S Cl2S 2.46(7) 2_575 ? C1S Cl2S 1.92(7) 2_575 ? 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 O1 U1 O2 178.3(4) . . ? O1 U1 N2 93.4(4) . . ? O2 U1 N2 88.3(4) . . ? O1 U1 N3 90.7(4) . . ? O2 U1 N3 90.3(4) . . ? N2 U1 N3 58.6(4) . . ? O1 U1 N1 90.5(4) . . ? O2 U1 N1 90.2(4) . . ? N2 U1 N1 60.1(4) . . ? N3 U1 N1 118.7(3) . . ? O1 U1 Cl1 92.4(3) . . ? O2 U1 Cl1 86.2(3) . . ? N2 U1 Cl1 143.5(3) . . ? N3 U1 Cl1 157.3(3) . . ? N1 U1 Cl1 83.8(3) . . ? O1 U1 Cl1 91.9(3) . 2_666 ? O2 U1 Cl1 86.8(3) . 2_666 ? N2 U1 Cl1 141.5(3) . 2_666 ? N3 U1 Cl1 83.2(2) . 2_666 ? N1 U1 Cl1 157.9(3) . 2_666 ? Cl1 U1 Cl1 74.15(11) . 2_666 ? O1 U1 P1 93.7(3) . . ? O2 U1 P1 87.8(3) . . ? N2 U1 P1 29.8(3) . . ? N3 U1 P1 88.4(2) . . ? N1 U1 P1 30.3(3) . . ? Cl1 U1 P1 113.81(10) . . ? Cl1 U1 P1 170.06(10) 2_666 . ? O1 U1 P2 94.6(3) . . ? O2 U1 P2 86.9(3) . . ? N2 U1 P2 29.5(3) . . ? N3 U1 P2 29.3(2) . . ? N1 U1 P2 89.6(3) . . ? Cl1 U1 P2 170.46(9) . . ? Cl1 U1 P2 112.08(10) 2_666 . ? P1 U1 P2 59.25(10) . . ? N1 Si1 C1 109.0(9) . . ? N1 Si1 C3 109.1(9) . . ? C1 Si1 C3 108.2(11) . . ? N1 Si1 C2 112.9(8) . . ? C1 Si1 C2 109.7(11) . . ? C3 Si1 C2 107.8(10) . . ? N3 Si2 C30 111.0(7) . . ? N3 Si2 C28 112.0(6) . . ? C30 Si2 C28 106.9(8) . . ? N3 Si2 C29 108.4(6) . . ? C30 Si2 C29 110.1(8) . . ? C28 Si2 C29 108.4(7) . . ? U1 Cl1 U1 105.85(11) . 2_666 ? P1 N1 Si1 132.6(7) . . ? P1 N1 U1 94.7(5) . . ? Si1 N1 U1 131.9(6) . . ? P2 N2 P1 157.4(8) . . ? P2 N2 U1 101.5(5) . . ? P1 N2 U1 100.7(6) . . ? P2 N3 Si2 127.1(6) . . ? P2 N3 U1 98.6(5) . . ? Si2 N3 U1 133.9(5) . . ? N2 P1 N1 104.3(6) . . ? N2 P1 C10 109.0(6) . . ? N1 P1 C10 114.3(6) . . ? N2 P1 C4 107.3(6) . . ? N1 P1 C4 114.4(6) . . ? C10 P1 C4 107.2(5) . . ? N2 P1 U1 49.5(4) . . ? N1 P1 U1 54.9(4) . . ? C10 P1 U1 129.7(3) . . ? C4 P1 U1 122.1(4) . . ? N3 P2 N2 100.8(6) . . ? N3 P2 C16 116.1(6) . . ? N2 P2 C16 109.2(5) . . ? N3 P2 C22 115.9(5) . . ? N2 P2 C22 106.6(6) . . ? C16 P2 C22 107.5(4) . . ? N3 P2 U1 52.1(4) . . ? N2 P2 U1 49.1(4) . . ? C16 P2 U1 122.2(3) . . ? C22 P2 U1 129.1(4) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 120.0 . . ? C5 C4 P1 118.3(6) . . ? C9 C4 P1 121.1(6) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C11 C10 C15 120.0 . . ? C11 C10 P1 123.2(6) . . ? C15 C10 P1 116.8(6) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C17 C16 C21 120.0 . . ? C17 C16 P2 116.2(5) . . ? C21 C16 P2 123.8(5) . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C23 C22 C27 120.0 . . ? C23 C22 P2 120.3(6) . . ? C27 C22 P2 119.0(5) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C1S Cl2S C1S 97(3) . 2_575 ? C1S Cl2S Cl2S 51(2) . 2_575 ? C1S Cl2S Cl2S 46(2) 2_575 2_575 ? Cl1S C1S Cl2S 147(6) . . ? Cl1S C1S Cl2S 110(4) . 2_575 ? Cl2S C1S Cl2S 83(3) . 2_575 ? 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 O1 U1 Cl1 U1 91.3(3) . . . 2_666 ? O2 U1 Cl1 U1 -87.8(3) . . . 2_666 ? N2 U1 Cl1 U1 -169.7(5) . . . 2_666 ? N3 U1 Cl1 U1 -6.2(7) . . . 2_666 ? N1 U1 Cl1 U1 -178.4(3) . . . 2_666 ? Cl1 U1 Cl1 U1 0.0 2_666 . . 2_666 ? P1 U1 Cl1 U1 -173.66(10) . . . 2_666 ? P2 U1 Cl1 U1 -132.0(6) . . . 2_666 ? C1 Si1 N1 P1 116.0(11) . . . . ? C3 Si1 N1 P1 -2.1(15) . . . . ? C2 Si1 N1 P1 -121.9(11) . . . . ? C1 Si1 N1 U1 -51.6(11) . . . . ? C3 Si1 N1 U1 -169.7(11) . . . . ? C2 Si1 N1 U1 70.5(10) . . . . ? O1 U1 N1 P1 -96.3(5) . . . . ? O2 U1 N1 P1 85.2(5) . . . . ? N2 U1 N1 P1 -2.7(4) . . . . ? N3 U1 N1 P1 -5.2(6) . . . . ? Cl1 U1 N1 P1 171.4(5) . . . . ? Cl1 U1 N1 P1 167.3(3) 2_666 . . . ? P2 U1 N1 P1 -1.8(4) . . . . ? O1 U1 N1 Si1 74.5(8) . . . . ? O2 U1 N1 Si1 -103.9(8) . . . . ? N2 U1 N1 Si1 168.2(9) . . . . ? N3 U1 N1 Si1 165.6(7) . . . . ? Cl1 U1 N1 Si1 -17.8(8) . . . . ? Cl1 U1 N1 Si1 -21.8(13) 2_666 . . . ? P1 U1 N1 Si1 170.9(12) . . . . ? P2 U1 N1 Si1 169.1(8) . . . . ? O1 U1 N2 P2 -93.3(6) . . . . ? O2 U1 N2 P2 86.8(6) . . . . ? N3 U1 N2 P2 -4.5(4) . . . . ? N1 U1 N2 P2 178.1(7) . . . . ? Cl1 U1 N2 P2 168.1(2) . . . . ? Cl1 U1 N2 P2 4.1(8) 2_666 . . . ? P1 U1 N2 P2 175.3(10) . . . . ? O1 U1 N2 P1 91.4(6) . . . . ? O2 U1 N2 P1 -88.5(6) . . . . ? N3 U1 N2 P1 -179.9(7) . . . . ? N1 U1 N2 P1 2.7(5) . . . . ? Cl1 U1 N2 P1 -7.2(9) . . . . ? Cl1 U1 N2 P1 -171.3(2) 2_666 . . . ? P2 U1 N2 P1 -175.3(10) . . . . ? C30 Si2 N3 P2 110.4(9) . . . . ? C28 Si2 N3 P2 -9.0(11) . . . . ? C29 Si2 N3 P2 -128.5(9) . . . . ? C30 Si2 N3 U1 -61.2(9) . . . . ? C28 Si2 N3 U1 179.4(8) . . . . ? C29 Si2 N3 U1 59.8(9) . . . . ? O1 U1 N3 P2 98.1(5) . . . . ? O2 U1 N3 P2 -83.3(5) . . . . ? N2 U1 N3 P2 4.6(4) . . . . ? N1 U1 N3 P2 7.1(6) . . . . ? Cl1 U1 N3 P2 -164.1(3) . . . . ? Cl1 U1 N3 P2 -170.1(5) 2_666 . . . ? P1 U1 N3 P2 4.5(4) . . . . ? O1 U1 N3 Si2 -88.6(8) . . . . ? O2 U1 N3 Si2 90.0(8) . . . . ? N2 U1 N3 Si2 177.8(9) . . . . ? N1 U1 N3 Si2 -179.6(7) . . . . ? Cl1 U1 N3 Si2 9.2(13) . . . . ? Cl1 U1 N3 Si2 3.2(7) 2_666 . . . ? P1 U1 N3 Si2 177.8(7) . . . . ? P2 U1 N3 Si2 173.3(11) . . . . ? P2 N2 P1 N1 -172(2) . . . . ? U1 N2 P1 N1 -4.0(7) . . . . ? P2 N2 P1 C10 65(2) . . . . ? U1 N2 P1 C10 -126.5(5) . . . . ? P2 N2 P1 C4 -50(2) . . . . ? U1 N2 P1 C4 117.8(5) . . . . ? P2 N2 P1 U1 -168(3) . . . . ? Si1 N1 P1 N2 -167.1(9) . . . . ? U1 N1 P1 N2 3.7(6) . . . . ? Si1 N1 P1 C10 -48.2(11) . . . . ? U1 N1 P1 C10 122.6(5) . . . . ? Si1 N1 P1 C4 76.0(11) . . . . ? U1 N1 P1 C4 -113.2(5) . . . . ? Si1 N1 P1 U1 -170.8(12) . . . . ? O1 U1 P1 N2 -90.5(6) . . . . ? O2 U1 P1 N2 90.4(6) . . . . ? N3 U1 P1 N2 0.1(6) . . . . ? N1 U1 P1 N2 -175.3(8) . . . . ? Cl1 U1 P1 N2 175.3(6) . . . . ? Cl1 U1 P1 N2 33.3(8) 2_666 . . . ? P2 U1 P1 N2 2.7(6) . . . . ? O1 U1 P1 N1 84.8(6) . . . . ? O2 U1 P1 N1 -94.3(6) . . . . ? N2 U1 P1 N1 175.3(8) . . . . ? N3 U1 P1 N1 175.4(6) . . . . ? Cl1 U1 P1 N1 -9.4(5) . . . . ? Cl1 U1 P1 N1 -151.4(7) 2_666 . . . ? P2 U1 P1 N1 178.0(5) . . . . ? O1 U1 P1 C10 -9.3(7) . . . . ? O2 U1 P1 C10 171.6(6) . . . . ? N2 U1 P1 C10 81.2(8) . . . . ? N3 U1 P1 C10 81.3(6) . . . . ? N1 U1 P1 C10 -94.1(8) . . . . ? Cl1 U1 P1 C10 -103.5(6) . . . . ? Cl1 U1 P1 C10 114.5(7) 2_666 . . . ? P2 U1 P1 C10 83.9(6) . . . . ? O1 U1 P1 C4 -176.2(6) . . . . ? O2 U1 P1 C4 4.7(6) . . . . ? N2 U1 P1 C4 -85.7(7) . . . . ? N3 U1 P1 C4 -85.6(5) . . . . ? N1 U1 P1 C4 99.0(7) . . . . ? Cl1 U1 P1 C4 89.6(5) . . . . ? Cl1 U1 P1 C4 -52.5(8) 2_666 . . . ? P2 U1 P1 C4 -83.1(5) . . . . ? Si2 N3 P2 N2 180.0(8) . . . . ? U1 N3 P2 N2 -6.1(6) . . . . ? Si2 N3 P2 C16 -62.2(9) . . . . ? U1 N3 P2 C16 111.8(5) . . . . ? Si2 N3 P2 C22 65.4(10) . . . . ? U1 N3 P2 C22 -120.7(5) . . . . ? Si2 N3 P2 U1 -173.9(10) . . . . ? P1 N2 P2 N3 174(2) . . . . ? U1 N2 P2 N3 6.4(6) . . . . ? P1 N2 P2 C16 52(2) . . . . ? U1 N2 P2 C16 -116.4(5) . . . . ? P1 N2 P2 C22 -64(2) . . . . ? U1 N2 P2 C22 127.7(5) . . . . ? P1 N2 P2 U1 168(3) . . . . ? O1 U1 P2 N3 -83.2(6) . . . . ? O2 U1 P2 N3 96.0(6) . . . . ? N2 U1 P2 N3 -172.1(8) . . . . ? N1 U1 P2 N3 -173.7(6) . . . . ? Cl1 U1 P2 N3 140.2(8) . . . . ? Cl1 U1 P2 N3 10.7(5) 2_666 . . . ? P1 U1 P2 N3 -174.8(5) . . . . ? O1 U1 P2 N2 88.9(6) . . . . ? O2 U1 P2 N2 -91.9(6) . . . . ? N3 U1 P2 N2 172.1(8) . . . . ? N1 U1 P2 N2 -1.7(6) . . . . ? Cl1 U1 P2 N2 -47.8(9) . . . . ? Cl1 U1 P2 N2 -177.2(6) 2_666 . . . ? P1 U1 P2 N2 -2.7(6) . . . . ? O1 U1 P2 C16 177.1(5) . . . . ? O2 U1 P2 C16 -3.7(5) . . . . ? N2 U1 P2 C16 88.2(7) . . . . ? N3 U1 P2 C16 -99.7(7) . . . . ? N1 U1 P2 C16 86.5(5) . . . . ? Cl1 U1 P2 C16 40.5(8) . . . . ? Cl1 U1 P2 C16 -89.0(4) 2_666 . . . ? P1 U1 P2 C16 85.5(4) . . . . ? O1 U1 P2 C22 11.4(6) . . . . ? O2 U1 P2 C22 -169.4(6) . . . . ? N2 U1 P2 C22 -77.5(7) . . . . ? N3 U1 P2 C22 94.6(7) . . . . ? N1 U1 P2 C22 -79.2(5) . . . . ? Cl1 U1 P2 C22 -125.3(7) . . . . ? Cl1 U1 P2 C22 105.3(5) 2_666 . . . ? P1 U1 P2 C22 -80.2(5) . . . . ? N2 P1 C4 C5 -104.7(8) . . . . ? N1 P1 C4 C5 10.4(9) . . . . ? C10 P1 C4 C5 138.3(8) . . . . ? U1 P1 C4 C5 -52.2(8) . . . . ? N2 P1 C4 C9 66.6(8) . . . . ? N1 P1 C4 C9 -178.3(7) . . . . ? C10 P1 C4 C9 -50.4(8) . . . . ? U1 P1 C4 C9 119.1(6) . . . . ? C9 C4 C5 C6 0.0 . . . . ? P1 C4 C5 C6 171.4(9) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C4 0.0 . . . . ? C5 C4 C9 C8 0.0 . . . . ? P1 C4 C9 C8 -171.1(9) . . . . ? N2 P1 C10 C11 -139.0(8) . . . . ? N1 P1 C10 C11 104.8(9) . . . . ? C4 P1 C10 C11 -23.2(10) . . . . ? U1 P1 C10 C11 168.4(6) . . . . ? N2 P1 C10 C15 39.9(9) . . . . ? N1 P1 C10 C15 -76.3(9) . . . . ? C4 P1 C10 C15 155.8(7) . . . . ? U1 P1 C10 C15 -12.7(9) . . . . ? C15 C10 C11 C12 0.0 . . . . ? P1 C10 C11 C12 178.9(10) . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C10 0.0 . . . . ? C11 C10 C15 C14 0.0 . . . . ? P1 C10 C15 C14 -179.0(9) . . . . ? N3 P2 C16 C17 -69.6(7) . . . . ? N2 P2 C16 C17 43.5(7) . . . . ? C22 P2 C16 C17 158.8(6) . . . . ? U1 P2 C16 C17 -9.6(7) . . . . ? N3 P2 C16 C21 112.5(7) . . . . ? N2 P2 C16 C21 -134.5(7) . . . . ? C22 P2 C16 C21 -19.1(8) . . . . ? U1 P2 C16 C21 172.5(5) . . . . ? C21 C16 C17 C18 0.0 . . . . ? P2 C16 C17 C18 -178.1(8) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C21 0.0 . . . . ? C19 C20 C21 C16 0.0 . . . . ? C17 C16 C21 C20 0.0 . . . . ? P2 C16 C21 C20 177.9(8) . . . . ? N3 P2 C22 C23 -176.5(8) . . . . ? N2 P2 C22 C23 72.2(9) . . . . ? C16 P2 C22 C23 -44.8(9) . . . . ? U1 P2 C22 C23 122.5(7) . . . . ? N3 P2 C22 C27 13.2(10) . . . . ? N2 P2 C22 C27 -98.0(8) . . . . ? C16 P2 C22 C27 144.9(8) . . . . ? U1 P2 C22 C27 -47.7(9) . . . . ? C27 C22 C23 C24 0.0 . . . . ? P2 C22 C23 C24 -170.2(10) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C22 0.0 . . . . ? C23 C22 C27 C26 0.0 . . . . ? P2 C22 C27 C26 170.3(10) . . . . ? C1S Cl2S C1S Cl1S 117(10) 2_575 . . . ? Cl2S Cl2S C1S Cl1S 117(10) 2_575 . . . ? C1S Cl2S C1S Cl2S 0.000(4) 2_575 . . 2_575 ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 24.39 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 5.043 _refine_diff_density_min -2.409 _refine_diff_density_rms 0.217 #===END data_s1364abs _database_code_CSD 209177 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_exptl_refinement ; The structure was solved by the Patterson method. The asymmetric unit contains the molecule, together with 0.5 MePh disordered over 2 sites related by a centre of symmetry. The non-H were refined anisotropically H atoms, except those on the solvent molecule were included in calculated positions. H1 was found by difference Fourier techniques and refined isotropically. ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.50 H61 N3 O2 P2 Si4 U' _chemical_formula_weight 1034.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' U U -9.6767 9.6646 '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 10.2914(13) _cell_length_b 12.7639(16) _cell_length_c 17.868(2) _cell_angle_alpha 84.831(2) _cell_angle_beta 83.767(2) _cell_angle_gamma 77.728(2) _cell_volume 2274.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7413 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.03 _exptl_crystal_description cubic _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1038 _exptl_absorpt_coefficient_mu 3.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.488 _exptl_absorpt_correction_T_max 0.488 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19949 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.32 _reflns_number_total 10410 _reflns_number_gt 9423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0296P)^2^+0.2641P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10410 _refine_ls_number_parameters 503 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.605763(11) 0.676326(9) 0.720257(6) 0.01080(4) Uani 1 1 d . . . O1 O 0.4586(2) 0.69633(17) 0.67300(12) 0.0161(5) Uani 1 1 d . . . O2 O 0.7509(2) 0.65913(17) 0.76994(12) 0.0147(5) Uani 1 1 d . . . N1 N 0.6344(3) 0.4930(2) 0.72376(15) 0.0140(5) Uani 1 1 d . . . N2 N 0.4949(3) 0.7899(2) 0.82491(14) 0.0126(5) Uani 1 1 d . . . N3 N 0.7321(3) 0.7538(2) 0.61025(14) 0.0121(5) Uani 1 1 d . . . C1 C 0.5795(3) 0.8919(2) 0.70024(17) 0.0109(6) Uani 1 1 d . . . H1 H 0.503(4) 0.900(3) 0.674(2) 0.031(11) Uiso 1 1 d . . . P1 P 0.72364(8) 0.87058(6) 0.63910(4) 0.01101(16) Uani 1 1 d . . . P2 P 0.53292(8) 0.90243(6) 0.79559(4) 0.01078(16) Uani 1 1 d . . . Si1 Si 0.51105(10) 0.42446(8) 0.70900(6) 0.0220(2) Uani 1 1 d . . . Si2 Si 0.78463(9) 0.41466(7) 0.75138(5) 0.01710(19) Uani 1 1 d . . . Si3 Si 0.42740(9) 0.73703(7) 0.90893(5) 0.01504(18) Uani 1 1 d . . . Si4 Si 0.79905(9) 0.69034(8) 0.52913(5) 0.01690(19) Uani 1 1 d . . . C2 C 0.3930(3) 1.0147(2) 0.81013(17) 0.0129(6) Uani 1 1 d . . . C3 C 0.3306(3) 1.0748(3) 0.75092(18) 0.0149(6) Uani 1 1 d . . . H3 H 0.3612 1.0588 0.7015 0.018 Uiso 1 1 calc R . . C4 C 0.2227(3) 1.1590(3) 0.76467(19) 0.0175(7) Uani 1 1 d . . . H4 H 0.1809 1.1983 0.7244 0.021 Uiso 1 1 calc R . . C5 C 0.1769(3) 1.1847(3) 0.83731(19) 0.0193(7) Uani 1 1 d . . . H5 H 0.1052 1.2416 0.8461 0.023 Uiso 1 1 calc R . . C6 C 0.2383(3) 1.1252(3) 0.89726(19) 0.0228(8) Uani 1 1 d . . . H6 H 0.2074 1.1416 0.9465 0.027 Uiso 1 1 calc R . . C7 C 0.3459(3) 1.0412(3) 0.88358(18) 0.0196(7) Uani 1 1 d . . . H7 H 0.3873 1.0020 0.9240 0.024 Uiso 1 1 calc R . . C8 C 0.6632(3) 0.9357(2) 0.84351(17) 0.0127(6) Uani 1 1 d . . . C9 C 0.6642(3) 1.0419(3) 0.85443(18) 0.0175(7) Uani 1 1 d . . . H9 H 0.5955 1.0965 0.8385 0.021 Uiso 1 1 calc R . . C10 C 0.7678(3) 1.0670(3) 0.88926(19) 0.0217(7) Uani 1 1 d . . . H10 H 0.7678 1.1381 0.8970 0.026 Uiso 1 1 calc R . . C11 C 0.8700(3) 0.9859(3) 0.91216(19) 0.0210(7) Uani 1 1 d . . . H11 H 0.9396 1.0024 0.9349 0.025 Uiso 1 1 calc R . . C12 C 0.8694(3) 0.8801(3) 0.90153(18) 0.0182(7) Uani 1 1 d . . . H12 H 0.9389 0.8259 0.9169 0.022 Uiso 1 1 calc R . . C13 C 0.7665(3) 0.8542(3) 0.86826(18) 0.0160(7) Uani 1 1 d . . . H13 H 0.7658 0.7827 0.8623 0.019 Uiso 1 1 calc R . . C14 C 0.8710(3) 0.8783(3) 0.68315(17) 0.0134(6) Uani 1 1 d . . . C15 C 0.8903(3) 0.9768(3) 0.70227(19) 0.0179(7) Uani 1 1 d . . . H15 H 0.8253 1.0386 0.6944 0.021 Uiso 1 1 calc R . . C16 C 1.0052(3) 0.9831(3) 0.73272(19) 0.0204(7) Uani 1 1 d . . . H16 H 1.0170 1.0489 0.7462 0.024 Uiso 1 1 calc R . . C17 C 1.1035(3) 0.8916(3) 0.74336(19) 0.0204(7) Uani 1 1 d . . . H17 H 1.1816 0.8963 0.7634 0.025 Uiso 1 1 calc R . . C18 C 1.0858(3) 0.7943(3) 0.72435(18) 0.0185(7) Uani 1 1 d . . . H18 H 1.1519 0.7331 0.7316 0.022 Uiso 1 1 calc R . . C19 C 0.9694(3) 0.7865(3) 0.69437(17) 0.0149(6) Uani 1 1 d . . . H19 H 0.9573 0.7202 0.6819 0.018 Uiso 1 1 calc R . . C20 C 0.7170(3) 0.9753(2) 0.56332(17) 0.0132(6) Uani 1 1 d . . . C21 C 0.8288(4) 0.9777(3) 0.5135(2) 0.0325(10) Uani 1 1 d . . . H21 H 0.9071 0.9271 0.5203 0.039 Uiso 1 1 calc R . . C22 C 0.8255(4) 1.0548(3) 0.4537(2) 0.0337(10) Uani 1 1 d . . . H22 H 0.9013 1.0553 0.4203 0.040 Uiso 1 1 calc R . . C23 C 0.7110(3) 1.1306(3) 0.44325(19) 0.0222(8) Uani 1 1 d . . . H23 H 0.7089 1.1832 0.4036 0.027 Uiso 1 1 calc R . . C24 C 0.6002(4) 1.1273(3) 0.4923(2) 0.0383(11) Uani 1 1 d . . . H24 H 0.5218 1.1774 0.4853 0.046 Uiso 1 1 calc R . . C25 C 0.6025(4) 1.0509(3) 0.5522(2) 0.0320(10) Uani 1 1 d . . . H25 H 0.5262 1.0505 0.5852 0.038 Uiso 1 1 calc R . . C26 C 0.4518(4) 0.5904(3) 0.8990(2) 0.0359(10) Uani 1 1 d . . . H26A H 0.4128 0.5786 0.8549 0.054 Uiso 1 1 calc R . . H26B H 0.4097 0.5575 0.9428 0.054 Uiso 1 1 calc R . . H26C H 0.5456 0.5594 0.8942 0.054 Uiso 1 1 calc R . . C27 C 0.5123(4) 0.7600(3) 0.99112(19) 0.0273(9) Uani 1 1 d . . . H27A H 0.6063 0.7312 0.9827 0.041 Uiso 1 1 calc R . . H27B H 0.4763 0.7250 1.0360 0.041 Uiso 1 1 calc R . . H27C H 0.4980 0.8358 0.9970 0.041 Uiso 1 1 calc R . . C28 C 0.2444(3) 0.7891(3) 0.92755(19) 0.0238(8) Uani 1 1 d . . . H28A H 0.2275 0.8656 0.9307 0.036 Uiso 1 1 calc R . . H28B H 0.2123 0.7561 0.9743 0.036 Uiso 1 1 calc R . . H28C H 0.1992 0.7726 0.8873 0.036 Uiso 1 1 calc R . . C29 C 0.7593(4) 0.7707(3) 0.4387(2) 0.0319(9) Uani 1 1 d . . . H29A H 0.6698 0.8121 0.4444 0.048 Uiso 1 1 calc R . . H29B H 0.7672 0.7231 0.3991 0.048 Uiso 1 1 calc R . . H29C H 0.8206 0.8181 0.4263 0.048 Uiso 1 1 calc R . . C30 C 0.9850(3) 0.6517(3) 0.5236(2) 0.0249(8) Uani 1 1 d . . . H30A H 1.0216 0.7153 0.5204 0.037 Uiso 1 1 calc R . . H30B H 1.0174 0.6124 0.4797 0.037 Uiso 1 1 calc R . . H30C H 1.0116 0.6076 0.5680 0.037 Uiso 1 1 calc R . . C31 C 0.7232(4) 0.5702(3) 0.5315(2) 0.0231(8) Uani 1 1 d . . . H31A H 0.7491 0.5228 0.5745 0.035 Uiso 1 1 calc R . . H31B H 0.7537 0.5335 0.4862 0.035 Uiso 1 1 calc R . . H31C H 0.6277 0.5923 0.5349 0.035 Uiso 1 1 calc R . . C32 C 0.9375(3) 0.4631(3) 0.7081(2) 0.0230(8) Uani 1 1 d . . . H32A H 0.9377 0.4694 0.6542 0.034 Uiso 1 1 calc R . . H32B H 1.0158 0.4127 0.7223 0.034 Uiso 1 1 calc R . . H32C H 0.9373 0.5320 0.7258 0.034 Uiso 1 1 calc R . . C33 C 0.7869(4) 0.4035(3) 0.8560(2) 0.0273(8) Uani 1 1 d . . . H33A H 0.7852 0.4729 0.8732 0.041 Uiso 1 1 calc R . . H33B H 0.8665 0.3544 0.8697 0.041 Uiso 1 1 calc R . . H33C H 0.7100 0.3773 0.8789 0.041 Uiso 1 1 calc R . . C34 C 0.8230(4) 0.2740(3) 0.7206(3) 0.0330(9) Uani 1 1 d . . . H34A H 0.7478 0.2410 0.7356 0.049 Uiso 1 1 calc R . . H34B H 0.8997 0.2334 0.7438 0.049 Uiso 1 1 calc R . . H34C H 0.8411 0.2756 0.6667 0.049 Uiso 1 1 calc R . . C35 C 0.4808(4) 0.3310(3) 0.7933(2) 0.0282(9) Uani 1 1 d . . . H35A H 0.5645 0.2882 0.8069 0.042 Uiso 1 1 calc R . . H35B H 0.4246 0.2849 0.7812 0.042 Uiso 1 1 calc R . . H35C H 0.4378 0.3721 0.8348 0.042 Uiso 1 1 calc R . . C36 C 0.5518(5) 0.3475(4) 0.6225(2) 0.0446(12) Uani 1 1 d . . . H36A H 0.5591 0.3963 0.5788 0.067 Uiso 1 1 calc R . . H36B H 0.4822 0.3095 0.6180 0.067 Uiso 1 1 calc R . . H36C H 0.6349 0.2970 0.6261 0.067 Uiso 1 1 calc R . . C37 C 0.3418(4) 0.5093(3) 0.6975(3) 0.0443(12) Uani 1 1 d . . . H37A H 0.3171 0.5568 0.7377 0.066 Uiso 1 1 calc R . . H37B H 0.2780 0.4639 0.6989 0.066 Uiso 1 1 calc R . . H37C H 0.3432 0.5507 0.6499 0.066 Uiso 1 1 calc R . . C1S C -0.0794(5) 0.5796(4) 0.9815(3) 0.0430(11) Uani 1 1 d . . . C2S C 0.1066(5) 0.5038(4) 0.8886(3) 0.0500(13) Uani 1 1 d . . . C3S C 0.0009(9) 0.5803(7) 0.9018(6) 0.042(2) Uani 0.50 1 d P . . C4S C 0.0263(8) 0.5042(8) 0.9694(5) 0.041(2) Uani 0.50 1 d P . . C5S C 0.1527(8) 0.4243(7) 0.9414(5) 0.037(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01258(6) 0.00765(6) 0.01181(6) -0.00023(4) -0.00176(4) -0.00115(4) O1 0.0176(12) 0.0123(11) 0.0189(12) 0.0017(9) -0.0062(9) -0.0029(9) O2 0.0150(11) 0.0134(11) 0.0158(11) -0.0023(9) -0.0024(9) -0.0018(9) N1 0.0163(13) 0.0093(13) 0.0168(14) -0.0007(10) -0.0021(11) -0.0032(11) N2 0.0143(13) 0.0088(13) 0.0146(13) 0.0002(10) 0.0005(10) -0.0033(10) N3 0.0144(13) 0.0090(13) 0.0120(13) -0.0019(10) 0.0010(10) -0.0011(10) C1 0.0119(15) 0.0094(15) 0.0112(15) -0.0015(11) -0.0003(12) -0.0021(12) P1 0.0108(4) 0.0098(4) 0.0111(4) 0.0006(3) 0.0004(3) -0.0001(3) P2 0.0119(4) 0.0091(4) 0.0106(4) -0.0008(3) -0.0004(3) -0.0006(3) Si1 0.0237(5) 0.0136(5) 0.0314(6) 0.0018(4) -0.0117(4) -0.0068(4) Si2 0.0164(5) 0.0102(4) 0.0233(5) 0.0004(4) -0.0034(4) 0.0005(4) Si3 0.0163(4) 0.0147(5) 0.0125(4) 0.0017(3) 0.0015(3) -0.0022(4) Si4 0.0174(5) 0.0189(5) 0.0122(4) -0.0038(4) 0.0008(3) 0.0013(4) C2 0.0127(15) 0.0097(15) 0.0162(16) -0.0009(12) -0.0010(12) -0.0022(12) C3 0.0164(16) 0.0164(16) 0.0115(15) -0.0034(12) 0.0003(12) -0.0021(13) C4 0.0160(16) 0.0149(16) 0.0197(17) 0.0013(13) -0.0037(13) 0.0013(13) C5 0.0139(16) 0.0155(17) 0.0270(19) -0.0043(14) -0.0007(14) 0.0010(13) C6 0.0260(19) 0.0220(19) 0.0167(17) -0.0041(14) 0.0041(14) 0.0018(15) C7 0.0226(18) 0.0201(18) 0.0132(16) 0.0012(13) -0.0018(13) 0.0014(14) C8 0.0139(15) 0.0123(15) 0.0118(15) -0.0011(12) 0.0015(12) -0.0035(12) C9 0.0197(17) 0.0132(16) 0.0190(17) -0.0013(13) -0.0033(13) -0.0008(13) C10 0.0265(19) 0.0192(18) 0.0227(18) -0.0044(14) -0.0029(15) -0.0102(15) C11 0.0214(18) 0.028(2) 0.0165(17) -0.0027(14) -0.0045(14) -0.0087(15) C12 0.0200(17) 0.0184(17) 0.0150(16) -0.0002(13) -0.0032(13) -0.0007(14) C13 0.0143(16) 0.0160(16) 0.0171(16) -0.0025(13) 0.0015(13) -0.0025(13) C14 0.0133(15) 0.0136(16) 0.0132(15) 0.0003(12) 0.0001(12) -0.0032(12) C15 0.0168(16) 0.0125(16) 0.0224(17) 0.0025(13) 0.0001(13) -0.0013(13) C16 0.0213(18) 0.0171(17) 0.0245(18) -0.0014(14) -0.0040(14) -0.0072(14) C17 0.0167(17) 0.0242(19) 0.0219(18) 0.0028(14) -0.0042(14) -0.0083(14) C18 0.0141(16) 0.0196(18) 0.0190(17) 0.0061(13) -0.0030(13) 0.0004(13) C19 0.0176(16) 0.0147(16) 0.0113(15) 0.0004(12) 0.0013(12) -0.0029(13) C20 0.0165(16) 0.0116(15) 0.0107(15) 0.0007(12) 0.0002(12) -0.0025(12) C21 0.0142(18) 0.035(2) 0.037(2) 0.0197(18) 0.0069(16) 0.0081(16) C22 0.0190(19) 0.040(2) 0.033(2) 0.0198(18) 0.0087(16) -0.0021(17) C23 0.0241(18) 0.0207(18) 0.0199(18) 0.0100(14) -0.0033(14) -0.0042(15) C24 0.026(2) 0.037(2) 0.036(2) 0.0225(19) 0.0068(17) 0.0136(18) C25 0.023(2) 0.033(2) 0.027(2) 0.0147(17) 0.0129(16) 0.0087(17) C26 0.043(3) 0.020(2) 0.040(2) 0.0044(17) 0.0168(19) -0.0080(18) C27 0.0199(18) 0.047(3) 0.0137(17) 0.0056(16) -0.0018(14) -0.0082(17) C28 0.0171(17) 0.035(2) 0.0181(17) 0.0043(15) 0.0001(14) -0.0060(16) C29 0.028(2) 0.049(3) 0.0149(18) 0.0034(17) 0.0013(15) -0.0035(19) C30 0.0200(18) 0.030(2) 0.0229(19) -0.0080(15) 0.0019(14) -0.0007(15) C31 0.0264(19) 0.0232(19) 0.0201(18) -0.0101(14) -0.0046(15) -0.0009(15) C32 0.0192(18) 0.0191(18) 0.0273(19) -0.0010(15) 0.0001(15) 0.0020(14) C33 0.0210(18) 0.032(2) 0.027(2) 0.0065(16) -0.0055(15) -0.0026(16) C34 0.025(2) 0.0147(18) 0.056(3) -0.0032(18) -0.0024(19) 0.0036(15) C35 0.0246(19) 0.0146(18) 0.047(2) 0.0051(16) -0.0088(17) -0.0076(15) C36 0.067(3) 0.035(3) 0.043(3) -0.010(2) -0.017(2) -0.028(2) C37 0.024(2) 0.026(2) 0.087(4) 0.017(2) -0.024(2) -0.0137(18) C1S 0.045(3) 0.033(3) 0.057(3) -0.012(2) -0.020(2) -0.010(2) C2S 0.054(3) 0.059(3) 0.044(3) -0.008(2) 0.000(2) -0.029(3) C3S 0.043(5) 0.028(5) 0.058(6) 0.005(4) -0.029(5) -0.007(4) C4S 0.029(5) 0.053(6) 0.053(6) -0.023(5) 0.007(4) -0.029(4) C5S 0.033(5) 0.033(5) 0.048(5) -0.010(4) -0.020(4) -0.003(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 U1 O1 1.774(2) . ? U1 O2 1.784(2) . ? U1 N1 2.291(3) . ? U1 N3 2.484(3) . ? U1 N2 2.495(3) . ? U1 C1 2.701(3) . ? U1 P1 3.1576(8) . ? U1 P2 3.2037(9) . ? N1 Si1 1.741(3) . ? N1 Si2 1.747(3) . ? N2 P2 1.597(3) . ? N2 Si3 1.727(3) . ? N3 P1 1.603(3) . ? N3 Si4 1.729(3) . ? C1 P2 1.728(3) . ? C1 P1 1.732(3) . ? C1 H1 0.94(4) . ? P1 C14 1.807(3) . ? P1 C20 1.811(3) . ? P2 C8 1.808(3) . ? P2 C2 1.817(3) . ? Si1 C37 1.867(4) . ? Si1 C36 1.868(4) . ? Si1 C35 1.876(4) . ? Si2 C33 1.863(4) . ? Si2 C34 1.873(4) . ? Si2 C32 1.876(4) . ? Si3 C26 1.856(4) . ? Si3 C28 1.863(3) . ? Si3 C27 1.863(4) . ? Si4 C31 1.858(4) . ? Si4 C30 1.866(4) . ? Si4 C29 1.869(4) . ? C2 C3 1.383(4) . ? C2 C7 1.395(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9300 . ? C4 C5 1.376(5) . ? C4 H4 0.9300 . ? C5 C6 1.386(5) . ? C5 H5 0.9300 . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.388(4) . ? C8 C13 1.399(4) . ? C9 C10 1.398(5) . ? C9 H9 0.9300 . ? C10 C11 1.378(5) . ? C10 H10 0.9300 . ? C11 C12 1.381(5) . ? C11 H11 0.9300 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.391(4) . ? C14 C19 1.392(4) . ? C15 C16 1.374(4) . ? C15 H15 0.9300 . ? C16 C17 1.387(5) . ? C16 H16 0.9300 . ? C17 C18 1.370(5) . ? C17 H17 0.9300 . ? C18 C19 1.389(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.376(4) . ? C20 C21 1.380(5) . ? C21 C22 1.385(5) . ? C21 H21 0.9300 . ? C22 C23 1.375(5) . ? C22 H22 0.9300 . ? C23 C24 1.366(5) . ? C23 H23 0.9300 . ? C24 C25 1.379(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C1S C4S 1.302(10) . ? C1S C4S 1.378(11) 2_567 ? C1S C5S 1.499(10) 2_567 ? C1S C3S 1.567(11) . ? C2S C3S 1.314(10) . ? C2S C5S 1.366(10) . ? C2S C4S 1.585(9) . ? C3S C4S 1.490(13) . ? C4S C4S 1.171(17) 2_567 ? C4S C1S 1.378(11) 2_567 ? C4S C5S 1.540(12) . ? C5S C1S 1.499(10) 2_567 ? 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 O1 U1 O2 178.16(10) . . ? O1 U1 N1 92.61(10) . . ? O2 U1 N1 88.56(10) . . ? O1 U1 N3 92.88(9) . . ? O2 U1 N3 87.96(9) . . ? N1 U1 N3 113.53(9) . . ? O1 U1 N2 93.61(9) . . ? O2 U1 N2 84.55(9) . . ? N1 U1 N2 125.11(9) . . ? N3 U1 N2 120.51(8) . . ? O1 U1 C1 85.46(10) . . ? O2 U1 C1 93.52(10) . . ? N1 U1 C1 173.92(9) . . ? N3 U1 C1 60.90(9) . . ? N2 U1 C1 60.83(9) . . ? O1 U1 P1 98.29(7) . . ? O2 U1 P1 81.63(7) . . ? N1 U1 P1 142.00(7) . . ? N3 U1 P1 30.09(6) . . ? N2 U1 P1 90.54(6) . . ? C1 U1 P1 33.23(7) . . ? O1 U1 P2 95.81(7) . . ? O2 U1 P2 82.53(7) . . ? N1 U1 P2 153.43(7) . . ? N3 U1 P2 91.20(6) . . ? N2 U1 P2 29.31(6) . . ? C1 U1 P2 32.65(6) . . ? P1 U1 P2 61.27(2) . . ? Si1 N1 Si2 116.61(15) . . ? Si1 N1 U1 124.61(14) . . ? Si2 N1 U1 118.51(13) . . ? P2 N2 Si3 135.51(17) . . ? P2 N2 U1 100.79(12) . . ? Si3 N2 U1 122.68(13) . . ? P1 N3 Si4 135.05(16) . . ? P1 N3 U1 98.89(12) . . ? Si4 N3 U1 126.04(13) . . ? P2 C1 P1 139.1(2) . . ? P2 C1 U1 89.88(12) . . ? P1 C1 U1 88.01(12) . . ? P2 C1 H1 110(2) . . ? P1 C1 H1 111(2) . . ? U1 C1 H1 93(2) . . ? N3 P1 C1 104.35(14) . . ? N3 P1 C14 112.07(14) . . ? C1 P1 C14 113.04(15) . . ? N3 P1 C20 113.18(14) . . ? C1 P1 C20 111.17(14) . . ? C14 P1 C20 103.31(15) . . ? N3 P1 U1 51.02(9) . . ? C1 P1 U1 58.75(10) . . ? C14 P1 U1 108.35(10) . . ? C20 P1 U1 148.17(11) . . ? N2 P2 C1 104.86(14) . . ? N2 P2 C8 114.18(14) . . ? C1 P2 C8 111.55(15) . . ? N2 P2 C2 112.19(14) . . ? C1 P2 C2 110.16(15) . . ? C8 P2 C2 104.03(14) . . ? N2 P2 U1 49.90(9) . . ? C1 P2 U1 57.47(10) . . ? C8 P2 U1 115.89(10) . . ? C2 P2 U1 140.03(10) . . ? N1 Si1 C37 115.88(16) . . ? N1 Si1 C36 112.96(18) . . ? C37 Si1 C36 104.4(2) . . ? N1 Si1 C35 110.28(15) . . ? C37 Si1 C35 103.17(19) . . ? C36 Si1 C35 109.57(19) . . ? N1 Si2 C33 111.42(15) . . ? N1 Si2 C34 114.53(16) . . ? C33 Si2 C34 106.62(19) . . ? N1 Si2 C32 114.39(14) . . ? C33 Si2 C32 108.51(17) . . ? C34 Si2 C32 100.58(17) . . ? N2 Si3 C26 105.85(15) . . ? N2 Si3 C28 113.21(14) . . ? C26 Si3 C28 107.04(18) . . ? N2 Si3 C27 112.14(15) . . ? C26 Si3 C27 109.4(2) . . ? C28 Si3 C27 108.95(17) . . ? N3 Si4 C31 105.84(14) . . ? N3 Si4 C30 112.26(15) . . ? C31 Si4 C30 111.21(17) . . ? N3 Si4 C29 115.21(16) . . ? C31 Si4 C29 106.67(18) . . ? C30 Si4 C29 105.60(17) . . ? C3 C2 C7 118.5(3) . . ? C3 C2 P2 122.4(2) . . ? C7 C2 P2 119.1(2) . . ? C2 C3 C4 120.5(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 119.8(3) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 121.0(3) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C9 C8 C13 119.3(3) . . ? C9 C8 P2 120.8(2) . . ? C13 C8 P2 119.9(2) . . ? C8 C9 C10 120.3(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 119.9(3) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C15 C14 C19 119.6(3) . . ? C15 C14 P1 120.3(2) . . ? C19 C14 P1 120.0(2) . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.1(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.4(3) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 119.6(3) . . ? C18 C19 H19 120.2 . . ? C14 C19 H19 120.2 . . ? C25 C20 C21 118.6(3) . . ? C25 C20 P1 122.1(2) . . ? C21 C20 P1 119.2(2) . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 118.7(3) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 121.3(3) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C20 C25 C24 120.4(3) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si3 C28 H28A 109.5 . . ? Si3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si4 C29 H29A 109.5 . . ? Si4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si4 C30 H30A 109.5 . . ? Si4 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si4 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si4 C31 H31A 109.5 . . ? Si4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C4S C1S C4S 51.7(7) . 2_567 ? C4S C1S C5S 116.3(7) . 2_567 ? C4S C1S C5S 64.5(5) 2_567 2_567 ? C4S C1S C3S 61.8(6) . . ? C4S C1S C3S 113.5(6) 2_567 . ? C5S C1S C3S 178.0(6) 2_567 . ? C3S C2S C5S 123.4(7) . . ? C3S C2S C4S 61.0(6) . . ? C5S C2S C4S 62.4(6) . . ? C2S C3S C4S 68.5(6) . . ? C2S C3S C1S 118.8(7) . . ? C4S C3S C1S 50.4(5) . . ? C4S C4S C1S 67.5(9) 2_567 . ? C4S C4S C1S 60.8(9) 2_567 2_567 ? C1S C4S C1S 128.3(7) . 2_567 ? C4S C4S C3S 135.3(14) 2_567 . ? C1S C4S C3S 67.9(7) . . ? C1S C4S C3S 163.9(8) 2_567 . ? C4S C4S C5S 122.3(14) 2_567 . ? C1S C4S C5S 170.2(9) . . ? C1S C4S C5S 61.5(6) 2_567 . ? C3S C4S C5S 102.3(7) . . ? C4S C4S C2S 174.1(15) 2_567 . ? C1S C4S C2S 118.4(8) . . ? C1S C4S C2S 113.4(7) 2_567 . ? C3S C4S C2S 50.5(5) . . ? C5S C4S C2S 51.8(5) . . ? C2S C5S C1S 119.7(7) . 2_567 ? C2S C5S C4S 65.8(6) . . ? C1S C5S C4S 53.9(5) 2_567 . ? 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 O1 U1 N1 Si1 -16.52(18) . . . . ? O2 U1 N1 Si1 162.06(17) . . . . ? N3 U1 N1 Si1 -110.80(16) . . . . ? N2 U1 N1 Si1 79.75(19) . . . . ? C1 U1 N1 Si1 -87.8(9) . . . . ? P1 U1 N1 Si1 -123.54(14) . . . . ? P2 U1 N1 Si1 92.0(2) . . . . ? O1 U1 N1 Si2 169.58(15) . . . . ? O2 U1 N1 Si2 -11.84(15) . . . . ? N3 U1 N1 Si2 75.30(16) . . . . ? N2 U1 N1 Si2 -94.15(16) . . . . ? C1 U1 N1 Si2 98.3(9) . . . . ? P1 U1 N1 Si2 62.56(19) . . . . ? P2 U1 N1 Si2 -81.9(2) . . . . ? O1 U1 N2 P2 -95.43(13) . . . . ? O2 U1 N2 P2 84.44(13) . . . . ? N1 U1 N2 P2 168.82(11) . . . . ? N3 U1 N2 P2 0.05(16) . . . . ? C1 U1 N2 P2 -12.68(11) . . . . ? P1 U1 N2 P2 2.91(11) . . . . ? O1 U1 N2 Si3 94.49(16) . . . . ? O2 U1 N2 Si3 -85.64(16) . . . . ? N1 U1 N2 Si3 -1.3(2) . . . . ? N3 U1 N2 Si3 -170.03(13) . . . . ? C1 U1 N2 Si3 177.24(19) . . . . ? P1 U1 N2 Si3 -167.17(14) . . . . ? P2 U1 N2 Si3 -170.1(2) . . . . ? O1 U1 N3 P1 101.60(13) . . . . ? O2 U1 N3 P1 -76.75(13) . . . . ? N1 U1 N3 P1 -164.29(11) . . . . ? N2 U1 N3 P1 5.70(16) . . . . ? C1 U1 N3 P1 18.42(11) . . . . ? P2 U1 N3 P1 5.73(11) . . . . ? O1 U1 N3 Si4 -76.82(17) . . . . ? O2 U1 N3 Si4 104.83(17) . . . . ? N1 U1 N3 Si4 17.29(19) . . . . ? N2 U1 N3 Si4 -172.72(13) . . . . ? C1 U1 N3 Si4 -160.0(2) . . . . ? P1 U1 N3 Si4 -178.4(3) . . . . ? P2 U1 N3 Si4 -172.69(15) . . . . ? O1 U1 C1 P2 108.19(13) . . . . ? O2 U1 C1 P2 -70.27(13) . . . . ? N1 U1 C1 P2 180(16) . . . . ? N3 U1 C1 P2 -155.96(15) . . . . ? N2 U1 C1 P2 11.49(10) . . . . ? P1 U1 C1 P2 -139.16(19) . . . . ? O1 U1 C1 P1 -112.65(13) . . . . ? O2 U1 C1 P1 68.89(13) . . . . ? N1 U1 C1 P1 -41.0(9) . . . . ? N3 U1 C1 P1 -16.81(10) . . . . ? N2 U1 C1 P1 150.65(15) . . . . ? P2 U1 C1 P1 139.16(19) . . . . ? Si4 N3 P1 C1 151.8(2) . . . . ? U1 N3 P1 C1 -26.40(15) . . . . ? Si4 N3 P1 C14 -85.6(2) . . . . ? U1 N3 P1 C14 96.26(14) . . . . ? Si4 N3 P1 C20 30.8(3) . . . . ? U1 N3 P1 C20 -147.39(12) . . . . ? Si4 N3 P1 U1 178.2(3) . . . . ? P2 C1 P1 N3 111.4(3) . . . . ? U1 C1 P1 N3 23.84(13) . . . . ? P2 C1 P1 C14 -10.7(3) . . . . ? U1 C1 P1 C14 -98.17(13) . . . . ? P2 C1 P1 C20 -126.3(3) . . . . ? U1 C1 P1 C20 146.17(12) . . . . ? P2 C1 P1 U1 87.5(3) . . . . ? O1 U1 P1 N3 -81.36(14) . . . . ? O2 U1 P1 N3 100.50(14) . . . . ? N1 U1 P1 N3 23.78(16) . . . . ? N2 U1 P1 N3 -175.09(13) . . . . ? C1 U1 P1 N3 -149.75(17) . . . . ? P2 U1 P1 N3 -173.47(12) . . . . ? O1 U1 P1 C1 68.39(14) . . . . ? O2 U1 P1 C1 -109.75(14) . . . . ? N1 U1 P1 C1 173.53(16) . . . . ? N3 U1 P1 C1 149.75(17) . . . . ? N2 U1 P1 C1 -25.34(14) . . . . ? P2 U1 P1 C1 -23.72(12) . . . . ? O1 U1 P1 C14 174.70(13) . . . . ? O2 U1 P1 C14 -3.44(13) . . . . ? N1 U1 P1 C14 -80.16(15) . . . . ? N3 U1 P1 C14 -103.94(16) . . . . ? N2 U1 P1 C14 80.97(12) . . . . ? C1 U1 P1 C14 106.32(16) . . . . ? P2 U1 P1 C14 82.59(11) . . . . ? O1 U1 P1 C20 -11.4(2) . . . . ? O2 U1 P1 C20 170.4(2) . . . . ? N1 U1 P1 C20 93.7(2) . . . . ? N3 U1 P1 C20 69.9(2) . . . . ? N2 U1 P1 C20 -105.2(2) . . . . ? C1 U1 P1 C20 -79.8(2) . . . . ? P2 U1 P1 C20 -103.6(2) . . . . ? Si3 N2 P2 C1 -173.9(2) . . . . ? U1 N2 P2 C1 18.05(15) . . . . ? Si3 N2 P2 C8 63.7(3) . . . . ? U1 N2 P2 C8 -104.34(14) . . . . ? Si3 N2 P2 C2 -54.3(3) . . . . ? U1 N2 P2 C2 137.61(12) . . . . ? Si3 N2 P2 U1 168.1(3) . . . . ? P1 C1 P2 N2 -103.2(3) . . . . ? U1 C1 P2 N2 -16.33(14) . . . . ? P1 C1 P2 C8 20.9(3) . . . . ? U1 C1 P2 C8 107.76(13) . . . . ? P1 C1 P2 C2 135.9(3) . . . . ? U1 C1 P2 C2 -137.24(12) . . . . ? P1 C1 P2 U1 -86.8(3) . . . . ? O1 U1 P2 N2 87.03(14) . . . . ? O2 U1 P2 N2 -92.17(14) . . . . ? N1 U1 P2 N2 -20.8(2) . . . . ? N3 U1 P2 N2 -179.95(14) . . . . ? C1 U1 P2 N2 159.19(18) . . . . ? P1 U1 P2 N2 -176.68(13) . . . . ? O1 U1 P2 C1 -72.16(14) . . . . ? O2 U1 P2 C1 108.64(14) . . . . ? N1 U1 P2 C1 -179.97(19) . . . . ? N3 U1 P2 C1 20.86(14) . . . . ? N2 U1 P2 C1 -159.19(18) . . . . ? P1 U1 P2 C1 24.13(12) . . . . ? O1 U1 P2 C8 -172.22(13) . . . . ? O2 U1 P2 C8 8.58(13) . . . . ? N1 U1 P2 C8 79.98(19) . . . . ? N3 U1 P2 C8 -79.20(13) . . . . ? N2 U1 P2 C8 100.75(17) . . . . ? C1 U1 P2 C8 -100.06(17) . . . . ? P1 U1 P2 C8 -75.93(11) . . . . ? O1 U1 P2 C2 10.68(18) . . . . ? O2 U1 P2 C2 -168.52(18) . . . . ? N1 U1 P2 C2 -97.1(2) . . . . ? N3 U1 P2 C2 103.70(17) . . . . ? N2 U1 P2 C2 -76.3(2) . . . . ? C1 U1 P2 C2 82.8(2) . . . . ? P1 U1 P2 C2 106.97(16) . . . . ? Si2 N1 Si1 C37 168.9(2) . . . . ? U1 N1 Si1 C37 -5.1(3) . . . . ? Si2 N1 Si1 C36 -70.8(2) . . . . ? U1 N1 Si1 C36 115.2(2) . . . . ? Si2 N1 Si1 C35 52.2(2) . . . . ? U1 N1 Si1 C35 -121.81(18) . . . . ? Si1 N1 Si2 C33 -95.0(2) . . . . ? U1 N1 Si2 C33 79.42(19) . . . . ? Si1 N1 Si2 C34 26.1(2) . . . . ? U1 N1 Si2 C34 -159.48(17) . . . . ? Si1 N1 Si2 C32 141.51(17) . . . . ? U1 N1 Si2 C32 -44.1(2) . . . . ? P2 N2 Si3 C26 -168.0(2) . . . . ? U1 N2 Si3 C26 -1.9(2) . . . . ? P2 N2 Si3 C28 75.1(3) . . . . ? U1 N2 Si3 C28 -118.90(18) . . . . ? P2 N2 Si3 C27 -48.7(3) . . . . ? U1 N2 Si3 C27 117.33(18) . . . . ? P1 N3 Si4 C31 -164.5(2) . . . . ? U1 N3 Si4 C31 13.3(2) . . . . ? P1 N3 Si4 C30 74.0(3) . . . . ? U1 N3 Si4 C30 -108.17(19) . . . . ? P1 N3 Si4 C29 -46.9(3) . . . . ? U1 N3 Si4 C29 130.91(18) . . . . ? N2 P2 C2 C3 -111.9(3) . . . . ? C1 P2 C2 C3 4.5(3) . . . . ? C8 P2 C2 C3 124.1(3) . . . . ? U1 P2 C2 C3 -58.5(3) . . . . ? N2 P2 C2 C7 67.7(3) . . . . ? C1 P2 C2 C7 -175.9(3) . . . . ? C8 P2 C2 C7 -56.2(3) . . . . ? U1 P2 C2 C7 121.1(2) . . . . ? C7 C2 C3 C4 -0.7(5) . . . . ? P2 C2 C3 C4 179.0(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? C4 C5 C6 C7 0.6(5) . . . . ? C5 C6 C7 C2 -0.6(5) . . . . ? C3 C2 C7 C6 0.6(5) . . . . ? P2 C2 C7 C6 -179.1(3) . . . . ? N2 P2 C8 C9 -147.6(3) . . . . ? C1 P2 C8 C9 93.7(3) . . . . ? C2 P2 C8 C9 -25.0(3) . . . . ? U1 P2 C8 C9 156.9(2) . . . . ? N2 P2 C8 C13 34.1(3) . . . . ? C1 P2 C8 C13 -84.6(3) . . . . ? C2 P2 C8 C13 156.7(2) . . . . ? U1 P2 C8 C13 -21.4(3) . . . . ? C13 C8 C9 C10 0.5(5) . . . . ? P2 C8 C9 C10 -177.8(2) . . . . ? C8 C9 C10 C11 0.6(5) . . . . ? C9 C10 C11 C12 -0.7(5) . . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? C11 C12 C13 C8 1.4(5) . . . . ? C9 C8 C13 C12 -1.5(5) . . . . ? P2 C8 C13 C12 176.8(2) . . . . ? N3 P1 C14 C15 171.1(2) . . . . ? C1 P1 C14 C15 -71.3(3) . . . . ? C20 P1 C14 C15 48.9(3) . . . . ? U1 P1 C14 C15 -134.4(2) . . . . ? N3 P1 C14 C19 -5.4(3) . . . . ? C1 P1 C14 C19 112.2(3) . . . . ? C20 P1 C14 C19 -127.6(3) . . . . ? U1 P1 C14 C19 49.1(3) . . . . ? C19 C14 C15 C16 -0.6(5) . . . . ? P1 C14 C15 C16 -177.2(3) . . . . ? C14 C15 C16 C17 1.1(5) . . . . ? C15 C16 C17 C18 -0.8(5) . . . . ? C16 C17 C18 C19 0.0(5) . . . . ? C17 C18 C19 C14 0.5(5) . . . . ? C15 C14 C19 C18 -0.2(5) . . . . ? P1 C14 C19 C18 176.4(2) . . . . ? N3 P1 C20 C25 108.3(3) . . . . ? C1 P1 C20 C25 -8.7(4) . . . . ? C14 P1 C20 C25 -130.3(3) . . . . ? U1 P1 C20 C25 55.7(4) . . . . ? N3 P1 C20 C21 -69.6(3) . . . . ? C1 P1 C20 C21 173.3(3) . . . . ? C14 P1 C20 C21 51.8(3) . . . . ? U1 P1 C20 C21 -122.2(3) . . . . ? C25 C20 C21 C22 0.0(6) . . . . ? P1 C20 C21 C22 178.0(3) . . . . ? C20 C21 C22 C23 0.5(7) . . . . ? C21 C22 C23 C24 -1.1(7) . . . . ? C22 C23 C24 C25 1.1(7) . . . . ? C21 C20 C25 C24 0.0(6) . . . . ? P1 C20 C25 C24 -177.9(3) . . . . ? C23 C24 C25 C20 -0.6(7) . . . . ? C5S C2S C3S C4S -0.8(8) . . . . ? C5S C2S C3S C1S -1.7(11) . . . . ? C4S C2S C3S C1S -0.8(6) . . . . ? C4S C1S C3S C2S 1.0(7) . . . . ? C4S C1S C3S C2S 0.8(9) 2_567 . . . ? C5S C1S C3S C2S 5(17) 2_567 . . . ? C4S C1S C3S C4S -0.3(8) 2_567 . . . ? C5S C1S C3S C4S 4(16) 2_567 . . . ? C5S C1S C4S C4S 0.4(9) 2_567 . . 2_567 ? C3S C1S C4S C4S -179.7(10) . . . 2_567 ? C4S C1S C4S C1S 0.000(2) 2_567 . . 2_567 ? C5S C1S C4S C1S 0.4(9) 2_567 . . 2_567 ? C3S C1S C4S C1S -179.7(10) . . . 2_567 ? C4S C1S C4S C3S 179.7(10) 2_567 . . . ? C5S C1S C4S C3S -179.9(6) 2_567 . . . ? C4S C1S C4S C5S 178(5) 2_567 . . . ? C5S C1S C4S C5S 178(4) 2_567 . . . ? C3S C1S C4S C5S -2(4) . . . . ? C4S C1S C4S C2S 178.9(12) 2_567 . . . ? C5S C1S C4S C2S 179.3(5) 2_567 . . . ? C3S C1S C4S C2S -0.8(6) . . . . ? C2S C3S C4S C4S -178.7(15) . . . 2_567 ? C1S C3S C4S C4S 0.4(13) . . . 2_567 ? C2S C3S C4S C1S -179.0(6) . . . . ? C2S C3S C4S C1S 0(3) . . . 2_567 ? C1S C3S C4S C1S 179(3) . . . 2_567 ? C2S C3S C4S C5S 0.6(6) . . . . ? C1S C3S C4S C5S 179.7(7) . . . . ? C1S C3S C4S C2S 179.0(6) . . . . ? C3S C2S C4S C4S 171(11) . . . 2_567 ? C5S C2S C4S C4S -10(10) . . . 2_567 ? C3S C2S C4S C1S 1.0(7) . . . . ? C5S C2S C4S C1S -179.8(8) . . . . ? C3S C2S C4S C1S -180.0(8) . . . 2_567 ? C5S C2S C4S C1S -0.7(6) . . . 2_567 ? C5S C2S C4S C3S 179.2(7) . . . . ? C3S C2S C4S C5S -179.2(7) . . . . ? C3S C2S C5S C1S 1.5(11) . . . 2_567 ? C4S C2S C5S C1S 0.7(6) . . . 2_567 ? C3S C2S C5S C4S 0.8(8) . . . . ? C4S C4S C5S C2S 178.8(12) 2_567 . . . ? C1S C4S C5S C2S 1(4) . . . . ? C1S C4S C5S C2S 179.2(6) 2_567 . . . ? C3S C4S C5S C2S -0.6(6) . . . . ? C4S C4S C5S C1S -0.5(10) 2_567 . . 2_567 ? C1S C4S C5S C1S -178(4) . . . 2_567 ? C3S C4S C5S C1S -179.8(7) . . . 2_567 ? C2S C4S C5S C1S -179.2(6) . . . 2_567 ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.194 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.120 #===END