Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Redshaw, Carl' 'Elsegood, Mark' 'Gibson, Vernon C.' _publ_contact_author_name 'Dr Carl Redshaw' _publ_contact_author_address ; Wolfson Materials and Catalysis Centre University of East Anglia School of Chemical Sciences Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email 'CARL.REDSHAW@UEA.AC.UK' _publ_section_title ; Novel Tungsten calix [8] arene complexes ; data_1.3MeCN _database_code_CSD 181731 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H113 Cl4 N3 O8 W2' _chemical_formula_weight 1922.37 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6346(8) _cell_length_b 17.6171(11) _cell_length_c 21.8873(14) _cell_angle_alpha 85.711(2) _cell_angle_beta 83.857(2) _cell_angle_gamma 87.482(2) _cell_volume 4827.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19838 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.31 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1956 _exptl_absorpt_coefficient_mu 2.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.487 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 45995 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16910 _reflns_number_gt 13580 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0759P)^2^+169.6872P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 16910 _refine_ls_number_parameters 1152 _refine_ls_number_restraints 523 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2675 _refine_ls_wR_factor_gt 0.2568 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.157 _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 W1 W 0.17330(5) 0.56259(3) 0.38192(3) 0.02917(19) Uani 1 1 d . . . W2 W 0.12613(5) 0.20303(3) 0.33709(3) 0.0350(2) Uani 1 1 d . . . Cl2 Cl 0.0582(3) 0.6076(2) 0.30555(18) 0.0390(9) Uani 1 1 d . . . Cl1 Cl 0.2720(3) 0.5350(2) 0.4612(2) 0.0444(10) Uani 1 1 d . . . Cl4 Cl 0.0099(4) 0.2012(2) 0.4271(2) 0.0507(11) Uani 1 1 d . . . Cl3 Cl -0.0291(4) 0.1867(3) 0.2867(2) 0.0530(11) Uani 1 1 d . . . O1 O 0.0451(7) 0.5211(5) 0.4200(5) 0.029(2) Uani 1 1 d . . . O2 O 0.1432(8) 0.6562(5) 0.4140(5) 0.033(2) Uani 1 1 d . . . O3 O 0.2775(7) 0.6136(5) 0.3261(4) 0.027(2) Uani 1 1 d . . . O4 O 0.2167(8) 0.4753(6) 0.3418(4) 0.032(2) Uani 1 1 d . . . O5 O 0.2378(9) 0.2170(5) 0.3818(5) 0.041(3) Uani 1 1 d . . . O6 O 0.1478(9) 0.0957(6) 0.3454(5) 0.039(3) Uani 1 1 d . . . O7 O 0.2019(9) 0.1922(6) 0.2603(5) 0.044(3) Uani 1 1 d . . . O8 O 0.1093(8) 0.3082(6) 0.3161(5) 0.034(2) Uani 1 1 d . . . C1 C -0.0607(11) 0.5305(8) 0.4136(6) 0.027(3) Uani 1 1 d . . . C2 C -0.1110(11) 0.4767(8) 0.3851(7) 0.029(3) Uani 1 1 d . . . C3 C -0.2163(11) 0.4888(8) 0.3756(7) 0.029(3) Uani 1 1 d . . . H3 H -0.2512 0.4509 0.3574 0.035 Uiso 1 1 calc R . . C4 C -0.2744(11) 0.5561(8) 0.3921(7) 0.030(3) Uani 1 1 d . A . C5 C -0.2216(11) 0.6070(8) 0.4225(7) 0.031(3) Uani 1 1 d . . . H5 H -0.2603 0.6511 0.4360 0.038 Uiso 1 1 calc R . . C6 C -0.1152(11) 0.5975(8) 0.4346(6) 0.027(3) Uani 1 1 d . . . C7 C -0.3897(13) 0.5686(11) 0.3781(8) 0.052(4) Uani 1 1 d DU . . C8 C -0.4475(18) 0.6335(14) 0.4087(14) 0.075(6) Uani 0.85(2) 1 d PDU A 1 H8A H -0.4429 0.6268 0.4532 0.112 Uiso 0.85(2) 1 calc PR A 1 H8B H -0.5224 0.6351 0.4006 0.112 Uiso 0.85(2) 1 calc PR A 1 H8C H -0.4150 0.6814 0.3923 0.112 Uiso 0.85(2) 1 calc PR A 1 C9 C -0.4518(17) 0.4944(14) 0.4004(13) 0.069(6) Uani 0.85(2) 1 d PDU A 1 H9A H -0.4146 0.4505 0.3818 0.104 Uiso 0.85(2) 1 calc PR A 1 H9B H -0.5242 0.4998 0.3879 0.104 Uiso 0.85(2) 1 calc PR A 1 H9C H -0.4554 0.4868 0.4454 0.104 Uiso 0.85(2) 1 calc PR A 1 C10 C -0.3932(18) 0.5792(17) 0.3100(10) 0.072(6) Uani 0.85(2) 1 d PDU A 1 H10A H -0.3567 0.5357 0.2905 0.107 Uiso 0.85(2) 1 calc PR A 1 H10B H -0.3577 0.6261 0.2941 0.107 Uiso 0.85(2) 1 calc PR A 1 H10C H -0.4676 0.5828 0.3008 0.107 Uiso 0.85(2) 1 calc PR A 1 C8X C -0.467(7) 0.573(7) 0.434(3) 0.067(12) Uani 0.15(2) 1 d PDU A 2 H8X1 H -0.4551 0.5285 0.4629 0.101 Uiso 0.15(2) 1 calc PR A 2 H8X2 H -0.5396 0.5736 0.4228 0.101 Uiso 0.15(2) 1 calc PR A 2 H8X3 H -0.4561 0.6195 0.4544 0.101 Uiso 0.15(2) 1 calc PR A 2 C9X C -0.429(8) 0.508(5) 0.337(4) 0.063(11) Uani 0.15(2) 1 d PDU A 2 H9X1 H -0.4474 0.4617 0.3634 0.094 Uiso 0.15(2) 1 calc PR A 2 H9X2 H -0.3719 0.4957 0.3053 0.094 Uiso 0.15(2) 1 calc PR A 2 H9X3 H -0.4916 0.5286 0.3183 0.094 Uiso 0.15(2) 1 calc PR A 2 C10X C -0.388(8) 0.643(3) 0.341(5) 0.063(11) Uani 0.15(2) 1 d PDU A 2 H10D H -0.3526 0.6364 0.2996 0.094 Uiso 0.15(2) 1 calc PR A 2 H10E H -0.3490 0.6796 0.3611 0.094 Uiso 0.15(2) 1 calc PR A 2 H10F H -0.4611 0.6630 0.3380 0.094 Uiso 0.15(2) 1 calc PR A 2 C11 C -0.0663(13) 0.6550(9) 0.4698(7) 0.036(4) Uani 1 1 d . . . H11A H -0.0078 0.6293 0.4911 0.044 Uiso 1 1 calc R . . H11B H -0.1209 0.6733 0.5018 0.044 Uiso 1 1 calc R . . C12 C 0.0825(12) 0.7221(8) 0.4030(7) 0.030(3) Uani 1 1 d . . . C13 C -0.0226(12) 0.7232(8) 0.4302(7) 0.032(3) Uani 1 1 d . . . C14 C -0.0807(11) 0.7919(9) 0.4208(7) 0.035(4) Uani 1 1 d . . . H14 H -0.1522 0.7952 0.4392 0.042 Uiso 1 1 calc R . . C15 C -0.0406(12) 0.8544(8) 0.3868(7) 0.033(3) Uani 1 1 d . . . C16 C 0.0665(11) 0.8482(8) 0.3601(7) 0.030(3) Uani 1 1 d . . . H16 H 0.0966 0.8912 0.3369 0.037 Uiso 1 1 calc R . . C17 C 0.1280(11) 0.7834(8) 0.3665(7) 0.030(3) Uani 1 1 d . . . C18 C -0.1031(12) 0.9305(8) 0.3831(7) 0.043(4) Uani 1 1 d D . . C19 C -0.0917(17) 0.9661(12) 0.3156(9) 0.076(7) Uani 1 1 d D . . H19A H -0.0187 0.9827 0.3046 0.114 Uiso 1 1 calc R . . H19B H -0.1416 1.0100 0.3120 0.114 Uiso 1 1 calc R . . H19C H -0.1076 0.9281 0.2878 0.114 Uiso 1 1 calc R . . C20 C -0.0618(15) 0.9836(11) 0.4255(11) 0.073(7) Uani 1 1 d D . . H20A H -0.0822 0.9656 0.4684 0.110 Uiso 1 1 calc R . . H20B H -0.0924 1.0350 0.4177 0.110 Uiso 1 1 calc R . . H20C H 0.0160 0.9846 0.4179 0.110 Uiso 1 1 calc R . . C21 C -0.2256(12) 0.9223(9) 0.4009(8) 0.044(4) Uani 1 1 d D . . H21A H -0.2515 0.8831 0.3774 0.066 Uiso 1 1 calc R . . H21B H -0.2628 0.9710 0.3915 0.066 Uiso 1 1 calc R . . H21C H -0.2390 0.9077 0.4451 0.066 Uiso 1 1 calc R . . C22 C 0.2451(12) 0.7744(9) 0.3378(7) 0.036(4) Uani 1 1 d . . . H22A H 0.2761 0.8254 0.3320 0.044 Uiso 1 1 calc R . . H22B H 0.2858 0.7433 0.3675 0.044 Uiso 1 1 calc R . . C23 C 0.2774(11) 0.6564(10) 0.2734(6) 0.035(4) Uani 1 1 d . . . C24 C 0.2602(10) 0.7378(8) 0.2761(7) 0.029(3) Uani 1 1 d . . . C25 C 0.2555(11) 0.7816(9) 0.2207(7) 0.034(3) Uani 1 1 d . . . H25 H 0.2450 0.8353 0.2213 0.040 Uiso 1 1 calc R . . C26 C 0.2657(13) 0.7491(9) 0.1649(8) 0.040(4) Uani 1 1 d . B . C27 C 0.2769(13) 0.6718(9) 0.1644(7) 0.039(4) Uani 1 1 d . . . H27 H 0.2819 0.6495 0.1260 0.047 Uiso 1 1 calc R . . C28 C 0.2815(11) 0.6235(8) 0.2186(6) 0.029(3) Uani 1 1 d . . . C29 C 0.2595(15) 0.7964(11) 0.1036(8) 0.060(4) Uani 1 1 d DU . . C30 C 0.173(2) 0.7705(15) 0.0684(12) 0.076(6) Uani 0.81(2) 1 d PDU B 1 H30A H 0.1818 0.7154 0.0644 0.113 Uiso 0.81(2) 1 calc PR B 1 H30B H 0.1779 0.7971 0.0273 0.113 Uiso 0.81(2) 1 calc PR B 1 H30C H 0.1033 0.7820 0.0905 0.113 Uiso 0.81(2) 1 calc PR B 1 C31 C 0.249(2) 0.8805(13) 0.1091(11) 0.064(6) Uani 0.81(2) 1 d PDU B 1 H31A H 0.2458 0.9065 0.0681 0.096 Uiso 0.81(2) 1 calc PR B 1 H31B H 0.3104 0.8975 0.1274 0.096 Uiso 0.81(2) 1 calc PR B 1 H31C H 0.1834 0.8926 0.1353 0.096 Uiso 0.81(2) 1 calc PR B 1 C32 C 0.356(2) 0.7825(15) 0.0582(11) 0.075(6) Uani 0.81(2) 1 d PDU B 1 H32A H 0.3703 0.7275 0.0563 0.112 Uiso 0.81(2) 1 calc PR B 1 H32B H 0.4178 0.8059 0.0716 0.112 Uiso 0.81(2) 1 calc PR B 1 H32C H 0.3424 0.8050 0.0174 0.112 Uiso 0.81(2) 1 calc PR B 1 C30X C 0.148(4) 0.830(5) 0.112(4) 0.066(11) Uani 0.19(2) 1 d PDU B 2 H30D H 0.0969 0.7922 0.1049 0.099 Uiso 0.19(2) 1 calc PR B 2 H30E H 0.1408 0.8747 0.0830 0.099 Uiso 0.19(2) 1 calc PR B 2 H30F H 0.1321 0.8459 0.1544 0.099 Uiso 0.19(2) 1 calc PR B 2 C31X C 0.335(6) 0.860(4) 0.091(4) 0.065(11) Uani 0.19(2) 1 d PDU B 2 H31D H 0.3984 0.8475 0.1125 0.097 Uiso 0.19(2) 1 calc PR B 2 H31E H 0.3001 0.9069 0.1059 0.097 Uiso 0.19(2) 1 calc PR B 2 H31F H 0.3558 0.8673 0.0467 0.097 Uiso 0.19(2) 1 calc PR B 2 C32X C 0.256(8) 0.756(5) 0.045(3) 0.074(11) Uani 0.19(2) 1 d PDU B 2 H32D H 0.2335 0.7041 0.0559 0.111 Uiso 0.19(2) 1 calc PR B 2 H32E H 0.3272 0.7555 0.0225 0.111 Uiso 0.19(2) 1 calc PR B 2 H32F H 0.2055 0.7837 0.0199 0.111 Uiso 0.19(2) 1 calc PR B 2 C33 C 0.2719(12) 0.5385(9) 0.2147(7) 0.032(3) Uani 1 1 d . . . H33A H 0.1964 0.5273 0.2275 0.039 Uiso 1 1 calc R . . H33B H 0.2852 0.5290 0.1704 0.039 Uiso 1 1 calc R . . C34 C 0.3062(11) 0.4465(8) 0.3075(7) 0.030(3) Uani 1 1 d . . . C35 C 0.3369(12) 0.4793(8) 0.2482(7) 0.032(3) Uani 1 1 d . . . C36 C 0.4290(11) 0.4465(9) 0.2168(7) 0.033(3) Uani 1 1 d . . . H36 H 0.4539 0.4683 0.1771 0.040 Uiso 1 1 calc R . . C37 C 0.4841(13) 0.3845(9) 0.2409(8) 0.043(4) Uani 1 1 d . C . C38 C 0.4501(12) 0.3541(8) 0.2997(8) 0.036(3) Uani 1 1 d . . . H38 H 0.4874 0.3109 0.3166 0.043 Uiso 1 1 calc R . . C39 C 0.3623(10) 0.3856(8) 0.3346(7) 0.028(3) Uani 1 1 d . . . C40 C 0.5786(14) 0.3460(9) 0.2013(8) 0.062(4) Uani 1 1 d DU . . C41 C 0.621(2) 0.2713(13) 0.2349(14) 0.078(8) Uani 0.68(2) 1 d PDU C 1 H41A H 0.5628 0.2362 0.2451 0.118 Uiso 0.68(2) 1 calc PR C 1 H41B H 0.6495 0.2835 0.2728 0.118 Uiso 0.68(2) 1 calc PR C 1 H41C H 0.6777 0.2474 0.2078 0.118 Uiso 0.68(2) 1 calc PR C 1 C42 C 0.6637(18) 0.4013(14) 0.1845(12) 0.060(6) Uani 0.68(2) 1 d PDU C 1 H42A H 0.7230 0.3772 0.1595 0.090 Uiso 0.68(2) 1 calc PR C 1 H42B H 0.6890 0.4177 0.2220 0.090 Uiso 0.68(2) 1 calc PR C 1 H42C H 0.6354 0.4457 0.1609 0.090 Uiso 0.68(2) 1 calc PR C 1 C43 C 0.5288(18) 0.3230(13) 0.1431(11) 0.056(5) Uani 0.68(2) 1 d PDU C 1 H43A H 0.4729 0.2866 0.1558 0.084 Uiso 0.68(2) 1 calc PR C 1 H43B H 0.5843 0.2996 0.1150 0.084 Uiso 0.68(2) 1 calc PR C 1 H43C H 0.4981 0.3685 0.1221 0.084 Uiso 0.68(2) 1 calc PR C 1 C41X C 0.678(3) 0.349(3) 0.238(2) 0.069(9) Uani 0.32(2) 1 d PDU C 2 H41D H 0.6612 0.3242 0.2799 0.103 Uiso 0.32(2) 1 calc PR C 2 H41E H 0.6953 0.4017 0.2415 0.103 Uiso 0.32(2) 1 calc PR C 2 H41F H 0.7386 0.3215 0.2172 0.103 Uiso 0.32(2) 1 calc PR C 2 C42X C 0.603(4) 0.383(3) 0.1383(15) 0.064(9) Uani 0.32(2) 1 d PDU C 2 H42D H 0.6634 0.3558 0.1166 0.096 Uiso 0.32(2) 1 calc PR C 2 H42E H 0.6223 0.4362 0.1415 0.096 Uiso 0.32(2) 1 calc PR C 2 H42F H 0.5410 0.3827 0.1154 0.096 Uiso 0.32(2) 1 calc PR C 2 C43X C 0.558(4) 0.2596(12) 0.197(3) 0.067(9) Uani 0.32(2) 1 d PDU C 2 H43D H 0.5425 0.2353 0.2387 0.100 Uiso 0.32(2) 1 calc PR C 2 H43E H 0.6207 0.2346 0.1762 0.100 Uiso 0.32(2) 1 calc PR C 2 H43F H 0.4964 0.2548 0.1738 0.100 Uiso 0.32(2) 1 calc PR C 2 C44 C 0.3269(12) 0.3545(8) 0.3997(7) 0.034(3) Uani 1 1 d . . . H44A H 0.3438 0.3917 0.4287 0.041 Uiso 1 1 calc R . . H44B H 0.2486 0.3501 0.4040 0.041 Uiso 1 1 calc R . . C45 C 0.3292(13) 0.2116(9) 0.4102(8) 0.039(4) Uani 1 1 d . . . C46 C 0.3763(12) 0.2791(9) 0.4181(7) 0.034(3) Uani 1 1 d . . . C47 C 0.4769(12) 0.2728(8) 0.4397(7) 0.034(3) Uani 1 1 d . . . H47 H 0.5123 0.3182 0.4443 0.041 Uiso 1 1 calc R . . C48 C 0.5275(14) 0.2032(9) 0.4547(7) 0.037(4) Uani 1 1 d . D . C49 C 0.4694(14) 0.1381(9) 0.4501(7) 0.041(4) Uani 1 1 d . . . H49 H 0.5007 0.0899 0.4618 0.049 Uiso 1 1 calc R . . C50 C 0.3687(13) 0.1398(8) 0.4296(7) 0.037(4) Uani 1 1 d . . . C51 C 0.6426(14) 0.1976(10) 0.4708(7) 0.055(4) Uani 1 1 d DU . . C52 C 0.633(4) 0.159(2) 0.5368(14) 0.060(8) Uani 0.56(7) 1 d PDU D 1 H52A H 0.7040 0.1531 0.5513 0.089 Uiso 0.56(7) 1 calc PR D 1 H52B H 0.6025 0.1090 0.5368 0.089 Uiso 0.56(7) 1 calc PR D 1 H52C H 0.5871 0.1909 0.5642 0.089 Uiso 0.56(7) 1 calc PR D 1 C53 C 0.700(4) 0.2717(19) 0.471(2) 0.055(9) Uani 0.56(7) 1 d PDU D 1 H53A H 0.7721 0.2607 0.4819 0.083 Uiso 0.56(7) 1 calc PR D 1 H53B H 0.6608 0.3041 0.5007 0.083 Uiso 0.56(7) 1 calc PR D 1 H53C H 0.7029 0.2980 0.4296 0.083 Uiso 0.56(7) 1 calc PR D 1 C54 C 0.709(3) 0.141(3) 0.432(2) 0.071(9) Uani 0.56(7) 1 d PDU D 1 H54A H 0.7822 0.1378 0.4428 0.106 Uiso 0.56(7) 1 calc PR D 1 H54B H 0.7091 0.1577 0.3880 0.106 Uiso 0.56(7) 1 calc PR D 1 H54C H 0.6781 0.0904 0.4391 0.106 Uiso 0.56(7) 1 calc PR D 1 C52X C 0.672(6) 0.138(3) 0.522(3) 0.073(11) Uani 0.44(7) 1 d PDU D 2 H52D H 0.7482 0.1407 0.5268 0.110 Uiso 0.44(7) 1 calc PR D 2 H52E H 0.6581 0.0869 0.5103 0.110 Uiso 0.44(7) 1 calc PR D 2 H52F H 0.6298 0.1482 0.5606 0.110 Uiso 0.44(7) 1 calc PR D 2 C53X C 0.679(5) 0.275(2) 0.485(3) 0.052(10) Uani 0.44(7) 1 d PDU D 2 H53D H 0.7524 0.2703 0.4956 0.078 Uiso 0.44(7) 1 calc PR D 2 H53E H 0.6324 0.2938 0.5201 0.078 Uiso 0.44(7) 1 calc PR D 2 H53F H 0.6747 0.3111 0.4491 0.078 Uiso 0.44(7) 1 calc PR D 2 C54X C 0.710(4) 0.173(4) 0.4122(19) 0.061(9) Uani 0.44(7) 1 d PDU D 2 H54D H 0.7854 0.1677 0.4197 0.092 Uiso 0.44(7) 1 calc PR D 2 H54E H 0.7017 0.2110 0.3781 0.092 Uiso 0.44(7) 1 calc PR D 2 H54F H 0.6866 0.1235 0.4016 0.092 Uiso 0.44(7) 1 calc PR D 2 C55 C 0.3101(14) 0.0674(9) 0.4255(8) 0.043(4) Uani 1 1 d . . . H55A H 0.3386 0.0272 0.4539 0.051 Uiso 1 1 calc R . . H55B H 0.2340 0.0767 0.4400 0.051 Uiso 1 1 calc R . . C56 C 0.2375(11) 0.0531(8) 0.3241(7) 0.032(3) Uani 1 1 d . . . C57 C 0.3173(13) 0.0386(8) 0.3630(8) 0.039(4) Uani 1 1 d . . . C58 C 0.4084(12) -0.0029(8) 0.3404(8) 0.038(4) Uani 1 1 d . . . H58 H 0.4626 -0.0147 0.3669 0.045 Uiso 1 1 calc R . . C59 C 0.4231(13) -0.0273(9) 0.2822(9) 0.044(4) Uani 1 1 d . . . C60 C 0.3383(13) -0.0112(9) 0.2439(8) 0.042(4) Uani 1 1 d . . . H60 H 0.3454 -0.0283 0.2034 0.051 Uiso 1 1 calc R . . C61 C 0.2459(12) 0.0289(9) 0.2652(8) 0.036(3) Uani 1 1 d . . . C62 C 0.5255(14) -0.0700(11) 0.2591(10) 0.056(5) Uani 1 1 d . . . C63 C 0.6185(17) -0.0177(14) 0.2586(12) 0.076(7) Uani 1 1 d . . . H63A H 0.6244 -0.0039 0.3007 0.114 Uiso 1 1 calc R . . H63B H 0.6062 0.0285 0.2322 0.114 Uiso 1 1 calc R . . H63C H 0.6845 -0.0441 0.2428 0.114 Uiso 1 1 calc R . . C64 C 0.5245(16) -0.0938(15) 0.1935(12) 0.079(7) Uani 1 1 d . . . H64A H 0.5887 -0.1251 0.1824 0.118 Uiso 1 1 calc R . . H64B H 0.5229 -0.0483 0.1650 0.118 Uiso 1 1 calc R . . H64C H 0.4613 -0.1233 0.1911 0.118 Uiso 1 1 calc R . . C65 C 0.5394(16) -0.1408(12) 0.3003(11) 0.069(6) Uani 1 1 d . . . H65A H 0.5338 -0.1276 0.3433 0.104 Uiso 1 1 calc R . . H65B H 0.6097 -0.1648 0.2893 0.104 Uiso 1 1 calc R . . H65C H 0.4840 -0.1763 0.2953 0.104 Uiso 1 1 calc R . . C66 C 0.1614(13) 0.0495(9) 0.2211(8) 0.040(4) Uani 1 1 d . . . H66A H 0.1526 0.0048 0.1975 0.048 Uiso 1 1 calc R . . H66B H 0.0927 0.0599 0.2458 0.048 Uiso 1 1 calc R . . C67 C 0.1988(13) 0.1872(10) 0.1994(7) 0.040(4) Uani 1 1 d . . . C68 C 0.1849(11) 0.1162(9) 0.1767(8) 0.037(4) Uani 1 1 d . . . C69 C 0.1881(16) 0.1164(12) 0.1126(10) 0.059(5) Uani 1 1 d . . . H69 H 0.1790 0.0699 0.0948 0.071 Uiso 1 1 calc R . . C70 C 0.2047(15) 0.1842(13) 0.0728(9) 0.058(5) Uani 1 1 d . E . C71 C 0.2200(15) 0.2502(12) 0.0988(9) 0.054(5) Uani 1 1 d . . . H71 H 0.2367 0.2947 0.0729 0.065 Uiso 1 1 calc R . . C72 C 0.2119(13) 0.2539(9) 0.1613(7) 0.039(4) Uani 1 1 d . . . C73 C 0.2038(19) 0.1788(15) 0.0026(11) 0.088(6) Uani 1 1 d DU . . C74 C 0.219(5) 0.097(2) -0.016(2) 0.114(11) Uani 0.56(2) 1 d PDU E 1 H74A H 0.2791 0.0722 0.0035 0.171 Uiso 0.56(2) 1 calc PR E 1 H74B H 0.2339 0.0973 -0.0608 0.171 Uiso 0.56(2) 1 calc PR E 1 H74C H 0.1542 0.0694 -0.0025 0.171 Uiso 0.56(2) 1 calc PR E 1 C75 C 0.321(3) 0.221(3) -0.0272(17) 0.091(10) Uani 0.56(2) 1 d PDU E 1 H75A H 0.3820 0.1907 -0.0131 0.137 Uiso 0.56(2) 1 calc PR E 1 H75B H 0.3219 0.2726 -0.0130 0.137 Uiso 0.56(2) 1 calc PR E 1 H75C H 0.3264 0.2242 -0.0723 0.137 Uiso 0.56(2) 1 calc PR E 1 C76 C 0.115(3) 0.230(3) -0.0205(19) 0.094(10) Uani 0.56(2) 1 d PDU E 1 H76A H 0.1163 0.2800 -0.0038 0.141 Uiso 0.56(2) 1 calc PR E 1 H76B H 0.0463 0.2072 -0.0071 0.141 Uiso 0.56(2) 1 calc PR E 1 H76C H 0.1251 0.2361 -0.0656 0.141 Uiso 0.56(2) 1 calc PR E 1 C74X C 0.302(4) 0.136(3) -0.025(2) 0.102(12) Uani 0.44(2) 1 d PDU E 2 H74D H 0.3658 0.1595 -0.0146 0.153 Uiso 0.44(2) 1 calc PR E 2 H74E H 0.3017 0.1369 -0.0694 0.153 Uiso 0.44(2) 1 calc PR E 2 H74F H 0.3011 0.0827 -0.0073 0.153 Uiso 0.44(2) 1 calc PR E 2 C75X C 0.209(4) 0.270(3) -0.032(2) 0.092(11) Uani 0.44(2) 1 d PDU E 2 H75D H 0.1460 0.3004 -0.0167 0.138 Uiso 0.44(2) 1 calc PR E 2 H75E H 0.2099 0.2681 -0.0770 0.138 Uiso 0.44(2) 1 calc PR E 2 H75F H 0.2734 0.2940 -0.0231 0.138 Uiso 0.44(2) 1 calc PR E 2 C76X C 0.095(3) 0.152(3) -0.008(2) 0.095(11) Uani 0.44(2) 1 d PDU E 2 H76D H 0.0388 0.1843 0.0121 0.142 Uiso 0.44(2) 1 calc PR E 2 H76E H 0.0869 0.0990 0.0085 0.142 Uiso 0.44(2) 1 calc PR E 2 H76F H 0.0881 0.1548 -0.0527 0.142 Uiso 0.44(2) 1 calc PR E 2 C77 C 0.2284(12) 0.3277(8) 0.1912(7) 0.034(3) Uani 1 1 d . . . H77A H 0.2702 0.3623 0.1611 0.041 Uiso 1 1 calc R . . H77B H 0.2703 0.3157 0.2267 0.041 Uiso 1 1 calc R . . C78 C 0.0741(11) 0.3612(8) 0.2734(7) 0.029(3) Uani 1 1 d . . . C79 C 0.1223(12) 0.3692(8) 0.2138(7) 0.034(3) Uani 1 1 d . . . C80 C 0.0773(12) 0.4214(8) 0.1724(7) 0.033(3) Uani 1 1 d . . . H80 H 0.1081 0.4259 0.1308 0.040 Uiso 1 1 calc R . . C81 C -0.0117(11) 0.4672(9) 0.1902(7) 0.036(4) Uani 1 1 d . . . C82 C -0.0525(12) 0.4617(9) 0.2510(7) 0.033(3) Uani 1 1 d . . . H82 H -0.1112 0.4943 0.2638 0.039 Uiso 1 1 calc R . . C83 C -0.0116(11) 0.4104(8) 0.2947(7) 0.029(3) Uani 1 1 d . . . C84 C -0.0551(14) 0.5271(11) 0.1438(8) 0.048(4) Uani 1 1 d . . . C85 C -0.0883(18) 0.4892(15) 0.0883(10) 0.076(7) Uani 1 1 d . . . H85A H -0.0290 0.4570 0.0710 0.114 Uiso 1 1 calc R . . H85B H -0.1073 0.5285 0.0568 0.114 Uiso 1 1 calc R . . H85C H -0.1500 0.4578 0.1015 0.114 Uiso 1 1 calc R . . C86 C 0.0329(17) 0.5844(12) 0.1220(12) 0.075(7) Uani 1 1 d . . . H86A H 0.0654 0.5996 0.1577 0.113 Uiso 1 1 calc R . . H86B H 0.0015 0.6295 0.1008 0.113 Uiso 1 1 calc R . . H86C H 0.0876 0.5605 0.0937 0.113 Uiso 1 1 calc R . . C87 C -0.1541(17) 0.5720(15) 0.1705(10) 0.074(7) Uani 1 1 d . . . H87A H -0.2105 0.5366 0.1853 0.111 Uiso 1 1 calc R . . H87B H -0.1790 0.6081 0.1384 0.111 Uiso 1 1 calc R . . H87C H -0.1358 0.5998 0.2048 0.111 Uiso 1 1 calc R . . C88 C -0.0522(12) 0.4054(8) 0.3628(7) 0.034(3) Uani 1 1 d . . . H88A H -0.1004 0.3622 0.3712 0.041 Uiso 1 1 calc R . . H88B H 0.0092 0.3940 0.3870 0.041 Uiso 1 1 calc R . . N1 N 0.286(3) 0.445(2) 0.0524(17) 0.163(14) Uani 1 1 d U . . C89 C 0.318(2) 0.493(2) 0.0257(12) 0.092(8) Uani 1 1 d U . . C90 C 0.359(4) 0.556(2) -0.0064(16) 0.138(13) Uani 1 1 d U . . H90A H 0.3103 0.5996 0.0010 0.207 Uiso 1 1 calc R . . H90B H 0.3668 0.5472 -0.0505 0.207 Uiso 1 1 calc R . . H90C H 0.4284 0.5650 0.0067 0.207 Uiso 1 1 calc R . . N2 N 0.557(2) 0.6959(16) 0.1733(13) 0.121(9) Uani 1 1 d U . . C91 C 0.553(2) 0.6354(15) 0.1321(13) 0.082(7) Uani 1 1 d U . . C92 C 0.545(3) 0.5841(14) 0.1000(15) 0.112(11) Uani 1 1 d U . . H92A H 0.6065 0.5487 0.1025 0.168 Uiso 1 1 calc R . . H92B H 0.5423 0.6045 0.0573 0.168 Uiso 1 1 calc R . . H92C H 0.4795 0.5572 0.1140 0.168 Uiso 1 1 calc R . . N3 N -0.217(3) 0.802(3) 0.1921(17) 0.22(2) Uani 1 1 d U . . C93 C -0.143(3) 0.785(3) 0.2152(19) 0.181(17) Uani 1 1 d U . . C94 C -0.042(3) 0.767(3) 0.238(2) 0.20(2) Uani 1 1 d U . . H94A H 0.0072 0.7469 0.2049 0.301 Uiso 1 1 calc R . . H94B H -0.0510 0.7295 0.2728 0.301 Uiso 1 1 calc R . . H94C H -0.0144 0.8139 0.2508 0.301 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 W1 0.0240(3) 0.0295(3) 0.0331(3) 0.0003(2) 0.0022(2) -0.0091(2) W2 0.0400(4) 0.0266(3) 0.0371(4) -0.0010(3) -0.0002(3) 0.0003(3) Cl2 0.0309(19) 0.039(2) 0.046(2) 0.0055(17) -0.0053(16) -0.0050(16) Cl1 0.037(2) 0.040(2) 0.055(2) 0.0123(18) -0.0093(18) -0.0006(17) Cl4 0.051(3) 0.040(2) 0.056(3) 0.0010(19) 0.010(2) -0.0005(19) Cl3 0.046(2) 0.050(3) 0.064(3) -0.004(2) -0.008(2) -0.009(2) O1 0.015(4) 0.028(5) 0.042(6) 0.007(4) 0.003(4) -0.001(4) O2 0.039(6) 0.025(5) 0.033(5) 0.000(4) 0.006(4) -0.016(4) O3 0.022(5) 0.021(5) 0.036(5) 0.006(4) -0.003(4) -0.005(4) O4 0.028(5) 0.035(6) 0.029(5) 0.008(4) 0.002(4) 0.002(4) O5 0.045(6) 0.016(5) 0.063(7) 0.016(5) -0.021(6) -0.001(4) O6 0.039(6) 0.024(5) 0.052(7) 0.001(5) -0.005(5) 0.006(4) O7 0.044(7) 0.033(6) 0.055(7) 0.000(5) -0.011(5) -0.006(5) O8 0.034(6) 0.030(5) 0.038(6) 0.003(4) -0.005(5) 0.007(4) C1 0.021(7) 0.033(8) 0.027(7) 0.007(6) 0.002(5) -0.006(6) C2 0.030(8) 0.024(7) 0.031(8) 0.005(6) -0.002(6) 0.000(6) C3 0.024(7) 0.028(7) 0.035(8) -0.003(6) -0.004(6) -0.004(6) C4 0.024(7) 0.031(8) 0.036(8) 0.000(6) -0.002(6) -0.004(6) C5 0.031(8) 0.022(7) 0.038(8) 0.006(6) 0.004(6) -0.005(6) C6 0.023(7) 0.027(7) 0.030(7) 0.004(6) 0.003(6) -0.007(6) C7 0.026(7) 0.062(9) 0.073(9) -0.016(8) -0.013(7) -0.005(6) C8 0.041(11) 0.074(11) 0.113(15) -0.030(12) -0.022(11) 0.014(10) C9 0.030(10) 0.074(11) 0.106(15) -0.012(11) -0.007(11) -0.016(9) C10 0.034(11) 0.105(16) 0.077(9) -0.003(9) -0.023(10) 0.012(11) C8X 0.04(2) 0.08(2) 0.088(19) -0.022(16) -0.002(15) 0.00(2) C9X 0.03(2) 0.083(19) 0.08(2) -0.025(17) -0.03(2) -0.01(2) C10X 0.03(2) 0.072(15) 0.09(2) -0.003(15) -0.03(2) 0.01(2) C11 0.042(9) 0.043(9) 0.023(7) -0.003(6) 0.009(6) -0.017(7) C12 0.038(8) 0.017(7) 0.035(8) 0.001(6) -0.006(6) -0.006(6) C13 0.037(8) 0.031(8) 0.027(7) -0.005(6) 0.005(6) -0.013(6) C14 0.018(7) 0.047(9) 0.041(9) -0.010(7) 0.005(6) -0.015(6) C15 0.036(8) 0.026(7) 0.037(8) -0.011(6) 0.003(7) -0.008(6) C16 0.030(8) 0.020(7) 0.041(8) 0.006(6) -0.006(6) -0.006(6) C17 0.030(8) 0.028(7) 0.034(8) -0.001(6) -0.005(6) -0.009(6) C18 0.039(9) 0.027(8) 0.062(11) 0.001(7) 0.004(8) -0.002(7) C19 0.067(14) 0.062(13) 0.082(15) 0.039(12) 0.030(12) 0.023(11) C20 0.043(11) 0.047(12) 0.14(2) -0.039(13) -0.031(12) 0.006(9) C21 0.039(9) 0.028(8) 0.063(11) 0.002(8) -0.007(8) 0.005(7) C22 0.027(8) 0.037(9) 0.046(9) -0.009(7) 0.004(7) -0.014(6) C23 0.022(7) 0.060(10) 0.025(7) 0.008(7) -0.006(6) -0.028(7) C24 0.018(7) 0.033(8) 0.037(8) 0.004(6) -0.009(6) -0.010(6) C25 0.028(8) 0.029(8) 0.044(9) 0.001(7) -0.005(6) -0.006(6) C26 0.041(9) 0.034(9) 0.043(9) 0.016(7) -0.006(7) -0.006(7) C27 0.045(9) 0.036(9) 0.036(9) -0.005(7) -0.005(7) 0.002(7) C28 0.025(7) 0.029(7) 0.030(8) 0.007(6) 0.003(6) -0.002(6) C29 0.098(12) 0.044(7) 0.037(8) 0.011(7) -0.017(7) -0.002(8) C30 0.117(14) 0.063(13) 0.051(13) 0.009(11) -0.040(12) 0.003(13) C31 0.099(16) 0.042(8) 0.052(12) 0.019(8) -0.023(11) 0.008(9) C32 0.115(14) 0.056(13) 0.048(12) 0.014(10) -0.002(10) 0.007(12) C30X 0.095(14) 0.05(2) 0.05(2) 0.008(19) -0.02(2) -0.004(14) C31X 0.097(19) 0.050(19) 0.05(2) 0.017(17) -0.016(19) -0.005(15) C32X 0.12(3) 0.06(2) 0.041(18) 0.003(15) -0.02(2) 0.00(2) C33 0.029(8) 0.038(8) 0.028(8) 0.007(6) 0.001(6) -0.004(6) C34 0.020(7) 0.028(7) 0.040(8) -0.001(6) -0.003(6) -0.001(6) C35 0.035(8) 0.024(7) 0.035(8) 0.002(6) 0.001(6) -0.007(6) C36 0.028(8) 0.036(8) 0.034(8) 0.002(6) 0.004(6) -0.007(6) C37 0.030(8) 0.037(9) 0.060(11) -0.004(8) 0.006(8) 0.005(7) C38 0.028(8) 0.022(7) 0.056(10) -0.004(7) -0.003(7) 0.004(6) C39 0.012(6) 0.024(7) 0.049(9) 0.003(6) -0.006(6) -0.003(5) C40 0.058(9) 0.039(8) 0.083(11) -0.002(8) 0.012(8) 0.017(7) C41 0.068(16) 0.067(13) 0.088(16) 0.008(12) 0.021(12) 0.043(12) C42 0.036(12) 0.066(13) 0.076(16) -0.013(11) 0.008(11) 0.013(8) C43 0.037(12) 0.028(11) 0.097(14) -0.005(10) 0.012(10) 0.014(9) C41X 0.056(18) 0.06(2) 0.09(2) -0.005(18) 0.012(14) 0.016(17) C42X 0.05(2) 0.053(18) 0.084(15) -0.002(16) 0.018(15) 0.015(18) C43X 0.06(2) 0.035(11) 0.10(2) -0.004(14) 0.002(18) 0.029(15) C44 0.035(8) 0.026(8) 0.041(9) 0.003(6) -0.005(7) 0.000(6) C45 0.045(9) 0.025(8) 0.046(9) 0.010(7) -0.010(7) -0.008(7) C46 0.036(8) 0.032(8) 0.032(8) 0.001(6) 0.000(6) -0.004(6) C47 0.033(8) 0.024(7) 0.044(9) -0.004(6) -0.003(7) 0.003(6) C48 0.054(10) 0.027(8) 0.032(8) -0.004(6) -0.013(7) 0.008(7) C49 0.054(10) 0.025(8) 0.043(9) 0.005(7) -0.013(8) 0.014(7) C50 0.051(10) 0.024(8) 0.037(9) 0.004(6) -0.008(7) 0.000(7) C51 0.054(10) 0.036(7) 0.080(10) -0.009(7) -0.036(8) 0.019(6) C52 0.06(2) 0.034(17) 0.092(12) 0.003(12) -0.052(14) 0.013(14) C53 0.04(2) 0.049(12) 0.08(2) -0.007(12) -0.019(17) 0.009(11) C54 0.050(17) 0.048(17) 0.117(19) -0.015(16) -0.029(16) 0.031(15) C52X 0.08(3) 0.051(17) 0.096(17) 0.013(17) -0.043(19) 0.00(2) C53X 0.03(2) 0.042(11) 0.08(2) -0.006(12) -0.014(19) 0.007(13) C54X 0.051(15) 0.050(18) 0.087(14) -0.012(13) -0.034(12) 0.028(15) C55 0.052(10) 0.024(8) 0.051(10) 0.010(7) -0.007(8) -0.001(7) C56 0.027(7) 0.015(7) 0.052(9) 0.003(6) -0.002(7) -0.003(6) C57 0.040(9) 0.019(7) 0.055(10) 0.005(7) 0.000(8) -0.001(6) C58 0.033(8) 0.020(7) 0.061(11) 0.005(7) -0.015(7) -0.003(6) C59 0.029(8) 0.037(9) 0.064(12) -0.006(8) 0.001(8) -0.005(7) C60 0.041(9) 0.037(9) 0.051(10) -0.010(8) -0.003(8) -0.008(7) C61 0.028(8) 0.030(8) 0.049(10) -0.002(7) -0.003(7) -0.003(6) C62 0.027(9) 0.056(12) 0.082(14) -0.006(10) 0.002(9) 0.009(8) C63 0.049(12) 0.090(17) 0.089(17) -0.008(14) 0.001(11) -0.020(12) C64 0.041(11) 0.092(17) 0.105(19) -0.044(15) -0.003(11) 0.029(11) C65 0.046(11) 0.059(13) 0.100(17) -0.015(12) -0.001(11) 0.020(10) C66 0.034(8) 0.036(9) 0.049(10) -0.010(7) 0.000(7) -0.006(7) C67 0.035(9) 0.045(10) 0.038(9) -0.007(7) 0.002(7) -0.002(7) C68 0.022(7) 0.041(9) 0.049(10) -0.010(7) -0.002(7) 0.003(6) C69 0.052(11) 0.056(12) 0.073(14) -0.031(11) -0.008(10) 0.003(9) C70 0.043(11) 0.082(15) 0.049(11) 0.001(10) -0.003(8) -0.007(10) C71 0.044(10) 0.071(13) 0.046(11) -0.011(9) 0.003(8) -0.001(9) C72 0.044(9) 0.034(8) 0.037(9) 0.002(7) -0.010(7) 0.012(7) C73 0.101(14) 0.112(16) 0.052(12) -0.013(10) -0.014(10) 0.024(12) C74 0.15(3) 0.132(18) 0.06(2) -0.041(19) 0.00(2) 0.032(17) C75 0.088(15) 0.13(2) 0.044(18) 0.015(19) 0.000(16) 0.048(16) C76 0.089(16) 0.13(2) 0.060(18) 0.000(19) -0.023(17) 0.014(17) C74X 0.111(19) 0.13(2) 0.06(2) 0.00(2) 0.00(2) 0.037(19) C75X 0.08(2) 0.14(2) 0.05(2) 0.020(19) -0.01(2) 0.035(17) C76X 0.107(17) 0.13(3) 0.05(2) -0.01(2) -0.035(19) 0.027(18) C77 0.029(8) 0.025(7) 0.044(9) 0.011(6) 0.005(7) 0.000(6) C78 0.030(7) 0.024(7) 0.035(8) -0.003(6) -0.005(6) -0.006(6) C79 0.029(8) 0.030(8) 0.044(9) -0.001(7) 0.000(7) -0.007(6) C80 0.033(8) 0.029(8) 0.037(8) 0.007(6) -0.003(6) -0.010(6) C81 0.023(7) 0.042(9) 0.045(9) -0.005(7) -0.004(6) -0.008(6) C82 0.031(8) 0.035(8) 0.032(8) 0.008(6) -0.013(6) 0.000(6) C83 0.023(7) 0.026(7) 0.038(8) -0.002(6) -0.005(6) -0.007(6) C84 0.047(10) 0.051(11) 0.044(10) 0.012(8) -0.009(8) 0.010(8) C85 0.062(14) 0.107(19) 0.058(13) 0.019(13) -0.019(11) 0.010(13) C86 0.054(12) 0.061(13) 0.101(18) 0.046(13) 0.002(12) 0.001(10) C87 0.055(13) 0.107(19) 0.053(12) 0.026(12) -0.005(10) 0.020(12) C88 0.036(8) 0.026(8) 0.040(9) 0.003(6) -0.008(7) -0.002(6) N1 0.15(3) 0.15(3) 0.16(3) 0.06(2) 0.05(2) 0.02(2) C89 0.10(2) 0.11(2) 0.057(15) 0.011(13) 0.008(13) 0.023(15) C90 0.20(4) 0.11(2) 0.10(2) -0.016(17) 0.01(2) -0.05(2) N2 0.13(2) 0.111(19) 0.13(2) -0.028(14) -0.015(17) 0.015(17) C91 0.077(15) 0.070(15) 0.091(18) 0.011(10) 0.013(13) -0.010(13) C92 0.15(3) 0.044(13) 0.12(2) 0.001(11) 0.05(2) 0.004(15) N3 0.14(3) 0.37(5) 0.17(3) -0.12(3) -0.07(2) 0.19(3) C93 0.13(3) 0.27(4) 0.16(3) -0.14(3) -0.08(2) 0.13(3) C94 0.15(3) 0.25(4) 0.24(4) -0.16(4) -0.13(3) 0.12(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 W1 O2 1.849(10) . ? W1 O4 1.861(10) . ? W1 O1 1.892(9) . ? W1 O3 1.905(9) . ? W1 Cl1 2.255(4) . ? W1 Cl2 2.400(4) . ? W2 O5 1.836(11) . ? W2 O7 1.861(12) . ? W2 O8 1.884(10) . ? W2 O6 1.896(10) . ? W2 Cl4 2.327(4) . ? W2 Cl3 2.389(5) . ? O1 C1 1.359(16) . ? O2 C12 1.384(17) . ? O3 C23 1.331(17) . ? O4 C34 1.387(17) . ? O5 C45 1.367(19) . ? O6 C56 1.389(18) . ? O7 C67 1.349(19) . ? O8 C78 1.366(17) . ? C1 C2 1.39(2) . ? C1 C6 1.42(2) . ? C2 C3 1.37(2) . ? C2 C88 1.52(2) . ? C3 C4 1.42(2) . ? C4 C5 1.39(2) . ? C4 C7 1.53(2) . ? C5 C6 1.40(2) . ? C6 C11 1.51(2) . ? C7 C8X 1.49(3) . ? C7 C8 1.49(2) . ? C7 C10 1.49(2) . ? C7 C10X 1.49(3) . ? C7 C9X 1.57(3) . ? C7 C9 1.57(3) . ? C11 C13 1.517(19) . ? C12 C13 1.40(2) . ? C12 C17 1.400(19) . ? C13 C14 1.40(2) . ? C14 C15 1.37(2) . ? C15 C16 1.42(2) . ? C15 C18 1.53(2) . ? C16 C17 1.36(2) . ? C17 C22 1.55(2) . ? C18 C20 1.51(2) . ? C18 C19 1.555(18) . ? C18 C21 1.565(17) . ? C22 C24 1.53(2) . ? C23 C28 1.37(2) . ? C23 C24 1.45(2) . ? C24 C25 1.39(2) . ? C25 C26 1.38(2) . ? C26 C27 1.36(2) . ? C26 C29 1.53(2) . ? C27 C28 1.41(2) . ? C28 C33 1.52(2) . ? C29 C31X 1.49(3) . ? C29 C31 1.49(3) . ? C29 C32X 1.51(3) . ? C29 C30 1.51(2) . ? C29 C30X 1.51(3) . ? C29 C32 1.51(2) . ? C33 C35 1.50(2) . ? C34 C39 1.39(2) . ? C34 C35 1.40(2) . ? C35 C36 1.41(2) . ? C36 C37 1.37(2) . ? C37 C38 1.39(2) . ? C37 C40 1.56(2) . ? C38 C39 1.40(2) . ? C39 C44 1.52(2) . ? C40 C42 1.48(2) . ? C40 C42X 1.49(2) . ? C40 C41 1.561(15) . ? C40 C43 1.564(15) . ? C40 C43X 1.567(16) . ? C40 C41X 1.570(16) . ? C44 C46 1.49(2) . ? C45 C46 1.38(2) . ? C45 C50 1.39(2) . ? C46 C47 1.40(2) . ? C47 C48 1.39(2) . ? C48 C49 1.40(2) . ? C48 C51 1.53(2) . ? C49 C50 1.39(2) . ? C50 C55 1.52(2) . ? C51 C53 1.52(3) . ? C51 C53X 1.52(3) . ? C51 C54 1.53(2) . ? C51 C52X 1.54(2) . ? C51 C54X 1.54(2) . ? C51 C52 1.54(2) . ? C55 C57 1.49(2) . ? C56 C61 1.38(2) . ? C56 C57 1.39(2) . ? C57 C58 1.40(2) . ? C58 C59 1.37(2) . ? C59 C60 1.44(2) . ? C59 C62 1.53(2) . ? C60 C61 1.39(2) . ? C61 C66 1.53(2) . ? C62 C65 1.50(3) . ? C62 C63 1.52(3) . ? C62 C64 1.53(3) . ? C66 C68 1.49(2) . ? C67 C72 1.40(2) . ? C67 C68 1.40(2) . ? C68 C69 1.40(3) . ? C69 C70 1.43(3) . ? C70 C71 1.36(3) . ? C70 C73 1.55(3) . ? C71 C72 1.37(2) . ? C72 C77 1.53(2) . ? C73 C74X 1.51(3) . ? C73 C76 1.51(3) . ? C73 C74 1.52(3) . ? C73 C76X 1.53(3) . ? C73 C75X 1.73(4) . ? C73 C75 1.73(4) . ? C77 C79 1.55(2) . ? C78 C79 1.38(2) . ? C78 C83 1.42(2) . ? C79 C80 1.39(2) . ? C80 C81 1.39(2) . ? C81 C82 1.37(2) . ? C81 C84 1.53(2) . ? C82 C83 1.39(2) . ? C83 C88 1.52(2) . ? C84 C85 1.53(3) . ? C84 C87 1.54(3) . ? C84 C86 1.55(3) . ? N1 C89 1.06(4) . ? C89 C90 1.35(4) . ? N2 C91 1.45(4) . ? C91 C92 1.20(4) . ? N3 C93 1.13(4) . ? C93 C94 1.42(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W1 O4 172.2(4) . . ? O2 W1 O1 93.3(4) . . ? O4 W1 O1 94.1(4) . . ? O2 W1 O3 86.0(4) . . ? O4 W1 O3 86.2(4) . . ? O1 W1 O3 163.9(4) . . ? O2 W1 Cl1 86.5(3) . . ? O4 W1 Cl1 95.1(3) . . ? O1 W1 Cl1 97.3(3) . . ? O3 W1 Cl1 98.7(3) . . ? O2 W1 Cl2 85.3(3) . . ? O4 W1 Cl2 93.3(3) . . ? O1 W1 Cl2 81.4(3) . . ? O3 W1 Cl2 82.5(3) . . ? Cl1 W1 Cl2 171.67(15) . . ? O5 W2 O7 99.1(5) . . ? O5 W2 O8 92.4(4) . . ? O7 W2 O8 89.1(5) . . ? O5 W2 O6 91.6(4) . . ? O7 W2 O6 82.8(5) . . ? O8 W2 O6 171.4(5) . . ? O5 W2 Cl4 89.9(4) . . ? O7 W2 Cl4 169.4(4) . . ? O8 W2 Cl4 96.2(3) . . ? O6 W2 Cl4 91.5(4) . . ? O5 W2 Cl3 175.1(4) . . ? O7 W2 Cl3 85.8(4) . . ? O8 W2 Cl3 87.3(3) . . ? O6 W2 Cl3 89.4(4) . . ? Cl4 W2 Cl3 85.28(17) . . ? C1 O1 W1 137.0(8) . . ? C12 O2 W1 139.5(9) . . ? C23 O3 W1 135.9(8) . . ? C34 O4 W1 138.7(9) . . ? C45 O5 W2 166.8(11) . . ? C56 O6 W2 127.5(9) . . ? C67 O7 W2 147.6(10) . . ? C78 O8 W2 144.3(9) . . ? O1 C1 C2 119.7(13) . . ? O1 C1 C6 118.3(12) . . ? C2 C1 C6 122.0(13) . . ? C3 C2 C1 119.3(13) . . ? C3 C2 C88 119.0(13) . . ? C1 C2 C88 121.7(13) . . ? C2 C3 C4 122.0(13) . . ? C5 C4 C3 116.4(13) . . ? C5 C4 C7 123.4(14) . . ? C3 C4 C7 120.1(13) . . ? C4 C5 C6 124.4(14) . . ? C5 C6 C1 115.7(13) . . ? C5 C6 C11 120.1(13) . . ? C1 C6 C11 124.1(13) . . ? C8X C7 C8 47(4) . . ? C8X C7 C10 137(5) . . ? C8 C7 C10 110(2) . . ? C8X C7 C10X 110(4) . . ? C8 C7 C10X 64(5) . . ? C10 C7 C10X 55(4) . . ? C8X C7 C4 113(5) . . ? C8 C7 C4 114.2(15) . . ? C10 C7 C4 109.4(14) . . ? C10X C7 C4 103(4) . . ? C8X C7 C9X 108(3) . . ? C8 C7 C9X 131(4) . . ? C10 C7 C9X 55(4) . . ? C10X C7 C9X 108(3) . . ? C4 C7 C9X 114(4) . . ? C8X C7 C9 63(4) . . ? C8 C7 C9 107.6(16) . . ? C10 C7 C9 106.5(16) . . ? C10X C7 C9 148(4) . . ? C4 C7 C9 108.7(16) . . ? C9X C7 C9 52(4) . . ? C6 C11 C13 114.3(12) . . ? O2 C12 C13 116.7(12) . . ? O2 C12 C17 119.7(13) . . ? C13 C12 C17 123.7(14) . . ? C12 C13 C14 115.5(13) . . ? C12 C13 C11 120.8(14) . . ? C14 C13 C11 123.7(13) . . ? C15 C14 C13 123.9(14) . . ? C14 C15 C16 117.0(14) . . ? C14 C15 C18 122.0(13) . . ? C16 C15 C18 120.6(12) . . ? C17 C16 C15 122.7(13) . . ? C16 C17 C12 117.1(14) . . ? C16 C17 C22 124.2(13) . . ? C12 C17 C22 118.7(13) . . ? C20 C18 C15 109.4(14) . . ? C20 C18 C19 110.3(15) . . ? C15 C18 C19 109.9(13) . . ? C20 C18 C21 108.7(13) . . ? C15 C18 C21 112.9(12) . . ? C19 C18 C21 105.5(14) . . ? C24 C22 C17 115.1(12) . . ? O3 C23 C28 120.5(15) . . ? O3 C23 C24 118.4(13) . . ? C28 C23 C24 120.8(13) . . ? C25 C24 C23 117.7(13) . . ? C25 C24 C22 121.1(14) . . ? C23 C24 C22 121.1(13) . . ? C26 C25 C24 121.7(14) . . ? C27 C26 C25 118.8(14) . . ? C27 C26 C29 118.7(16) . . ? C25 C26 C29 122.4(15) . . ? C26 C27 C28 122.8(15) . . ? C23 C28 C27 117.9(14) . . ? C23 C28 C33 122.7(13) . . ? C27 C28 C33 118.5(13) . . ? C31X C29 C31 46(3) . . ? C31X C29 C32X 109(3) . . ? C31 C29 C32X 126(4) . . ? C31X C29 C30 132(4) . . ? C31 C29 C30 110.4(16) . . ? C32X C29 C30 44(4) . . ? C31X C29 C30X 108(3) . . ? C31 C29 C30X 63(3) . . ? C32X C29 C30X 101(3) . . ? C30 C29 C30X 59(3) . . ? C31X C29 C32 64(3) . . ? C31 C29 C32 106.7(16) . . ? C32X C29 C32 56(3) . . ? C30 C29 C32 100(2) . . ? C30X C29 C32 146(4) . . ? C31X C29 C26 116(4) . . ? C31 C29 C26 114.5(17) . . ? C32X C29 C26 119(4) . . ? C30 C29 C26 112.0(16) . . ? C30X C29 C26 101(4) . . ? C32 C29 C26 112.2(16) . . ? C35 C33 C28 123.6(13) . . ? O4 C34 C39 117.2(13) . . ? O4 C34 C35 119.9(13) . . ? C39 C34 C35 122.9(13) . . ? C34 C35 C36 115.9(13) . . ? C34 C35 C33 124.4(13) . . ? C36 C35 C33 119.3(13) . . ? C37 C36 C35 123.0(14) . . ? C36 C37 C38 118.7(14) . . ? C36 C37 C40 120.4(15) . . ? C38 C37 C40 120.8(14) . . ? C37 C38 C39 121.6(14) . . ? C34 C39 C38 117.8(14) . . ? C34 C39 C44 120.2(13) . . ? C38 C39 C44 121.9(13) . . ? C42 C40 C42X 56(2) . . ? C42 C40 C37 109.4(16) . . ? C42X C40 C37 115(2) . . ? C42 C40 C41 111.8(13) . . ? C42X C40 C41 133(3) . . ? C37 C40 C41 111.8(16) . . ? C42 C40 C43 111.6(13) . . ? C42X C40 C43 56(2) . . ? C37 C40 C43 104.5(15) . . ? C41 C40 C43 107.5(16) . . ? C42 C40 C43X 140(3) . . ? C42X C40 C43X 110.1(15) . . ? C37 C40 C43X 110(2) . . ? C41 C40 C43X 47(2) . . ? C43 C40 C43X 62.5(19) . . ? C42 C40 C41X 57(2) . . ? C42X C40 C41X 109.6(16) . . ? C37 C40 C41X 106(2) . . ? C41 C40 C41X 60.5(18) . . ? C43 C40 C41X 150(3) . . ? C43X C40 C41X 106.3(19) . . ? C46 C44 C39 115.0(13) . . ? O5 C45 C46 116.9(13) . . ? O5 C45 C50 118.9(14) . . ? C46 C45 C50 124.2(15) . . ? C45 C46 C47 116.5(14) . . ? C45 C46 C44 121.8(14) . . ? C47 C46 C44 121.5(14) . . ? C48 C47 C46 123.0(15) . . ? C47 C48 C49 116.2(15) . . ? C47 C48 C51 121.9(15) . . ? C49 C48 C51 121.8(14) . . ? C50 C49 C48 124.0(14) . . ? C49 C50 C45 115.4(14) . . ? C49 C50 C55 121.6(14) . . ? C45 C50 C55 123.0(15) . . ? C53 C51 C53X 15(3) . . ? C53 C51 C54 111(2) . . ? C53X C51 C54 125(3) . . ? C53 C51 C48 117(3) . . ? C53X C51 C48 111(3) . . ? C54 C51 C48 111(2) . . ? C53 C51 C52X 113(4) . . ? C53X C51 C52X 109(2) . . ? C54 C51 C52X 80(3) . . ? C48 C51 C52X 119(3) . . ? C53 C51 C54X 94(3) . . ? C53X C51 C54X 108(2) . . ? C54 C51 C54X 25.5(18) . . ? C48 C51 C54X 106(2) . . ? C52X C51 C54X 104(3) . . ? C53 C51 C52 108.6(19) . . ? C53X C51 C52 98(3) . . ? C54 C51 C52 105(2) . . ? C48 C51 C52 104(2) . . ? C52X C51 C52 25(2) . . ? C54X C51 C52 129(3) . . ? C57 C55 C50 115.0(13) . . ? C61 C56 O6 119.5(13) . . ? C61 C56 C57 122.6(14) . . ? O6 C56 C57 117.9(14) . . ? C56 C57 C58 117.4(16) . . ? C56 C57 C55 122.5(14) . . ? C58 C57 C55 120.1(15) . . ? C59 C58 C57 123.2(15) . . ? C58 C59 C60 117.4(15) . . ? C58 C59 C62 121.2(16) . . ? C60 C59 C62 121.4(17) . . ? C61 C60 C59 120.9(16) . . ? C56 C61 C60 118.5(15) . . ? C56 C61 C66 122.3(14) . . ? C60 C61 C66 119.0(15) . . ? C65 C62 C63 111.4(18) . . ? C65 C62 C64 107.8(19) . . ? C63 C62 C64 107.2(18) . . ? C65 C62 C59 109.0(16) . . ? C63 C62 C59 108.7(17) . . ? C64 C62 C59 112.8(16) . . ? C68 C66 C61 115.1(13) . . ? O7 C67 C72 117.5(14) . . ? O7 C67 C68 119.6(15) . . ? C72 C67 C68 122.9(15) . . ? C69 C68 C67 115.3(16) . . ? C69 C68 C66 125.4(16) . . ? C67 C68 C66 119.1(15) . . ? C68 C69 C70 122.3(17) . . ? C71 C70 C69 118.3(18) . . ? C71 C70 C73 123(2) . . ? C69 C70 C73 118(2) . . ? C70 C71 C72 121.5(19) . . ? C71 C72 C67 119.4(16) . . ? C71 C72 C77 122.2(16) . . ? C67 C72 C77 118.1(14) . . ? C74X C73 C76 138(3) . . ? C74X C73 C74 49(2) . . ? C76 C73 C74 120(3) . . ? C74X C73 C76X 118(4) . . ? C76 C73 C76X 55(2) . . ? C74 C73 C76X 73(4) . . ? C74X C73 C70 111(3) . . ? C76 C73 C70 110(2) . . ? C74 C73 C70 112(2) . . ? C76X C73 C70 108(3) . . ? C74X C73 C75X 106(2) . . ? C76 C73 C75X 50(2) . . ? C74 C73 C75X 138(3) . . ? C76X C73 C75X 104(2) . . ? C70 C73 C75X 108(2) . . ? C74X C73 C75 56(3) . . ? C76 C73 C75 106(2) . . ? C74 C73 C75 104(2) . . ? C76X C73 C75 148(3) . . ? C70 C73 C75 103(2) . . ? C75X C73 C75 56.5(18) . . ? C72 C77 C79 113.0(13) . . ? O8 C78 C79 122.2(13) . . ? O8 C78 C83 116.0(13) . . ? C79 C78 C83 121.7(14) . . ? C78 C79 C80 118.3(14) . . ? C78 C79 C77 123.9(14) . . ? C80 C79 C77 117.6(13) . . ? C79 C80 C81 121.9(15) . . ? C82 C81 C80 118.0(15) . . ? C82 C81 C84 121.6(14) . . ? C80 C81 C84 120.1(14) . . ? C81 C82 C83 122.9(15) . . ? C82 C83 C78 116.7(14) . . ? C82 C83 C88 124.0(13) . . ? C78 C83 C88 119.3(13) . . ? C81 C84 C85 110.6(16) . . ? C81 C84 C87 113.4(15) . . ? C85 C84 C87 106.2(17) . . ? C81 C84 C86 108.6(14) . . ? C85 C84 C86 109.8(18) . . ? C87 C84 C86 108.1(18) . . ? C2 C88 C83 114.7(12) . . ? N1 C89 C90 178(4) . . ? C92 C91 N2 177(3) . . ? N3 C93 C94 172(7) . . ? 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 O2 W1 O1 C1 70.0(14) . . . . ? O4 W1 O1 C1 -107.5(14) . . . . ? O3 W1 O1 C1 -17(2) . . . . ? Cl1 W1 O1 C1 156.9(13) . . . . ? Cl2 W1 O1 C1 -14.8(13) . . . . ? O4 W1 O2 C12 81(4) . . . . ? O1 W1 O2 C12 -79.6(13) . . . . ? O3 W1 O2 C12 84.4(13) . . . . ? Cl1 W1 O2 C12 -176.6(13) . . . . ? Cl2 W1 O2 C12 1.6(13) . . . . ? O2 W1 O3 C23 -81.8(14) . . . . ? O4 W1 O3 C23 97.8(14) . . . . ? O1 W1 O3 C23 6(2) . . . . ? Cl1 W1 O3 C23 -167.7(14) . . . . ? Cl2 W1 O3 C23 4.0(14) . . . . ? O2 W1 O4 C34 28(4) . . . . ? O1 W1 O4 C34 -171.3(13) . . . . ? O3 W1 O4 C34 24.8(13) . . . . ? Cl1 W1 O4 C34 -73.6(13) . . . . ? Cl2 W1 O4 C34 107.1(13) . . . . ? O7 W2 O5 C45 -57(5) . . . . ? O8 W2 O5 C45 -146(5) . . . . ? O6 W2 O5 C45 26(5) . . . . ? Cl4 W2 O5 C45 117(5) . . . . ? Cl3 W2 O5 C45 128(5) . . . . ? O5 W2 O6 C56 -61.9(13) . . . . ? O7 W2 O6 C56 37.1(12) . . . . ? O8 W2 O6 C56 56(4) . . . . ? Cl4 W2 O6 C56 -151.9(12) . . . . ? Cl3 W2 O6 C56 122.9(12) . . . . ? O5 W2 O7 C67 -170.7(19) . . . . ? O8 W2 O7 C67 -78(2) . . . . ? O6 W2 O7 C67 99(2) . . . . ? Cl4 W2 O7 C67 41(3) . . . . ? Cl3 W2 O7 C67 8.9(19) . . . . ? O5 W2 O8 C78 153.8(16) . . . . ? O7 W2 O8 C78 54.7(16) . . . . ? O6 W2 O8 C78 36(4) . . . . ? Cl4 W2 O8 C78 -116.0(16) . . . . ? Cl3 W2 O8 C78 -31.1(16) . . . . ? W1 O1 C1 C2 103.8(15) . . . . ? W1 O1 C1 C6 -73.8(17) . . . . ? O1 C1 C2 C3 -176.2(12) . . . . ? C6 C1 C2 C3 1(2) . . . . ? O1 C1 C2 C88 2(2) . . . . ? C6 C1 C2 C88 179.9(13) . . . . ? C1 C2 C3 C4 2(2) . . . . ? C88 C2 C3 C4 -176.4(13) . . . . ? C2 C3 C4 C5 -4(2) . . . . ? C2 C3 C4 C7 177.3(14) . . . . ? C3 C4 C5 C6 3(2) . . . . ? C7 C4 C5 C6 -178.4(14) . . . . ? C4 C5 C6 C1 0(2) . . . . ? C4 C5 C6 C11 -178.0(13) . . . . ? O1 C1 C6 C5 175.2(12) . . . . ? C2 C1 C6 C5 -2.3(19) . . . . ? O1 C1 C6 C11 -7(2) . . . . ? C2 C1 C6 C11 175.5(13) . . . . ? C5 C4 C7 C8X -61(5) . . . . ? C3 C4 C7 C8X 117(5) . . . . ? C5 C4 C7 C8 -10(3) . . . . ? C3 C4 C7 C8 168.5(19) . . . . ? C5 C4 C7 C10 114.3(19) . . . . ? C3 C4 C7 C10 -68(2) . . . . ? C5 C4 C7 C10X 58(5) . . . . ? C3 C4 C7 C10X -124(5) . . . . ? C5 C4 C7 C9X 174(5) . . . . ? C3 C4 C7 C9X -8(5) . . . . ? C5 C4 C7 C9 -129.9(16) . . . . ? C3 C4 C7 C9 48.3(19) . . . . ? C5 C6 C11 C13 -85.5(17) . . . . ? C1 C6 C11 C13 96.8(17) . . . . ? W1 O2 C12 C13 87.3(17) . . . . ? W1 O2 C12 C17 -93.2(16) . . . . ? O2 C12 C13 C14 177.0(12) . . . . ? C17 C12 C13 C14 -2(2) . . . . ? O2 C12 C13 C11 0(2) . . . . ? C17 C12 C13 C11 -179.4(13) . . . . ? C6 C11 C13 C12 -89.3(18) . . . . ? C6 C11 C13 C14 94.0(18) . . . . ? C12 C13 C14 C15 1(2) . . . . ? C11 C13 C14 C15 177.8(14) . . . . ? C13 C14 C15 C16 0(2) . . . . ? C13 C14 C15 C18 -173.8(14) . . . . ? C14 C15 C16 C17 1(2) . . . . ? C18 C15 C16 C17 174.6(14) . . . . ? C15 C16 C17 C12 -2(2) . . . . ? C15 C16 C17 C22 179.7(14) . . . . ? O2 C12 C17 C16 -176.4(13) . . . . ? C13 C12 C17 C16 3(2) . . . . ? O2 C12 C17 C22 2(2) . . . . ? C13 C12 C17 C22 -178.8(14) . . . . ? C14 C15 C18 C20 101.1(18) . . . . ? C16 C15 C18 C20 -72.2(19) . . . . ? C14 C15 C18 C19 -137.7(17) . . . . ? C16 C15 C18 C19 49(2) . . . . ? C14 C15 C18 C21 -20(2) . . . . ? C16 C15 C18 C21 166.6(14) . . . . ? C16 C17 C22 C24 -96.2(17) . . . . ? C12 C17 C22 C24 85.9(17) . . . . ? W1 O3 C23 C28 -83.8(18) . . . . ? W1 O3 C23 C24 89.1(15) . . . . ? O3 C23 C24 C25 -177.2(12) . . . . ? C28 C23 C24 C25 -4.4(19) . . . . ? O3 C23 C24 C22 1.4(19) . . . . ? C28 C23 C24 C22 174.3(12) . . . . ? C17 C22 C24 C25 87.2(16) . . . . ? C17 C22 C24 C23 -91.4(16) . . . . ? C23 C24 C25 C26 1(2) . . . . ? C22 C24 C25 C26 -178.0(14) . . . . ? C24 C25 C26 C27 2(2) . . . . ? C24 C25 C26 C29 179.2(14) . . . . ? C25 C26 C27 C28 -2(2) . . . . ? C29 C26 C27 C28 -178.8(15) . . . . ? O3 C23 C28 C27 177.6(13) . . . . ? C24 C23 C28 C27 5(2) . . . . ? O3 C23 C28 C33 8(2) . . . . ? C24 C23 C28 C33 -164.5(13) . . . . ? C26 C27 C28 C23 -2(2) . . . . ? C26 C27 C28 C33 168.0(15) . . . . ? C27 C26 C29 C31X -128(4) . . . . ? C25 C26 C29 C31X 55(4) . . . . ? C27 C26 C29 C31 -179.2(17) . . . . ? C25 C26 C29 C31 4(2) . . . . ? C27 C26 C29 C32X 5(5) . . . . ? C25 C26 C29 C32X -172(4) . . . . ? C27 C26 C29 C30 54(2) . . . . ? C25 C26 C29 C30 -123(2) . . . . ? C27 C26 C29 C30X 115(4) . . . . ? C25 C26 C29 C30X -62(4) . . . . ? C27 C26 C29 C32 -57(2) . . . . ? C25 C26 C29 C32 126(2) . . . . ? C23 C28 C33 C35 -51(2) . . . . ? C27 C28 C33 C35 140.0(15) . . . . ? W1 O4 C34 C39 110.2(14) . . . . ? W1 O4 C34 C35 -69.4(19) . . . . ? O4 C34 C35 C36 179.9(13) . . . . ? C39 C34 C35 C36 0(2) . . . . ? O4 C34 C35 C33 -8(2) . . . . ? C39 C34 C35 C33 172.5(14) . . . . ? C28 C33 C35 C34 90.3(18) . . . . ? C28 C33 C35 C36 -97.8(17) . . . . ? C34 C35 C36 C37 2(2) . . . . ? C33 C35 C36 C37 -170.2(15) . . . . ? C35 C36 C37 C38 -2(3) . . . . ? C35 C36 C37 C40 173.9(15) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? C40 C37 C38 C39 -176.8(15) . . . . ? O4 C34 C39 C38 177.5(12) . . . . ? C35 C34 C39 C38 -3(2) . . . . ? O4 C34 C39 C44 -2(2) . . . . ? C35 C34 C39 C44 178.0(13) . . . . ? C37 C38 C39 C34 3(2) . . . . ? C37 C38 C39 C44 -177.9(15) . . . . ? C36 C37 C40 C42 62(2) . . . . ? C38 C37 C40 C42 -121.7(17) . . . . ? C36 C37 C40 C42X 2(3) . . . . ? C38 C37 C40 C42X 178(2) . . . . ? C36 C37 C40 C41 -173.4(18) . . . . ? C38 C37 C40 C41 3(2) . . . . ? C36 C37 C40 C43 -57(2) . . . . ? C38 C37 C40 C43 118.7(17) . . . . ? C36 C37 C40 C43X -123(3) . . . . ? C38 C37 C40 C43X 53(3) . . . . ? C36 C37 C40 C41X 123(3) . . . . ? C38 C37 C40 C41X -61(3) . . . . ? C34 C39 C44 C46 166.2(13) . . . . ? C38 C39 C44 C46 -13(2) . . . . ? W2 O5 C45 C46 149(4) . . . . ? W2 O5 C45 C50 -32(6) . . . . ? O5 C45 C46 C47 -171.7(14) . . . . ? C50 C45 C46 C47 9(2) . . . . ? O5 C45 C46 C44 3(2) . . . . ? C50 C45 C46 C44 -176.4(15) . . . . ? C39 C44 C46 C45 -91.5(18) . . . . ? C39 C44 C46 C47 83.3(18) . . . . ? C45 C46 C47 C48 -2(2) . . . . ? C44 C46 C47 C48 -177.0(15) . . . . ? C46 C47 C48 C49 -3(2) . . . . ? C46 C47 C48 C51 172.6(14) . . . . ? C47 C48 C49 C50 3(2) . . . . ? C51 C48 C49 C50 -173.1(15) . . . . ? C48 C49 C50 C45 3(2) . . . . ? C48 C49 C50 C55 179.8(16) . . . . ? O5 C45 C50 C49 171.3(15) . . . . ? C46 C45 C50 C49 -9(3) . . . . ? O5 C45 C50 C55 -5(2) . . . . ? C46 C45 C50 C55 174.2(16) . . . . ? C47 C48 C51 C53 1(3) . . . . ? C49 C48 C51 C53 177(2) . . . . ? C47 C48 C51 C53X 16(3) . . . . ? C49 C48 C51 C53X -169(3) . . . . ? C47 C48 C51 C54 -128(3) . . . . ? C49 C48 C51 C54 48(3) . . . . ? C47 C48 C51 C52X 142(3) . . . . ? C49 C48 C51 C52X -42(4) . . . . ? C47 C48 C51 C54X -101(3) . . . . ? C49 C48 C51 C54X 74(3) . . . . ? C47 C48 C51 C52 120(2) . . . . ? C49 C48 C51 C52 -64(2) . . . . ? C49 C50 C55 C57 -99.0(18) . . . . ? C45 C50 C55 C57 78(2) . . . . ? W2 O6 C56 C61 -88.2(15) . . . . ? W2 O6 C56 C57 89.8(15) . . . . ? C61 C56 C57 C58 -1(2) . . . . ? O6 C56 C57 C58 -178.6(12) . . . . ? C61 C56 C57 C55 177.5(14) . . . . ? O6 C56 C57 C55 0(2) . . . . ? C50 C55 C57 C56 -98.0(18) . . . . ? C50 C55 C57 C58 80.1(18) . . . . ? C56 C57 C58 C59 2(2) . . . . ? C55 C57 C58 C59 -176.1(14) . . . . ? C57 C58 C59 C60 -2(2) . . . . ? C57 C58 C59 C62 177.9(15) . . . . ? C58 C59 C60 C61 1(2) . . . . ? C62 C59 C60 C61 -178.9(16) . . . . ? O6 C56 C61 C60 177.6(13) . . . . ? C57 C56 C61 C60 0(2) . . . . ? O6 C56 C61 C66 2(2) . . . . ? C57 C56 C61 C66 -175.8(14) . . . . ? C59 C60 C61 C56 0(2) . . . . ? C59 C60 C61 C66 175.7(14) . . . . ? C58 C59 C62 C65 59(2) . . . . ? C60 C59 C62 C65 -121.0(19) . . . . ? C58 C59 C62 C63 -63(2) . . . . ? C60 C59 C62 C63 117(2) . . . . ? C58 C59 C62 C64 178.6(18) . . . . ? C60 C59 C62 C64 -1(3) . . . . ? C56 C61 C66 C68 96.7(18) . . . . ? C60 C61 C66 C68 -78.8(19) . . . . ? W2 O7 C67 C72 96(2) . . . . ? W2 O7 C67 C68 -86(2) . . . . ? O7 C67 C68 C69 -176.9(15) . . . . ? C72 C67 C68 C69 2(2) . . . . ? O7 C67 C68 C66 7(2) . . . . ? C72 C67 C68 C66 -174.3(15) . . . . ? C61 C66 C68 C69 124.9(17) . . . . ? C61 C66 C68 C67 -59.5(19) . . . . ? C67 C68 C69 C70 0(3) . . . . ? C66 C68 C69 C70 175.9(17) . . . . ? C68 C69 C70 C71 1(3) . . . . ? C68 C69 C70 C73 -178.4(17) . . . . ? C69 C70 C71 C72 -5(3) . . . . ? C73 C70 C71 C72 174.8(18) . . . . ? C70 C71 C72 C67 7(3) . . . . ? C70 C71 C72 C77 -179.7(17) . . . . ? O7 C67 C72 C71 173.5(15) . . . . ? C68 C67 C72 C71 -5(3) . . . . ? O7 C67 C72 C77 0(2) . . . . ? C68 C67 C72 C77 -178.9(14) . . . . ? C71 C70 C73 C74X 109(4) . . . . ? C69 C70 C73 C74X -71(4) . . . . ? C71 C70 C73 C76 -61(3) . . . . ? C69 C70 C73 C76 119(3) . . . . ? C71 C70 C73 C74 163(3) . . . . ? C69 C70 C73 C74 -18(3) . . . . ? C71 C70 C73 C76X -119(3) . . . . ? C69 C70 C73 C76X 60(3) . . . . ? C71 C70 C73 C75X -7(3) . . . . ? C69 C70 C73 C75X 173(2) . . . . ? C71 C70 C73 C75 51(3) . . . . ? C69 C70 C73 C75 -129(2) . . . . ? C71 C72 C77 C79 100.1(18) . . . . ? C67 C72 C77 C79 -86.4(17) . . . . ? W2 O8 C78 C79 -66(2) . . . . ? W2 O8 C78 C83 117.7(15) . . . . ? O8 C78 C79 C80 176.1(13) . . . . ? C83 C78 C79 C80 -7(2) . . . . ? O8 C78 C79 C77 -8(2) . . . . ? C83 C78 C79 C77 168.2(13) . . . . ? C72 C77 C79 C78 95.5(18) . . . . ? C72 C77 C79 C80 -88.9(16) . . . . ? C78 C79 C80 C81 3(2) . . . . ? C77 C79 C80 C81 -173.2(14) . . . . ? C79 C80 C81 C82 2(2) . . . . ? C79 C80 C81 C84 176.7(15) . . . . ? C80 C81 C82 C83 -3(2) . . . . ? C84 C81 C82 C83 -177.0(15) . . . . ? C81 C82 C83 C78 -2(2) . . . . ? C81 C82 C83 C88 177.3(14) . . . . ? O8 C78 C83 C82 -176.3(12) . . . . ? C79 C78 C83 C82 7(2) . . . . ? O8 C78 C83 C88 4.5(19) . . . . ? C79 C78 C83 C88 -172.2(13) . . . . ? C82 C81 C84 C85 -125.7(17) . . . . ? C80 C81 C84 C85 60(2) . . . . ? C82 C81 C84 C87 -7(2) . . . . ? C80 C81 C84 C87 179.3(17) . . . . ? C82 C81 C84 C86 113.6(19) . . . . ? C80 C81 C84 C86 -60(2) . . . . ? C3 C2 C88 C83 81.5(17) . . . . ? C1 C2 C88 C83 -97.1(16) . . . . ? C82 C83 C88 C2 -21(2) . . . . ? C78 C83 C88 C2 157.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 4.440 _refine_diff_density_min -5.716 _refine_diff_density_rms 0.245 #===END data_2 _database_code_CSD 181732 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H134 N10 Na2 O8 W2' _chemical_formula_weight 2113.93 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' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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 13.8499(9) _cell_length_b 14.8714(10) _cell_length_c 28.9308(19) _cell_angle_alpha 78.519(2) _cell_angle_beta 77.455(2) _cell_angle_gamma 65.342(2) _cell_volume 5246.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12243 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.95 _exptl_crystal_description 'thick needle' _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 2.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.481 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39366 _diffrn_reflns_av_R_equivalents 0.1002 _diffrn_reflns_av_sigmaI/netI 0.2514 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.92 _reflns_number_total 23757 _reflns_number_gt 11723 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23757 _refine_ls_number_parameters 1254 _refine_ls_number_restraints 260 _refine_ls_R_factor_all 0.1837 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.970 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.72226(3) 0.39443(3) 0.699471(15) 0.01733(13) Uani 1 1 d U . . W2 W 0.72870(3) 0.43722(3) 0.770469(15) 0.01733(13) Uani 1 1 d . . . O1 O 0.5627(5) 0.4512(5) 0.7091(2) 0.0219(17) Uani 1 1 d . . . O2 O 0.7036(5) 0.5166(5) 0.6519(2) 0.0144(12) Uani 1 1 d U . . O3 O 0.8723(5) 0.3346(5) 0.6690(2) 0.0168(16) Uani 1 1 d . . . O4 O 0.7385(5) 0.2575(5) 0.7304(2) 0.0193(17) Uani 1 1 d . . . O5 O 0.6319(5) 0.3697(5) 0.8083(2) 0.0183(16) Uani 1 1 d . . . O6 O 0.8407(5) 0.3158(5) 0.7998(2) 0.0209(17) Uani 1 1 d . . . O7 O 0.8353(5) 0.4990(5) 0.7562(2) 0.0226(17) Uani 1 1 d . . . O8 O 0.6155(5) 0.5733(5) 0.7586(2) 0.0160(16) Uani 1 1 d . . . C1 C 0.4787(8) 0.5426(7) 0.7039(3) 0.016(2) Uani 1 1 d U . . C2 C 0.4135(9) 0.5909(8) 0.7439(4) 0.024(3) Uani 1 1 d . . . C3 C 0.3283(9) 0.6825(8) 0.7338(4) 0.029(3) Uani 1 1 d . . . H3 H 0.2854 0.7175 0.7600 0.035 Uiso 1 1 calc R . . C4 C 0.3018(8) 0.7260(8) 0.6886(4) 0.028(3) Uani 1 1 d . . . C5 C 0.3698(8) 0.6725(8) 0.6511(4) 0.022(2) Uani 1 1 d U . . H5 H 0.3562 0.6993 0.6194 0.027 Uiso 1 1 calc R . . C6 C 0.4555(8) 0.5826(8) 0.6581(4) 0.0192(19) Uani 1 1 d U . . C7 C 0.2069(10) 0.8234(9) 0.6796(4) 0.038(3) Uani 1 1 d . . . C8 C 0.2432(12) 0.8963(10) 0.6435(5) 0.076(5) Uani 1 1 d . . . H8A H 0.3005 0.9053 0.6544 0.114 Uiso 1 1 calc R . . H8B H 0.1824 0.9605 0.6400 0.114 Uiso 1 1 calc R . . H8C H 0.2704 0.8701 0.6126 0.114 Uiso 1 1 calc R . . C9 C 0.1306(11) 0.8009(11) 0.6567(6) 0.080(6) Uani 1 1 d . . . H9A H 0.1663 0.7793 0.6253 0.120 Uiso 1 1 calc R . . H9B H 0.0653 0.8612 0.6530 0.120 Uiso 1 1 calc R . . H9C H 0.1115 0.7480 0.6771 0.120 Uiso 1 1 calc R . . C10 C 0.1455(12) 0.8715(11) 0.7242(5) 0.071(5) Uani 1 1 d . . . H10A H 0.1309 0.8215 0.7491 0.107 Uiso 1 1 calc R . . H10B H 0.0774 0.9253 0.7171 0.107 Uiso 1 1 calc R . . H10C H 0.1883 0.8989 0.7354 0.107 Uiso 1 1 calc R . . C11 C 0.5153(8) 0.5241(8) 0.6166(4) 0.025(2) Uani 1 1 d U . . H11A H 0.4624 0.5349 0.5958 0.030 Uiso 1 1 calc R . . H11B H 0.5425 0.4525 0.6293 0.030 Uiso 1 1 calc R . . C12 C 0.7023(8) 0.5278(7) 0.6045(3) 0.0171(14) Uani 1 1 d U . . C13 C 0.6086(8) 0.5445(8) 0.5853(4) 0.0181(17) Uani 1 1 d U . . C14 C 0.6077(9) 0.5689(8) 0.5363(4) 0.024(3) Uani 1 1 d . . . H14 H 0.5436 0.5829 0.5243 0.029 Uiso 1 1 calc R . . C15 C 0.6967(9) 0.5737(8) 0.5042(4) 0.025(3) Uani 1 1 d . . . C16 C 0.7922(8) 0.5470(8) 0.5226(4) 0.023(3) Uani 1 1 d . . . H16 H 0.8550 0.5466 0.5013 0.027 Uiso 1 1 calc R . . C17 C 0.7972(8) 0.5213(7) 0.5710(3) 0.0175(18) Uani 1 1 d U . . C18 C 0.6948(10) 0.5983(9) 0.4504(4) 0.031(3) Uani 1 1 d . . . C19 C 0.7345(13) 0.6843(11) 0.4307(4) 0.065(5) Uani 1 1 d . . . H19A H 0.7226 0.7073 0.3975 0.098 Uiso 1 1 calc R . . H19B H 0.8113 0.6600 0.4324 0.098 Uiso 1 1 calc R . . H19C H 0.6945 0.7397 0.4499 0.098 Uiso 1 1 calc R . . C20 C 0.7723(13) 0.5055(12) 0.4251(4) 0.072(5) Uani 1 1 d . . . H20A H 0.7548 0.4479 0.4400 0.107 Uiso 1 1 calc R . . H20B H 0.8466 0.4915 0.4280 0.107 Uiso 1 1 calc R . . H20C H 0.7642 0.5188 0.3913 0.107 Uiso 1 1 calc R . . C21 C 0.5865(10) 0.6306(10) 0.4369(4) 0.043(3) Uani 1 1 d . . . H21A H 0.5647 0.5740 0.4436 0.064 Uiso 1 1 calc R . . H21B H 0.5888 0.6553 0.4028 0.064 Uiso 1 1 calc R . . H21C H 0.5345 0.6840 0.4555 0.064 Uiso 1 1 calc R . . C22 C 0.9060(7) 0.4712(7) 0.5887(4) 0.018(2) Uani 1 1 d U . . H22A H 0.8991 0.4845 0.6218 0.021 Uiso 1 1 calc R . . H22B H 0.9586 0.4965 0.5680 0.021 Uiso 1 1 calc R . . C23 C 0.9121(8) 0.3001(8) 0.6257(4) 0.020(2) Uani 1 1 d . . . C24 C 0.9423(8) 0.3591(8) 0.5869(4) 0.020(2) Uani 1 1 d U . . C25 C 0.9963(8) 0.3200(8) 0.5441(4) 0.024(3) Uani 1 1 d . . . H25 H 1.0182 0.3612 0.5182 0.029 Uiso 1 1 calc R . . C26 C 1.0188(9) 0.2221(9) 0.5386(4) 0.032(3) Uani 1 1 d U A . C27 C 0.9847(8) 0.1645(8) 0.5770(4) 0.024(3) Uani 1 1 d . . . H27 H 0.9992 0.0975 0.5738 0.029 Uiso 1 1 calc R . . C28 C 0.9294(9) 0.2018(8) 0.6205(4) 0.025(3) Uani 1 1 d . . . C29 C 1.0840(10) 0.1780(9) 0.4925(4) 0.039(2) Uani 1 1 d U . . C30 C 1.0272(18) 0.2500(14) 0.4492(6) 0.062(5) Uani 0.745(15) 1 d PU A 1 H30A H 0.9538 0.2532 0.4528 0.092 Uiso 0.745(15) 1 calc PR A 1 H30B H 1.0679 0.2242 0.4191 0.092 Uiso 0.745(15) 1 calc PR A 1 H30C H 1.0248 0.3169 0.4489 0.092 Uiso 0.745(15) 1 calc PR A 1 C31 C 1.1928(15) 0.1776(16) 0.4838(7) 0.056(4) Uani 0.745(15) 1 d PU A 1 H31A H 1.1885 0.2434 0.4874 0.083 Uiso 0.745(15) 1 calc PR A 1 H31B H 1.2269 0.1620 0.4514 0.083 Uiso 0.745(15) 1 calc PR A 1 H31C H 1.2356 0.1272 0.5069 0.083 Uiso 0.745(15) 1 calc PR A 1 C32 C 1.0838(16) 0.0775(14) 0.4886(6) 0.043(4) Uani 0.745(15) 1 d PU A 1 H32A H 1.0096 0.0819 0.4946 0.064 Uiso 0.745(15) 1 calc PR A 1 H32B H 1.1245 0.0268 0.5122 0.064 Uiso 0.745(15) 1 calc PR A 1 H32C H 1.1171 0.0591 0.4565 0.064 Uiso 0.745(15) 1 calc PR A 1 C30X C 1.116(5) 0.253(4) 0.4562(17) 0.050(6) Uani 0.255(15) 1 d PU A 2 H30D H 1.1444 0.2875 0.4718 0.074 Uiso 0.255(15) 1 calc PR A 2 H30E H 1.0529 0.3018 0.4422 0.074 Uiso 0.255(15) 1 calc PR A 2 H30F H 1.1713 0.2185 0.4310 0.074 Uiso 0.255(15) 1 calc PR A 2 C31X C 1.200(4) 0.107(4) 0.5083(19) 0.051(7) Uani 0.255(15) 1 d PU A 2 H31D H 1.2332 0.1481 0.5156 0.076 Uiso 0.255(15) 1 calc PR A 2 H31E H 1.2460 0.0687 0.4823 0.076 Uiso 0.255(15) 1 calc PR A 2 H31F H 1.1905 0.0612 0.5367 0.076 Uiso 0.255(15) 1 calc PR A 2 C32X C 1.029(5) 0.135(5) 0.4738(19) 0.046(6) Uani 0.255(15) 1 d PU A 2 H32D H 1.0120 0.0862 0.4983 0.070 Uiso 0.255(15) 1 calc PR A 2 H32E H 1.0754 0.1024 0.4461 0.070 Uiso 0.255(15) 1 calc PR A 2 H32F H 0.9630 0.1876 0.4640 0.070 Uiso 0.255(15) 1 calc PR A 2 C33 C 0.8951(8) 0.1340(8) 0.6611(4) 0.024(3) Uani 1 1 d . . . H33A H 0.9143 0.1420 0.6906 0.029 Uiso 1 1 calc R . . H33B H 0.9387 0.0643 0.6546 0.029 Uiso 1 1 calc R . . C34 C 0.7053(8) 0.2071(8) 0.7073(3) 0.018(2) Uani 1 1 d . . . C35 C 0.7778(8) 0.1479(7) 0.6711(3) 0.019(3) Uani 1 1 d . . . C36 C 0.7358(9) 0.0977(8) 0.6498(4) 0.024(3) Uani 1 1 d . . . H36 H 0.7814 0.0585 0.6254 0.028 Uiso 1 1 calc R . . C37 C 0.6324(8) 0.1022(7) 0.6624(4) 0.018(2) Uani 1 1 d . . . C38 C 0.5653(9) 0.1583(8) 0.6995(3) 0.025(3) Uani 1 1 d . . . H38 H 0.4933 0.1633 0.7087 0.030 Uiso 1 1 calc R . . C39 C 0.6050(8) 0.2071(8) 0.7231(3) 0.017(2) Uani 1 1 d . . . C40 C 0.5977(9) 0.0437(8) 0.6366(4) 0.026(3) Uani 1 1 d . . . C41 C 0.4775(10) 0.0618(10) 0.6533(5) 0.048(4) Uani 1 1 d . . . H41A H 0.4331 0.1326 0.6458 0.072 Uiso 1 1 calc R . . H41B H 0.4658 0.0426 0.6878 0.072 Uiso 1 1 calc R . . H41C H 0.4578 0.0217 0.6369 0.072 Uiso 1 1 calc R . . C42 C 0.6632(10) -0.0668(8) 0.6460(4) 0.037(3) Uani 1 1 d . . . H42A H 0.6384 -0.1034 0.6298 0.056 Uiso 1 1 calc R . . H42B H 0.6546 -0.0882 0.6804 0.056 Uiso 1 1 calc R . . H42C H 0.7392 -0.0806 0.6339 0.056 Uiso 1 1 calc R . . C43 C 0.6094(11) 0.0758(10) 0.5831(4) 0.044(4) Uani 1 1 d . . . H43A H 0.5577 0.1443 0.5765 0.065 Uiso 1 1 calc R . . H43B H 0.5957 0.0312 0.5670 0.065 Uiso 1 1 calc R . . H43C H 0.6825 0.0727 0.5714 0.065 Uiso 1 1 calc R . . C44 C 0.5362(8) 0.2634(8) 0.7649(3) 0.018(2) Uani 1 1 d . . . H44A H 0.5212 0.3352 0.7557 0.022 Uiso 1 1 calc R . . H44B H 0.4666 0.2558 0.7719 0.022 Uiso 1 1 calc R . . C45 C 0.6351(7) 0.2792(7) 0.8281(3) 0.012(2) Uani 1 1 d . . . C46 C 0.5875(8) 0.2285(8) 0.8094(4) 0.018(2) Uani 1 1 d . . . C47 C 0.5883(8) 0.1373(8) 0.8353(4) 0.022(3) Uani 1 1 d . . . H47 H 0.5559 0.1032 0.8234 0.027 Uiso 1 1 calc R . . C48 C 0.6333(8) 0.0934(8) 0.8771(4) 0.024(3) Uani 1 1 d . . . C49 C 0.6806(8) 0.1451(8) 0.8934(3) 0.021(3) Uani 1 1 d . . . H49 H 0.7123 0.1181 0.9217 0.025 Uiso 1 1 calc R . . C50 C 0.6824(8) 0.2351(8) 0.8693(4) 0.021(3) Uani 1 1 d . . . C51 C 0.6188(9) -0.0002(9) 0.9047(4) 0.027(3) Uani 1 1 d . . . C52 C 0.5012(10) 0.0263(10) 0.9254(5) 0.050(4) Uani 1 1 d . . . H52A H 0.4819 0.0676 0.9511 0.075 Uiso 1 1 calc R . . H52B H 0.4890 -0.0349 0.9381 0.075 Uiso 1 1 calc R . . H52C H 0.4568 0.0633 0.9003 0.075 Uiso 1 1 calc R . . C53 C 0.6848(11) -0.0447(9) 0.9455(4) 0.048(4) Uani 1 1 d . . . H53A H 0.6578 0.0018 0.9694 0.071 Uiso 1 1 calc R . . H53B H 0.7603 -0.0568 0.9332 0.071 Uiso 1 1 calc R . . H53C H 0.6788 -0.1079 0.9602 0.071 Uiso 1 1 calc R . . C54 C 0.6552(11) -0.0820(9) 0.8715(4) 0.046(4) Uani 1 1 d . . . H54A H 0.6550 -0.1443 0.8906 0.069 Uiso 1 1 calc R . . H54B H 0.7280 -0.0926 0.8548 0.069 Uiso 1 1 calc R . . H54C H 0.6058 -0.0609 0.8482 0.069 Uiso 1 1 calc R . . C55 C 0.7253(8) 0.2896(8) 0.8928(3) 0.022(3) Uani 1 1 d . . . H55A H 0.6866 0.3618 0.8835 0.026 Uiso 1 1 calc R . . H55B H 0.7051 0.2766 0.9277 0.026 Uiso 1 1 calc R . . C56 C 0.8924(9) 0.2931(8) 0.8389(4) 0.025(3) Uani 1 1 d . . . C57 C 0.8408(8) 0.2690(7) 0.8837(4) 0.020(3) Uani 1 1 d . . . C58 C 0.9057(9) 0.2306(8) 0.9207(4) 0.025(3) Uani 1 1 d . . . H58 H 0.8740 0.2105 0.9514 0.030 Uiso 1 1 calc R . . C59 C 1.0117(9) 0.2202(8) 0.9155(4) 0.023(3) Uani 1 1 d . . . C60 C 1.0522(8) 0.2576(8) 0.8715(4) 0.022(3) Uani 1 1 d . . . H60 H 1.1226 0.2569 0.8669 0.026 Uiso 1 1 calc R . . C61 C 0.9927(8) 0.2965(8) 0.8334(4) 0.020(2) Uani 1 1 d . . . C62 C 1.0782(10) 0.1753(9) 0.9558(4) 0.032(3) Uani 1 1 d . . . C63 C 1.0231(12) 0.1393(12) 1.0011(5) 0.070(5) Uani 1 1 d . . . H63A H 1.0104 0.0820 0.9963 0.104 Uiso 1 1 calc R . . H63B H 0.9543 0.1929 1.0107 0.104 Uiso 1 1 calc R . . H63C H 1.0684 0.1193 1.0261 0.104 Uiso 1 1 calc R . . C64 C 1.1812(13) 0.0905(13) 0.9393(5) 0.093(7) Uani 1 1 d . . . H64A H 1.2258 0.0627 0.9648 0.139 Uiso 1 1 calc R . . H64B H 1.2206 0.1155 0.9110 0.139 Uiso 1 1 calc R . . H64C H 1.1639 0.0383 0.9313 0.139 Uiso 1 1 calc R . . C65 C 1.1107(13) 0.2566(12) 0.9678(5) 0.066(5) Uani 1 1 d . . . H65A H 1.0462 0.3172 0.9736 0.100 Uiso 1 1 calc R . . H65B H 1.1604 0.2721 0.9409 0.100 Uiso 1 1 calc R . . H65C H 1.1458 0.2313 0.9964 0.100 Uiso 1 1 calc R . . C66 C 1.0292(8) 0.3587(7) 0.7897(3) 0.021(3) Uani 1 1 d . . . H66A H 1.1082 0.3374 0.7847 0.026 Uiso 1 1 calc R . . H66B H 1.0074 0.3516 0.7607 0.026 Uiso 1 1 calc R . . C67 C 0.8705(8) 0.5257(8) 0.7886(3) 0.019(2) Uani 1 1 d . . . C68 C 0.9735(8) 0.4658(8) 0.8010(4) 0.019(2) Uani 1 1 d . . . C69 C 1.0177(8) 0.4997(8) 0.8288(4) 0.023(3) Uani 1 1 d . . . H69 H 1.0866 0.4574 0.8371 0.028 Uiso 1 1 calc R . . C70 C 0.9654(8) 0.5947(8) 0.8455(4) 0.025(2) Uani 1 1 d U . . C71 C 0.8625(8) 0.6482(8) 0.8348(4) 0.024(2) Uani 1 1 d U . . H71 H 0.8228 0.7104 0.8470 0.029 Uiso 1 1 calc R . . C72 C 0.8137(8) 0.6191(8) 0.8081(4) 0.022(2) Uani 1 1 d U . . C73 C 1.0195(9) 0.6300(9) 0.8735(4) 0.030(3) Uani 1 1 d . . . C74 C 1.0538(11) 0.5562(10) 0.9185(5) 0.054(4) Uani 1 1 d . . . H74A H 1.0937 0.5787 0.9345 0.081 Uiso 1 1 calc R . . H74B H 1.0998 0.4898 0.9092 0.081 Uiso 1 1 calc R . . H74C H 0.9898 0.5535 0.9402 0.081 Uiso 1 1 calc R . . C75 C 0.9527(9) 0.7319(10) 0.8894(4) 0.044(4) Uani 1 1 d . . . H75A H 0.9361 0.7817 0.8613 0.066 Uiso 1 1 calc R . . H75B H 0.9931 0.7484 0.9080 0.066 Uiso 1 1 calc R . . H75C H 0.8857 0.7315 0.9091 0.066 Uiso 1 1 calc R . . C76 C 1.1250(11) 0.6339(11) 0.8419(5) 0.061(4) Uani 1 1 d . . . H76A H 1.1074 0.6803 0.8129 0.091 Uiso 1 1 calc R . . H76B H 1.1726 0.5672 0.8333 0.091 Uiso 1 1 calc R . . H76C H 1.1614 0.6566 0.8598 0.091 Uiso 1 1 calc R . . C77 C 0.7009(8) 0.6858(8) 0.7971(4) 0.023(3) Uani 1 1 d . . . H77A H 0.7016 0.6884 0.7625 0.027 Uiso 1 1 calc R . . H77B H 0.6855 0.7541 0.8031 0.027 Uiso 1 1 calc R . . C78 C 0.5657(8) 0.6088(8) 0.8022(4) 0.020(2) Uani 1 1 d . . . C79 C 0.6064(8) 0.6574(8) 0.8245(4) 0.019(2) Uani 1 1 d . . . C80 C 0.5547(9) 0.6866(8) 0.8680(4) 0.026(3) Uani 1 1 d . . . H80 H 0.5834 0.7185 0.8835 0.031 Uiso 1 1 calc R . . C81 C 0.4626(9) 0.6725(10) 0.8908(4) 0.033(3) Uani 1 1 d U B . C82 C 0.4197(9) 0.6288(9) 0.8662(4) 0.028(3) Uani 1 1 d . . . H82 H 0.3552 0.6200 0.8807 0.034 Uiso 1 1 calc R . . C83 C 0.4681(8) 0.5975(8) 0.8211(4) 0.020(3) Uani 1 1 d . . . C84 C 0.4073(11) 0.7038(11) 0.9402(4) 0.047(3) Uani 1 1 d U . . C85 C 0.4906(17) 0.659(2) 0.9738(7) 0.063(5) Uani 0.694(18) 1 d PU B 1 H85A H 0.5192 0.5862 0.9763 0.094 Uiso 0.694(18) 1 calc PR B 1 H85B H 0.4570 0.6802 1.0055 0.094 Uiso 0.694(18) 1 calc PR B 1 H85C H 0.5492 0.6821 0.9615 0.094 Uiso 0.694(18) 1 calc PR B 1 C86 C 0.360(2) 0.8162(16) 0.9366(7) 0.063(5) Uani 0.694(18) 1 d PU B 1 H86A H 0.3246 0.8368 0.9683 0.095 Uiso 0.694(18) 1 calc PR B 1 H86B H 0.3063 0.8435 0.9147 0.095 Uiso 0.694(18) 1 calc PR B 1 H86C H 0.4166 0.8413 0.9246 0.095 Uiso 0.694(18) 1 calc PR B 1 C87 C 0.3164(18) 0.6644(19) 0.9621(8) 0.053(5) Uani 0.694(18) 1 d PU B 1 H87A H 0.3467 0.5914 0.9646 0.079 Uiso 0.694(18) 1 calc PR B 1 H87B H 0.2605 0.6917 0.9415 0.079 Uiso 0.694(18) 1 calc PR B 1 H87C H 0.2850 0.6854 0.9939 0.079 Uiso 0.694(18) 1 calc PR B 1 C85X C 0.451(4) 0.609(4) 0.9755(16) 0.063(7) Uani 0.306(18) 1 d PU B 2 H85D H 0.4196 0.6243 1.0082 0.095 Uiso 0.306(18) 1 calc PR B 2 H85E H 0.5297 0.5861 0.9721 0.095 Uiso 0.306(18) 1 calc PR B 2 H85F H 0.4329 0.5567 0.9687 0.095 Uiso 0.306(18) 1 calc PR B 2 C86X C 0.436(4) 0.780(4) 0.9554(16) 0.057(5) Uani 0.306(18) 1 d PU B 2 H86D H 0.3968 0.7953 0.9874 0.086 Uiso 0.306(18) 1 calc PR B 2 H86E H 0.4153 0.8409 0.9328 0.086 Uiso 0.306(18) 1 calc PR B 2 H86F H 0.5131 0.7532 0.9560 0.086 Uiso 0.306(18) 1 calc PR B 2 C87X C 0.291(4) 0.726(5) 0.9489(19) 0.058(6) Uani 0.306(18) 1 d PU B 2 H87D H 0.2606 0.7457 0.9809 0.087 Uiso 0.306(18) 1 calc PR B 2 H87E H 0.2798 0.6664 0.9463 0.087 Uiso 0.306(18) 1 calc PR B 2 H87F H 0.2556 0.7804 0.9252 0.087 Uiso 0.306(18) 1 calc PR B 2 C88 C 0.4255(8) 0.5485(8) 0.7949(3) 0.021(3) Uani 1 1 d . . . H88A H 0.3544 0.5521 0.8123 0.025 Uiso 1 1 calc R . . H88B H 0.4740 0.4771 0.7956 0.025 Uiso 1 1 calc R . . Na1 Na 0.6174(4) 0.6711(3) 0.68248(15) 0.0333(12) Uani 1 1 d . . . Na2 Na 0.8555(4) 0.1673(3) 0.78322(16) 0.0359(12) Uani 1 1 d . . . N1 N 0.5642(10) 0.7733(8) 0.6081(4) 0.054(3) Uani 1 1 d . . . C89 C 0.5292(11) 0.8105(10) 0.5738(5) 0.042(3) Uani 1 1 d . . . C90 C 0.4830(14) 0.8579(12) 0.5311(5) 0.081(6) Uani 1 1 d . . . H90A H 0.4410 0.9290 0.5337 0.122 Uiso 1 1 calc R . . H90B H 0.4360 0.8270 0.5267 0.122 Uiso 1 1 calc R . . H90C H 0.5404 0.8502 0.5037 0.122 Uiso 1 1 calc R . . N2 N 0.7922(9) 0.6873(8) 0.6698(4) 0.042(3) Uani 1 1 d . . . C91 C 0.8787(11) 0.6428(10) 0.6742(4) 0.036(3) Uani 1 1 d . . . C92 C 0.9928(10) 0.5820(11) 0.6780(5) 0.054(4) Uani 1 1 d . . . H92A H 1.0062 0.5112 0.6806 0.081 Uiso 1 1 calc R . . H92B H 1.0105 0.5950 0.7063 0.081 Uiso 1 1 calc R . . H92C H 1.0378 0.5994 0.6495 0.081 Uiso 1 1 calc R . . N3 N 0.4960(10) 0.8137(8) 0.7249(4) 0.051(3) Uani 1 1 d . . . C93 C 0.4405(15) 0.8528(13) 0.7582(7) 0.079(6) Uani 1 1 d . . . C94 C 0.374(2) 0.904(2) 0.7994(7) 0.202(16) Uani 1 1 d . . . N4 N 0.8635(9) 0.0044(8) 0.7802(4) 0.046(3) Uani 1 1 d . . . C95 C 0.8479(11) -0.0492(11) 0.7647(5) 0.046(4) Uani 1 1 d . . . C96 C 0.8262(15) -0.1191(12) 0.7446(5) 0.080(6) Uani 1 1 d . . . H96A H 0.7741 -0.0825 0.7224 0.120 Uiso 1 1 calc R . . H96B H 0.7967 -0.1587 0.7702 0.120 Uiso 1 1 calc R . . H96C H 0.8930 -0.1634 0.7274 0.120 Uiso 1 1 calc R . . N5 N 1.0491(10) 0.1243(8) 0.7548(4) 0.056(3) Uani 1 1 d . . . C97 C 1.0942(12) 0.1495(11) 0.7206(6) 0.052(4) Uani 1 1 d . . . C98 C 1.1517(13) 0.1825(13) 0.6768(6) 0.081(6) Uani 1 1 d . . . H98A H 1.2099 0.1955 0.6844 0.122 Uiso 1 1 calc R . . H98B H 1.1019 0.2437 0.6609 0.122 Uiso 1 1 calc R . . H98C H 1.1819 0.1304 0.6555 0.122 Uiso 1 1 calc R . . N6 N 0.7530(13) 0.6377(13) 0.9724(5) 0.102(6) Uani 1 1 d . . . C99 C 0.7708(13) 0.5713(14) 0.9543(5) 0.062(5) Uani 1 1 d . . . C100 C 0.7943(12) 0.4854(10) 0.9292(5) 0.060(4) Uani 1 1 d . . . H10D H 0.8715 0.4557 0.9176 0.090 Uiso 1 1 calc R . . H10E H 0.7543 0.5080 0.9021 0.090 Uiso 1 1 calc R . . H10F H 0.7725 0.4356 0.9512 0.090 Uiso 1 1 calc R . . N7 N 0.6967(13) 0.2455(14) 0.4737(5) 0.105(6) Uani 1 1 d . . . C101 C 0.7096(11) 0.2712(12) 0.5055(5) 0.053(4) Uani 1 1 d . . . C102 C 0.7212(11) 0.3030(10) 0.5473(4) 0.048(4) Uani 1 1 d . . . H10G H 0.6587 0.3081 0.5719 0.072 Uiso 1 1 calc R . . H10H H 0.7263 0.3682 0.5388 0.072 Uiso 1 1 calc R . . H10I H 0.7866 0.2542 0.5596 0.072 Uiso 1 1 calc R . . N8 N -0.0067(13) 1.0089(12) 0.8725(6) 0.107(5) Uani 1 1 d . . . C103 C 0.0898(17) 0.9207(14) 0.8635(7) 0.081(6) Uani 1 1 d . . . C104 C 0.1603(15) 0.8531(14) 0.8584(8) 0.119(9) Uani 1 1 d . . . H10J H 0.2215 0.8699 0.8421 0.178 Uiso 1 1 calc R . . H10K H 0.1473 0.8134 0.8390 0.178 Uiso 1 1 calc R . . H10L H 0.1761 0.8146 0.8895 0.178 Uiso 1 1 calc R . . N9 N 0.2918(10) 0.3305(11) 0.8478(5) 0.071(4) Uani 1 1 d . . . C105 C 0.3367(11) 0.3347(11) 0.8747(5) 0.047(4) Uani 1 1 d . . . C106 C 0.3911(12) 0.3436(11) 0.9093(5) 0.061(4) Uani 1 1 d . . . H10M H 0.4092 0.4023 0.8991 0.092 Uiso 1 1 calc R . . H10N H 0.4571 0.2838 0.9124 0.092 Uiso 1 1 calc R . . H10O H 0.3442 0.3508 0.9402 0.092 Uiso 1 1 calc R . . N10 N 1.2802(11) 0.3195(11) 0.6970(4) 0.069(4) Uani 1 1 d . . . C107 C 1.2720(10) 0.3866(11) 0.7123(4) 0.039(3) Uani 1 1 d . . . C108 C 1.2617(11) 0.4725(11) 0.7314(5) 0.055(4) Uani 1 1 d . . . H10P H 1.2833 0.5175 0.7058 0.082 Uiso 1 1 calc R . . H10Q H 1.3079 0.4516 0.7561 0.082 Uiso 1 1 calc R . . H10R H 1.1867 0.5071 0.7454 0.082 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 W1 0.0148(3) 0.0169(3) 0.0204(3) -0.0066(2) -0.0003(2) -0.0055(2) W2 0.0151(3) 0.0175(3) 0.0200(3) -0.0061(2) -0.0003(2) -0.0064(2) O1 0.021(4) 0.012(4) 0.037(4) -0.004(3) -0.011(3) -0.006(3) O2 0.013(3) 0.017(2) 0.022(2) -0.0073(15) 0.001(2) -0.013(2) O3 0.020(4) 0.018(4) 0.018(4) -0.007(3) 0.006(3) -0.014(3) O4 0.010(4) 0.025(4) 0.028(4) -0.011(3) -0.001(3) -0.010(3) O5 0.017(4) 0.023(4) 0.018(4) -0.009(3) 0.002(3) -0.010(3) O6 0.012(4) 0.028(4) 0.022(4) -0.008(3) -0.004(3) -0.004(3) O7 0.017(4) 0.028(5) 0.030(4) -0.016(3) 0.001(3) -0.013(4) O8 0.009(4) 0.014(4) 0.021(4) -0.012(3) 0.002(3) 0.001(3) C1 0.014(5) 0.014(5) 0.027(4) -0.007(3) -0.002(4) -0.009(4) C2 0.024(6) 0.034(7) 0.026(6) -0.005(5) 0.002(5) -0.025(6) C3 0.027(7) 0.023(7) 0.041(7) -0.016(6) 0.003(6) -0.012(6) C4 0.015(6) 0.025(7) 0.038(7) -0.003(5) -0.002(5) -0.003(5) C5 0.021(5) 0.026(5) 0.023(5) -0.003(3) -0.004(4) -0.012(3) C6 0.016(3) 0.025(3) 0.026(3) -0.008(3) -0.004(3) -0.014(3) C7 0.035(8) 0.032(8) 0.040(8) -0.006(6) -0.007(6) -0.004(6) C8 0.057(11) 0.046(10) 0.078(12) 0.017(8) -0.004(9) 0.012(8) C9 0.036(10) 0.056(11) 0.136(16) -0.027(10) -0.035(10) 0.013(8) C10 0.062(11) 0.049(10) 0.057(10) -0.012(8) -0.012(8) 0.028(8) C11 0.019(5) 0.034(5) 0.027(4) -0.010(4) -0.003(4) -0.013(4) C12 0.017(3) 0.017(3) 0.022(2) -0.0055(17) -0.001(2) -0.011(3) C13 0.018(3) 0.018(4) 0.022(4) -0.009(3) -0.002(3) -0.008(4) C14 0.025(7) 0.022(6) 0.031(7) -0.013(5) -0.002(5) -0.012(5) C15 0.038(7) 0.015(6) 0.029(7) -0.007(5) -0.005(5) -0.016(6) C16 0.017(6) 0.031(7) 0.023(6) -0.008(5) 0.001(5) -0.012(5) C17 0.020(3) 0.016(4) 0.021(3) -0.007(3) 0.001(3) -0.011(4) C18 0.038(8) 0.032(7) 0.020(6) -0.007(5) 0.000(5) -0.011(6) C19 0.108(14) 0.086(12) 0.033(8) 0.016(8) -0.019(8) -0.073(11) C20 0.085(13) 0.084(13) 0.024(8) -0.029(8) 0.007(8) -0.010(10) C21 0.048(9) 0.059(10) 0.030(7) -0.007(6) -0.010(6) -0.026(8) C22 0.010(5) 0.019(4) 0.028(5) -0.010(4) 0.008(4) -0.012(4) C23 0.011(5) 0.030(7) 0.027(6) -0.012(5) 0.001(4) -0.013(5) C24 0.010(5) 0.016(4) 0.034(6) -0.009(4) -0.001(4) -0.003(4) C25 0.025(6) 0.034(7) 0.024(6) -0.009(5) 0.001(5) -0.022(6) C26 0.037(6) 0.029(6) 0.033(5) -0.020(4) 0.011(4) -0.017(5) C27 0.022(6) 0.017(6) 0.034(7) -0.007(5) -0.001(5) -0.009(5) C28 0.020(6) 0.026(7) 0.029(7) -0.001(5) -0.005(5) -0.010(5) C29 0.044(5) 0.041(5) 0.035(5) -0.023(4) 0.016(4) -0.022(5) C30 0.080(10) 0.056(8) 0.032(5) -0.017(6) 0.012(7) -0.015(9) C31 0.049(6) 0.059(10) 0.064(10) -0.037(8) 0.030(5) -0.032(7) C32 0.051(10) 0.044(6) 0.037(9) -0.032(5) 0.025(7) -0.025(7) C30X 0.059(12) 0.049(10) 0.041(9) -0.022(8) 0.023(9) -0.029(8) C31X 0.040(8) 0.054(13) 0.050(14) -0.025(10) 0.020(8) -0.015(9) C32X 0.053(12) 0.053(13) 0.041(12) -0.038(10) 0.022(10) -0.028(10) C33 0.009(6) 0.026(7) 0.028(6) -0.010(5) 0.003(5) 0.002(5) C34 0.016(6) 0.020(6) 0.020(6) 0.000(4) -0.006(4) -0.010(5) C35 0.020(6) 0.010(6) 0.022(6) -0.002(4) 0.000(5) -0.002(5) C36 0.030(7) 0.017(6) 0.022(6) -0.004(5) 0.000(5) -0.008(5) C37 0.009(5) 0.007(6) 0.041(7) -0.014(5) -0.004(5) -0.001(5) C38 0.039(7) 0.019(6) 0.019(6) -0.001(5) 0.002(5) -0.017(6) C39 0.007(5) 0.028(7) 0.021(6) -0.004(5) -0.003(4) -0.010(5) C40 0.026(7) 0.019(6) 0.028(6) -0.001(5) -0.016(5) 0.002(5) C41 0.033(8) 0.049(9) 0.077(10) -0.036(8) -0.015(7) -0.014(7) C42 0.041(8) 0.026(7) 0.051(8) -0.015(6) -0.011(6) -0.013(6) C43 0.068(10) 0.052(9) 0.024(7) -0.004(6) -0.016(7) -0.032(8) C44 0.015(6) 0.019(6) 0.022(6) -0.008(5) 0.004(4) -0.008(5) C45 0.008(5) 0.013(6) 0.020(5) -0.009(4) 0.002(4) -0.006(4) C46 0.008(5) 0.017(6) 0.023(6) -0.011(5) 0.007(4) -0.001(5) C47 0.018(6) 0.027(7) 0.023(6) -0.007(5) 0.001(5) -0.010(5) C48 0.015(6) 0.028(7) 0.021(6) -0.002(5) 0.006(5) -0.006(5) C49 0.016(6) 0.028(7) 0.017(6) -0.009(5) 0.000(4) -0.006(5) C50 0.012(6) 0.024(7) 0.028(6) -0.005(5) 0.000(5) -0.007(5) C51 0.033(7) 0.037(8) 0.024(6) 0.000(5) 0.003(5) -0.029(6) C52 0.048(9) 0.038(8) 0.066(10) -0.003(7) 0.015(7) -0.032(7) C53 0.061(10) 0.029(8) 0.059(9) 0.014(7) -0.023(8) -0.026(7) C54 0.059(10) 0.019(7) 0.050(9) -0.002(6) 0.006(7) -0.014(7) C55 0.021(6) 0.030(7) 0.021(6) -0.012(5) 0.000(5) -0.015(5) C56 0.024(6) 0.016(6) 0.027(6) -0.009(5) -0.008(5) 0.005(5) C57 0.019(6) 0.010(6) 0.029(6) -0.012(5) -0.002(5) 0.000(5) C58 0.029(7) 0.014(6) 0.025(6) -0.007(5) 0.001(5) -0.003(5) C59 0.023(6) 0.025(7) 0.027(6) -0.008(5) -0.010(5) -0.010(5) C60 0.007(5) 0.033(7) 0.028(6) -0.016(5) -0.001(4) -0.007(5) C61 0.013(6) 0.017(6) 0.037(7) -0.006(5) -0.003(5) -0.012(5) C62 0.036(8) 0.037(8) 0.027(7) 0.000(5) -0.012(6) -0.018(6) C63 0.074(12) 0.100(14) 0.056(10) 0.030(9) -0.039(9) -0.058(11) C64 0.070(13) 0.110(16) 0.058(11) -0.019(10) -0.037(9) 0.021(11) C65 0.090(13) 0.078(12) 0.059(10) 0.000(8) -0.029(9) -0.054(11) C66 0.023(6) 0.022(6) 0.014(5) -0.007(4) 0.001(4) -0.004(5) C67 0.025(6) 0.029(7) 0.013(5) 0.003(5) 0.001(4) -0.022(5) C68 0.013(6) 0.018(6) 0.028(6) -0.004(5) 0.002(5) -0.009(5) C69 0.012(6) 0.030(7) 0.028(6) -0.008(5) 0.004(5) -0.010(5) C70 0.019(4) 0.029(6) 0.027(5) -0.010(4) -0.003(4) -0.005(4) C71 0.018(3) 0.023(4) 0.028(4) -0.007(3) -0.002(3) -0.004(3) C72 0.018(5) 0.017(5) 0.030(5) -0.001(4) -0.003(4) -0.006(4) C73 0.015(6) 0.038(8) 0.045(8) -0.021(6) -0.003(5) -0.013(6) C74 0.048(9) 0.052(10) 0.074(11) -0.024(8) -0.029(8) -0.014(8) C75 0.031(8) 0.071(10) 0.049(8) -0.037(7) 0.003(6) -0.029(7) C76 0.052(10) 0.067(11) 0.089(12) -0.044(9) 0.013(8) -0.045(9) C77 0.023(6) 0.014(6) 0.029(6) -0.007(5) -0.001(5) -0.005(5) C78 0.017(6) 0.018(6) 0.025(6) -0.001(5) -0.001(5) -0.009(5) C79 0.010(5) 0.021(6) 0.025(6) -0.009(5) -0.006(4) -0.001(5) C80 0.030(7) 0.027(7) 0.029(7) -0.013(5) -0.002(5) -0.016(6) C81 0.026(6) 0.051(7) 0.038(5) -0.030(5) 0.010(4) -0.028(5) C82 0.015(6) 0.035(8) 0.030(7) -0.008(5) 0.001(5) -0.006(6) C83 0.012(6) 0.016(6) 0.033(6) -0.006(5) -0.003(5) -0.006(5) C84 0.043(6) 0.068(6) 0.040(5) -0.034(5) 0.015(4) -0.030(5) C85 0.056(8) 0.106(12) 0.038(7) -0.041(8) 0.009(6) -0.038(8) C86 0.070(11) 0.070(7) 0.059(10) -0.050(7) 0.022(8) -0.033(7) C87 0.048(9) 0.082(11) 0.037(9) -0.035(10) 0.023(7) -0.035(9) C85X 0.063(13) 0.084(11) 0.040(7) -0.022(9) 0.020(12) -0.033(11) C86X 0.062(11) 0.082(11) 0.043(11) -0.047(8) 0.010(11) -0.034(9) C87X 0.045(6) 0.087(15) 0.046(13) -0.033(13) 0.028(7) -0.036(10) C88 0.013(6) 0.022(6) 0.028(6) -0.012(5) 0.003(5) -0.005(5) Na1 0.042(3) 0.027(3) 0.032(3) -0.007(2) -0.003(2) -0.014(2) Na2 0.040(3) 0.024(3) 0.045(3) -0.013(2) -0.010(2) -0.007(2) N1 0.067(9) 0.036(7) 0.067(9) -0.001(6) -0.024(7) -0.024(7) C89 0.053(10) 0.038(9) 0.043(9) -0.013(7) -0.005(7) -0.023(8) C90 0.103(15) 0.084(13) 0.055(10) 0.021(9) -0.031(10) -0.040(12) N2 0.032(7) 0.029(7) 0.062(8) 0.002(5) -0.009(6) -0.013(6) C91 0.045(9) 0.033(8) 0.038(8) -0.011(6) 0.006(6) -0.025(7) C92 0.038(9) 0.070(11) 0.057(10) -0.002(8) -0.002(7) -0.029(8) N3 0.054(8) 0.035(7) 0.050(8) 0.000(6) 0.000(6) -0.011(6) C93 0.068(13) 0.064(13) 0.083(14) 0.025(10) -0.018(11) -0.018(10) C94 0.17(3) 0.24(3) 0.062(15) -0.047(17) 0.040(15) 0.04(2) N4 0.037(7) 0.029(7) 0.064(8) -0.003(6) 0.002(6) -0.010(6) C95 0.052(10) 0.046(10) 0.053(9) 0.013(7) -0.013(7) -0.038(8) C96 0.146(18) 0.081(13) 0.051(10) 0.000(9) -0.025(10) -0.081(13) N5 0.066(9) 0.036(7) 0.068(9) -0.021(6) 0.001(7) -0.020(7) C97 0.041(9) 0.045(10) 0.074(12) -0.015(8) -0.010(8) -0.016(8) C98 0.065(12) 0.096(15) 0.105(15) 0.004(11) -0.027(10) -0.054(11) N6 0.095(13) 0.123(16) 0.108(13) -0.080(12) 0.022(9) -0.052(11) C99 0.070(12) 0.080(14) 0.042(9) -0.019(9) 0.022(8) -0.046(10) C100 0.077(12) 0.041(9) 0.049(9) -0.008(7) 0.016(8) -0.023(8) N7 0.113(14) 0.177(19) 0.059(10) -0.029(11) -0.010(9) -0.085(13) C101 0.041(9) 0.075(12) 0.053(10) -0.004(9) -0.013(8) -0.031(9) C102 0.058(10) 0.042(9) 0.044(9) 0.003(7) -0.009(7) -0.022(8) N8 0.099(14) 0.091(13) 0.121(14) -0.015(10) -0.028(11) -0.020(11) C103 0.077(15) 0.053(12) 0.104(15) -0.013(11) -0.024(11) -0.010(11) C104 0.059(14) 0.057(14) 0.23(3) -0.042(15) -0.009(15) -0.008(11) N9 0.038(8) 0.086(11) 0.079(10) -0.022(8) -0.008(7) -0.009(8) C105 0.025(8) 0.053(10) 0.047(9) -0.013(8) 0.010(7) -0.006(7) C106 0.064(11) 0.064(11) 0.058(10) -0.014(8) -0.001(8) -0.030(9) N10 0.077(10) 0.087(12) 0.061(9) -0.031(8) 0.000(7) -0.044(9) C107 0.030(7) 0.063(11) 0.029(7) -0.018(7) 0.005(6) -0.023(8) C108 0.046(9) 0.055(10) 0.069(10) -0.004(8) -0.016(8) -0.024(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 1.965(6) . ? W1 O1 1.986(7) . ? W1 O4 1.995(7) . ? W1 O2 2.008(6) . ? W1 W2 2.2976(6) . ? W2 O7 1.977(7) . ? W2 O8 1.996(6) . ? W2 O6 2.002(7) . ? W2 O5 2.012(7) . ? O1 C1 1.378(11) . ? O2 C12 1.352(11) . ? O2 Na1 2.355(8) . ? O3 C23 1.362(11) . ? O4 C34 1.358(11) . ? O4 Na2 2.282(8) . ? O5 C45 1.341(11) . ? O6 C56 1.381(12) . ? O6 Na2 2.268(8) . ? O7 C67 1.335(11) . ? O8 C78 1.387(11) . ? O8 Na1 2.386(8) . ? C1 C6 1.385(13) . ? C1 C2 1.418(14) . ? C1 Na1 3.130(11) . ? C2 C3 1.409(15) . ? C2 C88 1.498(13) . ? C3 C4 1.394(14) . ? C4 C5 1.403(14) . ? C4 C7 1.518(15) . ? C5 C6 1.383(14) . ? C6 C11 1.507(13) . ? C7 C10 1.511(16) . ? C7 C8 1.515(18) . ? C7 C9 1.535(18) . ? C11 C13 1.513(14) . ? C12 C13 1.429(14) . ? C12 C17 1.432(13) . ? C12 Na1 3.112(11) . ? C13 C14 1.394(13) . ? C14 C15 1.391(14) . ? C15 C16 1.406(14) . ? C15 C18 1.528(14) . ? C16 C17 1.386(13) . ? C17 C22 1.529(13) . ? C18 C21 1.487(16) . ? C18 C20 1.555(16) . ? C18 C19 1.556(16) . ? C22 C24 1.537(13) . ? C23 C24 1.384(14) . ? C23 C28 1.413(14) . ? C24 C25 1.396(13) . ? C25 C26 1.392(14) . ? C26 C27 1.386(15) . ? C26 C29 1.533(14) . ? C27 C28 1.409(14) . ? C28 C33 1.519(14) . ? C29 C32X 1.41(5) . ? C29 C31 1.47(2) . ? C29 C30X 1.51(5) . ? C29 C32 1.52(2) . ? C29 C30 1.59(2) . ? C29 C31X 1.62(5) . ? C33 C35 1.519(14) . ? C34 C39 1.364(13) . ? C34 C35 1.431(13) . ? C35 C36 1.406(14) . ? C36 C37 1.374(14) . ? C37 C38 1.412(13) . ? C37 C40 1.520(14) . ? C38 C39 1.409(14) . ? C39 C44 1.520(13) . ? C40 C42 1.511(15) . ? C40 C43 1.518(14) . ? C40 C41 1.550(16) . ? C44 C46 1.503(13) . ? C45 C50 1.396(13) . ? C45 C46 1.423(13) . ? C45 Na2 2.945(10) . ? C46 C47 1.410(14) . ? C47 C48 1.398(14) . ? C48 C49 1.392(14) . ? C48 C51 1.530(15) . ? C49 C50 1.388(14) . ? C50 C55 1.506(14) . ? C50 Na2 3.059(11) . ? C51 C52 1.516(15) . ? C51 C53 1.524(15) . ? C51 C54 1.549(15) . ? C55 C57 1.470(14) . ? C56 C61 1.384(14) . ? C56 C57 1.394(14) . ? C56 Na2 2.951(12) . ? C57 C58 1.425(14) . ? C58 C59 1.388(14) . ? C59 C60 1.384(14) . ? C59 C62 1.516(14) . ? C60 C61 1.403(13) . ? C61 C66 1.535(13) . ? C62 C63 1.486(16) . ? C62 C64 1.517(18) . ? C62 C65 1.574(17) . ? C66 C68 1.520(14) . ? C67 C68 1.412(14) . ? C67 C72 1.441(14) . ? C68 C69 1.381(14) . ? C69 C70 1.422(14) . ? C70 C71 1.381(14) . ? C70 C73 1.500(15) . ? C71 C72 1.358(14) . ? C72 C77 1.524(14) . ? C73 C75 1.512(15) . ? C73 C74 1.545(16) . ? C73 C76 1.563(16) . ? C77 C79 1.549(14) . ? C78 C79 1.394(14) . ? C78 C83 1.409(14) . ? C79 C80 1.361(13) . ? C80 C81 1.382(15) . ? C81 C82 1.404(15) . ? C81 C84 1.529(15) . ? C82 C83 1.404(14) . ? C83 C88 1.493(14) . ? C84 C87X 1.48(5) . ? C84 C86X 1.51(4) . ? C84 C86 1.51(2) . ? C84 C85 1.52(2) . ? C84 C85X 1.54(5) . ? C84 C87 1.57(2) . ? Na1 N1 2.437(13) . ? Na1 N3 2.449(12) . ? Na1 N2 2.474(12) . ? Na2 N4 2.397(13) . ? Na2 N5 2.469(14) . ? N1 C89 1.137(15) . ? C89 C90 1.432(17) . ? N2 C91 1.122(15) . ? C91 C92 1.474(18) . ? N3 C93 1.177(19) . ? C93 C94 1.46(2) . ? N4 C95 1.102(15) . ? C95 C96 1.444(18) . ? N5 C97 1.135(17) . ? C97 C98 1.46(2) . ? N6 C99 1.120(18) . ? C99 C100 1.48(2) . ? N7 C101 1.137(17) . ? C101 C102 1.446(18) . ? N8 C103 1.45(2) . ? C103 C104 1.08(2) . ? N9 C105 1.122(17) . ? C105 C106 1.433(19) . ? N10 C107 1.126(16) . ? C107 C108 1.431(18) . ? 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 O3 W1 O1 160.8(3) . . ? O3 W1 O4 87.1(3) . . ? O1 W1 O4 95.6(3) . . ? O3 W1 O2 88.8(3) . . ? O1 W1 O2 83.2(3) . . ? O4 W1 O2 163.4(3) . . ? O3 W1 W2 105.94(19) . . ? O1 W1 W2 93.08(19) . . ? O4 W1 W2 90.69(19) . . ? O2 W1 W2 105.95(18) . . ? O7 W2 O8 88.1(3) . . ? O7 W2 O6 87.1(3) . . ? O8 W2 O6 163.3(3) . . ? O7 W2 O5 159.7(3) . . ? O8 W2 O5 97.8(3) . . ? O6 W2 O5 81.7(3) . . ? O7 W2 W1 106.17(19) . . ? O8 W2 W1 92.25(18) . . ? O6 W2 W1 104.49(19) . . ? O5 W2 W1 93.10(18) . . ? C1 O1 W1 139.0(6) . . ? C12 O2 W1 128.9(6) . . ? C12 O2 Na1 111.3(6) . . ? W1 O2 Na1 116.5(3) . . ? C23 O3 W1 129.4(6) . . ? C34 O4 W1 115.4(6) . . ? C34 O4 Na2 117.9(6) . . ? W1 O4 Na2 123.2(3) . . ? C45 O5 W2 140.8(6) . . ? C56 O6 W2 135.4(6) . . ? C56 O6 Na2 105.4(6) . . ? W2 O6 Na2 116.0(3) . . ? C67 O7 W2 125.2(6) . . ? C78 O8 W2 108.6(6) . . ? C78 O8 Na1 126.5(6) . . ? W2 O8 Na1 121.5(3) . . ? O1 C1 C6 117.4(9) . . ? O1 C1 C2 121.5(9) . . ? C6 C1 C2 120.9(9) . . ? O1 C1 Na1 96.5(6) . . ? C6 C1 Na1 83.8(6) . . ? C2 C1 Na1 93.5(6) . . ? C3 C2 C1 115.9(10) . . ? C3 C2 C88 119.3(9) . . ? C1 C2 C88 124.8(10) . . ? C4 C3 C2 125.4(10) . . ? C3 C4 C5 114.9(10) . . ? C3 C4 C7 123.4(10) . . ? C5 C4 C7 121.7(10) . . ? C6 C5 C4 123.1(10) . . ? C5 C6 C1 119.8(9) . . ? C5 C6 C11 119.3(9) . . ? C1 C6 C11 120.6(9) . . ? C10 C7 C8 109.8(12) . . ? C10 C7 C4 113.9(10) . . ? C8 C7 C4 110.4(11) . . ? C10 C7 C9 108.8(12) . . ? C8 C7 C9 106.3(12) . . ? C4 C7 C9 107.4(11) . . ? C6 C11 C13 119.2(9) . . ? O2 C12 C13 122.4(9) . . ? O2 C12 C17 120.6(9) . . ? C13 C12 C17 117.0(9) . . ? O2 C12 Na1 44.8(4) . . ? C13 C12 Na1 104.2(6) . . ? C17 C12 Na1 120.8(7) . . ? C14 C13 C12 119.6(9) . . ? C14 C13 C11 119.1(9) . . ? C12 C13 C11 121.0(9) . . ? C15 C14 C13 122.9(10) . . ? C14 C15 C16 117.3(10) . . ? C14 C15 C18 122.0(10) . . ? C16 C15 C18 120.5(10) . . ? C17 C16 C15 121.8(10) . . ? C16 C17 C12 120.5(9) . . ? C16 C17 C22 120.2(9) . . ? C12 C17 C22 118.7(9) . . ? C21 C18 C15 113.8(10) . . ? C21 C18 C20 108.2(11) . . ? C15 C18 C20 109.7(9) . . ? C21 C18 C19 107.4(10) . . ? C15 C18 C19 109.4(10) . . ? C20 C18 C19 108.1(11) . . ? C17 C22 C24 105.9(8) . . ? O3 C23 C24 120.2(10) . . ? O3 C23 C28 120.6(9) . . ? C24 C23 C28 119.1(9) . . ? C23 C24 C25 120.6(10) . . ? C23 C24 C22 120.0(9) . . ? C25 C24 C22 119.1(9) . . ? C26 C25 C24 121.5(10) . . ? C27 C26 C25 117.6(10) . . ? C27 C26 C29 121.3(10) . . ? C25 C26 C29 121.0(10) . . ? C26 C27 C28 122.4(11) . . ? C27 C28 C23 118.6(10) . . ? C27 C28 C33 119.3(10) . . ? C23 C28 C33 122.0(9) . . ? C32X C29 C30X 112(3) . . ? C31 C29 C32 112.8(13) . . ? C32X C29 C26 111(2) . . ? C31 C29 C26 111.7(12) . . ? C30X C29 C26 112(2) . . ? C32 C29 C26 114.1(11) . . ? C31 C29 C30 105.4(14) . . ? C32 C29 C30 104.2(13) . . ? C26 C29 C30 107.7(11) . . ? C32X C29 C31X 119(3) . . ? C30X C29 C31X 99(3) . . ? C26 C29 C31X 103(2) . . ? C28 C33 C35 118.3(9) . . ? O4 C34 C39 117.5(9) . . ? O4 C34 C35 120.4(9) . . ? C39 C34 C35 121.8(10) . . ? C36 C35 C34 115.9(10) . . ? C36 C35 C33 123.5(9) . . ? C34 C35 C33 120.3(10) . . ? C37 C36 C35 123.7(10) . . ? C36 C37 C38 118.2(10) . . ? C36 C37 C40 118.2(9) . . ? C38 C37 C40 123.5(10) . . ? C39 C38 C37 120.1(10) . . ? C34 C39 C38 119.8(10) . . ? C34 C39 C44 119.1(9) . . ? C38 C39 C44 121.0(9) . . ? C42 C40 C43 109.2(9) . . ? C42 C40 C37 110.7(9) . . ? C43 C40 C37 111.3(10) . . ? C42 C40 C41 108.0(10) . . ? C43 C40 C41 106.4(9) . . ? C37 C40 C41 111.1(9) . . ? C46 C44 C39 113.5(8) . . ? O5 C45 C50 119.2(9) . . ? O5 C45 C46 121.8(9) . . ? C50 C45 C46 119.0(9) . . ? O5 C45 Na2 95.9(5) . . ? C50 C45 Na2 81.1(6) . . ? C46 C45 Na2 94.9(6) . . ? C47 C46 C45 116.9(9) . . ? C47 C46 C44 117.0(10) . . ? C45 C46 C44 126.1(9) . . ? C48 C47 C46 124.6(10) . . ? C49 C48 C47 116.2(10) . . ? C49 C48 C51 123.8(10) . . ? C47 C48 C51 119.7(10) . . ? C50 C49 C48 121.6(10) . . ? C49 C50 C45 121.7(10) . . ? C49 C50 C55 117.0(10) . . ? C45 C50 C55 120.9(9) . . ? C49 C50 Na2 101.9(7) . . ? C45 C50 Na2 72.1(6) . . ? C55 C50 Na2 102.9(6) . . ? C52 C51 C53 108.4(10) . . ? C52 C51 C48 109.1(10) . . ? C53 C51 C48 112.2(10) . . ? C52 C51 C54 109.5(10) . . ? C53 C51 C54 107.0(10) . . ? C48 C51 C54 110.7(9) . . ? C57 C55 C50 120.0(9) . . ? O6 C56 C61 120.1(10) . . ? O6 C56 C57 118.8(10) . . ? C61 C56 C57 121.1(10) . . ? O6 C56 Na2 47.8(5) . . ? C61 C56 Na2 120.4(7) . . ? C57 C56 Na2 99.5(7) . . ? C56 C57 C58 115.4(10) . . ? C56 C57 C55 122.2(10) . . ? C58 C57 C55 122.3(10) . . ? C59 C58 C57 125.0(10) . . ? C60 C59 C58 115.7(10) . . ? C60 C59 C62 121.6(10) . . ? C58 C59 C62 122.7(10) . . ? C59 C60 C61 122.1(10) . . ? C56 C61 C60 119.5(10) . . ? C56 C61 C66 119.7(10) . . ? C60 C61 C66 119.8(9) . . ? C63 C62 C59 115.2(11) . . ? C63 C62 C64 109.4(12) . . ? C59 C62 C64 109.1(10) . . ? C63 C62 C65 106.8(11) . . ? C59 C62 C65 108.8(10) . . ? C64 C62 C65 107.2(13) . . ? C68 C66 C61 105.3(8) . . ? O7 C67 C68 119.4(10) . . ? O7 C67 C72 123.2(10) . . ? C68 C67 C72 117.0(9) . . ? C69 C68 C67 120.1(10) . . ? C69 C68 C66 119.5(9) . . ? C67 C68 C66 119.9(9) . . ? C68 C69 C70 123.3(10) . . ? C71 C70 C69 114.5(10) . . ? C71 C70 C73 124.4(10) . . ? C69 C70 C73 121.1(10) . . ? C72 C71 C70 125.2(11) . . ? C71 C72 C67 119.7(10) . . ? C71 C72 C77 120.8(10) . . ? C67 C72 C77 119.5(9) . . ? C70 C73 C75 114.7(10) . . ? C70 C73 C74 111.5(10) . . ? C75 C73 C74 107.4(10) . . ? C70 C73 C76 108.7(9) . . ? C75 C73 C76 107.8(10) . . ? C74 C73 C76 106.4(10) . . ? C72 C77 C79 118.1(9) . . ? O8 C78 C79 122.2(9) . . ? O8 C78 C83 115.7(9) . . ? C79 C78 C83 122.0(10) . . ? C80 C79 C78 118.3(10) . . ? C80 C79 C77 122.2(10) . . ? C78 C79 C77 119.1(9) . . ? C79 C80 C81 123.5(11) . . ? C80 C81 C82 117.0(10) . . ? C80 C81 C84 122.6(11) . . ? C82 C81 C84 120.5(11) . . ? C83 C82 C81 122.7(11) . . ? C82 C83 C78 116.2(10) . . ? C82 C83 C88 123.6(10) . . ? C78 C83 C88 120.0(9) . . ? C87X C84 C86X 114(3) . . ? C86 C84 C85 110.8(15) . . ? C87X C84 C81 114(2) . . ? C86X C84 C81 115.2(19) . . ? C86 C84 C81 109.0(13) . . ? C85 C84 C81 108.4(12) . . ? C87X C84 C85X 102(3) . . ? C86X C84 C85X 105(3) . . ? C81 C84 C85X 105(2) . . ? C86 C84 C87 108.9(14) . . ? C85 C84 C87 106.7(15) . . ? C81 C84 C87 113.0(12) . . ? C83 C88 C2 116.2(9) . . ? O2 Na1 O8 85.1(3) . . ? O2 Na1 N1 97.1(3) . . ? O8 Na1 N1 162.6(4) . . ? O2 Na1 N3 165.8(4) . . ? O8 Na1 N3 85.8(3) . . ? N1 Na1 N3 88.5(4) . . ? O2 Na1 N2 89.8(3) . . ? O8 Na1 N2 102.9(3) . . ? N1 Na1 N2 94.3(4) . . ? N3 Na1 N2 102.9(4) . . ? O2 Na1 C12 23.9(2) . . ? O8 Na1 C12 108.1(3) . . ? N1 Na1 C12 73.2(3) . . ? N3 Na1 C12 158.0(4) . . ? N2 Na1 C12 90.8(3) . . ? O2 Na1 C1 65.8(3) . . ? O8 Na1 C1 62.6(3) . . ? N1 Na1 C1 102.5(4) . . ? N3 Na1 C1 100.3(4) . . ? N2 Na1 C1 151.7(3) . . ? C12 Na1 C1 72.8(3) . . ? O6 Na2 O4 86.6(3) . . ? O6 Na2 N4 170.2(4) . . ? O4 Na2 N4 99.4(4) . . ? O6 Na2 N5 89.4(3) . . ? O4 Na2 N5 118.0(4) . . ? N4 Na2 N5 94.7(4) . . ? O6 Na2 C45 69.7(3) . . ? O4 Na2 C45 65.8(3) . . ? N4 Na2 C45 105.5(4) . . ? N5 Na2 C45 158.8(4) . . ? O6 Na2 C56 26.8(2) . . ? O4 Na2 C56 113.0(3) . . ? N4 Na2 C56 145.4(4) . . ? N5 Na2 C56 81.0(4) . . ? C45 Na2 C56 78.7(3) . . ? O6 Na2 C50 69.4(3) . . ? O4 Na2 C50 92.6(3) . . ? N4 Na2 C50 102.3(4) . . ? N5 Na2 C50 142.1(4) . . ? C45 Na2 C50 26.8(3) . . ? C56 Na2 C50 65.8(3) . . ? C89 N1 Na1 167.5(11) . . ? N1 C89 C90 178.8(16) . . ? C91 N2 Na1 141.4(10) . . ? N2 C91 C92 177.3(14) . . ? C93 N3 Na1 154.9(12) . . ? N3 C93 C94 178(2) . . ? C95 N4 Na2 153.0(12) . . ? N4 C95 C96 179.3(18) . . ? C97 N5 Na2 132.0(12) . . ? N5 C97 C98 180(2) . . ? N6 C99 C100 178.5(18) . . ? N7 C101 C102 177.1(17) . . ? C104 C103 N8 177(3) . . ? N9 C105 C106 177.9(17) . . ? N10 C107 C108 179.4(15) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 4.076 _refine_diff_density_min -2.184 _refine_diff_density_rms 0.207 #===END data_3.4MeCN _database_code_CSD 181733 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H116 Cl10 N4 O8 W3' _chemical_formula_weight 2359.98 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' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 15.880(2) _cell_length_b 32.197(5) _cell_length_c 20.141(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.955(3) _cell_angle_gamma 90.00 _cell_volume 10143(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 19137 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 27.42 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4704 _exptl_absorpt_coefficient_mu 3.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.781 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.6928 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 17 _diffrn_reflns_number 56311 _diffrn_reflns_av_R_equivalents 0.1414 _diffrn_reflns_av_sigmaI/netI 0.1235 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 22.50 _reflns_number_total 14555 _reflns_number_gt 9795 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1087P)^2^+290.4081P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14555 _refine_ls_number_parameters 1119 _refine_ls_number_restraints 1081 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.2416 _refine_ls_wR_factor_gt 0.2173 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.46443(5) 0.90627(2) 0.38249(4) 0.0216(2) Uani 1 1 d U . . Cl1 Cl 0.4904(3) 0.9053(2) 0.5010(2) 0.0452(15) Uani 1 1 d U . . Cl2 Cl 0.3201(3) 0.91242(19) 0.3776(3) 0.0395(13) Uani 1 1 d U . . Cl3 Cl 0.4678(4) 0.97896(17) 0.3902(3) 0.0462(14) Uani 1 1 d U . . Cl4 Cl 0.4502(4) 0.83555(16) 0.3869(3) 0.0452(14) Uani 1 1 d U . . W2 W 0.79796(5) 0.76999(2) 0.36335(4) 0.0198(2) Uani 1 1 d U . . Cl5 Cl 0.8078(4) 0.74129(19) 0.2593(3) 0.0428(14) Uani 1 1 d U . . Cl6 Cl 0.6979(3) 0.81800(16) 0.3112(2) 0.0292(11) Uani 1 1 d U . . Cl7 Cl 0.9102(4) 0.81389(19) 0.3512(3) 0.0529(16) Uani 1 1 d U . . W3 W 0.26099(5) 0.74249(3) 0.27961(4) 0.0214(2) Uani 1 1 d U . . Cl8 Cl 0.1410(3) 0.74550(19) 0.1932(3) 0.0410(14) Uani 1 1 d U . . Cl9 Cl 0.3473(3) 0.73079(16) 0.1965(2) 0.0302(11) Uani 1 1 d U . . Cl10 Cl 0.2358(3) 0.67170(16) 0.2860(3) 0.0359(12) Uani 1 1 d U . . O1 O 0.4536(7) 0.9035(4) 0.2894(6) 0.025(3) Uani 1 1 d U . . O2 O 0.5798(7) 0.9054(4) 0.3852(6) 0.024(2) Uani 1 1 d U . . O3 O 0.7953(7) 0.7950(4) 0.4445(6) 0.022(2) Uani 1 1 d U . . O4 O 0.8776(7) 0.7314(4) 0.4039(6) 0.026(2) Uani 1 1 d U . . O5 O 0.7137(7) 0.7319(4) 0.3716(6) 0.021(2) Uani 1 1 d U . . O6 O 0.3557(7) 0.7382(4) 0.3463(6) 0.020(2) Uani 1 1 d U . . O7 O 0.1922(7) 0.7525(4) 0.3448(6) 0.026(3) Uani 1 1 d U . . O8 O 0.2688(8) 0.7978(4) 0.2692(6) 0.025(2) Uani 1 1 d U . . C1 C 0.4831(11) 0.9024(6) 0.2297(9) 0.022(3) Uani 1 1 d U . . C2 C 0.4435(11) 0.8743(6) 0.1813(9) 0.024(3) Uani 1 1 d U . . C3 C 0.4624(11) 0.8760(6) 0.1181(9) 0.025(3) Uani 1 1 d U . . H3 H 0.4338 0.8576 0.0848 0.030 Uiso 1 1 calc R . . C4 C 0.5233(12) 0.9041(7) 0.1001(10) 0.033(3) Uani 1 1 d U . . C5 C 0.5673(11) 0.9287(6) 0.1534(10) 0.028(3) Uani 1 1 d U . . H5 H 0.6122 0.9462 0.1445 0.033 Uiso 1 1 calc R . . C6 C 0.5479(11) 0.9285(6) 0.2177(10) 0.025(3) Uani 1 1 d U . . C7 C 0.5331(15) 0.9093(8) 0.0260(11) 0.046(3) Uani 1 1 d U . . C8 C 0.4434(15) 0.9238(9) -0.0119(12) 0.064(5) Uani 1 1 d U . . H8A H 0.4249 0.9482 0.0108 0.096 Uiso 1 1 calc R . . H8B H 0.4019 0.9013 -0.0117 0.096 Uiso 1 1 calc R . . H8C H 0.4474 0.9309 -0.0586 0.096 Uiso 1 1 calc R . . C9 C 0.5950(16) 0.9415(8) 0.0151(11) 0.055(5) Uani 1 1 d U . . H9A H 0.6508 0.9352 0.0424 0.083 Uiso 1 1 calc R . . H9B H 0.5752 0.9686 0.0283 0.083 Uiso 1 1 calc R . . H9C H 0.6003 0.9421 -0.0327 0.083 Uiso 1 1 calc R . . C10 C 0.5555(18) 0.8690(8) -0.0008(13) 0.062(5) Uani 1 1 d U . . H10A H 0.5496 0.8708 -0.0500 0.093 Uiso 1 1 calc R . . H10B H 0.5171 0.8475 0.0111 0.093 Uiso 1 1 calc R . . H10C H 0.6147 0.8620 0.0186 0.093 Uiso 1 1 calc R . . C11 C 0.5958(12) 0.9576(6) 0.2702(10) 0.025(4) Uani 1 1 d U . . H11A H 0.5541 0.9693 0.2965 0.029 Uiso 1 1 calc R . . H11B H 0.6176 0.9810 0.2462 0.029 Uiso 1 1 calc R . . C12 C 0.6596(10) 0.9142(6) 0.3743(8) 0.020(3) Uani 1 1 d U . . C13 C 0.6711(11) 0.9398(6) 0.3203(9) 0.021(4) Uani 1 1 d U . . C14 C 0.7531(11) 0.9522(5) 0.3162(9) 0.017(3) Uani 1 1 d U . . H14 H 0.7619 0.9702 0.2806 0.021 Uiso 1 1 calc R . . C15 C 0.8236(11) 0.9392(6) 0.3629(10) 0.024(4) Uani 1 1 d U . . C16 C 0.8089(11) 0.9109(6) 0.4140(10) 0.024(4) Uani 1 1 d U . . H16 H 0.8565 0.9009 0.4451 0.029 Uiso 1 1 calc R . . C17 C 0.7276(11) 0.8975(6) 0.4202(9) 0.021(4) Uani 1 1 d U . . C18 C 0.9128(12) 0.9575(7) 0.3643(11) 0.035(4) Uani 1 1 d U . . C19 C 0.9157(15) 0.9864(8) 0.3039(13) 0.056(6) Uani 1 1 d U . . H19A H 0.8880 0.9727 0.2624 0.084 Uiso 1 1 calc R . . H19B H 0.9753 0.9926 0.3009 0.084 Uiso 1 1 calc R . . H19C H 0.8855 1.0123 0.3101 0.084 Uiso 1 1 calc R . . C20 C 0.9744(12) 0.9224(7) 0.3623(13) 0.047(5) Uani 1 1 d U . . H20A H 0.9529 0.8974 0.3817 0.070 Uiso 1 1 calc R . . H20B H 1.0302 0.9299 0.3884 0.070 Uiso 1 1 calc R . . H20C H 0.9802 0.9169 0.3155 0.070 Uiso 1 1 calc R . . C21 C 0.9381(16) 0.9811(8) 0.4298(12) 0.056(6) Uani 1 1 d U . . H21A H 0.9001 1.0051 0.4303 0.085 Uiso 1 1 calc R . . H21B H 0.9973 0.9907 0.4337 0.085 Uiso 1 1 calc R . . H21C H 0.9331 0.9628 0.4678 0.085 Uiso 1 1 calc R . . C22 C 0.7079(11) 0.8676(6) 0.4722(9) 0.022(3) Uani 1 1 d U . . H22A H 0.6757 0.8439 0.4490 0.026 Uiso 1 1 calc R . . H22B H 0.6701 0.8815 0.4996 0.026 Uiso 1 1 calc R . . C23 C 0.8271(11) 0.8161(6) 0.5028(9) 0.021(3) Uani 1 1 d U . . C24 C 0.7856(11) 0.8507(6) 0.5195(9) 0.019(3) Uani 1 1 d U . . C25 C 0.8129(12) 0.8714(6) 0.5796(9) 0.023(3) Uani 1 1 d U . . H25 H 0.7835 0.8956 0.5902 0.028 Uiso 1 1 calc R . . C26 C 0.8847(12) 0.8567(6) 0.6254(10) 0.026(4) Uani 1 1 d U . . C27 C 0.9243(11) 0.8214(6) 0.6076(9) 0.022(4) Uani 1 1 d U . . H27 H 0.9716 0.8110 0.6385 0.027 Uiso 1 1 calc R . . C28 C 0.9003(11) 0.8002(6) 0.5486(8) 0.019(3) Uani 1 1 d U . . C29 C 0.9127(12) 0.8803(6) 0.6894(9) 0.027(4) Uani 1 1 d U . . C30 C 0.8376(14) 0.8926(7) 0.7245(11) 0.044(5) Uani 1 1 d U . . H30A H 0.8075 0.9164 0.7013 0.067 Uiso 1 1 calc R . . H30B H 0.8595 0.8999 0.7716 0.067 Uiso 1 1 calc R . . H30C H 0.7980 0.8691 0.7231 0.067 Uiso 1 1 calc R . . C31 C 0.9633(16) 0.9194(7) 0.6755(12) 0.054(6) Uani 1 1 d U . . H31A H 1.0105 0.9114 0.6527 0.081 Uiso 1 1 calc R . . H31B H 0.9862 0.9331 0.7182 0.081 Uiso 1 1 calc R . . H31C H 0.9252 0.9386 0.6467 0.081 Uiso 1 1 calc R . . C32 C 0.9742(15) 0.8531(7) 0.7407(11) 0.046(6) Uani 1 1 d U . . H32A H 0.9439 0.8282 0.7517 0.069 Uiso 1 1 calc R . . H32B H 0.9933 0.8692 0.7819 0.069 Uiso 1 1 calc R . . H32C H 1.0238 0.8450 0.7208 0.069 Uiso 1 1 calc R . . C33 C 0.9498(11) 0.7638(6) 0.5302(10) 0.027(3) Uani 1 1 d U . . H33A H 1.0024 0.7612 0.5644 0.032 Uiso 1 1 calc R . . H33B H 0.9678 0.7700 0.4865 0.032 Uiso 1 1 calc R . . C34 C 0.8700(11) 0.7059(6) 0.4605(9) 0.023(3) Uani 1 1 d U . . C35 C 0.9046(11) 0.7219(6) 0.5241(10) 0.027(3) Uani 1 1 d U . . C36 C 0.8944(12) 0.6971(6) 0.5771(10) 0.030(4) Uani 1 1 d U . . H36 H 0.9151 0.7072 0.6213 0.036 Uiso 1 1 calc R . . C37 C 0.8561(12) 0.6587(6) 0.5709(10) 0.027(3) Uani 1 1 d U . . C38 C 0.8225(11) 0.6447(6) 0.5068(9) 0.024(3) Uani 1 1 d U . . H38 H 0.7934 0.6188 0.5018 0.028 Uiso 1 1 calc R . . C39 C 0.8302(11) 0.6676(6) 0.4492(9) 0.023(3) Uani 1 1 d U . . C40 C 0.8492(14) 0.6300(7) 0.6334(11) 0.042(4) Uani 1 1 d U . . C41 C 0.927(2) 0.6392(13) 0.6874(16) 0.125(13) Uani 1 1 d U . . H41A H 0.9732 0.6504 0.6661 0.187 Uiso 1 1 calc R . . H41B H 0.9463 0.6134 0.7113 0.187 Uiso 1 1 calc R . . H41C H 0.9116 0.6595 0.7194 0.187 Uiso 1 1 calc R . . C42 C 0.850(3) 0.5862(8) 0.6147(15) 0.112(12) Uani 1 1 d U . . H42A H 0.8451 0.5689 0.6539 0.168 Uiso 1 1 calc R . . H42B H 0.9040 0.5798 0.5993 0.168 Uiso 1 1 calc R . . H42C H 0.8022 0.5804 0.5783 0.168 Uiso 1 1 calc R . . C43 C 0.7713(19) 0.6405(10) 0.6596(15) 0.086(9) Uani 1 1 d U . . H43A H 0.7215 0.6368 0.6239 0.128 Uiso 1 1 calc R . . H43B H 0.7743 0.6695 0.6747 0.128 Uiso 1 1 calc R . . H43C H 0.7662 0.6223 0.6976 0.128 Uiso 1 1 calc R . . C44 C 0.7992(11) 0.6522(6) 0.3787(9) 0.022(4) Uani 1 1 d U . . H44A H 0.8113 0.6221 0.3777 0.026 Uiso 1 1 calc R . . H44B H 0.8333 0.6660 0.3484 0.026 Uiso 1 1 calc R . . C45 C 0.6641(11) 0.6967(5) 0.3491(8) 0.016(2) Uani 1 1 d U . . C46 C 0.7060(11) 0.6586(5) 0.3502(8) 0.017(2) Uani 1 1 d U . . C47 C 0.6562(12) 0.6248(6) 0.3250(8) 0.021(3) Uani 1 1 d U . . H47 H 0.6825 0.5982 0.3253 0.025 Uiso 1 1 calc R . . C48 C 0.5679(12) 0.6283(6) 0.2989(8) 0.021(2) Uani 1 1 d U . . C49 C 0.5312(12) 0.6669(5) 0.3028(8) 0.019(2) Uani 1 1 d U . . H49 H 0.4715 0.6699 0.2873 0.022 Uiso 1 1 calc R . . C50 C 0.5772(11) 0.7008(6) 0.3281(8) 0.018(2) Uani 1 1 d U . . C51 C 0.5220(13) 0.5910(6) 0.2631(10) 0.031(3) Uani 1 1 d U . . C52 C 0.538(2) 0.5883(10) 0.1922(13) 0.095(10) Uani 1 1 d U . . H52A H 0.4992 0.5679 0.1672 0.143 Uiso 1 1 calc R . . H52B H 0.5974 0.5798 0.1925 0.143 Uiso 1 1 calc R . . H52C H 0.5282 0.6155 0.1705 0.143 Uiso 1 1 calc R . . C53 C 0.5468(17) 0.5508(7) 0.2999(15) 0.068(8) Uani 1 1 d U . . H53A H 0.5401 0.5537 0.3471 0.102 Uiso 1 1 calc R . . H53B H 0.6065 0.5443 0.2976 0.102 Uiso 1 1 calc R . . H53C H 0.5099 0.5284 0.2788 0.102 Uiso 1 1 calc R . . C54 C 0.4274(15) 0.5944(9) 0.2639(18) 0.089(10) Uani 1 1 d U . . H54A H 0.3994 0.6089 0.2233 0.134 Uiso 1 1 calc R . . H54B H 0.4184 0.6101 0.3039 0.134 Uiso 1 1 calc R . . H54C H 0.4029 0.5666 0.2652 0.134 Uiso 1 1 calc R . . C55 C 0.5314(11) 0.7416(6) 0.3369(9) 0.019(3) Uani 1 1 d U . . H55A H 0.5714 0.7650 0.3358 0.023 Uiso 1 1 calc R . . H55B H 0.4831 0.7452 0.2990 0.023 Uiso 1 1 calc R . . C56 C 0.4124(11) 0.7389(6) 0.4055(9) 0.018(2) Uani 1 1 d U . . C57 C 0.4990(11) 0.7421(6) 0.4010(9) 0.019(2) Uani 1 1 d U . . C58 C 0.5556(11) 0.7457(5) 0.4632(9) 0.019(2) Uani 1 1 d U . . H58 H 0.6152 0.7469 0.4625 0.022 Uiso 1 1 calc R . . C59 C 0.5287(11) 0.7477(6) 0.5251(9) 0.021(2) Uani 1 1 d U . . C60 C 0.4408(11) 0.7412(6) 0.5248(9) 0.021(3) Uani 1 1 d U . . H60 H 0.4213 0.7395 0.5667 0.025 Uiso 1 1 calc R . . C61 C 0.3819(11) 0.7373(6) 0.4660(9) 0.019(2) Uani 1 1 d U . . C62 C 0.5908(12) 0.7560(6) 0.5913(9) 0.026(3) Uani 1 1 d U . . C63 C 0.6910(14) 0.7510(8) 0.5841(16) 0.068(8) Uani 1 1 d U . . H63A H 0.7113 0.7769 0.5669 0.102 Uiso 1 1 calc R . . H63B H 0.6967 0.7283 0.5527 0.102 Uiso 1 1 calc R . . H63C H 0.7250 0.7447 0.6283 0.102 Uiso 1 1 calc R . . C64 C 0.5733(16) 0.7258(7) 0.6452(10) 0.046(6) Uani 1 1 d U . . H64A H 0.6088 0.7331 0.6885 0.069 Uiso 1 1 calc R . . H64B H 0.5871 0.6975 0.6326 0.069 Uiso 1 1 calc R . . H64C H 0.5128 0.7273 0.6494 0.069 Uiso 1 1 calc R . . C65 C 0.5754(16) 0.7994(7) 0.6134(11) 0.046(5) Uani 1 1 d U . . H65A H 0.5899 0.8192 0.5802 0.070 Uiso 1 1 calc R . . H65B H 0.6112 0.8048 0.6573 0.070 Uiso 1 1 calc R . . H65C H 0.5151 0.8026 0.6172 0.070 Uiso 1 1 calc R . . C66 C 0.2875(11) 0.7320(6) 0.4713(9) 0.021(3) Uani 1 1 d U . . H66A H 0.2611 0.7113 0.4376 0.025 Uiso 1 1 calc R . . H66B H 0.2830 0.7212 0.5166 0.025 Uiso 1 1 calc R . . C67 C 0.1933(11) 0.7832(6) 0.3923(9) 0.022(3) Uani 1 1 d U . . C68 C 0.2396(11) 0.7725(6) 0.4596(10) 0.024(3) Uani 1 1 d U . . C69 C 0.2406(12) 0.8029(6) 0.5071(10) 0.026(4) Uani 1 1 d U . . H69 H 0.2696 0.7973 0.5515 0.031 Uiso 1 1 calc R . . C70 C 0.2017(12) 0.8419(6) 0.4945(10) 0.025(3) Uani 1 1 d U . . C71 C 0.1601(11) 0.8495(6) 0.4287(9) 0.024(3) Uani 1 1 d U . . H71 H 0.1319 0.8753 0.4190 0.029 Uiso 1 1 calc R . . C72 C 0.1582(11) 0.8208(6) 0.3766(9) 0.022(2) Uani 1 1 d U . . C73 C 0.2039(14) 0.8735(6) 0.5512(10) 0.033(4) Uani 1 1 d U . . C74 C 0.2979(19) 0.8810(11) 0.5841(18) 0.100(11) Uani 1 1 d U . . H74A H 0.3279 0.8951 0.5519 0.151 Uiso 1 1 calc R . . H74B H 0.3256 0.8543 0.5969 0.151 Uiso 1 1 calc R . . H74C H 0.2998 0.8983 0.6243 0.151 Uiso 1 1 calc R . . C75 C 0.162(2) 0.8560(10) 0.6074(15) 0.093(10) Uani 1 1 d U . . H75A H 0.1497 0.8786 0.6367 0.139 Uiso 1 1 calc R . . H75B H 0.2014 0.8362 0.6339 0.139 Uiso 1 1 calc R . . H75C H 0.1092 0.8418 0.5881 0.139 Uiso 1 1 calc R . . C76 C 0.165(3) 0.9141(8) 0.5264(15) 0.102(11) Uani 1 1 d U . . H76A H 0.1777 0.9198 0.4814 0.153 Uiso 1 1 calc R . . H76B H 0.1887 0.9363 0.5574 0.153 Uiso 1 1 calc R . . H76C H 0.1029 0.9129 0.5242 0.153 Uiso 1 1 calc R . . C77 C 0.1130(11) 0.8308(6) 0.3075(9) 0.025(3) Uani 1 1 d U . . H77A H 0.0611 0.8472 0.3106 0.030 Uiso 1 1 calc R . . H77B H 0.0946 0.8046 0.2835 0.030 Uiso 1 1 calc R . . C78 C 0.2437(11) 0.8379(6) 0.2502(9) 0.018(3) Uani 1 1 d U . . C79 C 0.1690(11) 0.8552(6) 0.2667(9) 0.023(3) Uani 1 1 d U . . C80 C 0.1478(12) 0.8959(6) 0.2477(9) 0.028(3) Uani 1 1 d U . . H80 H 0.0981 0.9078 0.2602 0.034 Uiso 1 1 calc R . . C81 C 0.1965(12) 0.9202(7) 0.2109(10) 0.031(3) Uani 1 1 d U . . C82 C 0.2723(11) 0.9018(6) 0.1952(10) 0.028(3) Uani 1 1 d U . . H82 H 0.3078 0.9174 0.1710 0.033 Uiso 1 1 calc R . . C83 C 0.2950(11) 0.8615(6) 0.2146(10) 0.025(4) Uani 1 1 d U . . C84 C 0.1761(14) 0.9657(7) 0.1901(12) 0.042(4) Uani 1 1 d U . . C85 C 0.0948(19) 0.9806(9) 0.2113(18) 0.087(9) Uani 1 1 d U . . H85A H 0.1029 0.9821 0.2606 0.130 Uiso 1 1 calc R . . H85B H 0.0483 0.9612 0.1948 0.130 Uiso 1 1 calc R . . H85C H 0.0803 1.0083 0.1923 0.130 Uiso 1 1 calc R . . C86 C 0.165(3) 0.9680(11) 0.1138(16) 0.128(13) Uani 1 1 d U . . H86A H 0.1840 0.9952 0.1005 0.192 Uiso 1 1 calc R . . H86B H 0.1040 0.9644 0.0946 0.192 Uiso 1 1 calc R . . H86C H 0.1982 0.9461 0.0971 0.192 Uiso 1 1 calc R . . C87 C 0.248(2) 0.9939(10) 0.222(2) 0.127(13) Uani 1 1 d U . . H87A H 0.2510 0.9938 0.2710 0.191 Uiso 1 1 calc R . . H87B H 0.2364 1.0222 0.2048 0.191 Uiso 1 1 calc R . . H87C H 0.3018 0.9841 0.2107 0.191 Uiso 1 1 calc R . . C88 C 0.3787(12) 0.8431(6) 0.1985(10) 0.027(4) Uani 1 1 d U . . H88A H 0.4061 0.8266 0.2379 0.033 Uiso 1 1 calc R . . H88B H 0.3641 0.8237 0.1601 0.033 Uiso 1 1 calc R . . N1 N 0.241(2) 0.6335(10) 0.5220(15) 0.100(9) Uani 1 1 d U . . C89 C 0.183(2) 0.6440(11) 0.5451(18) 0.086(10) Uani 1 1 d U . . C90 C 0.115(2) 0.6604(12) 0.5744(18) 0.104(12) Uani 1 1 d U . . H90A H 0.1219 0.6522 0.6219 0.156 Uiso 1 1 calc R . . H90B H 0.0601 0.6495 0.5504 0.156 Uiso 1 1 calc R . . H90C H 0.1145 0.6908 0.5712 0.156 Uiso 1 1 calc R . . N2 N 1.013(2) 0.6137(14) 0.425(2) 0.143(14) Uani 1 1 d U . . C91 C 1.033(2) 0.6479(15) 0.4112(13) 0.083(10) Uani 1 1 d U . . C92 C 1.063(2) 0.6903(14) 0.396(2) 0.120(13) Uani 1 1 d U . . H92A H 1.0604 0.7087 0.4347 0.180 Uiso 1 1 calc R . . H92B H 1.0264 0.7014 0.3560 0.180 Uiso 1 1 calc R . . H92C H 1.1221 0.6887 0.3884 0.180 Uiso 1 1 calc R . . N3 N 0.187(3) 1.0085(13) 0.411(2) 0.142(14) Uani 1 1 d U . . C93 C 0.245(3) 1.0081(10) 0.4494(19) 0.085(10) Uani 1 1 d U . . C94 C 0.3208(18) 1.0050(9) 0.5016(17) 0.076(9) Uani 1 1 d U . . H94A H 0.3039 1.0051 0.5461 0.114 Uiso 1 1 calc R . . H94B H 0.3585 1.0287 0.4980 0.114 Uiso 1 1 calc R . . H94C H 0.3512 0.9791 0.4956 0.114 Uiso 1 1 calc R . . N4 N 0.276(2) 0.9884(9) -0.1610(15) 0.105(10) Uani 1 1 d U . . C95 C 0.241(3) 0.9630(11) -0.144(2) 0.112(13) Uani 1 1 d U . . C96 C 0.191(4) 0.9279(15) -0.120(3) 0.20(2) Uani 1 1 d U . . H96A H 0.1347 0.9383 -0.1132 0.305 Uiso 1 1 calc R . . H96B H 0.2219 0.9173 -0.0769 0.305 Uiso 1 1 calc R . . H96C H 0.1829 0.9055 -0.1532 0.305 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 W1 0.0091(4) 0.0386(5) 0.0187(4) 0.0038(3) 0.0067(3) 0.0029(3) Cl1 0.029(3) 0.103(5) 0.003(2) 0.001(2) 0.000(2) 0.000(3) Cl2 0.009(2) 0.080(4) 0.030(3) -0.012(3) 0.005(2) 0.001(2) Cl3 0.048(4) 0.039(3) 0.057(4) -0.006(3) 0.025(3) 0.000(3) Cl4 0.057(4) 0.033(3) 0.052(4) 0.009(2) 0.026(3) 0.001(3) W2 0.0070(4) 0.0389(5) 0.0135(4) -0.0005(3) 0.0016(3) -0.0030(3) Cl5 0.044(4) 0.070(4) 0.017(3) 0.000(2) 0.014(2) 0.014(3) Cl6 0.023(3) 0.045(3) 0.017(3) 0.003(2) -0.004(2) -0.001(2) Cl7 0.026(3) 0.064(4) 0.072(4) 0.009(3) 0.018(3) -0.016(3) W3 0.0051(4) 0.0427(5) 0.0155(4) -0.0012(3) -0.0005(3) -0.0025(3) Cl8 0.016(3) 0.071(4) 0.031(3) -0.006(3) -0.011(2) -0.004(2) Cl9 0.019(3) 0.053(3) 0.018(3) -0.008(2) 0.0023(19) -0.004(2) Cl10 0.032(3) 0.037(3) 0.040(3) -0.003(2) 0.009(2) -0.007(2) O1 0.005(6) 0.063(7) 0.010(4) 0.005(4) 0.006(4) 0.001(6) O2 0.003(4) 0.058(7) 0.011(5) 0.010(5) 0.003(4) 0.005(4) O3 0.007(6) 0.033(7) 0.022(5) -0.008(4) -0.007(4) -0.003(5) O4 0.002(5) 0.052(5) 0.022(5) 0.000(4) -0.006(4) 0.000(4) O5 0.007(5) 0.033(5) 0.023(7) -0.006(5) 0.005(5) -0.003(4) O6 0.002(5) 0.045(7) 0.011(5) 0.004(5) 0.000(4) -0.002(5) O7 0.006(6) 0.048(6) 0.024(5) -0.005(5) 0.004(4) 0.003(5) O8 0.024(3) 0.026(2) 0.024(3) -0.0005(10) 0.0042(10) 0.0003(10) C1 0.006(6) 0.043(7) 0.019(5) 0.008(5) 0.010(4) 0.005(4) C2 0.003(5) 0.047(7) 0.023(5) 0.005(5) 0.007(4) 0.005(4) C3 0.003(6) 0.052(7) 0.022(4) 0.003(5) 0.004(5) 0.003(4) C4 0.013(6) 0.059(7) 0.030(4) 0.007(4) 0.013(4) -0.001(5) C5 0.008(6) 0.046(7) 0.033(5) 0.011(5) 0.014(4) -0.002(5) C6 0.008(6) 0.041(7) 0.029(5) 0.010(5) 0.009(4) 0.004(4) C7 0.036(7) 0.076(8) 0.032(4) 0.007(5) 0.019(5) -0.007(6) C8 0.042(8) 0.120(15) 0.035(9) 0.048(11) 0.022(7) -0.003(8) C9 0.057(10) 0.091(11) 0.019(10) 0.013(9) 0.009(9) -0.025(10) C10 0.068(13) 0.086(10) 0.037(10) -0.010(9) 0.026(11) -0.011(9) C11 0.018(7) 0.027(9) 0.031(8) 0.017(6) 0.009(6) 0.000(6) C12 0.003(4) 0.048(8) 0.009(7) 0.002(5) -0.001(5) -0.002(6) C13 0.008(6) 0.026(9) 0.030(9) 0.009(6) 0.005(5) 0.002(6) C14 0.012(6) 0.027(10) 0.012(9) -0.004(6) 0.003(6) -0.003(7) C15 0.012(6) 0.031(10) 0.029(10) 0.001(7) -0.001(6) -0.003(6) C16 0.006(6) 0.035(10) 0.030(10) 0.005(7) -0.002(7) 0.001(7) C17 0.005(6) 0.041(10) 0.015(8) 0.002(6) -0.002(6) -0.002(7) C18 0.012(6) 0.052(10) 0.038(9) 0.008(7) -0.005(7) -0.010(6) C19 0.029(11) 0.079(13) 0.056(11) 0.029(9) -0.001(10) -0.015(9) C20 0.008(8) 0.057(10) 0.074(12) 0.007(8) 0.004(9) -0.010(7) C21 0.037(14) 0.079(17) 0.050(11) -0.014(10) -0.002(11) -0.027(11) C22 0.015(6) 0.031(8) 0.019(6) 0.001(5) 0.001(5) -0.001(5) C23 0.009(7) 0.030(7) 0.021(6) -0.003(5) -0.003(5) -0.005(5) C24 0.010(6) 0.032(6) 0.017(5) 0.000(4) 0.003(4) -0.004(4) C25 0.016(7) 0.032(8) 0.020(6) -0.002(5) 0.001(5) -0.002(6) C26 0.016(9) 0.031(9) 0.026(8) -0.010(6) -0.009(6) -0.012(6) C27 0.009(9) 0.046(10) 0.011(8) -0.003(6) -0.001(6) 0.000(7) C28 0.005(8) 0.040(8) 0.011(8) -0.002(6) 0.000(5) -0.002(6) C29 0.028(10) 0.040(10) 0.013(8) -0.001(6) 0.006(6) -0.006(7) C30 0.035(11) 0.060(15) 0.040(13) -0.001(10) 0.009(9) 0.017(10) C31 0.064(16) 0.049(12) 0.049(15) -0.025(9) 0.011(12) -0.036(11) C32 0.041(13) 0.060(13) 0.032(11) -0.019(9) -0.010(9) 0.020(10) C33 0.007(7) 0.048(7) 0.021(8) -0.008(6) -0.011(6) 0.007(5) C34 0.005(6) 0.044(6) 0.019(5) -0.003(4) -0.004(5) 0.006(5) C35 0.008(7) 0.045(7) 0.024(6) -0.007(5) -0.006(6) 0.010(6) C36 0.017(10) 0.047(9) 0.023(7) -0.008(6) -0.006(8) 0.009(7) C37 0.014(7) 0.045(7) 0.021(4) -0.003(5) -0.003(6) 0.013(6) C38 0.005(6) 0.043(6) 0.021(5) -0.002(4) -0.004(5) 0.010(5) C39 0.006(6) 0.041(6) 0.021(5) -0.004(4) -0.002(5) 0.009(5) C40 0.036(11) 0.062(10) 0.026(8) 0.008(8) -0.004(8) 0.003(10) C41 0.083(16) 0.21(3) 0.062(18) 0.079(19) -0.050(15) -0.07(2) C42 0.24(4) 0.055(10) 0.044(18) 0.027(10) 0.024(19) 0.044(17) C43 0.073(15) 0.13(2) 0.07(2) 0.041(17) 0.044(13) 0.026(17) C44 0.015(7) 0.036(10) 0.016(7) -0.006(7) 0.006(7) 0.005(6) C45 0.015(4) 0.032(4) 0.002(6) -0.001(5) 0.004(5) -0.003(3) C46 0.017(5) 0.031(5) 0.004(6) 0.001(5) 0.006(5) -0.004(3) C47 0.022(5) 0.034(5) 0.006(6) -0.005(5) 0.000(5) -0.003(4) C48 0.022(5) 0.034(4) 0.006(6) -0.002(5) -0.002(5) -0.006(4) C49 0.017(5) 0.035(5) 0.003(6) 0.000(5) 0.002(5) -0.006(3) C50 0.016(4) 0.034(5) 0.004(6) 0.000(5) -0.001(5) -0.004(4) C51 0.029(7) 0.037(5) 0.024(7) -0.006(6) -0.005(6) -0.008(6) C52 0.14(3) 0.11(2) 0.027(10) -0.041(10) -0.005(14) -0.04(2) C53 0.059(16) 0.035(9) 0.097(18) 0.004(11) -0.021(16) -0.010(11) C54 0.019(8) 0.09(2) 0.15(3) -0.04(2) -0.028(12) -0.008(9) C55 0.004(6) 0.036(6) 0.016(4) -0.003(6) -0.003(4) -0.003(5) C56 0.006(4) 0.033(7) 0.015(4) -0.004(6) -0.002(3) 0.000(5) C57 0.006(4) 0.033(6) 0.017(4) -0.002(5) -0.001(3) -0.001(5) C58 0.003(4) 0.036(7) 0.016(4) -0.003(6) 0.000(3) 0.004(6) C59 0.007(4) 0.041(6) 0.016(4) -0.002(5) 0.001(3) 0.003(5) C60 0.008(4) 0.040(7) 0.014(4) 0.001(6) 0.001(3) 0.002(6) C61 0.008(4) 0.032(6) 0.016(4) 0.003(5) -0.001(3) 0.001(5) C62 0.011(5) 0.052(8) 0.015(4) -0.003(6) 0.002(4) -0.005(7) C63 0.014(8) 0.075(17) 0.11(2) -0.009(16) -0.005(9) -0.014(10) C64 0.056(14) 0.057(12) 0.016(9) 0.006(9) -0.016(9) -0.008(12) C65 0.056(15) 0.050(9) 0.026(12) -0.005(8) -0.014(11) -0.004(10) C66 0.010(4) 0.035(7) 0.017(7) 0.004(6) 0.001(4) -0.004(6) C67 0.011(7) 0.036(6) 0.022(6) 0.005(4) 0.012(5) 0.002(5) C68 0.003(7) 0.040(8) 0.029(7) 0.002(6) 0.005(6) 0.002(6) C69 0.012(9) 0.042(8) 0.025(8) 0.005(6) 0.006(7) 0.005(7) C70 0.016(7) 0.039(7) 0.024(5) 0.002(5) 0.011(5) -0.002(6) C71 0.010(6) 0.039(6) 0.026(5) 0.002(4) 0.011(5) 0.004(5) C72 0.008(5) 0.037(5) 0.023(4) 0.005(3) 0.010(4) 0.003(4) C73 0.043(11) 0.034(9) 0.024(8) -0.002(7) 0.012(8) -0.004(9) C74 0.052(13) 0.11(2) 0.13(3) -0.08(2) -0.002(12) -0.012(13) C75 0.14(2) 0.10(2) 0.065(18) -0.009(14) 0.08(2) 0.000(19) C76 0.19(3) 0.052(13) 0.053(18) -0.010(10) -0.021(19) 0.042(18) C77 0.009(7) 0.046(7) 0.023(5) 0.006(5) 0.011(5) 0.008(6) C78 0.007(7) 0.037(6) 0.010(8) -0.006(7) 0.003(6) -0.006(6) C79 0.004(8) 0.046(8) 0.021(9) 0.002(7) 0.008(7) 0.000(6) C80 0.012(7) 0.054(7) 0.023(8) 0.004(6) 0.011(6) 0.007(6) C81 0.010(6) 0.052(6) 0.032(7) 0.007(5) 0.009(5) 0.003(4) C82 0.006(6) 0.050(7) 0.029(8) 0.009(7) 0.007(6) 0.000(5) C83 0.007(7) 0.044(8) 0.026(10) 0.005(8) 0.008(7) -0.002(6) C84 0.023(8) 0.054(7) 0.052(9) 0.012(7) 0.017(7) 0.008(5) C85 0.060(14) 0.079(18) 0.13(2) 0.008(19) 0.052(18) 0.029(13) C86 0.22(4) 0.11(2) 0.066(11) 0.044(13) 0.057(17) 0.10(2) C87 0.075(17) 0.073(15) 0.23(3) 0.02(2) 0.01(2) -0.039(17) C88 0.019(9) 0.047(10) 0.019(10) -0.002(8) 0.012(7) -0.001(5) N1 0.09(2) 0.13(2) 0.08(2) 0.018(17) 0.026(15) 0.038(18) C89 0.07(2) 0.10(2) 0.10(2) 0.029(19) 0.036(17) 0.010(17) C90 0.06(2) 0.15(3) 0.10(3) -0.03(2) 0.007(17) 0.02(2) N2 0.09(2) 0.19(3) 0.16(3) 0.05(3) 0.07(2) 0.03(2) C91 0.07(2) 0.17(3) 0.014(14) -0.006(18) 0.014(13) 0.02(2) C92 0.04(2) 0.19(3) 0.13(3) -0.01(3) 0.01(2) -0.01(2) N3 0.14(3) 0.15(3) 0.12(3) -0.01(3) -0.022(19) 0.02(3) C93 0.09(2) 0.071(19) 0.09(3) -0.018(19) 0.020(14) 0.01(2) C94 0.050(16) 0.070(19) 0.11(2) -0.043(18) 0.033(13) -0.023(15) N4 0.13(3) 0.08(2) 0.10(2) 0.036(17) 0.011(19) -0.025(16) C95 0.12(3) 0.07(2) 0.15(3) 0.01(2) 0.04(2) -0.028(19) C96 0.21(5) 0.14(4) 0.27(6) 0.04(4) 0.07(4) -0.09(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 W1 O2 1.824(11) . ? W1 O1 1.856(11) . ? W1 Cl2 2.286(5) . ? W1 Cl4 2.291(5) . ? W1 Cl3 2.345(6) . ? W1 Cl1 2.352(5) . ? W2 O3 1.830(12) . ? W2 O5 1.845(11) . ? W2 O4 1.858(12) . ? W2 Cl5 2.321(5) . ? W2 Cl7 2.321(5) . ? W2 Cl6 2.332(5) . ? W3 O8 1.799(12) . ? W3 O6 1.841(11) . ? W3 O7 1.875(12) . ? W3 Cl10 2.321(5) . ? W3 Cl8 2.351(5) . ? W3 Cl9 2.370(5) . ? O1 C1 1.36(2) . ? O2 C12 1.35(2) . ? O3 C23 1.37(2) . ? O4 C34 1.43(2) . ? O5 C45 1.41(2) . ? O6 C56 1.36(2) . ? O7 C67 1.37(2) . ? O8 C78 1.39(2) . ? C1 C6 1.38(3) . ? C1 C2 1.40(3) . ? C2 C3 1.36(3) . ? C2 C88 1.52(3) . ? C3 C4 1.42(3) . ? C4 C5 1.42(3) . ? C4 C7 1.54(3) . ? C5 C6 1.38(3) . ? C6 C11 1.52(3) . ? C7 C10 1.47(3) . ? C7 C9 1.47(3) . ? C7 C8 1.57(3) . ? C11 C13 1.54(2) . ? C12 C13 1.40(2) . ? C12 C17 1.40(2) . ? C13 C14 1.38(2) . ? C14 C15 1.40(2) . ? C15 C16 1.42(3) . ? C15 C18 1.53(3) . ? C16 C17 1.39(2) . ? C17 C22 1.50(2) . ? C18 C20 1.50(3) . ? C18 C21 1.52(3) . ? C18 C19 1.54(3) . ? C22 C24 1.52(2) . ? C23 C24 1.36(3) . ? C23 C28 1.45(2) . ? C24 C25 1.38(3) . ? C25 C26 1.42(3) . ? C26 C27 1.38(3) . ? C26 C29 1.50(3) . ? C27 C28 1.37(2) . ? C28 C33 1.49(3) . ? C29 C30 1.54(3) . ? C29 C31 1.55(3) . ? C29 C32 1.56(3) . ? C33 C35 1.52(3) . ? C34 C39 1.39(3) . ? C34 C35 1.40(3) . ? C35 C36 1.37(3) . ? C36 C37 1.38(3) . ? C37 C38 1.39(3) . ? C37 C40 1.58(3) . ? C38 C39 1.40(3) . ? C39 C44 1.50(2) . ? C40 C42 1.46(3) . ? C40 C43 1.47(3) . ? C40 C41 1.53(3) . ? C44 C46 1.51(2) . ? C45 C50 1.38(2) . ? C45 C46 1.39(2) . ? C46 C47 1.39(2) . ? C47 C48 1.41(3) . ? C48 C49 1.38(3) . ? C48 C51 1.52(3) . ? C49 C50 1.36(2) . ? C50 C55 1.53(2) . ? C51 C52 1.50(3) . ? C51 C53 1.51(3) . ? C51 C54 1.51(3) . ? C55 C57 1.47(2) . ? C56 C61 1.39(3) . ? C56 C57 1.40(2) . ? C57 C58 1.41(2) . ? C58 C59 1.39(3) . ? C59 C60 1.41(2) . ? C59 C62 1.54(3) . ? C60 C61 1.38(2) . ? C61 C66 1.53(2) . ? C62 C65 1.50(3) . ? C62 C64 1.52(3) . ? C62 C63 1.63(3) . ? C66 C68 1.51(3) . ? C67 C72 1.35(3) . ? C67 C68 1.47(3) . ? C68 C69 1.37(3) . ? C69 C70 1.40(3) . ? C70 C71 1.40(3) . ? C70 C73 1.52(3) . ? C71 C72 1.39(3) . ? C72 C77 1.49(3) . ? C73 C76 1.50(3) . ? C73 C75 1.51(3) . ? C73 C74 1.54(3) . ? C77 C79 1.53(2) . ? C78 C83 1.40(2) . ? C78 C79 1.40(2) . ? C79 C80 1.39(3) . ? C80 C81 1.40(3) . ? C81 C82 1.43(3) . ? C81 C84 1.54(3) . ? C82 C83 1.38(3) . ? C83 C88 1.54(3) . ? C84 C85 1.51(3) . ? C84 C87 1.51(4) . ? C84 C86 1.52(4) . ? N1 C89 1.16(4) . ? C89 C90 1.43(4) . ? N2 C91 1.19(5) . ? C91 C92 1.50(5) . ? N3 C93 1.09(4) . ? C93 C94 1.46(4) . ? N4 C95 1.08(4) . ? C95 C96 1.52(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 W1 O1 87.0(5) . . ? O2 W1 Cl2 175.8(4) . . ? O1 W1 Cl2 92.4(4) . . ? O2 W1 Cl4 95.1(4) . . ? O1 W1 Cl4 89.9(4) . . ? Cl2 W1 Cl4 89.0(2) . . ? O2 W1 Cl3 90.1(4) . . ? O1 W1 Cl3 96.4(4) . . ? Cl2 W1 Cl3 85.9(2) . . ? Cl4 W1 Cl3 172.0(2) . . ? O2 W1 Cl1 88.3(4) . . ? O1 W1 Cl1 174.2(4) . . ? Cl2 W1 Cl1 92.50(19) . . ? Cl4 W1 Cl1 87.1(2) . . ? Cl3 W1 Cl1 87.0(2) . . ? O3 W2 O5 94.8(5) . . ? O3 W2 O4 91.2(5) . . ? O5 W2 O4 88.0(5) . . ? O3 W2 Cl5 176.4(4) . . ? O5 W2 Cl5 88.8(4) . . ? O4 W2 Cl5 89.0(4) . . ? O3 W2 Cl7 87.9(4) . . ? O5 W2 Cl7 175.8(4) . . ? O4 W2 Cl7 88.7(4) . . ? Cl5 W2 Cl7 88.5(2) . . ? O3 W2 Cl6 89.5(4) . . ? O5 W2 Cl6 91.9(4) . . ? O4 W2 Cl6 179.3(4) . . ? Cl5 W2 Cl6 90.22(18) . . ? Cl7 W2 Cl6 91.4(2) . . ? O8 W3 O6 95.5(5) . . ? O8 W3 O7 88.4(6) . . ? O6 W3 O7 90.2(5) . . ? O8 W3 Cl10 173.6(4) . . ? O6 W3 Cl10 90.7(4) . . ? O7 W3 Cl10 90.2(4) . . ? O8 W3 Cl8 86.3(4) . . ? O6 W3 Cl8 177.9(4) . . ? O7 W3 Cl8 90.9(4) . . ? Cl10 W3 Cl8 87.5(2) . . ? O8 W3 Cl9 90.8(4) . . ? O6 W3 Cl9 90.3(4) . . ? O7 W3 Cl9 179.2(4) . . ? Cl10 W3 Cl9 90.52(18) . . ? Cl8 W3 Cl9 88.68(18) . . ? C1 O1 W1 154.9(11) . . ? C12 O2 W1 163.0(12) . . ? C23 O3 W2 156.8(11) . . ? C34 O4 W2 126.1(10) . . ? C45 O5 W2 151.7(11) . . ? C56 O6 W3 165.7(11) . . ? C67 O7 W3 132.2(11) . . ? C78 O8 W3 158.8(11) . . ? O1 C1 C6 121.2(17) . . ? O1 C1 C2 116.7(15) . . ? C6 C1 C2 122.1(17) . . ? C3 C2 C1 118.8(17) . . ? C3 C2 C88 120.6(18) . . ? C1 C2 C88 120.6(16) . . ? C2 C3 C4 122.5(19) . . ? C3 C4 C5 115.6(17) . . ? C3 C4 C7 120.4(19) . . ? C5 C4 C7 123.7(18) . . ? C6 C5 C4 123.0(17) . . ? C1 C6 C5 117.5(18) . . ? C1 C6 C11 123.6(17) . . ? C5 C6 C11 118.9(16) . . ? C10 C7 C9 111(2) . . ? C10 C7 C4 109(2) . . ? C9 C7 C4 114(2) . . ? C10 C7 C8 110(2) . . ? C9 C7 C8 107(2) . . ? C4 C7 C8 105.6(17) . . ? C6 C11 C13 117.8(15) . . ? O2 C12 C13 120.0(15) . . ? O2 C12 C17 116.7(15) . . ? C13 C12 C17 123.3(16) . . ? C14 C13 C12 118.0(16) . . ? C14 C13 C11 119.2(16) . . ? C12 C13 C11 122.6(15) . . ? C13 C14 C15 121.8(17) . . ? C14 C15 C16 117.9(16) . . ? C14 C15 C18 121.9(17) . . ? C16 C15 C18 119.9(16) . . ? C17 C16 C15 122.4(17) . . ? C16 C17 C12 116.3(16) . . ? C16 C17 C22 125.0(16) . . ? C12 C17 C22 118.6(15) . . ? C20 C18 C21 109.1(19) . . ? C20 C18 C15 108.4(17) . . ? C21 C18 C15 108.3(18) . . ? C20 C18 C19 109(2) . . ? C21 C18 C19 110(2) . . ? C15 C18 C19 111.8(16) . . ? C17 C22 C24 115.1(15) . . ? C24 C23 O3 119.5(16) . . ? C24 C23 C28 120.0(16) . . ? O3 C23 C28 120.3(16) . . ? C23 C24 C25 121.2(17) . . ? C23 C24 C22 120.6(16) . . ? C25 C24 C22 118.2(16) . . ? C24 C25 C26 120.1(17) . . ? C27 C26 C25 117.4(17) . . ? C27 C26 C29 124.3(17) . . ? C25 C26 C29 118.3(17) . . ? C28 C27 C26 124.6(17) . . ? C27 C28 C23 116.7(16) . . ? C27 C28 C33 121.9(16) . . ? C23 C28 C33 121.3(15) . . ? C26 C29 C30 112.8(17) . . ? C26 C29 C31 110.2(16) . . ? C30 C29 C31 110.0(18) . . ? C26 C29 C32 110.1(16) . . ? C30 C29 C32 106.5(16) . . ? C31 C29 C32 107.0(18) . . ? C28 C33 C35 116.9(16) . . ? C39 C34 C35 125.0(19) . . ? C39 C34 O4 118.6(16) . . ? C35 C34 O4 116.3(17) . . ? C36 C35 C34 114.7(19) . . ? C36 C35 C33 125.0(17) . . ? C34 C35 C33 120.3(18) . . ? C35 C36 C37 124.5(19) . . ? C36 C37 C38 118.0(19) . . ? C36 C37 C40 123.0(18) . . ? C38 C37 C40 119.1(18) . . ? C37 C38 C39 121.9(19) . . ? C34 C39 C38 115.8(17) . . ? C34 C39 C44 121.0(17) . . ? C38 C39 C44 123.2(18) . . ? C42 C40 C43 111(3) . . ? C42 C40 C41 109(3) . . ? C43 C40 C41 109(3) . . ? C42 C40 C37 111(2) . . ? C43 C40 C37 109.3(19) . . ? C41 C40 C37 107.2(19) . . ? C39 C44 C46 117.1(15) . . ? C50 C45 C46 122.6(16) . . ? C50 C45 O5 119.8(16) . . ? C46 C45 O5 117.6(15) . . ? C47 C46 C45 116.4(17) . . ? C47 C46 C44 119.4(16) . . ? C45 C46 C44 124.2(16) . . ? C46 C47 C48 122.5(17) . . ? C49 C48 C47 116.9(16) . . ? C49 C48 C51 124.4(17) . . ? C47 C48 C51 118.4(17) . . ? C50 C49 C48 122.6(18) . . ? C49 C50 C45 118.8(17) . . ? C49 C50 C55 119.8(16) . . ? C45 C50 C55 121.2(16) . . ? C52 C51 C53 110(2) . . ? C52 C51 C54 110(2) . . ? C53 C51 C54 104(2) . . ? C52 C51 C48 110.5(19) . . ? C53 C51 C48 112.4(17) . . ? C54 C51 C48 109.4(18) . . ? C57 C55 C50 111.0(15) . . ? O6 C56 C61 119.3(15) . . ? O6 C56 C57 116.9(15) . . ? C61 C56 C57 123.8(16) . . ? C56 C57 C58 115.5(16) . . ? C56 C57 C55 123.6(16) . . ? C58 C57 C55 120.9(16) . . ? C59 C58 C57 123.6(16) . . ? C58 C59 C60 116.5(16) . . ? C58 C59 C62 122.4(16) . . ? C60 C59 C62 121.0(16) . . ? C61 C60 C59 122.7(17) . . ? C60 C61 C56 117.5(16) . . ? C60 C61 C66 118.4(16) . . ? C56 C61 C66 124.1(16) . . ? C65 C62 C64 109.0(18) . . ? C65 C62 C59 107.9(16) . . ? C64 C62 C59 109.8(16) . . ? C65 C62 C63 109.4(18) . . ? C64 C62 C63 107.5(19) . . ? C59 C62 C63 113.2(17) . . ? C68 C66 C61 111.4(15) . . ? C72 C67 O7 121.9(17) . . ? C72 C67 C68 123.1(18) . . ? O7 C67 C68 114.9(16) . . ? C69 C68 C67 115.1(17) . . ? C69 C68 C66 124.4(17) . . ? C67 C68 C66 120.3(17) . . ? C68 C69 C70 124.2(19) . . ? C71 C70 C69 116.6(18) . . ? C71 C70 C73 122.8(18) . . ? C69 C70 C73 120.6(18) . . ? C72 C71 C70 123.0(18) . . ? C67 C72 C71 117.7(18) . . ? C67 C72 C77 121.7(18) . . ? C71 C72 C77 120.5(17) . . ? C76 C73 C75 112(2) . . ? C76 C73 C70 112.2(19) . . ? C75 C73 C70 110.8(19) . . ? C76 C73 C74 109(2) . . ? C75 C73 C74 105(2) . . ? C70 C73 C74 108.7(19) . . ? C72 C77 C79 112.5(15) . . ? O8 C78 C83 118.9(15) . . ? O8 C78 C79 121.3(15) . . ? C83 C78 C79 119.8(17) . . ? C80 C79 C78 118.9(16) . . ? C80 C79 C77 119.9(16) . . ? C78 C79 C77 121.2(17) . . ? C79 C80 C81 122.9(17) . . ? C80 C81 C82 116.8(18) . . ? C80 C81 C84 124.4(17) . . ? C82 C81 C84 118.7(17) . . ? C83 C82 C81 121.0(17) . . ? C82 C83 C78 120.5(17) . . ? C82 C83 C88 119.6(16) . . ? C78 C83 C88 119.9(17) . . ? C85 C84 C87 108(3) . . ? C85 C84 C86 108(2) . . ? C87 C84 C86 111(3) . . ? C85 C84 C81 112.1(19) . . ? C87 C84 C81 110(2) . . ? C86 C84 C81 108(2) . . ? C2 C88 C83 115.8(16) . . ? N1 C89 C90 175(4) . . ? N2 C91 C92 177(4) . . ? N3 C93 C94 177(5) . . ? N4 C95 C96 179(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 W1 O1 C1 -3(3) . . . . ? Cl2 W1 O1 C1 173(3) . . . . ? Cl4 W1 O1 C1 -98(3) . . . . ? Cl3 W1 O1 C1 87(3) . . . . ? Cl1 W1 O1 C1 -39(6) . . . . ? O1 W1 O2 C12 53(4) . . . . ? Cl2 W1 O2 C12 -29(9) . . . . ? Cl4 W1 O2 C12 142(4) . . . . ? Cl3 W1 O2 C12 -44(4) . . . . ? Cl1 W1 O2 C12 -131(4) . . . . ? O5 W2 O3 C23 150(3) . . . . ? O4 W2 O3 C23 62(3) . . . . ? Cl5 W2 O3 C23 -32(9) . . . . ? Cl7 W2 O3 C23 -27(3) . . . . ? Cl6 W2 O3 C23 -118(3) . . . . ? O3 W2 O4 C34 52.5(14) . . . . ? O5 W2 O4 C34 -42.3(13) . . . . ? Cl5 W2 O4 C34 -131.1(13) . . . . ? Cl7 W2 O4 C34 140.3(13) . . . . ? Cl6 W2 O4 C34 -125(34) . . . . ? O3 W2 O5 C45 -173(2) . . . . ? O4 W2 O5 C45 -82(2) . . . . ? Cl5 W2 O5 C45 7(2) . . . . ? Cl7 W2 O5 C45 -44(7) . . . . ? Cl6 W2 O5 C45 97(2) . . . . ? O8 W3 O6 C56 77(5) . . . . ? O7 W3 O6 C56 -11(5) . . . . ? Cl10 W3 O6 C56 -102(5) . . . . ? Cl8 W3 O6 C56 -132(9) . . . . ? Cl9 W3 O6 C56 168(5) . . . . ? O8 W3 O7 C67 -35.3(15) . . . . ? O6 W3 O7 C67 60.2(15) . . . . ? Cl10 W3 O7 C67 151.0(15) . . . . ? Cl8 W3 O7 C67 -121.6(15) . . . . ? Cl9 W3 O7 C67 -63(30) . . . . ? O6 W3 O8 C78 -161(3) . . . . ? O7 W3 O8 C78 -71(3) . . . . ? Cl10 W3 O8 C78 6(6) . . . . ? Cl8 W3 O8 C78 20(3) . . . . ? Cl9 W3 O8 C78 108(3) . . . . ? W1 O1 C1 C6 -44(4) . . . . ? W1 O1 C1 C2 138(2) . . . . ? O1 C1 C2 C3 171.0(16) . . . . ? C6 C1 C2 C3 -8(3) . . . . ? O1 C1 C2 C88 -7(3) . . . . ? C6 C1 C2 C88 174.0(17) . . . . ? C1 C2 C3 C4 2(3) . . . . ? C88 C2 C3 C4 -179.1(18) . . . . ? C2 C3 C4 C5 4(3) . . . . ? C2 C3 C4 C7 -171.1(19) . . . . ? C3 C4 C5 C6 -6(3) . . . . ? C7 C4 C5 C6 169.2(19) . . . . ? O1 C1 C6 C5 -172.7(16) . . . . ? C2 C1 C6 C5 6(3) . . . . ? O1 C1 C6 C11 5(3) . . . . ? C2 C1 C6 C11 -176.4(17) . . . . ? C4 C5 C6 C1 1(3) . . . . ? C4 C5 C6 C11 -176.9(18) . . . . ? C3 C4 C7 C10 -59(3) . . . . ? C5 C4 C7 C10 127(2) . . . . ? C3 C4 C7 C9 176(2) . . . . ? C5 C4 C7 C9 2(3) . . . . ? C3 C4 C7 C8 59(3) . . . . ? C5 C4 C7 C8 -115(2) . . . . ? C1 C6 C11 C13 84(2) . . . . ? C5 C6 C11 C13 -99(2) . . . . ? W1 O2 C12 C13 -14(5) . . . . ? W1 O2 C12 C17 164(3) . . . . ? O2 C12 C13 C14 171.8(16) . . . . ? C17 C12 C13 C14 -7(3) . . . . ? O2 C12 C13 C11 -2(3) . . . . ? C17 C12 C13 C11 179.6(18) . . . . ? C6 C11 C13 C14 110.9(19) . . . . ? C6 C11 C13 C12 -75(2) . . . . ? C12 C13 C14 C15 2(3) . . . . ? C11 C13 C14 C15 175.8(17) . . . . ? C13 C14 C15 C16 3(3) . . . . ? C13 C14 C15 C18 -171.5(18) . . . . ? C14 C15 C16 C17 -3(3) . . . . ? C18 C15 C16 C17 171.7(18) . . . . ? C15 C16 C17 C12 -2(3) . . . . ? C15 C16 C17 C22 179.4(18) . . . . ? O2 C12 C17 C16 -171.9(16) . . . . ? C13 C12 C17 C16 6(3) . . . . ? O2 C12 C17 C22 7(3) . . . . ? C13 C12 C17 C22 -174.6(18) . . . . ? C14 C15 C18 C20 -128(2) . . . . ? C16 C15 C18 C20 58(2) . . . . ? C14 C15 C18 C21 114(2) . . . . ? C16 C15 C18 C21 -60(2) . . . . ? C14 C15 C18 C19 -7(3) . . . . ? C16 C15 C18 C19 179(2) . . . . ? C16 C17 C22 C24 -2(3) . . . . ? C12 C17 C22 C24 179.5(16) . . . . ? W2 O3 C23 C24 129(3) . . . . ? W2 O3 C23 C28 -56(4) . . . . ? O3 C23 C24 C25 176.4(16) . . . . ? C28 C23 C24 C25 1(3) . . . . ? O3 C23 C24 C22 -4(3) . . . . ? C28 C23 C24 C22 -179.3(16) . . . . ? C17 C22 C24 C23 -88(2) . . . . ? C17 C22 C24 C25 92(2) . . . . ? C23 C24 C25 C26 -1(3) . . . . ? C22 C24 C25 C26 179.6(16) . . . . ? C24 C25 C26 C27 0(3) . . . . ? C24 C25 C26 C29 179.3(17) . . . . ? C25 C26 C27 C28 1(3) . . . . ? C29 C26 C27 C28 -178.4(18) . . . . ? C26 C27 C28 C23 -1(3) . . . . ? C26 C27 C28 C33 175.4(19) . . . . ? C24 C23 C28 C27 0(3) . . . . ? O3 C23 C28 C27 -175.6(16) . . . . ? C24 C23 C28 C33 -176.7(17) . . . . ? O3 C23 C28 C33 8(3) . . . . ? C27 C26 C29 C30 -135(2) . . . . ? C25 C26 C29 C30 45(2) . . . . ? C27 C26 C29 C31 102(2) . . . . ? C25 C26 C29 C31 -78(2) . . . . ? C27 C26 C29 C32 -16(3) . . . . ? C25 C26 C29 C32 164.1(18) . . . . ? C27 C28 C33 C35 116(2) . . . . ? C23 C28 C33 C35 -68(2) . . . . ? W2 O4 C34 C39 88.7(18) . . . . ? W2 O4 C34 C35 -91.8(17) . . . . ? C39 C34 C35 C36 -2(3) . . . . ? O4 C34 C35 C36 178.6(15) . . . . ? C39 C34 C35 C33 177.7(17) . . . . ? O4 C34 C35 C33 -2(2) . . . . ? C28 C33 C35 C36 -79(2) . . . . ? C28 C33 C35 C34 101(2) . . . . ? C34 C35 C36 C37 2(3) . . . . ? C33 C35 C36 C37 -177.5(18) . . . . ? C35 C36 C37 C38 -3(3) . . . . ? C35 C36 C37 C40 177.1(18) . . . . ? C36 C37 C38 C39 3(3) . . . . ? C40 C37 C38 C39 -176.8(17) . . . . ? C35 C34 C39 C38 2(3) . . . . ? O4 C34 C39 C38 -178.2(14) . . . . ? C35 C34 C39 C44 -176.7(17) . . . . ? O4 C34 C39 C44 3(2) . . . . ? C37 C38 C39 C34 -3(3) . . . . ? C37 C38 C39 C44 176.2(17) . . . . ? C36 C37 C40 C42 -150(3) . . . . ? C38 C37 C40 C42 30(3) . . . . ? C36 C37 C40 C43 88(3) . . . . ? C38 C37 C40 C43 -93(3) . . . . ? C36 C37 C40 C41 -31(3) . . . . ? C38 C37 C40 C41 149(2) . . . . ? C34 C39 C44 C46 -97(2) . . . . ? C38 C39 C44 C46 84(2) . . . . ? W2 O5 C45 C50 -115(2) . . . . ? W2 O5 C45 C46 66(3) . . . . ? C50 C45 C46 C47 4(2) . . . . ? O5 C45 C46 C47 -177.2(14) . . . . ? C50 C45 C46 C44 -174.1(16) . . . . ? O5 C45 C46 C44 5(2) . . . . ? C39 C44 C46 C47 -125.7(18) . . . . ? C39 C44 C46 C45 52(2) . . . . ? C45 C46 C47 C48 1(2) . . . . ? C44 C46 C47 C48 178.5(16) . . . . ? C46 C47 C48 C49 -4(3) . . . . ? C46 C47 C48 C51 171.0(16) . . . . ? C47 C48 C49 C50 2(3) . . . . ? C51 C48 C49 C50 -171.8(17) . . . . ? C48 C49 C50 C45 2(3) . . . . ? C48 C49 C50 C55 -174.5(16) . . . . ? C46 C45 C50 C49 -5(3) . . . . ? O5 C45 C50 C49 176.1(15) . . . . ? C46 C45 C50 C55 171.3(15) . . . . ? O5 C45 C50 C55 -8(2) . . . . ? C49 C48 C51 C52 94(3) . . . . ? C47 C48 C51 C52 -80(3) . . . . ? C49 C48 C51 C53 -142(2) . . . . ? C47 C48 C51 C53 43(3) . . . . ? C49 C48 C51 C54 -28(3) . . . . ? C47 C48 C51 C54 158(2) . . . . ? C49 C50 C55 C57 83.9(19) . . . . ? C45 C50 C55 C57 -92.1(19) . . . . ? W3 O6 C56 C61 25(6) . . . . ? W3 O6 C56 C57 -154(4) . . . . ? O6 C56 C57 C58 175.7(15) . . . . ? C61 C56 C57 C58 -3(3) . . . . ? O6 C56 C57 C55 -5(3) . . . . ? C61 C56 C57 C55 176.7(17) . . . . ? C50 C55 C57 C56 -108(2) . . . . ? C50 C55 C57 C58 72(2) . . . . ? C56 C57 C58 C59 -3(3) . . . . ? C55 C57 C58 C59 178.0(18) . . . . ? C57 C58 C59 C60 7(3) . . . . ? C57 C58 C59 C62 -173.6(18) . . . . ? C58 C59 C60 C61 -6(3) . . . . ? C62 C59 C60 C61 174.1(18) . . . . ? C59 C60 C61 C56 2(3) . . . . ? C59 C60 C61 C66 -177.8(17) . . . . ? O6 C56 C61 C60 -175.3(16) . . . . ? C57 C56 C61 C60 3(3) . . . . ? O6 C56 C61 C66 4(3) . . . . ? C57 C56 C61 C66 -177.4(17) . . . . ? C58 C59 C62 C65 107(2) . . . . ? C60 C59 C62 C65 -73(2) . . . . ? C58 C59 C62 C64 -134(2) . . . . ? C60 C59 C62 C64 45(3) . . . . ? C58 C59 C62 C63 -14(3) . . . . ? C60 C59 C62 C63 165.4(19) . . . . ? C60 C61 C66 C68 99(2) . . . . ? C56 C61 C66 C68 -80(2) . . . . ? W3 O7 C67 C72 81(2) . . . . ? W3 O7 C67 C68 -95.5(18) . . . . ? C72 C67 C68 C69 4(3) . . . . ? O7 C67 C68 C69 -179.8(15) . . . . ? C72 C67 C68 C66 -171.7(17) . . . . ? O7 C67 C68 C66 5(2) . . . . ? C61 C66 C68 C69 -80(2) . . . . ? C61 C66 C68 C67 95(2) . . . . ? C67 C68 C69 C70 0(3) . . . . ? C66 C68 C69 C70 174.6(17) . . . . ? C68 C69 C70 C71 0(3) . . . . ? C68 C69 C70 C73 178.2(18) . . . . ? C69 C70 C71 C72 -2(3) . . . . ? C73 C70 C71 C72 179.8(17) . . . . ? O7 C67 C72 C71 178.0(15) . . . . ? C68 C67 C72 C71 -6(3) . . . . ? O7 C67 C72 C77 3(3) . . . . ? C68 C67 C72 C77 178.9(16) . . . . ? C70 C71 C72 C67 5(3) . . . . ? C70 C71 C72 C77 -179.8(17) . . . . ? C71 C70 C73 C76 -6(3) . . . . ? C69 C70 C73 C76 176(2) . . . . ? C71 C70 C73 C75 119(2) . . . . ? C69 C70 C73 C75 -59(3) . . . . ? C71 C70 C73 C74 -126(2) . . . . ? C69 C70 C73 C74 55(3) . . . . ? C67 C72 C77 C79 -100(2) . . . . ? C71 C72 C77 C79 85(2) . . . . ? W3 O8 C78 C83 -130(3) . . . . ? W3 O8 C78 C79 51(4) . . . . ? O8 C78 C79 C80 178.7(16) . . . . ? C83 C78 C79 C80 0(3) . . . . ? O8 C78 C79 C77 1(3) . . . . ? C83 C78 C79 C77 -178.0(17) . . . . ? C72 C77 C79 C80 -114(2) . . . . ? C72 C77 C79 C78 64(2) . . . . ? C78 C79 C80 C81 2(3) . . . . ? C77 C79 C80 C81 179.5(18) . . . . ? C79 C80 C81 C82 -2(3) . . . . ? C79 C80 C81 C84 -179(2) . . . . ? C80 C81 C82 C83 1(3) . . . . ? C84 C81 C82 C83 177.8(19) . . . . ? C81 C82 C83 C78 0(3) . . . . ? C81 C82 C83 C88 -178.4(18) . . . . ? O8 C78 C83 C82 -179.6(17) . . . . ? C79 C78 C83 C82 -1(3) . . . . ? O8 C78 C83 C88 -1(3) . . . . ? C79 C78 C83 C88 177.9(17) . . . . ? C80 C81 C84 C85 -3(3) . . . . ? C82 C81 C84 C85 -179(2) . . . . ? C80 C81 C84 C87 118(3) . . . . ? C82 C81 C84 C87 -59(3) . . . . ? C80 C81 C84 C86 -122(3) . . . . ? C82 C81 C84 C86 62(3) . . . . ? C3 C2 C88 C83 -113(2) . . . . ? C1 C2 C88 C83 66(2) . . . . ? C82 C83 C88 C2 18(3) . . . . ? C78 C83 C88 C2 -160.6(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 7.268 _refine_diff_density_min -3.547 _refine_diff_density_rms 0.571 #===END data_4.4C2H4Cl2.2H2O _database_code_CSD 181734 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H124 Cl24 O10 W4' _chemical_formula_weight 3024.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9255(8) _cell_length_b 24.9463(14) _cell_length_c 18.0215(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.937(2) _cell_angle_gamma 90.00 _cell_volume 5956.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 28055 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 29.45 _exptl_crystal_description block _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 4.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 0.809 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.6884 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 23 _diffrn_reflns_number 36959 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8539 _reflns_number_gt 6438 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0037(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8539 _refine_ls_number_parameters 753 _refine_ls_number_restraints 451 _refine_ls_R_factor_all 0.1449 _refine_ls_R_factor_gt 0.1256 _refine_ls_wR_factor_ref 0.3744 _refine_ls_wR_factor_gt 0.3664 _refine_ls_goodness_of_fit_ref 1.538 _refine_ls_restrained_S_all 1.505 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.0391(12) 0.7321(6) 0.5505(5) 0.0287(16) Uani 0.56(5) 1 d PDU A 1 Cl1 Cl 0.063(3) 0.7457(14) 0.6842(9) 0.060(6) Uani 0.56(5) 1 d PDU A 1 Cl2 Cl 0.2062(16) 0.7526(13) 0.570(2) 0.060(5) Uani 0.56(5) 1 d PDU A 1 Cl3 Cl 0.084(2) 0.6446(8) 0.5841(15) 0.046(5) Uani 0.56(5) 1 d PDU A 1 Cl4 Cl 0.001(2) 0.8229(7) 0.5290(15) 0.051(5) Uani 0.56(5) 1 d PDU A 1 W1X W 0.0176(14) 0.7405(5) 0.5515(6) 0.0229(17) Uani 0.44(5) 1 d PDU A 2 Cl1X Cl 0.044(4) 0.7582(13) 0.6847(10) 0.046(6) Uani 0.44(5) 1 d PDU A 2 Cl2X Cl 0.1843(19) 0.7585(14) 0.566(3) 0.047(5) Uani 0.44(5) 1 d PDU A 2 Cl3X Cl 0.062(3) 0.6536(8) 0.590(2) 0.046(6) Uani 0.44(5) 1 d PDU A 2 Cl4X Cl -0.019(3) 0.8312(8) 0.525(2) 0.054(6) Uani 0.44(5) 1 d PDU A 2 W2 W -0.21776(11) 0.51538(5) 0.52655(7) 0.0709(6) Uani 1 1 d U . . Cl5 Cl -0.1656(14) 0.4597(4) 0.4447(7) 0.163(5) Uani 1 1 d U . . Cl6 Cl -0.1770(7) 0.5853(3) 0.4614(5) 0.086(2) Uani 1 1 d U . . Cl7 Cl -0.0524(6) 0.5179(4) 0.6130(8) 0.109(3) Uani 1 1 d U . . Cl8 Cl -0.3760(10) 0.5124(4) 0.4413(6) 0.130(4) Uani 1 1 d U . . O1 O 0.0084(11) 0.7167(6) 0.4503(7) 0.037(3) Uani 1 1 d . . . O2 O -0.1026(12) 0.7196(6) 0.5374(8) 0.044(4) Uani 1 1 d . . . O3 O -0.2538(13) 0.5610(6) 0.5952(9) 0.052(4) Uani 1 1 d . . . O4 O -0.2366(12) 0.4550(6) 0.5782(9) 0.051(4) Uani 1 1 d . . . C1 C -0.0472(15) 0.6870(8) 0.3850(11) 0.037(5) Uani 1 1 d . A . C2 C 0.0004(17) 0.6473(8) 0.3590(10) 0.037(5) Uani 1 1 d . . . C3 C -0.0582(19) 0.6151(9) 0.3013(13) 0.049(6) Uani 1 1 d . A . H3 H -0.0267 0.5870 0.2819 0.059 Uiso 1 1 calc R . . C4 C -0.161(2) 0.6219(9) 0.2700(11) 0.054(7) Uani 1 1 d . . . C5 C -0.2027(18) 0.6685(9) 0.2950(12) 0.050(6) Uani 1 1 d . A . H5 H -0.2715 0.6771 0.2698 0.059 Uiso 1 1 calc R . . C6 C -0.1498(19) 0.6999(8) 0.3515(13) 0.045(5) Uani 1 1 d . . . C7 C -0.229(3) 0.5826(11) 0.2031(16) 0.080(7) Uani 1 1 d DU A . C8 C -0.200(4) 0.583(2) 0.140(2) 0.111(12) Uani 0.82(5) 1 d PDU A 1 H8A H -0.1357 0.5638 0.1510 0.167 Uiso 0.82(5) 1 calc PR A 1 H8B H -0.1915 0.6200 0.1256 0.167 Uiso 0.82(5) 1 calc PR A 1 H8C H -0.2512 0.5652 0.0975 0.167 Uiso 0.82(5) 1 calc PR A 1 C9 C -0.328(3) 0.589(2) 0.181(3) 0.109(12) Uani 0.82(5) 1 d PDU A 1 H9A H -0.3468 0.6199 0.1458 0.163 Uiso 0.82(5) 1 calc PR A 1 H9B H -0.3495 0.5961 0.2276 0.163 Uiso 0.82(5) 1 calc PR A 1 H9C H -0.3614 0.5568 0.1550 0.163 Uiso 0.82(5) 1 calc PR A 1 C10 C -0.206(3) 0.5259(12) 0.241(3) 0.093(14) Uani 0.82(5) 1 d PDU A 1 H10A H -0.1325 0.5211 0.2625 0.139 Uiso 0.82(5) 1 calc PR A 1 H10B H -0.2337 0.4984 0.2015 0.139 Uiso 0.82(5) 1 calc PR A 1 H10C H -0.2363 0.5226 0.2831 0.139 Uiso 0.82(5) 1 calc PR A 1 C8X C -0.248(13) 0.611(5) 0.138(5) 0.09(2) Uani 0.18(5) 1 d PDU A 2 H8D H -0.1849 0.6168 0.1259 0.142 Uiso 0.18(5) 1 calc PR A 2 H8E H -0.2771 0.6455 0.1454 0.142 Uiso 0.18(5) 1 calc PR A 2 H8F H -0.2957 0.5913 0.0954 0.142 Uiso 0.18(5) 1 calc PR A 2 C9X C -0.318(7) 0.567(7) 0.208(10) 0.10(2) Uani 0.18(5) 1 d PDU A 2 H9D H -0.3690 0.5939 0.1853 0.147 Uiso 0.18(5) 1 calc PR A 2 H9E H -0.3129 0.5617 0.2634 0.147 Uiso 0.18(5) 1 calc PR A 2 H9F H -0.3370 0.5327 0.1805 0.147 Uiso 0.18(5) 1 calc PR A 2 C10X C -0.175(11) 0.531(5) 0.187(9) 0.09(2) Uani 0.18(5) 1 d PDU A 2 H10D H -0.1043 0.5388 0.1925 0.136 Uiso 0.18(5) 1 calc PR A 2 H10E H -0.2091 0.5175 0.1347 0.136 Uiso 0.18(5) 1 calc PR A 2 H10F H -0.1774 0.5029 0.2255 0.136 Uiso 0.18(5) 1 calc PR A 2 C11 C -0.1983(19) 0.7469(9) 0.3796(12) 0.044(5) Uani 1 1 d . A . H11A H -0.2458 0.7655 0.3346 0.053 Uiso 1 1 calc R . . H11B H -0.1459 0.7728 0.4079 0.053 Uiso 1 1 calc R . . C12 C -0.2004(15) 0.7107(8) 0.5107(11) 0.032(4) Uani 1 1 d . A . C13 C -0.2560(18) 0.7249(8) 0.4349(12) 0.040(5) Uani 1 1 d . . . C14 C -0.3588(18) 0.7147(10) 0.4108(12) 0.050(6) Uani 1 1 d . A . H14 H -0.3971 0.7245 0.3592 0.060 Uiso 1 1 calc R . . C15 C -0.4063(18) 0.6920(10) 0.4561(16) 0.060(7) Uani 1 1 d . . . C16 C -0.3440(18) 0.6750(8) 0.5391(13) 0.043(5) Uani 1 1 d . A . H16 H -0.3763 0.6585 0.5726 0.052 Uiso 1 1 calc R . . C17 C -0.2454(14) 0.6832(7) 0.5636(12) 0.031(4) Uani 1 1 d . . . C18 C -0.5197(19) 0.6804(11) 0.4315(13) 0.077(7) Uani 1 1 d DU A . C19 C -0.578(3) 0.695(2) 0.350(2) 0.078(13) Uani 0.52(4) 1 d PDU A 1 H19A H -0.5493 0.6764 0.3139 0.117 Uiso 0.52(4) 1 calc PR A 1 H19B H -0.5760 0.7335 0.3432 0.117 Uiso 0.52(4) 1 calc PR A 1 H19C H -0.6487 0.6832 0.3399 0.117 Uiso 0.52(4) 1 calc PR A 1 C20 C -0.533(5) 0.611(2) 0.441(3) 0.098(18) Uani 0.52(4) 1 d PDU A 1 H20A H -0.5047 0.5917 0.4049 0.147 Uiso 0.52(4) 1 calc PR A 1 H20B H -0.6052 0.6017 0.4282 0.147 Uiso 0.52(4) 1 calc PR A 1 H20C H -0.4980 0.5996 0.4945 0.147 Uiso 0.52(4) 1 calc PR A 1 C21 C -0.565(3) 0.706(2) 0.487(2) 0.071(11) Uani 0.52(4) 1 d PDU A 1 H21A H -0.5282 0.6946 0.5406 0.106 Uiso 0.52(4) 1 calc PR A 1 H21B H -0.6359 0.6954 0.4748 0.106 Uiso 0.52(4) 1 calc PR A 1 H21C H -0.5607 0.7451 0.4835 0.106 Uiso 0.52(4) 1 calc PR A 1 C19X C -0.577(3) 0.7311(17) 0.420(4) 0.077(13) Uani 0.48(4) 1 d PDU A 2 H19D H -0.5476 0.7565 0.3916 0.116 Uiso 0.48(4) 1 calc PR A 2 H19E H -0.5741 0.7462 0.4708 0.116 Uiso 0.48(4) 1 calc PR A 2 H19F H -0.6475 0.7241 0.3898 0.116 Uiso 0.48(4) 1 calc PR A 2 C20X C -0.534(4) 0.652(2) 0.339(3) 0.082(15) Uani 0.48(4) 1 d PDU A 2 H20D H -0.4944 0.6188 0.3452 0.123 Uiso 0.48(4) 1 calc PR A 2 H20E H -0.5093 0.6774 0.3073 0.123 Uiso 0.48(4) 1 calc PR A 2 H20F H -0.6051 0.6441 0.3129 0.123 Uiso 0.48(4) 1 calc PR A 2 C21X C -0.553(5) 0.640(2) 0.477(3) 0.091(16) Uani 0.48(4) 1 d PDU A 2 H21D H -0.5195 0.6055 0.4745 0.137 Uiso 0.48(4) 1 calc PR A 2 H21E H -0.6264 0.6350 0.4559 0.137 Uiso 0.48(4) 1 calc PR A 2 H21F H -0.5358 0.6512 0.5317 0.137 Uiso 0.48(4) 1 calc PR A 2 C22 C -0.1766(17) 0.6659(9) 0.6388(13) 0.044(5) Uani 1 1 d . A . H22A H -0.1462 0.6980 0.6694 0.053 Uiso 1 1 calc R . . H22B H -0.1213 0.6447 0.6295 0.053 Uiso 1 1 calc R . . C23 C -0.2661(19) 0.5823(8) 0.6601(12) 0.044(5) Uani 1 1 d . A . C24 C -0.2272(17) 0.6321(8) 0.6872(12) 0.041(5) Uani 1 1 d . . . C25 C -0.237(2) 0.6524(10) 0.7532(15) 0.064(7) Uani 1 1 d . A . H25 H -0.2135 0.6875 0.7696 0.077 Uiso 1 1 calc R . . C26 C -0.284(2) 0.6208(10) 0.7986(15) 0.059(7) Uani 1 1 d . . . C27 C -0.3161(18) 0.5700(10) 0.7755(13) 0.050(6) Uani 1 1 d . A . H27 H -0.3423 0.5481 0.8079 0.059 Uiso 1 1 calc R . . C28 C -0.3105(17) 0.5499(8) 0.7043(13) 0.043(5) Uani 1 1 d . . . C29 C -0.294(3) 0.6437(13) 0.8766(18) 0.085(10) Uani 1 1 d . A . C30 C -0.179(3) 0.6475(15) 0.9380(16) 0.088(10) Uani 1 1 d . . . H30A H -0.1505 0.6114 0.9489 0.132 Uiso 1 1 calc R A . H30B H -0.1812 0.6642 0.9867 0.132 Uiso 1 1 calc R . . H30C H -0.1370 0.6692 0.9149 0.132 Uiso 1 1 calc R . . C31 C -0.337(3) 0.6979(12) 0.8603(16) 0.076(8) Uani 1 1 d . . . H31A H -0.3405 0.7143 0.9088 0.114 Uiso 1 1 calc R A . H31B H -0.4048 0.6958 0.8228 0.114 Uiso 1 1 calc R . . H31C H -0.2937 0.7197 0.8384 0.114 Uiso 1 1 calc R . . C32 C -0.360(2) 0.6115(13) 0.9114(15) 0.076(9) Uani 1 1 d . . . H32A H -0.3323 0.5752 0.9224 0.115 Uiso 1 1 calc R A . H32B H -0.4283 0.6097 0.8746 0.115 Uiso 1 1 calc R . . H32C H -0.3619 0.6284 0.9600 0.115 Uiso 1 1 calc R . . C33 C -0.3513(19) 0.4928(8) 0.6764(14) 0.048(6) Uani 1 1 d . A . H33A H -0.4080 0.4847 0.6968 0.058 Uiso 1 1 calc R . . H33B H -0.3784 0.4929 0.6187 0.058 Uiso 1 1 calc R . . C34 C -0.2222(16) 0.4297(7) 0.6479(11) 0.034(5) Uani 1 1 d U A . C35 C -0.2741(17) 0.4486(7) 0.7011(13) 0.040(5) Uani 1 1 d . . . C36 C -0.261(2) 0.4238(9) 0.7680(13) 0.052(6) Uani 1 1 d . A . H36 H -0.2965 0.4359 0.8019 0.063 Uiso 1 1 calc R . . C37 C -0.1975(18) 0.3817(10) 0.7898(13) 0.049(6) Uani 1 1 d . . . C38 C -0.1496(19) 0.3616(9) 0.7362(13) 0.049(6) Uani 1 1 d . A . H38 H -0.1080 0.3307 0.7502 0.059 Uiso 1 1 calc R . . C39 C -0.1607(17) 0.3841(8) 0.6680(12) 0.039(5) Uani 1 1 d . . . C40 C -0.169(2) 0.3524(10) 0.8717(14) 0.078(6) Uani 1 1 d DU A . C41 C -0.103(4) 0.3019(19) 0.881(3) 0.083(10) Uani 0.53(3) 1 d PDU A 1 H41A H -0.0914 0.2867 0.9330 0.125 Uiso 0.53(3) 1 calc PR A 1 H41B H -0.0377 0.3113 0.8740 0.125 Uiso 0.53(3) 1 calc PR A 1 H41C H -0.1370 0.2754 0.8415 0.125 Uiso 0.53(3) 1 calc PR A 1 C42 C -0.280(4) 0.332(2) 0.879(3) 0.085(11) Uani 0.53(3) 1 d PDU A 1 H42A H -0.2699 0.3137 0.9283 0.127 Uiso 0.53(3) 1 calc PR A 1 H42B H -0.3121 0.3080 0.8354 0.127 Uiso 0.53(3) 1 calc PR A 1 H42C H -0.3236 0.3636 0.8760 0.127 Uiso 0.53(3) 1 calc PR A 1 C43 C -0.125(5) 0.394(2) 0.937(3) 0.090(11) Uani 0.53(3) 1 d PDU A 1 H43A H -0.1083 0.3760 0.9875 0.134 Uiso 0.53(3) 1 calc PR A 1 H43B H -0.1743 0.4221 0.9335 0.134 Uiso 0.53(3) 1 calc PR A 1 H43C H -0.0631 0.4094 0.9300 0.134 Uiso 0.53(3) 1 calc PR A 1 C41X C -0.211(5) 0.2955(18) 0.861(3) 0.078(10) Uani 0.47(3) 1 d PDU A 2 H41D H -0.1953 0.2777 0.9116 0.116 Uiso 0.47(3) 1 calc PR A 2 H41E H -0.1809 0.2753 0.8269 0.116 Uiso 0.47(3) 1 calc PR A 2 H41F H -0.2845 0.2969 0.8367 0.116 Uiso 0.47(3) 1 calc PR A 2 C42X C -0.217(5) 0.386(2) 0.932(3) 0.091(12) Uani 0.47(3) 1 d PDU A 2 H42D H -0.1910 0.4229 0.9374 0.136 Uiso 0.47(3) 1 calc PR A 2 H42E H -0.1970 0.3685 0.9829 0.136 Uiso 0.47(3) 1 calc PR A 2 H42F H -0.2905 0.3866 0.9103 0.136 Uiso 0.47(3) 1 calc PR A 2 C43X C -0.053(3) 0.354(3) 0.906(3) 0.089(11) Uani 0.47(3) 1 d PDU A 2 H43D H -0.0301 0.3912 0.9123 0.134 Uiso 0.47(3) 1 calc PR A 2 H43E H -0.0229 0.3354 0.8706 0.134 Uiso 0.47(3) 1 calc PR A 2 H43F H -0.0326 0.3359 0.9568 0.134 Uiso 0.47(3) 1 calc PR A 2 C44 C -0.1112(19) 0.3622(9) 0.6077(12) 0.047(6) Uani 1 1 d . . . H44A H -0.1445 0.3280 0.5861 0.057 Uiso 1 1 calc R . . H44B H -0.1232 0.3880 0.5641 0.057 Uiso 1 1 calc R . . Cl9 Cl -0.0680(16) 0.3469(6) 1.1590(9) 0.184(7) Uani 1 1 d DU . . C45 C -0.059(4) 0.4099(13) 1.189(3) 0.187(15) Uani 1 1 d DU . . H45A H -0.1223 0.4289 1.1617 0.224 Uiso 1 1 calc R . . H45B H -0.0516 0.4104 1.2457 0.224 Uiso 1 1 calc R . . C46 C 0.021(4) 0.4368(16) 1.177(3) 0.199(17) Uani 1 1 d DU . . H46A H 0.0691 0.4099 1.1695 0.239 Uiso 1 1 calc R . . H46B H 0.0553 0.4570 1.2252 0.239 Uiso 1 1 calc R . . Cl10 Cl -0.006(3) 0.4789(13) 1.103(3) 0.344(18) Uani 1 1 d DU . . Cl11 Cl 0.0369(18) 0.1175(13) 0.8130(15) 0.157(11) Uani 0.50 1 d PDU . . C47 C 0.158(3) 0.130(2) 0.828(4) 0.16(2) Uani 0.50 1 d PDU . . H47A H 0.1966 0.1226 0.8829 0.192 Uiso 0.50 1 calc PR . . H47B H 0.1844 0.1059 0.7947 0.192 Uiso 0.50 1 calc PR . . C48 C 0.174(4) 0.182(3) 0.811(6) 0.17(2) Uani 0.50 1 d PDU . . H48A H 0.1979 0.1834 0.7642 0.208 Uiso 0.50 1 calc PR . . H48B H 0.2271 0.1984 0.8549 0.208 Uiso 0.50 1 calc PR . . Cl12 Cl 0.068(3) 0.2179(16) 0.793(4) 0.28(2) Uani 0.50 1 d PDU . . Cl13 Cl -0.383(2) 0.4680(7) 0.9649(19) 0.263(13) Uani 1 1 d DU . . C49 C -0.470(6) 0.486(3) 1.006(6) 0.26(3) Uani 1 1 d DU . . H49A H -0.5046 0.4515 1.0097 0.318 Uiso 1 1 calc R . . H49B H -0.4299 0.4943 1.0606 0.318 Uiso 1 1 calc R . . O1W O 0.1526(14) 0.1182(7) 0.6815(13) 0.078(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.019(3) 0.047(3) 0.0251(13) -0.0066(16) 0.0137(17) 0.003(2) Cl1 0.045(12) 0.102(15) 0.030(4) -0.024(6) 0.009(5) -0.013(12) Cl2 0.023(6) 0.103(10) 0.053(10) -0.006(9) 0.010(8) -0.007(7) Cl3 0.038(11) 0.064(6) 0.039(8) 0.017(7) 0.016(7) 0.028(6) Cl4 0.060(11) 0.036(5) 0.060(9) -0.026(6) 0.022(8) -0.005(6) W1X 0.020(4) 0.038(2) 0.0168(15) -0.0007(14) 0.0138(19) 0.013(2) Cl1X 0.056(16) 0.065(11) 0.020(5) -0.005(5) 0.018(7) 0.003(9) Cl2X 0.026(7) 0.083(9) 0.032(9) 0.002(8) 0.010(9) -0.004(7) Cl3X 0.048(16) 0.046(6) 0.054(10) 0.014(6) 0.034(9) 0.025(6) Cl4X 0.079(15) 0.044(6) 0.052(10) 0.012(9) 0.039(10) 0.021(8) W2 0.1006(11) 0.0713(9) 0.0481(8) 0.0040(5) 0.0334(7) 0.0108(6) Cl5 0.342(16) 0.081(5) 0.119(7) 0.020(5) 0.148(9) 0.064(8) Cl6 0.145(7) 0.069(4) 0.071(5) 0.026(4) 0.073(5) 0.022(4) Cl7 0.062(4) 0.098(6) 0.159(8) 0.057(5) 0.022(5) 0.009(4) Cl8 0.151(7) 0.118(7) 0.069(6) 0.014(5) -0.042(6) -0.023(6) O1 0.047(8) 0.050(8) 0.011(7) -0.003(6) 0.003(6) 0.003(7) O2 0.050(10) 0.056(9) 0.031(8) -0.002(7) 0.020(7) -0.003(7) O3 0.069(11) 0.061(9) 0.031(8) 0.008(7) 0.021(8) 0.006(8) O4 0.051(9) 0.042(8) 0.054(10) -0.015(7) 0.006(8) 0.019(7) C1 0.038(12) 0.047(12) 0.020(10) 0.014(9) 0.000(9) -0.018(9) C2 0.061(14) 0.037(11) 0.014(9) 0.006(8) 0.014(9) 0.003(10) C3 0.061(16) 0.048(12) 0.035(12) 0.004(10) 0.011(12) 0.013(11) C4 0.078(18) 0.060(14) 0.010(10) -0.004(10) -0.009(11) -0.017(13) C5 0.050(14) 0.065(14) 0.021(11) 0.013(11) -0.007(10) 0.017(12) C6 0.067(16) 0.034(11) 0.037(12) 0.006(10) 0.017(12) 0.000(10) C7 0.097(15) 0.064(12) 0.045(12) -0.013(11) -0.028(13) -0.006(13) C8 0.15(3) 0.11(3) 0.054(17) -0.026(17) -0.005(17) 0.00(2) C9 0.100(16) 0.10(2) 0.08(2) 0.01(2) -0.031(16) 0.014(18) C10 0.11(3) 0.047(14) 0.08(2) -0.023(13) -0.04(2) -0.002(15) C8X 0.11(5) 0.08(4) 0.06(4) 0.00(3) -0.02(4) -0.01(4) C9X 0.10(3) 0.09(4) 0.08(4) 0.01(3) -0.01(3) 0.00(3) C10X 0.12(4) 0.08(3) 0.04(4) -0.02(3) -0.02(4) 0.01(3) C11 0.064(15) 0.057(13) 0.017(10) 0.009(9) 0.021(10) 0.016(11) C12 0.035(12) 0.038(10) 0.028(11) -0.008(8) 0.017(9) -0.006(8) C13 0.058(15) 0.038(11) 0.027(11) 0.007(9) 0.016(11) 0.002(9) C14 0.053(15) 0.065(14) 0.016(11) 0.004(10) -0.015(10) -0.002(12) C15 0.035(13) 0.069(16) 0.065(17) -0.011(14) -0.001(12) -0.001(11) C16 0.062(16) 0.034(11) 0.041(13) -0.006(9) 0.025(11) -0.012(10) C17 0.032(11) 0.028(9) 0.039(12) -0.005(8) 0.017(9) -0.008(8) C18 0.031(13) 0.107(17) 0.074(15) 0.005(13) -0.013(10) -0.016(11) C19 0.03(2) 0.13(3) 0.069(17) 0.03(2) 0.012(18) -0.02(2) C20 0.07(4) 0.116(19) 0.09(4) 0.02(2) -0.01(3) -0.03(3) C21 0.017(19) 0.12(3) 0.07(2) 0.04(2) 0.005(17) -0.01(2) C19X 0.013(19) 0.13(2) 0.08(3) 0.00(2) 0.00(2) -0.002(18) C20X 0.05(3) 0.10(4) 0.09(3) -0.01(2) 0.00(3) -0.02(3) C21X 0.03(3) 0.14(3) 0.10(3) 0.01(3) 0.01(3) -0.02(3) C22 0.053(14) 0.045(12) 0.045(13) 0.003(10) 0.031(11) -0.003(10) C23 0.076(16) 0.041(12) 0.026(11) -0.008(9) 0.032(11) 0.007(11) C24 0.058(14) 0.044(12) 0.029(11) 0.010(9) 0.025(10) -0.006(10) C25 0.09(2) 0.053(14) 0.038(14) -0.008(11) 0.006(13) 0.006(13) C26 0.081(19) 0.059(15) 0.053(16) -0.003(12) 0.046(15) 0.001(13) C27 0.059(15) 0.058(14) 0.027(12) -0.007(10) 0.006(11) 0.009(11) C28 0.052(13) 0.047(12) 0.043(13) 0.000(10) 0.034(11) 0.004(10) C29 0.12(3) 0.09(2) 0.07(2) -0.050(17) 0.06(2) -0.016(19) C30 0.10(2) 0.12(3) 0.037(15) -0.018(16) 0.010(16) 0.01(2) C31 0.11(2) 0.09(2) 0.044(16) -0.006(14) 0.037(16) 0.009(18) C32 0.10(2) 0.11(2) 0.031(14) 0.004(14) 0.048(15) 0.028(18) C33 0.073(16) 0.042(12) 0.053(15) 0.001(10) 0.053(14) 0.000(11) C34 0.064(13) 0.028(9) 0.019(10) 0.014(8) 0.024(9) -0.005(9) C35 0.058(14) 0.023(9) 0.052(14) 0.001(9) 0.037(12) -0.001(9) C36 0.077(17) 0.055(14) 0.037(13) 0.009(11) 0.034(12) 0.006(13) C37 0.053(14) 0.075(16) 0.028(12) 0.004(11) 0.024(11) -0.009(12) C38 0.060(15) 0.055(13) 0.030(12) 0.002(10) 0.011(11) 0.002(11) C39 0.049(13) 0.036(11) 0.039(12) 0.005(9) 0.023(10) -0.001(9) C40 0.105(16) 0.104(15) 0.029(11) 0.015(11) 0.028(11) 0.001(12) C41 0.12(2) 0.101(19) 0.025(17) 0.032(16) 0.016(19) 0.007(17) C42 0.11(2) 0.10(3) 0.04(2) 0.04(2) 0.021(18) -0.009(17) C43 0.12(2) 0.10(2) 0.037(17) 0.016(14) 0.02(2) -0.010(19) C41X 0.12(2) 0.099(17) 0.026(18) 0.024(17) 0.03(2) 0.004(18) C42X 0.13(3) 0.11(2) 0.04(2) 0.008(19) 0.04(2) 0.00(2) C43X 0.108(17) 0.11(2) 0.04(2) 0.00(2) 0.007(18) 0.009(18) C44 0.072(16) 0.048(12) 0.027(11) 0.004(10) 0.023(11) 0.015(11) Cl9 0.27(2) 0.129(10) 0.135(11) 0.016(8) 0.029(12) -0.035(11) C45 0.19(4) 0.19(2) 0.22(4) -0.08(2) 0.12(3) -0.04(3) C46 0.21(4) 0.16(2) 0.26(4) -0.05(2) 0.13(4) -0.04(2) Cl10 0.36(4) 0.30(3) 0.44(5) 0.12(3) 0.24(4) 0.07(3) Cl11 0.096(15) 0.25(3) 0.106(17) 0.006(19) 0.003(13) -0.060(17) C47 0.11(2) 0.30(5) 0.06(3) -0.01(4) 0.01(3) -0.10(3) C48 0.11(3) 0.31(6) 0.09(4) 0.02(5) 0.02(3) -0.08(3) Cl12 0.15(3) 0.40(6) 0.26(5) 0.05(4) 0.02(3) -0.02(3) Cl13 0.29(3) 0.136(12) 0.44(4) -0.043(17) 0.23(3) -0.054(14) C49 0.35(6) 0.17(5) 0.32(7) -0.12(5) 0.17(5) 0.03(5) O1W 0.050(11) 0.071(12) 0.098(16) 0.019(11) 0.003(10) -0.005(9) _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 W1 O1 1.766(16) . ? W1 O2 1.94(2) . ? W1 Cl3 2.298(10) . ? W1 Cl2 2.301(11) . ? W1 Cl4 2.330(10) . ? W1 Cl1 2.354(11) . ? W1X O2 1.70(2) . ? W1X O1 1.887(17) . ? W1X Cl2X 2.297(13) . ? W1X Cl3X 2.302(12) . ? W1X Cl4X 2.335(12) . ? W1X Cl1X 2.353(13) . ? W2 O4 1.831(17) . ? W2 O3 1.861(16) . ? W2 Cl8 2.266(11) . ? W2 Cl6 2.271(7) . ? W2 Cl5 2.301(9) . ? W2 Cl7 2.351(10) . ? O1 C1 1.40(2) . ? O2 C12 1.32(2) . ? O3 C23 1.34(2) . ? O4 C34 1.37(2) . ? C1 C2 1.35(3) . ? C1 C6 1.41(3) . ? C2 C3 1.37(3) . ? C2 C44 1.49(3) 3_566 ? C3 C4 1.38(4) . ? C4 C5 1.43(3) . ? C4 C7 1.61(3) . ? C5 C6 1.32(3) . ? C6 C11 1.52(3) . ? C7 C8 1.31(5) . ? C7 C8X 1.32(6) . ? C7 C9 1.32(5) . ? C7 C9X 1.33(5) . ? C7 C10 1.56(4) . ? C7 C10X 1.57(5) . ? C11 C13 1.56(3) . ? C12 C13 1.39(3) . ? C12 C17 1.46(3) . ? C13 C14 1.38(3) . ? C14 C15 1.33(4) . ? C15 C18 1.53(3) . ? C15 C16 1.54(3) . ? C16 C17 1.32(3) . ? C17 C22 1.46(3) . ? C18 C21X 1.47(3) . ? C18 C19X 1.48(3) . ? C18 C19 1.48(3) . ? C18 C21 1.49(3) . ? C18 C20 1.77(5) . ? C18 C20X 1.77(5) . ? C22 C24 1.53(3) . ? C23 C24 1.38(3) . ? C23 C28 1.41(3) . ? C24 C25 1.34(3) . ? C25 C26 1.43(4) . ? C26 C27 1.37(3) . ? C26 C29 1.57(3) . ? C27 C28 1.40(3) . ? C28 C33 1.56(3) . ? C29 C31 1.47(4) . ? C29 C32 1.49(4) . ? C29 C30 1.65(5) . ? C33 C35 1.51(3) . ? C34 C39 1.40(3) . ? C34 C35 1.45(3) . ? C35 C36 1.32(3) . ? C36 C37 1.35(3) . ? C37 C38 1.42(3) . ? C37 C40 1.58(3) . ? C38 C39 1.32(3) . ? C39 C44 1.56(3) . ? C40 C41X 1.53(4) . ? C40 C43X 1.53(4) . ? C40 C41 1.54(4) . ? C40 C43 1.54(4) . ? C40 C42X 1.67(5) . ? C40 C42 1.67(5) . ? C44 C2 1.49(3) 3_566 ? Cl9 C45 1.66(3) . ? C45 C46 1.37(6) . ? C46 Cl10 1.65(3) . ? Cl11 C47 1.66(3) . ? C47 C48 1.37(6) . ? C48 Cl12 1.66(3) . ? Cl13 C49 1.66(3) . ? C49 C49 1.07(14) 3_467 ? 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 W1 O2 85.7(8) . . ? O1 W1 Cl3 91.3(9) . . ? O2 W1 Cl3 93.5(9) . . ? O1 W1 Cl2 96.9(13) . . ? O2 W1 Cl2 175.9(12) . . ? Cl3 W1 Cl2 89.6(7) . . ? O1 W1 Cl4 94.1(9) . . ? O2 W1 Cl4 88.1(9) . . ? Cl3 W1 Cl4 174.5(7) . . ? Cl2 W1 Cl4 88.6(5) . . ? O1 W1 Cl1 172.8(11) . . ? O2 W1 Cl1 87.9(11) . . ? Cl3 W1 Cl1 85.8(6) . . ? Cl2 W1 Cl1 89.7(7) . . ? Cl4 W1 Cl1 89.0(6) . . ? O2 W1X O1 89.3(8) . . ? O2 W1X Cl2X 173.0(12) . . ? O1 W1X Cl2X 86.5(14) . . ? O2 W1X Cl3X 85.1(11) . . ? O1 W1X Cl3X 85.7(10) . . ? Cl2X W1X Cl3X 89.0(8) . . ? O2 W1X Cl4X 97.2(12) . . ? O1 W1X Cl4X 99.5(10) . . ? Cl2X W1X Cl4X 89.1(7) . . ? Cl3X W1X Cl4X 174.3(10) . . ? O2 W1X Cl1X 92.9(14) . . ? O1 W1X Cl1X 171.0(10) . . ? Cl2X W1X Cl1X 90.4(7) . . ? Cl3X W1X Cl1X 85.8(6) . . ? Cl4X W1X Cl1X 88.9(7) . . ? O4 W2 O3 93.1(7) . . ? O4 W2 Cl8 93.2(5) . . ? O3 W2 Cl8 93.8(6) . . ? O4 W2 Cl6 173.0(5) . . ? O3 W2 Cl6 92.0(5) . . ? Cl8 W2 Cl6 91.2(4) . . ? O4 W2 Cl5 87.3(5) . . ? O3 W2 Cl5 177.4(7) . . ? Cl8 W2 Cl5 88.8(6) . . ? Cl6 W2 Cl5 87.4(3) . . ? O4 W2 Cl7 87.1(5) . . ? O3 W2 Cl7 87.3(6) . . ? Cl8 W2 Cl7 178.9(5) . . ? Cl6 W2 Cl7 88.4(3) . . ? Cl5 W2 Cl7 90.2(6) . . ? C1 O1 W1 150.4(13) . . ? C1 O1 W1X 146.4(14) . . ? W1 O1 W1X 11.0(4) . . ? C12 O2 W1X 165.7(15) . . ? C12 O2 W1 166.3(13) . . ? W1X O2 W1 8.9(5) . . ? C23 O3 W2 162.6(15) . . ? C34 O4 W2 147.7(13) . . ? C2 C1 O1 118.2(18) . . ? C2 C1 C6 124.2(19) . . ? O1 C1 C6 117.6(19) . . ? C1 C2 C3 117(2) . . ? C1 C2 C44 122.2(18) . 3_566 ? C3 C2 C44 120.9(19) . 3_566 ? C2 C3 C4 123(2) . . ? C3 C4 C5 116(2) . . ? C3 C4 C7 122(2) . . ? C5 C4 C7 122(2) . . ? C6 C5 C4 123(2) . . ? C5 C6 C1 117(2) . . ? C5 C6 C11 121(2) . . ? C1 C6 C11 122(2) . . ? C8 C7 C8X 43(6) . . ? C8 C7 C9 108(4) . . ? C8X C7 C9 76(7) . . ? C8 C7 C9X 127(8) . . ? C8X C7 C9X 107(5) . . ? C9 C7 C9X 32(7) . . ? C8 C7 C10 108(4) . . ? C8X C7 C10 146(7) . . ? C9 C7 C10 107(4) . . ? C9X C7 C10 77(8) . . ? C8 C7 C10X 64(7) . . ? C8X C7 C10X 105(5) . . ? C9 C7 C10X 124(7) . . ? C9X C7 C10X 106(4) . . ? C10 C7 C10X 44(6) . . ? C8 C7 C4 112(3) . . ? C8X C7 C4 104(7) . . ? C9 C7 C4 117(3) . . ? C9X C7 C4 118(8) . . ? C10 C7 C4 103(2) . . ? C10X C7 C4 116(6) . . ? C6 C11 C13 108.2(18) . . ? O2 C12 C13 121.0(18) . . ? O2 C12 C17 116.3(17) . . ? C13 C12 C17 122.6(18) . . ? C14 C13 C12 118.0(19) . . ? C14 C13 C11 123.4(19) . . ? C12 C13 C11 118(2) . . ? C15 C14 C13 123(2) . . ? C14 C15 C18 125(2) . . ? C14 C15 C16 119(2) . . ? C18 C15 C16 117(2) . . ? C17 C16 C15 120(2) . . ? C16 C17 C12 117.6(19) . . ? C16 C17 C22 125.4(19) . . ? C12 C17 C22 116.9(17) . . ? C21X C18 C19X 115(3) . . ? C21X C18 C19 123(4) . . ? C19X C18 C19 63(3) . . ? C21X C18 C21 69(3) . . ? C19X C18 C21 53(3) . . ? C19 C18 C21 110(3) . . ? C21X C18 C15 116(3) . . ? C19X C18 C15 110(3) . . ? C19 C18 C15 117(3) . . ? C21 C18 C15 110(2) . . ? C21X C18 C20 37(3) . . ? C19X C18 C20 142(3) . . ? C19 C18 C20 107(2) . . ? C21 C18 C20 106(2) . . ? C15 C18 C20 107(3) . . ? C21X C18 C20X 107(2) . . ? C19X C18 C20X 108(2) . . ? C19 C18 C20X 45(3) . . ? C21 C18 C20X 150(3) . . ? C15 C18 C20X 99(3) . . ? C20 C18 C20X 73(2) . . ? C17 C22 C24 114.0(19) . . ? O3 C23 C24 122(2) . . ? O3 C23 C28 117.5(19) . . ? C24 C23 C28 120.6(18) . . ? C25 C24 C23 121(2) . . ? C25 C24 C22 119(2) . . ? C23 C24 C22 119.4(19) . . ? C24 C25 C26 119(2) . . ? C27 C26 C25 120(2) . . ? C27 C26 C29 120(2) . . ? C25 C26 C29 120(2) . . ? C26 C27 C28 120(2) . . ? C27 C28 C23 118(2) . . ? C27 C28 C33 120.3(19) . . ? C23 C28 C33 121.5(18) . . ? C31 C29 C32 109(3) . . ? C31 C29 C26 107(3) . . ? C32 C29 C26 115(2) . . ? C31 C29 C30 109(3) . . ? C32 C29 C30 110(3) . . ? C26 C29 C30 106(2) . . ? C35 C33 C28 115(2) . . ? O4 C34 C39 121.2(17) . . ? O4 C34 C35 119.9(17) . . ? C39 C34 C35 118.9(16) . . ? C36 C35 C34 119.6(19) . . ? C36 C35 C33 120.2(19) . . ? C34 C35 C33 119.9(18) . . ? C35 C36 C37 122(2) . . ? C36 C37 C38 118(2) . . ? C36 C37 C40 126(2) . . ? C38 C37 C40 116(2) . . ? C39 C38 C37 123(2) . . ? C38 C39 C34 118(2) . . ? C38 C39 C44 124(2) . . ? C34 C39 C44 118.1(17) . . ? C41X C40 C43X 113(3) . . ? C41X C40 C41 56(3) . . ? C43X C40 C41 57(4) . . ? C41X C40 C43 140(3) . . ? C43X C40 C43 64(3) . . ? C41 C40 C43 113(3) . . ? C41X C40 C37 109(3) . . ? C43X C40 C37 107(3) . . ? C41 C40 C37 117(2) . . ? C43 C40 C37 109(3) . . ? C41X C40 C42X 110(2) . . ? C43X C40 C42X 108(2) . . ? C41 C40 C42X 134(3) . . ? C43 C40 C42X 47(3) . . ? C37 C40 C42X 110(3) . . ? C41X C40 C42 53(3) . . ? C43X C40 C42 149(3) . . ? C41 C40 C42 106(2) . . ? C43 C40 C42 108(2) . . ? C37 C40 C42 103(2) . . ? C42X C40 C42 62(2) . . ? C2 C44 C39 113.6(18) 3_566 . ? C46 C45 Cl9 113(3) . . ? C45 C46 Cl10 117(3) . . ? C48 C47 Cl11 112(2) . . ? C47 C48 Cl12 110.9(19) . . ? C49 C49 Cl13 135(10) 3_467 . ? 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 O2 W1 O1 C1 -36(3) . . . . ? Cl3 W1 O1 C1 57(3) . . . . ? Cl2 W1 O1 C1 147(3) . . . . ? Cl4 W1 O1 C1 -124(3) . . . . ? Cl1 W1 O1 C1 -8(10) . . . . ? O2 W1 O1 W1X 42(3) . . . . ? Cl3 W1 O1 W1X 135(3) . . . . ? Cl2 W1 O1 W1X -135(3) . . . . ? Cl4 W1 O1 W1X -46(3) . . . . ? Cl1 W1 O1 W1X 69(8) . . . . ? O2 W1X O1 C1 -11(3) . . . . ? Cl2X W1X O1 C1 163(2) . . . . ? Cl3X W1X O1 C1 74(2) . . . . ? Cl4X W1X O1 C1 -109(2) . . . . ? Cl1X W1X O1 C1 93(9) . . . . ? O2 W1X O1 W1 -131(3) . . . . ? Cl2X W1X O1 W1 43(3) . . . . ? Cl3X W1X O1 W1 -46(3) . . . . ? Cl4X W1X O1 W1 132(4) . . . . ? Cl1X W1X O1 W1 -27(8) . . . . ? O1 W1X O2 C12 -53(6) . . . . ? Cl2X W1X O2 C12 -106(11) . . . . ? Cl3X W1X O2 C12 -139(6) . . . . ? Cl4X W1X O2 C12 47(6) . . . . ? Cl1X W1X O2 C12 136(6) . . . . ? O1 W1X O2 W1 59(4) . . . . ? Cl2X W1X O2 W1 5(9) . . . . ? Cl3X W1X O2 W1 -27(4) . . . . ? Cl4X W1X O2 W1 158(4) . . . . ? Cl1X W1X O2 W1 -113(4) . . . . ? O1 W1 O2 C12 -9(6) . . . . ? Cl3 W1 O2 C12 -100(6) . . . . ? Cl2 W1 O2 C12 120(16) . . . . ? Cl4 W1 O2 C12 85(6) . . . . ? Cl1 W1 O2 C12 174(6) . . . . ? O1 W1 O2 W1X -114(4) . . . . ? Cl3 W1 O2 W1X 155(4) . . . . ? Cl2 W1 O2 W1X 16(15) . . . . ? Cl4 W1 O2 W1X -20(4) . . . . ? Cl1 W1 O2 W1X 69(4) . . . . ? O4 W2 O3 C23 34(6) . . . . ? Cl8 W2 O3 C23 128(5) . . . . ? Cl6 W2 O3 C23 -141(5) . . . . ? Cl5 W2 O3 C23 -64(14) . . . . ? Cl7 W2 O3 C23 -53(5) . . . . ? O3 W2 O4 C34 -44(3) . . . . ? Cl8 W2 O4 C34 -138(3) . . . . ? Cl6 W2 O4 C34 93(5) . . . . ? Cl5 W2 O4 C34 133(3) . . . . ? Cl7 W2 O4 C34 43(3) . . . . ? W1 O1 C1 C2 -105(3) . . . . ? W1X O1 C1 C2 -125(2) . . . . ? W1 O1 C1 C6 74(3) . . . . ? W1X O1 C1 C6 54(3) . . . . ? O1 C1 C2 C3 172.6(17) . . . . ? C6 C1 C2 C3 -6(3) . . . . ? O1 C1 C2 C44 -6(3) . . . 3_566 ? C6 C1 C2 C44 175.0(19) . . . 3_566 ? C1 C2 C3 C4 0(3) . . . . ? C44 C2 C3 C4 179(2) 3_566 . . . ? C2 C3 C4 C5 7(3) . . . . ? C2 C3 C4 C7 -179(2) . . . . ? C3 C4 C5 C6 -8(3) . . . . ? C7 C4 C5 C6 177(2) . . . . ? C4 C5 C6 C1 3(3) . . . . ? C4 C5 C6 C11 -176(2) . . . . ? C2 C1 C6 C5 5(3) . . . . ? O1 C1 C6 C5 -173.9(18) . . . . ? C2 C1 C6 C11 -176.3(19) . . . . ? O1 C1 C6 C11 5(3) . . . . ? C3 C4 C7 C8 -59(4) . . . . ? C5 C4 C7 C8 115(4) . . . . ? C3 C4 C7 C8X -104(9) . . . . ? C5 C4 C7 C8X 70(9) . . . . ? C3 C4 C7 C9 174(4) . . . . ? C5 C4 C7 C9 -12(5) . . . . ? C3 C4 C7 C9X 138(9) . . . . ? C5 C4 C7 C9X -48(9) . . . . ? C3 C4 C7 C10 56(4) . . . . ? C5 C4 C7 C10 -130(3) . . . . ? C3 C4 C7 C10X 11(9) . . . . ? C5 C4 C7 C10X -175(8) . . . . ? C5 C6 C11 C13 79(3) . . . . ? C1 C6 C11 C13 -100(2) . . . . ? W1X O2 C12 C13 13(7) . . . . ? W1 O2 C12 C13 -24(7) . . . . ? W1X O2 C12 C17 -170(5) . . . . ? W1 O2 C12 C17 153(5) . . . . ? O2 C12 C13 C14 -179.6(19) . . . . ? C17 C12 C13 C14 3(3) . . . . ? O2 C12 C13 C11 5(3) . . . . ? C17 C12 C13 C11 -171.7(18) . . . . ? C6 C11 C13 C14 -98(3) . . . . ? C6 C11 C13 C12 77(2) . . . . ? C12 C13 C14 C15 0(4) . . . . ? C11 C13 C14 C15 174(2) . . . . ? C13 C14 C15 C18 180(2) . . . . ? C13 C14 C15 C16 -1(4) . . . . ? C14 C15 C16 C17 0(3) . . . . ? C18 C15 C16 C17 179(2) . . . . ? C15 C16 C17 C12 3(3) . . . . ? C15 C16 C17 C22 -176(2) . . . . ? O2 C12 C17 C16 178.3(18) . . . . ? C13 C12 C17 C16 -4(3) . . . . ? O2 C12 C17 C22 -3(3) . . . . ? C13 C12 C17 C22 174.1(19) . . . . ? C14 C15 C18 C21X 160(4) . . . . ? C16 C15 C18 C21X -19(4) . . . . ? C14 C15 C18 C19X -67(4) . . . . ? C16 C15 C18 C19X 114(3) . . . . ? C14 C15 C18 C19 2(5) . . . . ? C16 C15 C18 C19 -177(3) . . . . ? C14 C15 C18 C21 -124(3) . . . . ? C16 C15 C18 C21 57(3) . . . . ? C14 C15 C18 C20 121(3) . . . . ? C16 C15 C18 C20 -58(3) . . . . ? C14 C15 C18 C20X 46(3) . . . . ? C16 C15 C18 C20X -133(3) . . . . ? C16 C17 C22 C24 5(3) . . . . ? C12 C17 C22 C24 -173.6(17) . . . . ? W2 O3 C23 C24 121(5) . . . . ? W2 O3 C23 C28 -53(7) . . . . ? O3 C23 C24 C25 -178(2) . . . . ? C28 C23 C24 C25 -5(4) . . . . ? O3 C23 C24 C22 5(3) . . . . ? C28 C23 C24 C22 178(2) . . . . ? C17 C22 C24 C25 -112(2) . . . . ? C17 C22 C24 C23 65(3) . . . . ? C23 C24 C25 C26 4(4) . . . . ? C22 C24 C25 C26 -180(2) . . . . ? C24 C25 C26 C27 1(4) . . . . ? C24 C25 C26 C29 179(3) . . . . ? C25 C26 C27 C28 -5(4) . . . . ? C29 C26 C27 C28 177(3) . . . . ? C26 C27 C28 C23 3(4) . . . . ? C26 C27 C28 C33 -177(2) . . . . ? O3 C23 C28 C27 175(2) . . . . ? C24 C23 C28 C27 1(3) . . . . ? O3 C23 C28 C33 -4(3) . . . . ? C24 C23 C28 C33 -178(2) . . . . ? C27 C26 C29 C31 -134(3) . . . . ? C25 C26 C29 C31 49(4) . . . . ? C27 C26 C29 C32 -13(4) . . . . ? C25 C26 C29 C32 170(3) . . . . ? C27 C26 C29 C30 110(3) . . . . ? C25 C26 C29 C30 -68(4) . . . . ? C27 C28 C33 C35 -91(2) . . . . ? C23 C28 C33 C35 88(3) . . . . ? W2 O4 C34 C39 -114(2) . . . . ? W2 O4 C34 C35 68(3) . . . . ? O4 C34 C35 C36 179(2) . . . . ? C39 C34 C35 C36 2(3) . . . . ? O4 C34 C35 C33 6(3) . . . . ? C39 C34 C35 C33 -172(2) . . . . ? C28 C33 C35 C36 89(3) . . . . ? C28 C33 C35 C34 -97(2) . . . . ? C34 C35 C36 C37 2(4) . . . . ? C33 C35 C36 C37 175(2) . . . . ? C35 C36 C37 C38 -4(4) . . . . ? C35 C36 C37 C40 174(2) . . . . ? C36 C37 C38 C39 3(4) . . . . ? C40 C37 C38 C39 -175(2) . . . . ? C37 C38 C39 C34 0(4) . . . . ? C37 C38 C39 C44 -178(2) . . . . ? O4 C34 C39 C38 180(2) . . . . ? C35 C34 C39 C38 -3(3) . . . . ? O4 C34 C39 C44 -2(3) . . . . ? C35 C34 C39 C44 176(2) . . . . ? C36 C37 C40 C41X 113(4) . . . . ? C38 C37 C40 C41X -68(4) . . . . ? C36 C37 C40 C43X -124(4) . . . . ? C38 C37 C40 C43X 54(3) . . . . ? C36 C37 C40 C41 174(3) . . . . ? C38 C37 C40 C41 -7(4) . . . . ? C36 C37 C40 C43 -56(4) . . . . ? C38 C37 C40 C43 122(3) . . . . ? C36 C37 C40 C42X -7(4) . . . . ? C38 C37 C40 C42X 172(3) . . . . ? C36 C37 C40 C42 58(3) . . . . ? C38 C37 C40 C42 -124(3) . . . . ? C38 C39 C44 C2 -52(3) . . . 3_566 ? C34 C39 C44 C2 130(2) . . . 3_566 ? Cl9 C45 C46 Cl10 103(5) . . . . ? Cl11 C47 C48 Cl12 8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.845 _refine_diff_density_min -4.124 _refine_diff_density_rms 0.428 #===END