Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Douthwaite, Richard E.' 'Lobkovsky, Emil B.' 'Sydora, Orson L.' 'Vaid, Thomas P.' 'Wolczanski, Peter T.' _publ_contact_author_name 'Prof Peter T Wolczanski' _publ_contact_author_address ; Prof Peter T Wolczanski Department of Chemistry and Chemical Biology Baker Laboratory Cornell University Ithaca, NY 14853-1301 USA ; data_woph6 _database_code_CSD 156504 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H52 O14 W' _chemical_formula_weight 1060.77 _chemical_melting_point ? _chemical_compound_source ? 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' '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 10.3360(10) _cell_length_b 11.8990(10) _cell_length_c 21.761(3) _cell_angle_alpha 97.120(10) _cell_angle_beta 102.200(10) _cell_angle_gamma 108.510(10) _cell_volume 2427.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 3.924 _cell_measurement_theta_max 24.765 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method ? _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 2.444 _exptl_absorpt_correction_type 'empirical by \y-scans' _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.947 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.46 _diffrn_reflns_number 6719 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6303 _reflns_number_observed 5608 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+4.6551P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6287 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_obs 0.0326 _refine_ls_wR_factor_all 0.0987 _refine_ls_wR_factor_obs 0.0835 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_goodness_of_fit_obs 0.986 _refine_ls_restrained_S_all 1.093 _refine_ls_restrained_S_obs 0.986 _refine_ls_shift/esd_max 1.078 _refine_ls_shift/esd_mean 0.262 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.19904(2) 0.39635(2) 0.247912(11) 0.03880(12) Uani 1 d . . O1 O 0.2955(4) 0.4355(4) 0.3351(2) 0.0525(11) Uani 1 d . . O2 O 0.3693(4) 0.4582(4) 0.2201(2) 0.0448(10) Uani 1 d . . O3 O 0.0975(4) 0.3565(4) 0.1595(2) 0.0544(11) Uani 1 d . . O4 O 0.2262(4) 0.2463(4) 0.2421(2) 0.0494(11) Uani 1 d . . O5 O 0.0223(4) 0.3276(4) 0.2662(2) 0.0525(11) Uani 1 d . . O6 O 0.1808(4) 0.5496(4) 0.2569(2) 0.0503(11) Uani 1 d . . O7 O 0.3311(7) 0.3188(5) 0.5733(2) 0.080(2) Uani 1 d . . H7A H 0.3479(97) 0.3783(18) 0.6013(6) 0.096 Uiso 1 calc R . O8 O 0.5594(6) 0.7082(6) 0.0402(3) 0.079(2) Uani 1 d . . H8O H 0.6402(35) 0.7115(69) 0.0410(30) 0.094 Uiso 1 calc R . O9 O -0.4519(4) 0.1357(4) 0.0115(2) 0.0535(11) Uani 1 d . . H9O H -0.4817(28) 0.1848(11) -0.0041(27) 0.064 Uiso 1 calc R . O10 O 0.4560(8) -0.0373(6) 0.1152(3) 0.094(2) Uani 1 d . . H10O H 0.4384(95) -0.0379(77) 0.0766(8) 0.113 Uiso 1 calc R . O11 O -0.3901(5) 0.4864(5) 0.3267(2) 0.0710(15) Uani 1 d . . H11O H -0.4680(15) 0.4467(48) 0.3019(25) 0.085 Uiso 1 calc R . O12 O 0.3961(8) 1.0225(5) 0.3886(3) 0.099(2) Uani 1 d . . H12B H 0.4689(54) 1.0372(24) 0.4170(29) 0.080 Uiso 1 calc R . C1 C 0.3039(6) 0.4064(6) 0.3948(3) 0.047(2) Uani 1 d . . C2 C 0.3145(7) 0.4924(6) 0.4459(3) 0.053(2) Uani 1 d . . H2 H 0.3161(7) 0.5632(61) 0.4408(5) 0.064 Uiso 1 d R . C3 C 0.3226(7) 0.4631(7) 0.5056(3) 0.056(2) Uani 1 d . . H3 H 0.3292(9) 0.5231(50) 0.5420(30) 0.068 Uiso 1 d R . C4 C 0.3217(7) 0.3517(7) 0.5147(3) 0.056(2) Uani 1 d . . C5 C 0.3134(9) 0.2665(7) 0.4633(4) 0.074(2) Uani 1 d . . H5 H 0.3139(9) 0.1949(70) 0.4687(6) 0.089 Uiso 1 d R . C6 C 0.3042(9) 0.2944(7) 0.4028(4) 0.067(2) Uani 1 d . . H6 H 0.2987(10) 0.2342(49) 0.3660(30) 0.080 Uiso 1 d R . C7 C 0.4133(6) 0.5194(6) 0.1742(3) 0.0434(15) Uani 1 d . . C8 C 0.5273(8) 0.5073(7) 0.1551(4) 0.066(2) Uani 1 d . . H8A H 0.5690(39) 0.4606(44) 0.1713(16) 0.079 Uiso 1 d R . C9 C 0.5763(8) 0.5697(8) 0.1106(4) 0.073(2) Uani 1 d . . H9A H 0.6583(71) 0.5595(12) 0.0965(13) 0.088 Uiso 1 d R . C10 C 0.5131(7) 0.6440(7) 0.0850(3) 0.055(2) Uani 1 d . . C11 C 0.3986(7) 0.6555(7) 0.1036(4) 0.061(2) Uani 1 d . . H11A H 0.3574(39) 0.7023(45) 0.0872(16) 0.074 Uiso 1 d R . C12 C 0.3466(7) 0.5928(6) 0.1478(3) 0.055(2) Uani 1 d . . H12A H 0.2643(63) 0.6002(9) 0.1602(10) 0.066 Uiso 1 d R . C13 C -0.0404(6) 0.3014(6) 0.1242(3) 0.0432(14) Uani 1 d . . C14 C -0.0965(7) 0.1792(6) 0.1043(4) 0.060(2) Uani 1 d . . H14 H -0.0408(46) 0.1321(39) 0.1151(9) 0.072 Uiso 1 d R . C15 C -0.2355(7) 0.1248(6) 0.0677(4) 0.061(2) Uani 1 d . . H15 H -0.2722(33) 0.0466(69) 0.0562(11) 0.073 Uiso 1 d R . C16 C -0.3164(6) 0.1942(5) 0.0497(3) 0.0412(14) Uani 1 d . . C17 C -0.2585(7) 0.3166(6) 0.0711(3) 0.054(2) Uani 1 d . . H17 H -0.3081(43) 0.3602(38) 0.0618(9) 0.065 Uiso 1 d R . C18 C -0.1211(7) 0.3696(6) 0.1076(3) 0.060(2) Uani 1 d . . H18 H -0.0892(33) 0.4379(70) 0.1185(12) 0.072 Uiso 1 d R . C19 C 0.2797(6) 0.1749(5) 0.2083(3) 0.0425(14) Uani 1 d . . C20 C 0.2897(7) 0.1863(6) 0.1471(3) 0.054(2) Uani 1 d . . H20 H 0.2572(26) 0.2442(45) 0.1267(16) 0.065 Uiso 1 d R . C21 C 0.3475(8) 0.1153(6) 0.1148(3) 0.059(2) Uani 1 d . . H21 H 0.3527(9) 0.1208(8) 0.0750(36) 0.071 Uiso 1 d R . C22 C 0.3968(8) 0.0356(7) 0.1446(4) 0.063(2) Uani 1 d . . C23 C 0.3853(9) 0.0245(7) 0.2046(4) 0.069(2) Uani 1 d . . H23 H 0.4100(29) -0.0194(49) 0.2199(18) 0.083 Uiso 1 d R . C24 C 0.3268(7) 0.0950(6) 0.2379(3) 0.054(2) Uani 1 d . . H24 H 0.3201(9) 0.0878(8) 0.2801(32) 0.065 Uiso 1 d R . C25 C -0.0809(6) 0.3662(6) 0.2826(3) 0.0430(15) Uani 1 d . . C26 C -0.2201(6) 0.3028(6) 0.2490(3) 0.048(2) Uani 1 d . . H26 H -0.2415(18) 0.2400(51) 0.2190(24) 0.058 Uiso 1 d R . C27 C -0.3251(7) 0.3410(6) 0.2643(3) 0.054(2) Uani 1 d . . H27 H -0.4166(73) 0.2993(34) 0.2435(17) 0.064 Uiso 1 d R . C28 C -0.2899(6) 0.4427(7) 0.3110(3) 0.052(2) Uani 1 d . . C29 C -0.1515(6) 0.5044(7) 0.3450(3) 0.055(2) Uani 1 d . . H29 H -0.1268(19) 0.5767(53) 0.3791(25) 0.066 Uiso 1 d R . C30 C -0.0456(7) 0.4650(7) 0.3311(3) 0.056(2) Uani 1 d . . H30 H 0.0503(76) 0.5055(33) 0.3551(19) 0.067 Uiso 1 d R . C31 C 0.2399(7) 0.6678(6) 0.2901(3) 0.048(2) Uani 1 d . . C32 C 0.3794(8) 0.7167(6) 0.3244(4) 0.064(2) Uani 1 d . . H32 H 0.4316(50) 0.6740(41) 0.3249(4) 0.077 Uiso 1 d R . C33 C 0.4348(9) 0.8351(7) 0.3577(4) 0.073(2) Uani 1 d . . H33 H 0.5226(87) 0.8661(31) 0.3792(21) 0.087 Uiso 1 d R . C34 C 0.3494(10) 0.9039(7) 0.3571(4) 0.072(2) Uani 1 d . . C35 C 0.2099(9) 0.8534(7) 0.3222(4) 0.072(2) Uani 1 d . . H35 H 0.1447(52) 0.9056(41) 0.3217(4) 0.086 Uiso 1 d R . C36 C 0.1541(8) 0.7358(7) 0.2884(4) 0.061(2) Uani 1 d . . H36 H 0.0599(80) 0.7029(29) 0.2645(20) 0.073 Uiso 1 d R . O1S O 0.6823(9) 1.1211(7) 0.4395(4) 0.140(3) Uani 1 d . . C1S C 0.7625(18) 1.2159(14) 0.4149(8) 0.177(6) Uani 1 d . . C2S C 0.7725(19) 1.1067(16) 0.4934(7) 0.207(8) Uani 1 d . . C3S C 0.8960(17) 1.2793(16) 0.4645(10) 0.208(9) Uani 1 d . . C4S C 0.9006(19) 1.2124(18) 0.5100(9) 0.238(11) Uani 1 d . . O2S O 0.1748(8) 0.2574(10) -0.0403(5) 0.152(3) Uani 1 d . . C5S C 0.0642(29) 0.1681(15) -0.0919(15) 0.266(14) Uani 1 d . . C6S C -0.0313(23) 0.2274(24) -0.1062(11) 0.232(11) Uani 1 d . . C7S C -0.0246(16) 0.3033(21) -0.0527(9) 0.184(7) Uani 1 d . . C8S C 0.1194(13) 0.3344(15) -0.0117(6) 0.155(5) Uani 1 d . . C1P C -0.0430 0.0280 0.3090 0.095 Uiso 0.33 d P . C2P C -0.0770 -0.0670 0.3420 0.219 Uiso 0.33 d P . C3P C -0.1280 0.0250 0.2530 0.094 Uiso 0.33 d P . C4P C -0.2100 -0.1610 0.3090 0.115 Uiso 0.33 d P . C5P C -0.2540 -0.0740 0.2280 0.142 Uiso 0.33 d P . C6P C -0.2890 -0.1690 0.2600 0.318 Uiso 0.33 d P . C1AP C -0.0490 -0.0140 0.3420 0.064 Uiso 0.33 d P . C2AP C -0.1410 -0.1310 0.3390 0.093 Uiso 0.33 d P . C3AP C -0.0680 0.0430 0.2940 0.124 Uiso 0.33 d P . C4AP C -0.2530 -0.1760 0.2800 0.126 Uiso 0.33 d P . C5AP C -0.1820 -0.0150 0.2390 0.142 Uiso 0.33 d P . C6AP C -0.2750 -0.1310 0.2360 0.181 Uiso 0.33 d P . C1BP C -0.0420 0.0090 0.3280 0.205 Uiso 0.33 d P . C2BP C -0.1070 -0.1010 0.3440 0.152 Uiso 0.33 d P . C3BP C -0.1000 0.0350 0.2730 0.109 Uiso 0.33 d P . C4BP C -0.2360 -0.1760 0.2980 0.132 Uiso 0.33 d P . C5BP C -0.2260 -0.0490 0.2320 0.145 Uiso 0.33 d P . C6BP C -0.2910 -0.1580 0.2490 0.062 Uiso 0.33 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0318(2) 0.0442(2) 0.0404(2) 0.00930(11) 0.01082(10) 0.01254(11) O1 0.049(3) 0.059(3) 0.042(3) 0.008(2) 0.008(2) 0.013(2) O2 0.035(2) 0.056(3) 0.049(2) 0.023(2) 0.014(2) 0.018(2) O3 0.044(3) 0.067(3) 0.042(2) 0.012(2) 0.005(2) 0.009(2) O4 0.050(3) 0.052(3) 0.056(3) 0.016(2) 0.026(2) 0.020(2) O5 0.044(3) 0.056(3) 0.066(3) 0.017(2) 0.028(2) 0.018(2) O6 0.046(2) 0.050(3) 0.056(3) 0.008(2) 0.018(2) 0.018(2) O7 0.110(5) 0.090(4) 0.050(3) 0.026(3) 0.024(3) 0.043(4) O8 0.067(3) 0.113(4) 0.098(4) 0.073(4) 0.050(3) 0.053(3) O9 0.041(2) 0.047(3) 0.064(3) 0.012(2) 0.003(2) 0.011(2) O10 0.133(5) 0.089(4) 0.090(4) 0.009(4) 0.062(4) 0.062(4) O11 0.042(3) 0.110(4) 0.062(3) -0.001(3) 0.011(2) 0.037(3) O12 0.129(6) 0.052(3) 0.107(5) -0.003(3) 0.026(4) 0.031(4) C1 0.037(3) 0.056(4) 0.044(4) 0.010(3) 0.010(3) 0.013(3) C2 0.057(4) 0.050(4) 0.053(4) 0.009(3) 0.012(3) 0.022(3) C3 0.057(4) 0.073(5) 0.041(4) 0.003(4) 0.012(3) 0.030(4) C4 0.058(4) 0.066(5) 0.048(4) 0.019(4) 0.015(3) 0.023(4) C5 0.107(7) 0.053(5) 0.063(5) 0.019(4) 0.023(4) 0.027(4) C6 0.093(6) 0.055(5) 0.047(4) 0.001(3) 0.017(4) 0.023(4) C7 0.035(3) 0.050(4) 0.051(4) 0.016(3) 0.016(3) 0.017(3) C8 0.065(5) 0.085(6) 0.085(6) 0.049(5) 0.042(4) 0.050(4) C9 0.071(5) 0.091(6) 0.104(6) 0.061(5) 0.058(5) 0.053(5) C10 0.051(4) 0.073(5) 0.056(4) 0.033(4) 0.024(3) 0.029(4) C11 0.057(4) 0.079(5) 0.074(5) 0.042(4) 0.029(4) 0.042(4) C12 0.050(4) 0.071(5) 0.060(4) 0.024(4) 0.022(3) 0.032(4) C13 0.040(4) 0.047(4) 0.039(3) 0.008(3) 0.008(3) 0.013(3) C14 0.051(4) 0.050(4) 0.075(5) 0.017(4) 0.006(4) 0.020(4) C15 0.053(4) 0.038(4) 0.081(5) 0.007(3) 0.007(4) 0.013(3) C16 0.036(3) 0.044(4) 0.041(3) 0.012(3) 0.011(3) 0.009(3) C17 0.055(4) 0.046(4) 0.059(4) 0.007(3) 0.001(3) 0.024(3) C18 0.061(5) 0.036(4) 0.065(5) 0.000(3) -0.001(4) 0.009(3) C19 0.038(3) 0.040(3) 0.051(4) 0.007(3) 0.017(3) 0.013(3) C20 0.055(4) 0.059(4) 0.058(4) 0.021(3) 0.023(3) 0.025(4) C21 0.069(5) 0.065(5) 0.046(4) 0.009(3) 0.027(4) 0.021(4) C22 0.072(5) 0.058(4) 0.066(5) 0.002(4) 0.038(4) 0.023(4) C23 0.089(6) 0.059(5) 0.077(6) 0.021(4) 0.033(5) 0.042(4) C24 0.072(5) 0.045(4) 0.052(4) 0.014(3) 0.026(4) 0.021(4) C25 0.034(3) 0.049(4) 0.051(4) 0.017(3) 0.020(3) 0.014(3) C26 0.040(4) 0.047(4) 0.055(4) 0.009(3) 0.013(3) 0.012(3) C27 0.031(3) 0.065(4) 0.052(4) 0.014(4) 0.004(3) 0.004(3) C28 0.037(4) 0.074(5) 0.048(4) 0.019(4) 0.015(3) 0.021(3) C29 0.040(4) 0.074(5) 0.045(4) -0.002(3) 0.011(3) 0.019(3) C30 0.035(4) 0.075(5) 0.046(4) 0.002(3) 0.008(3) 0.010(3) C31 0.049(4) 0.045(4) 0.057(4) 0.015(3) 0.023(3) 0.018(3) C32 0.054(4) 0.052(4) 0.085(5) 0.012(4) 0.010(4) 0.023(4) C33 0.069(5) 0.056(5) 0.080(5) 0.006(4) 0.006(4) 0.017(4) C34 0.101(7) 0.048(5) 0.066(5) 0.009(4) 0.030(5) 0.021(5) C35 0.079(6) 0.058(5) 0.094(6) 0.023(4) 0.034(5) 0.035(5) C36 0.053(4) 0.054(5) 0.083(5) 0.021(4) 0.023(4) 0.023(4) O1S 0.140(7) 0.104(5) 0.122(6) 0.028(5) 0.003(5) -0.009(5) C1S 0.181(14) 0.158(12) 0.179(14) 0.117(11) 0.039(11) 0.019(11) C2S 0.197(16) 0.224(17) 0.129(11) 0.107(12) -0.002(11) -0.016(13) C3S 0.135(13) 0.176(15) 0.232(20) 0.103(14) -0.029(13) -0.024(11) C4S 0.174(15) 0.212(18) 0.193(17) 0.087(14) -0.057(13) -0.058(13) O2S 0.077(5) 0.192(9) 0.212(10) 0.063(8) 0.063(6) 0.057(6) C5S 0.202(24) 0.112(11) 0.426(38) -0.068(16) 0.065(24) 0.035(13) C6S 0.164(18) 0.276(27) 0.165(18) -0.059(18) -0.017(14) 0.034(16) C7S 0.110(11) 0.311(24) 0.184(16) 0.096(16) 0.048(11) 0.120(14) C8S 0.094(8) 0.243(16) 0.126(10) 0.008(10) 0.050(8) 0.056(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 1.870(4) . ? W1 O4 1.887(4) . ? W1 O6 1.883(4) . ? W1 O5 1.898(4) . ? W1 O3 1.906(4) . ? W1 O2 1.934(4) . ? O1 C1 1.378(7) . ? O2 C7 1.378(7) . ? O3 C13 1.368(7) . ? O4 C19 1.372(7) . ? O5 C25 1.381(7) . ? O6 C31 1.374(8) . ? O7 C4 1.372(8) . ? O8 C10 1.383(8) . ? O9 C16 1.372(7) . ? O10 C22 1.379(8) . ? O11 C28 1.381(8) . ? O12 C34 1.372(9) . ? C1 C6 1.366(10) . ? C1 C2 1.375(9) . ? C2 C3 1.379(9) . ? C3 C4 1.362(10) . ? C4 C5 1.382(10) . ? C5 C6 1.386(10) . ? C7 C8 1.372(9) . ? C7 C12 1.381(9) . ? C8 C9 1.377(10) . ? C9 C10 1.360(9) . ? C10 C11 1.370(9) . ? C11 C12 1.382(9) . ? C13 C14 1.356(9) . ? C13 C18 1.365(9) . ? C14 C15 1.384(9) . ? C15 C16 1.385(9) . ? C16 C17 1.362(9) . ? C17 C18 1.369(9) . ? C19 C24 1.369(9) . ? C19 C20 1.378(9) . ? C20 C21 1.384(9) . ? C21 C22 1.378(10) . ? C22 C23 1.355(10) . ? C23 C24 1.396(10) . ? C25 C30 1.373(9) . ? C25 C26 1.379(8) . ? C26 C27 1.388(9) . ? C27 C28 1.373(10) . ? C28 C29 1.372(9) . ? C29 C30 1.393(9) . ? C31 C32 1.371(9) . ? C31 C36 1.375(9) . ? C32 C33 1.378(10) . ? C33 C34 1.381(11) . ? C34 C35 1.375(12) . ? C35 C36 1.373(11) . ? O1S C2S 1.40(2) . ? O1S C1S 1.41(2) . ? C1S C3S 1.46(3) . ? C2S C4S 1.45(3) . ? C3S C4S 1.35(3) . ? O2S C8S 1.38(2) . ? O2S C5S 1.44(3) . ? C5S C6S 1.39(3) . ? C6S C7S 1.36(3) . ? C7S C8S 1.47(2) . ? C1P C3BP 0.91 . ? C1P C1AP 0.93 . ? C1P C3P 1.33 . ? C1P C2P 1.40 . ? C1P C5AP 1.75 . ? C1P C2BP 1.80 . ? C2P C1AP 0.60 . ? C2P C2AP 0.82 . ? C2P C1BP 0.97 . ? C2P C4P 1.44 . ? C2P C4BP 1.72 . ? C2P C3AP 1.77 . ? C2P C4AP 1.96 . ? C3P C5AP 0.60 . ? C3P C3AP 0.93 . ? C3P C5BP 1.07 . ? C3P C5P 1.40 . ? C3P C1BP 1.75 . ? C3P C6AP 1.92 . ? C4P C4AP 0.66 . ? C4P C2AP 0.80 . ? C4P C2BP 1.12 . ? C4P C6P 1.17 . ? C4P C6BP 1.41 . ? C4P C6AP 1.72 . ? C4P C1AP 1.92 . ? C5P C6AP 0.70 . ? C5P C5AP 0.81 . ? C5P C6BP 1.14 . ? C5P C6P 1.39 . ? C5P C3BP 1.70 . ? C5P C4AP 1.76 . ? C6P C4AP 0.54 . ? C6P C6AP 0.74 . ? C6P C4BP 0.92 . ? C6P C5BP 1.62 . ? C6P C2AP 1.94 . ? C6P C5AP 1.98 . ? C1AP C2BP 1.03 . ? C1AP C3AP 1.33 . ? C1AP C2AP 1.40 . ? C1AP C3BP 1.72 . ? C2AP C4BP 1.11 . ? C2AP C4AP 1.44 . ? C2AP C1BP 1.73 . ? C3AP C1BP 0.92 . ? C3AP C5AP 1.41 . ? C3AP C5BP 1.80 . ? C4AP C6BP 0.80 . ? C4AP C6AP 1.17 . ? C4AP C2BP 1.72 . ? C4AP C5BP 1.92 . ? C5AP C3BP 0.96 . ? C5AP C6AP 1.39 . ? C5AP C6BP 1.79 . ? C6AP C5BP 0.97 . ? C6AP C4BP 1.53 . ? C1BP C3BP 1.34 . ? C1BP C2BP 1.39 . ? C2BP C4BP 1.43 . ? C3BP C5BP 1.40 . ? C4BP C6BP 1.18 . ? C5BP C6BP 1.39 . ? 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 O4 88.8(2) . . ? O1 W1 O6 88.8(2) . . ? O4 W1 O6 177.1(2) . . ? O1 W1 O5 91.6(2) . . ? O4 W1 O5 91.0(2) . . ? O6 W1 O5 90.7(2) . . ? O1 W1 O3 178.9(2) . . ? O4 W1 O3 91.7(2) . . ? O6 W1 O3 90.8(2) . . ? O5 W1 O3 87.4(2) . . ? O1 W1 O2 94.1(2) . . ? O4 W1 O2 87.7(2) . . ? O6 W1 O2 90.9(2) . . ? O5 W1 O2 174.1(2) . . ? O3 W1 O2 86.9(2) . . ? C1 O1 W1 148.0(4) . . ? C7 O2 W1 138.7(4) . . ? C13 O3 W1 136.8(4) . . ? C19 O4 W1 141.9(4) . . ? C25 O5 W1 137.9(4) . . ? C31 O6 W1 145.2(4) . . ? C6 C1 O1 120.1(6) . . ? C6 C1 C2 121.0(6) . . ? O1 C1 C2 118.9(6) . . ? C3 C2 C1 118.9(7) . . ? C4 C3 C2 121.2(7) . . ? C3 C4 O7 123.3(7) . . ? C3 C4 C5 119.4(7) . . ? O7 C4 C5 117.2(7) . . ? C6 C5 C4 120.0(7) . . ? C1 C6 C5 119.5(7) . . ? C8 C7 C12 119.8(6) . . ? C8 C7 O2 118.5(6) . . ? C12 C7 O2 121.7(5) . . ? C9 C8 C7 120.0(7) . . ? C10 C9 C8 120.9(7) . . ? C9 C10 C11 119.2(6) . . ? C9 C10 O8 122.5(6) . . ? C11 C10 O8 118.3(6) . . ? C10 C11 C12 121.0(7) . . ? C7 C12 C11 119.1(6) . . ? C14 C13 C18 119.7(6) . . ? C14 C13 O3 120.3(6) . . ? C18 C13 O3 120.0(6) . . ? C13 C14 C15 119.7(7) . . ? C16 C15 C14 120.5(6) . . ? C17 C16 O9 123.3(6) . . ? C17 C16 C15 118.7(6) . . ? O9 C16 C15 118.0(6) . . ? C16 C17 C18 120.3(6) . . ? C13 C18 C17 121.0(6) . . ? C24 C19 O4 118.1(6) . . ? C24 C19 C20 121.0(6) . . ? O4 C19 C20 120.9(6) . . ? C21 C20 C19 119.6(7) . . ? C20 C21 C22 119.7(7) . . ? C23 C22 O10 117.3(7) . . ? C23 C22 C21 120.1(7) . . ? O10 C22 C21 122.6(7) . . ? C22 C23 C24 121.0(7) . . ? C19 C24 C23 118.5(7) . . ? C30 C25 C26 121.0(6) . . ? C30 C25 O5 120.8(5) . . ? C26 C25 O5 118.2(6) . . ? C25 C26 C27 119.0(6) . . ? C28 C27 C26 120.2(6) . . ? C29 C28 C27 120.6(6) . . ? C29 C28 O11 117.1(6) . . ? C27 C28 O11 122.3(6) . . ? C28 C29 C30 119.7(7) . . ? C25 C30 C29 119.5(6) . . ? C32 C31 O6 121.5(6) . . ? C32 C31 C36 120.8(7) . . ? O6 C31 C36 117.8(6) . . ? C31 C32 C33 119.9(7) . . ? C34 C33 C32 120.0(8) . . ? C35 C34 C33 119.3(7) . . ? C35 C34 O12 117.0(8) . . ? C33 C34 O12 123.7(9) . . ? C36 C35 C34 121.1(8) . . ? C35 C36 C31 119.0(8) . . ? C2S O1S C1S 108.1(15) . . ? O1S C1S C3S 106.6(17) . . ? O1S C2S C4S 106.3(20) . . ? C4S C3S C1S 107.3(22) . . ? C3S C4S C2S 109.8(24) . . ? C8S O2S C5S 109.1(15) . . ? C6S C5S O2S 101.5(21) . . ? C7S C6S C5S 110.3(25) . . ? C6S C7S C8S 104.7(20) . . ? O2S C8S C7S 105.6(15) . . ? C3BP C1P C1AP 139.4 . . ? C3BP C1P C3P 6.9 . . ? C1AP C1P C3P 136.7 . . ? C3BP C1P C2P 125.5 . . ? C1AP C1P C2P 18.6 . . ? C3P C1P C2P 121.2 . . ? C3BP C1P C5AP 21.1 . . ? C1AP C1P C5AP 121.1 . . ? C3P C1P C5AP 16.0 . . ? C2P C1P C5AP 105.2 . . ? C3BP C1P C2BP 118.5 . . ? C1AP C1P C2BP 24.6 . . ? C3P C1P C2BP 114.3 . . ? C2P C1P C2BP 7.0 . . ? C5AP C1P C2BP 98.3 . . ? C1AP C2P C2AP 158.3 . . ? C1AP C2P C1BP 17.4 . . ? C2AP C2P C1BP 149.8 . . ? C1AP C2P C1P 29.3 . . ? C2AP C2P C1P 139.7 . . ? C1BP C2P C1P 12.0 . . ? C1AP C2P C4P 136.0 . . ? C2AP C2P C4P 27.4 . . ? C1BP C2P C4P 123.0 . . ? C1P C2P C4P 112.4 . . ? C1AP C2P C4BP 133.1 . . ? C2AP C2P C4BP 31.1 . . ? C1BP C2P C4BP 119.6 . . ? C1P C2P C4BP 108.8 . . ? C4P C2P C4BP 3.7 . . ? C1AP C2P C3AP 36.4 . . ? C2AP C2P C3AP 129.8 . . ? C1BP C2P C3AP 20.4 . . ? C1P C2P C3AP 10.5 . . ? C4P C2P C3AP 102.6 . . ? C4BP C2P C3AP 99.2 . . ? C1AP C2P C4AP 124.6 . . ? C2AP C2P C4AP 40.8 . . ? C1BP C2P C4AP 110.2 . . ? C1P C2P C4AP 99.2 . . ? C4P C2P C4AP 13.5 . . ? C4BP C2P C4AP 9.8 . . ? C3AP C2P C4AP 89.8 . . ? C5AP C3P C3AP 133.8 . . ? C5AP C3P C5BP 5.3 . . ? C3AP C3P C5BP 128.7 . . ? C5AP C3P C1P 126.0 . . ? C3AP C3P C1P 11.5 . . ? C5BP C3P C1P 121.2 . . ? C5AP C3P C5P 7.7 . . ? C3AP C3P C5P 126.1 . . ? C5BP C3P C5P 2.7 . . ? C1P C3P C5P 118.6 . . ? C5AP C3P C1BP 116.4 . . ? C3AP C3P C1BP 18.5 . . ? C5BP C3P C1BP 111.6 . . ? C1P C3P C1BP 10.0 . . ? C5P C3P C1BP 108.9 . . ? C5AP C3P C6AP 23.1 . . ? C3AP C3P C6AP 111.4 . . ? C5BP C3P C6AP 18.8 . . ? C1P C3P C6AP 103.0 . . ? C5P C3P C6AP 16.2 . . ? C1BP C3P C6AP 93.6 . . ? C4AP C4P C2AP 162.5 . . ? C4AP C4P C2BP 149.3 . . ? C2AP C4P C2BP 14.2 . . ? C4AP C4P C6P 11.5 . . ? C2AP C4P C6P 157.6 . . ? C2BP C4P C6P 143.5 . . ? C4AP C4P C6BP 16.0 . . ? C2AP C4P C6BP 150.4 . . ? C2BP C4P C6BP 136.3 . . ? C6P C4P C6BP 7.4 . . ? C4AP C4P C2P 135.6 . . ? C2AP C4P C2P 28.0 . . ? C2BP C4P C2P 13.9 . . ? C6P C4P C2P 129.7 . . ? C6BP C4P C2P 122.4 . . ? C4AP C4P C6AP 27.0 . . ? C2AP C4P C6AP 137.7 . . ? C2BP C4P C6AP 123.6 . . ? C6P C4P C6AP 20.3 . . ? C6BP C4P C6AP 13.0 . . ? C2P C4P C6AP 109.7 . . ? C4AP C4P C1AP 125.0 . . ? C2AP C4P C1AP 39.8 . . ? C2BP C4P C1AP 25.8 . . ? C6P C4P C1AP 117.8 . . ? C6BP C4P C1AP 110.8 . . ? C2P C4P C1AP 12.6 . . ? C6AP C4P C1AP 98.3 . . ? C6AP C5P C5AP 134.8 . . ? C6AP C5P C6BP 10.3 . . ? C5AP C5P C6BP 132.1 . . ? C6AP C5P C6P 15.2 . . ? C5AP C5P C6P 126.3 . . ? C6BP C5P C6P 6.3 . . ? C6AP C5P C3P 130.0 . . ? C5AP C5P C3P 5.7 . . ? C6BP C5P C3P 126.8 . . ? C6P C5P C3P 120.9 . . ? C6AP C5P C3BP 119.3 . . ? C5AP C5P C3BP 17.8 . . ? C6BP C5P C3BP 115.1 . . ? C6P C5P C3BP 109.1 . . ? C3P C5P C3BP 12.2 . . ? C6AP C5P C4AP 25.7 . . ? C5AP C5P C4AP 111.8 . . ? C6BP C5P C4AP 20.2 . . ? C6P C5P C4AP 14.6 . . ? C3P C5P C4AP 106.5 . . ? C3BP C5P C4AP 94.9 . . ? C4AP C6P C6AP 130.8 . . ? C4AP C6P C4BP 9.5 . . ? C6AP C6P C4BP 135.1 . . ? C4AP C6P C4P 13.9 . . ? C6AP C6P C4P 126.4 . . ? C4BP C6P C4P 9.6 . . ? C4AP C6P C5P 125.0 . . ? C6AP C6P C5P 14.4 . . ? C4BP C6P C5P 126.7 . . ? C4P C6P C5P 117.3 . . ? C4AP C6P C5BP 116.2 . . ? C6AP C6P C5BP 21.4 . . ? C4BP C6P C5BP 117.7 . . ? C4P C6P C5BP 108.3 . . ? C5P C6P C5BP 9.0 . . ? C4AP C6P C2AP 20.8 . . ? C6AP C6P C2AP 117.6 . . ? C4BP C6P C2AP 18.6 . . ? C4P C6P C2AP 9.1 . . ? C5P C6P C2AP 108.2 . . ? C5BP C6P C2AP 99.2 . . ? C4AP C6P C5AP 106.0 . . ? C6AP C6P C5AP 30.3 . . ? C4BP C6P C5AP 107.5 . . ? C4P C6P C5AP 98.1 . . ? C5P C6P C5AP 19.2 . . ? C5BP C6P C5AP 10.3 . . ? C2AP C6P C5AP 89.0 . . ? C2P C1AP C1P 132.0 . . ? C2P C1AP C2BP 7.7 . . ? C1P C1AP C2BP 133.5 . . ? C2P C1AP C3AP 127.9 . . ? C1P C1AP C3AP 11.8 . . ? C2BP C1AP C3AP 127.5 . . ? C2P C1AP C2AP 12.5 . . ? C1P C1AP C2AP 127.7 . . ? C2BP C1AP C2AP 7.0 . . ? C3AP C1AP C2AP 121.1 . . ? C2P C1AP C3BP 117.3 . . ? C1P C1AP C3BP 20.1 . . ? C2BP C1AP C3BP 116.8 . . ? C3AP C1AP C3BP 10.8 . . ? C2AP C1AP C3BP 110.3 . . ? C2P C1AP C4P 31.3 . . ? C1P C1AP C4P 106.9 . . ? C2BP C1AP C4P 28.4 . . ? C3AP C1AP C4P 99.6 . . ? C2AP C1AP C4P 21.6 . . ? C3BP C1AP C4P 88.8 . . ? C4P C2AP C2P 124.5 . . ? C4P C2AP C4BP 2.3 . . ? C2P C2AP C4BP 126.5 . . ? C4P C2AP C1AP 118.6 . . ? C2P C2AP C1AP 9.2 . . ? C4BP C2AP C1AP 120.7 . . ? C4P C2AP C4AP 7.9 . . ? C2P C2AP C4AP 117.4 . . ? C4BP C2AP C4AP 9.3 . . ? C1AP C2AP C4AP 112.0 . . ? C4P C2AP C1BP 108.7 . . ? C2P C2AP C1BP 16.4 . . ? C4BP C2AP C1BP 110.7 . . ? C1AP C2AP C1BP 10.4 . . ? C4AP C2AP C1BP 101.9 . . ? C4P C2AP C6P 13.3 . . ? C2P C2AP C6P 111.3 . . ? C4BP C2AP C6P 15.4 . . ? C1AP C2AP C6P 105.3 . . ? C4AP C2AP C6P 7.7 . . ? C1BP C2AP C6P 95.4 . . ? C1BP C3AP C3P 142.9 . . ? C1BP C3AP C1AP 7.8 . . ? C3P C3AP C1AP 137.1 . . ? C1BP C3AP C5AP 126.0 . . ? C3P C3AP C5AP 17.8 . . ? C1AP C3AP C5AP 119.7 . . ? C1BP C3AP C2P 21.8 . . ? C3P C3AP C2P 121.5 . . ? C1AP C3AP C2P 15.7 . . ? C5AP C3AP C2P 104.3 . . ? C1BP C3AP C5BP 116.8 . . ? C3P C3AP C5BP 27.6 . . ? C1AP C3AP C5BP 110.2 . . ? C5AP C3AP C5BP 9.9 . . ? C2P C3AP C5BP 95.0 . . ? C6P C4AP C4P 154.7 . . ? C6P C4AP C6BP 11.9 . . ? C4P C4AP C6BP 150.9 . . ? C6P C4AP C6AP 28.6 . . ? C4P C4AP C6AP 138.3 . . ? C6BP C4AP C6AP 16.8 . . ? C6P C4AP C2AP 151.5 . . ? C4P C4AP C2AP 9.6 . . ? C6BP C4AP C2AP 144.6 . . ? C6AP C4AP C2AP 130.2 . . ? C6P C4AP C2BP 142.9 . . ? C4P C4AP C2BP 19.5 . . ? C6BP C4AP C2BP 134.8 . . ? C6AP C4AP C2BP 120.0 . . ? C2AP C4AP C2BP 10.3 . . ? C6P C4AP C5P 40.4 . . ? C4P C4AP C5P 123.3 . . ? C6BP C4AP C5P 29.7 . . ? C6AP C4AP C5P 15.0 . . ? C2AP C4AP C5P 115.6 . . ? C2BP C4AP C5P 105.5 . . ? C6P C4AP C5BP 49.1 . . ? C4P C4AP C5BP 114.8 . . ? C6BP C4AP C5BP 38.6 . . ? C6AP C4AP C5BP 23.5 . . ? C2AP C4AP C5BP 106.8 . . ? C2BP C4AP C5BP 96.6 . . ? C5P C4AP C5BP 8.9 . . ? C6P C4AP C2P 132.7 . . ? C4P C4AP C2P 30.8 . . ? C6BP C4AP C2P 123.7 . . ? C6AP C4AP C2P 108.6 . . ? C2AP C4AP C2P 21.8 . . ? C2BP C4AP C2P 11.5 . . ? C5P C4AP C2P 94.2 . . ? C5BP C4AP C2P 85.3 . . ? C3P C5AP C5P 166.6 . . ? C3P C5AP C3BP 19.4 . . ? C5P C5AP C3BP 147.2 . . ? C3P C5AP C6AP 147.3 . . ? C5P C5AP C6AP 20.9 . . ? C3BP C5AP C6AP 128.7 . . ? C3P C5AP C3AP 28.4 . . ? C5P C5AP C3AP 138.2 . . ? C3BP C5AP C3AP 9.2 . . ? C6AP C5AP C3AP 119.5 . . ? C3P C5AP C1P 38.0 . . ? C5P C5AP C1P 129.0 . . ? C3BP C5AP C1P 19.8 . . ? C6AP C5AP C1P 109.3 . . ? C3AP C5AP C1P 11.3 . . ? C3P C5AP C6BP 139.0 . . ? C5P C5AP C6BP 28.3 . . ? C3BP C5AP C6BP 120.0 . . ? C6AP C5AP C6BP 9.3 . . ? C3AP C5AP C6BP 110.8 . . ? C1P C5AP C6BP 101.0 . . ? C3P C5AP C6P 132.6 . . ? C5P C5AP C6P 34.5 . . ? C3BP C5AP C6P 113.6 . . ? C6AP C5AP C6P 15.5 . . ? C3AP C5AP C6P 104.4 . . ? C1P C5AP C6P 94.6 . . ? C6BP C5AP C6P 6.4 . . ? C5P C6AP C6P 150.4 . . ? C5P C6AP C5BP 13.0 . . ? C6P C6AP C5BP 142.4 . . ? C5P C6AP C4AP 139.3 . . ? C6P C6AP C4AP 20.6 . . ? C5BP C6AP C4AP 127.7 . . ? C5P C6AP C5AP 24.4 . . ? C6P C6AP C5AP 134.1 . . ? C5BP C6AP C5AP 11.4 . . ? C4AP C6AP C5AP 117.5 . . ? C5P C6AP C4BP 133.0 . . ? C6P C6AP C4BP 25.0 . . ? C5BP C6AP C4BP 121.6 . . ? C4AP C6AP C4BP 6.3 . . ? C5AP C6AP C4BP 111.5 . . ? C5P C6AP C4P 124.6 . . ? C6P C6AP C4P 33.3 . . ? C5BP C6AP C4P 113.0 . . ? C4AP C6AP C4P 14.8 . . ? C5AP C6AP C4P 102.8 . . ? C4BP C6AP C4P 8.7 . . ? C5P C6AP C3P 33.8 . . ? C6P C6AP C3P 125.2 . . ? C5BP C6AP C3P 20.8 . . ? C4AP C6AP C3P 107.9 . . ? C5AP C6AP C3P 9.6 . . ? C4BP C6AP C3P 102.0 . . ? C4P C6AP C3P 93.3 . . ? C3AP C1BP C2P 137.8 . . ? C3AP C1BP C3BP 12.1 . . ? C2P C1BP C3BP 125.8 . . ? C3AP C1BP C2BP 132.0 . . ? C2P C1BP C2BP 6.4 . . ? C3BP C1BP C2BP 120.1 . . ? C3AP C1BP C2AP 124.4 . . ? C2P C1BP C2AP 13.8 . . ? C3BP C1BP C2AP 112.6 . . ? C2BP C1BP C2AP 7.6 . . ? C3AP C1BP C3P 18.7 . . ? C2P C1BP C3P 119.5 . . ? C3BP C1BP C3P 6.6 . . ? C2BP C1BP C3P 113.9 . . ? C2AP C1BP C3P 106.4 . . ? C1AP C2BP C4P 125.8 . . ? C1AP C2BP C1BP 11.6 . . ? C4P C2BP C1BP 115.2 . . ? C1AP C2BP C4BP 124.5 . . ? C4P C2BP C4BP 1.8 . . ? C1BP C2BP C4BP 113.8 . . ? C1AP C2BP C4AP 115.6 . . ? C4P C2BP C4AP 11.2 . . ? C1BP C2BP C4AP 104.6 . . ? C4BP C2BP C4AP 9.6 . . ? C1AP C2BP C1P 21.9 . . ? C4P C2BP C1P 105.5 . . ? C1BP C2BP C1P 10.3 . . ? C4BP C2BP C1P 104.0 . . ? C4AP C2BP C1P 94.7 . . ? C1P C3BP C5AP 139.1 . . ? C1P C3BP C1BP 12.4 . . ? C5AP C3BP C1BP 129.0 . . ? C1P C3BP C5BP 130.2 . . ? C5AP C3BP C5BP 10.2 . . ? C1BP C3BP C5BP 119.5 . . ? C1P C3BP C5P 125.6 . . ? C5AP C3BP C5P 14.9 . . ? C1BP C3BP C5P 114.7 . . ? C5BP C3BP C5P 4.8 . . ? C1P C3BP C1AP 20.6 . . ? C5AP C3BP C1AP 121.3 . . ? C1BP C3BP C1AP 8.2 . . ? C5BP C3BP C1AP 111.6 . . ? C5P C3BP C1AP 106.8 . . ? C6P C4BP C2AP 146.0 . . ? C6P C4BP C6BP 7.0 . . ? C2AP C4BP C6BP 139.5 . . ? C6P C4BP C2BP 135.4 . . ? C2AP C4BP C2BP 10.7 . . ? C6BP C4BP C2BP 128.8 . . ? C6P C4BP C6AP 19.9 . . ? C2AP C4BP C6AP 127.1 . . ? C6BP C4BP C6AP 12.9 . . ? C2BP C4BP C6AP 116.4 . . ? C6P C4BP C2P 123.7 . . ? C2AP C4BP C2P 22.5 . . ? C6BP C4BP C2P 117.1 . . ? C2BP C4BP C2P 11.8 . . ? C6AP C4BP C2P 104.7 . . ? C6AP C5BP C3P 140.4 . . ? C6AP C5BP C6BP 9.9 . . ? C3P C5BP C6BP 133.6 . . ? C6AP C5BP C3BP 127.4 . . ? C3P C5BP C3BP 14.3 . . ? C6BP C5BP C3BP 119.9 . . ? C6AP C5BP C6P 16.2 . . ? C3P C5BP C6P 127.2 . . ? C6BP C5BP C6P 6.7 . . ? C3BP C5BP C6P 113.3 . . ? C6AP C5BP C3AP 118.3 . . ? C3P C5BP C3AP 23.7 . . ? C6BP C5BP C3AP 110.5 . . ? C3BP C5BP C3AP 9.4 . . ? C6P C5BP C3AP 104.0 . . ? C6AP C5BP C4AP 28.7 . . ? C3P C5BP C4AP 112.7 . . ? C6BP C5BP C4AP 20.9 . . ? C3BP C5BP C4AP 99.1 . . ? C6P C5BP C4AP 14.7 . . ? C3AP C5BP C4AP 89.8 . . ? C4AP C6BP C5P 130.0 . . ? C4AP C6BP C4BP 5.9 . . ? C5P C6BP C4BP 127.4 . . ? C4AP C6BP C5BP 120.5 . . ? C5P C6BP C5BP 9.5 . . ? C4BP C6BP C5BP 117.9 . . ? C4AP C6BP C4P 13.1 . . ? C5P C6BP C4P 118.4 . . ? C4BP C6BP C4P 9.0 . . ? C5BP C6BP C4P 108.9 . . ? C4AP C6BP C5AP 110.4 . . ? C5P C6BP C5AP 19.7 . . ? C4BP C6BP C5AP 107.9 . . ? C5BP C6BP C5AP 10.2 . . ? C4P C6BP C5AP 98.9 . . ? _refine_diff_density_max 0.666 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.083 #===END data_final2 _database_code_CSD 156505 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 N4 O12 W' _chemical_formula_weight 1206.92 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' '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5723(3) _cell_length_b 11.2623(4) _cell_length_c 26.9897(9) _cell_angle_alpha 86.9380(10) _cell_angle_beta 83.5980(10) _cell_angle_gamma 88.5040(10) _cell_volume 2886.79(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 2.064 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.702253 _exptl_absorpt_correction_T_max 0.962273 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker 1K CCD' _diffrn_measurement_method '0.3 degree omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16628 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 0.76 _diffrn_reflns_theta_max 26.15 _reflns_number_total 9721 _reflns_number_gt 7605 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9721 _refine_ls_number_parameters 451 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 3.433 _refine_ls_shift/su_mean 0.114 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 0.08230(5) 0.07271(4) -0.271884(16) 0.04128(18) Uani 1 1 d . A . O1 O 0.0017(8) -0.0780(6) -0.2631(3) 0.0526(18) Uani 1 1 d . . . C2 C -0.0249(10) -0.1781(9) -0.2881(4) 0.042(2) Uiso 1 1 d D . . O3 O 0.0921(7) 0.0646(7) -0.2016(3) 0.0505(18) Uani 1 1 d . . . C3 C 0.0553(11) -0.2067(9) -0.3312(4) 0.051(3) Uiso 1 1 d D . . H3A H 0.1300 -0.1595 -0.3444 0.061 Uiso 1 1 calc R . . C4 C -0.1370(12) -0.2461(10) -0.2670(4) 0.055(3) Uiso 1 1 d D . . H4A H -0.1900 -0.2260 -0.2375 0.066 Uiso 1 1 calc R . . C5 C 0.0224(11) -0.3092(9) -0.3552(4) 0.054(3) Uiso 1 1 d D . . H5A H 0.0758 -0.3310 -0.3843 0.065 Uiso 1 1 calc R . . C6 C -0.1668(13) -0.3471(11) -0.2923(4) 0.063(3) Uiso 1 1 d D . . H6A H -0.2416 -0.3945 -0.2793 0.075 Uiso 1 1 calc R . . C7 C -0.0903(11) -0.3767(10) -0.3347(4) 0.052(3) Uiso 1 1 d D . . O8 O -0.1163(10) -0.4748(8) -0.3601(4) 0.081(3) Uiso 1 1 d . . . H8A H -0.2014 -0.4816 -0.3600 0.122 Uiso 1 1 calc R . . O9 O 0.2617(8) 0.0015(6) -0.2802(2) 0.0475(17) Uani 1 1 d . . . C10 C 0.3455(10) -0.0694(8) -0.2510(4) 0.041(2) Uiso 1 1 d D A . C11 C 0.4117(11) -0.0183(11) -0.2153(4) 0.057(3) Uiso 1 1 d D . . H11A H 0.4001 0.0629 -0.2110 0.068 Uiso 1 1 calc R A . C12 C 0.3623(12) -0.1886(10) -0.2573(4) 0.054(3) Uiso 1 1 d D . . H12A H 0.3162 -0.2230 -0.2813 0.065 Uiso 1 1 calc R A . C13 C 0.4956(13) -0.0856(11) -0.1858(5) 0.067(3) Uiso 1 1 d D A . H13A H 0.5399 -0.0504 -0.1615 0.080 Uiso 1 1 calc R . . C14 C 0.4472(12) -0.2596(10) -0.2287(4) 0.056(3) Uiso 1 1 d D A . H14A H 0.4591 -0.3405 -0.2336 0.067 Uiso 1 1 calc R . . C15 C 0.5130(11) -0.2071(9) -0.1928(4) 0.047(3) Uiso 1 1 d D . . O16 O 0.5971(10) -0.2703(9) -0.1621(4) 0.083(3) Uiso 1 1 d . A . H16A H 0.5846 -0.3417 -0.1636 0.125 Uiso 1 1 calc R . . O17 O 0.1663(7) 0.2217(6) -0.2806(3) 0.0516(18) Uani 1 1 d . . . C18 C 0.2745(10) 0.2956(8) -0.2988(3) 0.038(2) Uiso 1 1 d D A . C19 C 0.4080(11) 0.2545(10) -0.3092(4) 0.053(3) Uiso 1 1 d D . . H19A H 0.4278 0.1738 -0.3041 0.064 Uiso 1 1 calc R A . C20 C 0.2444(13) 0.4165(10) -0.3057(4) 0.058(3) Uiso 1 1 d D . . H20A H 0.1531 0.4459 -0.2988 0.069 Uiso 1 1 calc R A . C21 C 0.5142(13) 0.3290(10) -0.3272(4) 0.060(3) Uiso 1 1 d D A . H21A H 0.6052 0.2989 -0.3345 0.072 Uiso 1 1 calc R . . C22 C 0.3533(12) 0.4926(11) -0.3231(4) 0.061(3) Uiso 1 1 d D A . H22A H 0.3341 0.5738 -0.3269 0.073 Uiso 1 1 calc R . . C23 C 0.4852(11) 0.4518(9) -0.3345(4) 0.048(3) Uiso 1 1 d D . . O24 O 0.5972(9) 0.5211(8) -0.3543(3) 0.075(2) Uiso 1 1 d . A . H24A H 0.5708 0.5908 -0.3570 0.113 Uiso 1 1 calc R . . O25 O 0.0630(8) 0.0676(6) -0.3407(3) 0.0507(18) Uani 1 1 d . . . C26 C -0.0108(10) 0.1135(9) -0.3779(4) 0.045(2) Uiso 1 1 d D A . C27 C -0.0486(11) 0.2349(11) -0.3797(5) 0.066(3) Uiso 1 1 d D . . H27A H -0.0293 0.2829 -0.3544 0.079 Uiso 1 1 calc R A . C28 C -0.0425(12) 0.0437(11) -0.4150(4) 0.058(3) Uiso 1 1 d D . . H28A H -0.0203 -0.0372 -0.4134 0.070 Uiso 1 1 calc R A . C29 C -0.1149(12) 0.2825(12) -0.4197(4) 0.066(3) Uiso 1 1 d D A . H29A H -0.1413 0.3626 -0.4210 0.079 Uiso 1 1 calc R . . C30 C -0.1073(13) 0.0928(11) -0.4547(5) 0.067(3) Uiso 1 1 d D A . H30A H -0.1274 0.0448 -0.4799 0.080 Uiso 1 1 calc R . . C31 C -0.1419(13) 0.2110(11) -0.4574(5) 0.064(3) Uiso 1 1 d D . . O32 O -0.1993(12) 0.2598(10) -0.4981(4) 0.099(3) Uiso 1 1 d . A . H32A H -0.2096 0.2076 -0.5173 0.148 Uiso 1 1 calc R . . O33 O -0.0945(8) 0.1465(6) -0.2614(3) 0.0506(18) Uani 1 1 d . . . C34 C -0.1768(11) 0.2331(9) -0.2352(4) 0.044(2) Uiso 1 1 d D A . C35 C -0.3182(13) 0.2159(11) -0.2248(5) 0.065(3) Uiso 1 1 d D . . H35A H -0.3556 0.1453 -0.2333 0.078 Uiso 1 1 calc R A . C36 C -0.1215(14) 0.3327(10) -0.2192(4) 0.066(3) Uiso 1 1 d D . . H36A H -0.0251 0.3444 -0.2248 0.079 Uiso 1 1 calc R A . C37 C -0.4060(16) 0.2998(12) -0.2023(5) 0.078(4) Uiso 1 1 d D A . H37A H -0.5025 0.2885 -0.1972 0.093 Uiso 1 1 calc R . . C38 C -0.2075(13) 0.4169(11) -0.1946(4) 0.065(3) Uiso 1 1 d D A . H38A H -0.1686 0.4838 -0.1833 0.077 Uiso 1 1 calc R . . C39 C -0.3492(12) 0.4014(10) -0.1871(4) 0.052(3) Uiso 1 1 d D . . O40 O -0.4330(9) 0.4861(8) -0.1633(3) 0.073(2) Uiso 1 1 d . A . H40A H -0.3982 0.5516 -0.1698 0.109 Uiso 1 1 calc R . . C42A C 0.019(2) 0.0460(19) -0.1568(8) 0.043(5) Uiso 0.50 1 d PD A 1 C42B C 0.042(2) -0.0168(19) -0.1611(8) 0.043(5) Uiso 0.50 1 d PD A 2 C43A C -0.117(2) 0.007(2) -0.1500(8) 0.048(5) Uiso 0.50 1 d PD A 1 H43A H -0.1636 -0.0008 -0.1780 0.057 Uiso 0.50 1 calc PR A 1 C43B C -0.095(2) -0.052(2) -0.1575(8) 0.052(6) Uiso 0.50 1 d PD A 2 H43B H -0.1509 -0.0319 -0.1829 0.062 Uiso 0.50 1 calc PR A 2 C44A C 0.090(2) 0.0554(18) -0.1149(8) 0.057(6) Uiso 0.50 1 d PD A 1 H44A H 0.1821 0.0806 -0.1178 0.068 Uiso 0.50 1 calc PR A 1 C44B C 0.123(3) -0.0434(18) -0.1226(8) 0.058(6) Uiso 0.50 1 d PD A 2 H44B H 0.2151 -0.0170 -0.1254 0.070 Uiso 0.50 1 calc PR A 2 C45A C 0.017(3) 0.0260(17) -0.0685(10) 0.073(7) Uiso 0.50 1 d PD A 1 H45A H 0.0635 0.0318 -0.0402 0.088 Uiso 0.50 1 calc PR A 1 C45B C 0.071(2) -0.1081(18) -0.0803(9) 0.068(7) Uiso 0.50 1 d PD A 2 H45B H 0.1267 -0.1263 -0.0549 0.082 Uiso 0.50 1 calc PR A 2 C46A C -0.186(3) -0.020(2) -0.1040(8) 0.057(6) Uiso 0.50 1 d PD A 1 H46A H -0.2790 -0.0440 -0.1010 0.069 Uiso 0.50 1 calc PR A 1 C46B C -0.149(2) -0.1176(19) -0.1144(8) 0.056(6) Uiso 0.50 1 d PD A 2 H46B H -0.2411 -0.1429 -0.1116 0.067 Uiso 0.50 1 calc PR A 2 C47A C -0.118(3) -0.011(2) -0.0626(10) 0.069(7) Uiso 0.50 1 d PD A 1 C47B C -0.068(2) -0.146(2) -0.0760(9) 0.063(6) Uiso 0.50 1 d PD A 2 O48A O -0.177(2) -0.038(2) -0.0160(8) 0.100(7) Uiso 0.50 1 d P A 1 H48A H -0.1717 -0.1104 -0.0103 0.150 Uiso 0.50 1 calc PR A 1 O48B O -0.116(2) -0.2163(17) -0.0331(7) 0.085(6) Uiso 0.50 1 d P A 2 H48B H -0.1984 -0.2331 -0.0343 0.127 Uiso 0.50 1 calc PR A 2 N50 N 0.5302(12) 0.7462(10) -0.3789(4) 0.075(3) Uiso 1 1 d D . . C51 C 0.6028(14) 0.8383(12) -0.3666(5) 0.071(4) Uiso 1 1 d D . . H51A H 0.6770 0.8236 -0.3474 0.086 Uiso 1 1 calc R . . C52 C 0.4242(14) 0.7743(13) -0.4062(5) 0.076(4) Uiso 1 1 d D . . H52A H 0.3725 0.7119 -0.4155 0.092 Uiso 1 1 calc R . . C53 C 0.5710(15) 0.9555(12) -0.3816(5) 0.076(4) Uiso 1 1 d D B . H53A H 0.6249 1.0168 -0.3727 0.091 Uiso 1 1 calc R . . C54 C 0.3859(15) 0.8874(12) -0.4217(5) 0.080(4) Uiso 1 1 d D B . H54A H 0.3105 0.9005 -0.4404 0.096 Uiso 1 1 calc R . . C55 C 0.4625(14) 0.9813(12) -0.4089(5) 0.073(4) Uiso 1 1 d D . . C56 C 0.394(3) 1.104(2) -0.4144(11) 0.067(7) Uiso 0.50 1 d P B 1 H56A H 0.3260 1.1152 -0.3855 0.080 Uiso 0.50 1 calc PR B 1 H56B H 0.4661 1.1633 -0.4139 0.080 Uiso 0.50 1 calc PR B 1 C57 C 0.325(3) 1.128(2) -0.4580(9) 0.059(6) Uiso 0.50 1 d P B 1 H57A H 0.2416 1.0799 -0.4549 0.071 Uiso 0.50 1 calc PR B 1 H57B H 0.3870 1.1002 -0.4863 0.071 Uiso 0.50 1 calc PR B 1 C58 C 0.283(3) 1.254(2) -0.4699(9) 0.060(7) Uiso 0.50 1 d PD B 1 C59 C 0.292(2) 1.340(2) -0.4371(11) 0.080(8) Uiso 0.50 1 d PD B 1 H59A H 0.3267 1.3238 -0.4066 0.096 Uiso 0.50 1 calc PR B 1 C61 C 0.245(3) 1.454(3) -0.4523(12) 0.099(10) Uiso 0.50 1 d PD B 1 H61A H 0.2539 1.5142 -0.4307 0.118 Uiso 0.50 1 calc PR B 1 N63 N 0.194(2) 1.4826(19) -0.4918(8) 0.060(5) Uiso 0.50 1 d PD B 1 C56A C 0.469(4) 1.111(3) -0.4329(15) 0.093(10) Uiso 0.50 1 d P B 2 H56C H 0.4443 1.1627 -0.4055 0.111 Uiso 0.50 1 calc PR B 2 H56D H 0.5682 1.1243 -0.4436 0.111 Uiso 0.50 1 calc PR B 2 C57A C 0.416(5) 1.147(4) -0.4623(18) 0.130(15) Uiso 0.50 1 d P B 2 H57C H 0.3353 1.0961 -0.4622 0.156 Uiso 0.50 1 calc PR B 2 H57D H 0.4770 1.1298 -0.4923 0.156 Uiso 0.50 1 calc PR B 2 C58A C 0.353(4) 1.285(3) -0.4729(13) 0.090(10) Uiso 0.50 1 d P B 2 C59A C 0.448(4) 1.370(3) -0.4633(13) 0.100(10) Uiso 0.50 1 d P B 2 H59B H 0.5284 1.3507 -0.4481 0.120 Uiso 0.50 1 calc PR B 2 C61A C 0.411(4) 1.487(3) -0.4781(14) 0.109(11) Uiso 0.50 1 d P . 2 H61B H 0.4725 1.5470 -0.4736 0.131 Uiso 0.50 1 calc PR . 2 N63A N 0.281(3) 1.519(3) -0.5007(11) 0.096(8) Uiso 0.50 1 d P B 2 C60 C 0.230(2) 1.291(2) -0.5108(8) 0.128(7) Uiso 1 1 d D . . H60A H 0.172(19) 1.224(16) -0.553(7) 0.153 Uiso 1 1 d . . . C62 C 0.197(2) 1.410(2) -0.5205(9) 0.133(7) Uiso 1 1 d D B . H62A H 0.05(2) 1.429(16) -0.525(7) 0.159 Uiso 1 1 d . . . C71A C -1.279(4) -0.395(3) 0.0918(13) 0.255(16) Uiso 1 1 d D . . H71A H -1.3632 -0.4233 0.0808 0.306 Uiso 1 1 d R C . C73A C -1.136(4) -0.373(3) 0.0677(15) 0.30(2) Uiso 1 1 d D C . H73A H -1.1928 -0.3637 0.0405 0.355 Uiso 1 1 d R . . N70 N -1.318(4) -0.392(3) 0.1317(13) 0.111(10) Uiso 0.50 1 d PD C 1 C72 C -1.229(4) -0.346(3) 0.1526(16) 0.120(12) Uiso 0.50 1 d PD C 1 H72B H -1.2492 -0.3395 0.1869 0.143 Uiso 0.50 1 calc PR C 1 C74 C -1.107(5) -0.303(3) 0.1323(19) 0.162(18) Uiso 0.50 1 d PD C 1 H74A H -1.0519 -0.2668 0.1530 0.194 Uiso 0.50 1 calc PR C 1 C75 C -1.061(5) -0.308(3) 0.0863(19) 0.151(16) Uiso 0.50 1 d PD C 1 C76 C -0.939(9) -0.222(8) 0.035(3) 0.28(4) Uiso 0.50 1 d P C 1 H76A H -0.9057 -0.2672 0.0066 0.339 Uiso 0.50 1 calc PR C 1 H76B H -0.9742 -0.1436 0.0256 0.339 Uiso 0.50 1 calc PR C 1 C77 C -0.848(7) -0.224(6) 0.073(2) 0.19(2) Uiso 0.50 1 d P C 1 H77A H -0.8326 -0.3034 0.0868 0.232 Uiso 0.50 1 calc PR C 1 H77B H -0.8812 -0.1716 0.0993 0.232 Uiso 0.50 1 calc PR C 1 C78 C -0.618(4) -0.132(4) 0.0678(19) 0.151(17) Uiso 0.50 1 d PD C 1 H78B H -0.6407 -0.1222 0.1017 0.181 Uiso 0.50 1 calc PR C 1 C79 C -0.485(5) -0.102(3) 0.0454(16) 0.132(14) Uiso 0.50 1 d PD C 1 H79B H -0.4207 -0.0715 0.0647 0.158 Uiso 0.50 1 calc PR C 1 C80 C -0.715(4) -0.176(3) 0.0416(15) 0.114(12) Uiso 0.50 1 d PD C 1 C81 C -0.682(5) -0.188(3) -0.0098(17) 0.156(18) Uiso 0.50 1 d PD C 1 H81B H -0.7469 -0.2154 -0.0297 0.187 Uiso 0.50 1 calc PR C 1 C82 C -0.547(5) -0.158(3) -0.0290(18) 0.142(16) Uiso 0.50 1 d PD C 1 H82B H -0.5229 -0.1673 -0.0629 0.170 Uiso 0.50 1 calc PR C 1 N83 N -0.447(3) -0.115(2) -0.0035(11) 0.105(9) Uiso 0.50 1 d PD C 1 N70A N -1.293(3) -0.471(2) 0.1357(10) 0.088(7) Uiso 0.50 1 d PD C 2 C72A C -1.179(4) -0.560(4) 0.1377(14) 0.143(14) Uiso 0.50 1 d PD C 2 H72A H -1.2092 -0.6301 0.1545 0.172 Uiso 0.50 1 calc PR C 2 C74A C -1.040(5) -0.564(3) 0.1209(13) 0.154(16) Uiso 0.50 1 d PD C 2 H74B H -0.9724 -0.6200 0.1298 0.185 Uiso 0.50 1 calc PR C 2 C75A C -1.021(3) -0.462(3) 0.0858(11) 0.093(9) Uiso 0.50 1 d PD C 2 C76A C -0.823(6) -0.510(5) 0.059(2) 0.18(2) Uiso 0.50 1 d P C 2 H76C H -0.7648 -0.5445 0.0836 0.217 Uiso 0.50 1 calc PR C 2 H76D H -0.8135 -0.5510 0.0283 0.217 Uiso 0.50 1 calc PR C 2 C77A C -0.831(5) -0.333(4) 0.0525(17) 0.138(14) Uiso 0.50 1 d P C 2 H77C H -0.9018 -0.3049 0.0313 0.165 Uiso 0.50 1 calc PR C 2 H77D H -0.8502 -0.2985 0.0848 0.165 Uiso 0.50 1 calc PR C 2 C78A C -0.594(5) -0.233(4) 0.0511(17) 0.139(15) Uiso 0.50 1 d PD C 2 H78A H -0.6275 -0.1985 0.0809 0.167 Uiso 0.50 1 calc PR C 2 C79A C -0.459(6) -0.217(5) 0.0272(19) 0.18(2) Uiso 0.50 1 d PD C 2 H79A H -0.4040 -0.1643 0.0417 0.216 Uiso 0.50 1 calc PR C 2 C80A C -0.672(4) -0.304(3) 0.0265(12) 0.091(9) Uiso 0.50 1 d PD C 2 C81A C -0.615(6) -0.361(4) -0.0154(16) 0.17(2) Uiso 0.50 1 d PD C 2 H81A H -0.6707 -0.4125 -0.0298 0.205 Uiso 0.50 1 calc PR C 2 C82A C -0.473(6) -0.342(4) -0.037(2) 0.19(2) Uiso 0.50 1 d PD C 2 H82A H -0.4360 -0.3799 -0.0659 0.229 Uiso 0.50 1 calc PR C 2 N83A N -0.396(3) -0.268(3) -0.0145(11) 0.109(9) Uiso 0.50 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0467(3) 0.0346(2) 0.0427(3) 0.00024(17) -0.00477(18) -0.00965(17) O1 0.066(5) 0.040(4) 0.052(5) -0.007(3) -0.005(4) -0.017(4) O3 0.041(4) 0.073(5) 0.039(4) -0.001(4) -0.003(3) -0.020(4) O9 0.064(5) 0.045(4) 0.031(4) 0.012(3) -0.005(3) 0.002(3) O17 0.050(4) 0.033(4) 0.070(5) -0.004(3) 0.006(4) -0.007(3) O25 0.063(5) 0.050(4) 0.039(4) 0.000(3) -0.009(3) 0.010(4) O33 0.053(4) 0.053(4) 0.046(4) -0.002(3) -0.005(3) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O33 1.866(7) . ? W1 O17 1.871(7) . ? W1 O9 1.872(7) . ? W1 O1 1.875(7) . ? W1 O25 1.890(7) . ? W1 O3 1.906(7) . ? O1 C2 1.388(12) . ? C2 C3 1.369(14) . ? C2 C4 1.386(14) . ? O3 C42A 1.34(2) . ? O3 C42B 1.44(2) . ? C3 C5 1.413(14) . ? C4 C6 1.409(15) . ? C5 C7 1.383(15) . ? C6 C7 1.341(15) . ? C7 O8 1.372(13) . ? O9 C10 1.395(11) . ? C10 C12 1.366(13) . ? C10 C11 1.368(14) . ? C11 C13 1.379(15) . ? C12 C14 1.392(14) . ? C13 C15 1.395(15) . ? C14 C15 1.379(14) . ? C15 O16 1.378(13) . ? O17 C18 1.377(12) . ? C18 C19 1.353(13) . ? C18 C20 1.391(14) . ? C19 C21 1.365(15) . ? C20 C22 1.391(15) . ? C21 C23 1.412(14) . ? C22 C23 1.341(14) . ? C23 O24 1.384(14) . ? O25 C26 1.363(12) . ? C26 C28 1.371(14) . ? C26 C27 1.405(15) . ? C27 C29 1.388(15) . ? C28 C30 1.380(15) . ? C29 C31 1.381(15) . ? C30 C31 1.364(15) . ? C31 O32 1.365(15) . ? O33 C34 1.408(12) . ? C34 C36 1.363(15) . ? C34 C35 1.368(15) . ? C35 C37 1.370(16) . ? C36 C38 1.385(16) . ? C37 C39 1.379(16) . ? C38 C39 1.364(15) . ? C39 O40 1.370(13) . ? C42A C43A 1.37(2) . ? C42A C44A 1.39(2) . ? C42B C43B 1.37(2) . ? C42B C44B 1.38(2) . ? C43A C46A 1.36(3) . ? C43B C46B 1.40(3) . ? C44A C45A 1.39(3) . ? C44B C45B 1.37(3) . ? C45A C47A 1.36(3) . ? C45B C47B 1.39(3) . ? C46A C47A 1.36(3) . ? C46B C47B 1.38(3) . ? C47A O48A 1.34(3) . ? C47B O48B 1.41(3) . ? N50 C51 1.340(16) . ? N50 C52 1.341(15) . ? C51 C53 1.396(18) . ? C52 C54 1.373(17) . ? C53 C55 1.355(17) . ? C54 C55 1.384(17) . ? C55 C56 1.52(3) . ? C55 C56A 1.57(4) . ? C56 C57 1.42(4) . ? C57 C58 1.50(3) . ? C58 C60 1.31(3) . ? C58 C59 1.35(3) . ? C59 C61 1.41(3) . ? C61 N63 1.25(3) . ? C61 C62 2.03(4) . ? N63 C62 1.15(2) . ? C56A C57A 1.05(5) . ? C57A C58A 1.68(5) . ? C58A C59A 1.38(4) . ? C58A C60 1.65(4) . ? C59A C61A 1.40(5) . ? C61A N63A 1.48(4) . ? C61A C61A 1.98(7) 2_684 ? N63A C62 1.63(3) . ? C60 C62 1.38(2) . ? C71A N70 1.10(4) . ? C71A N70A 1.42(4) . ? C71A C73A 1.46(3) . ? C71A C72 1.87(5) . ? C73A C75 1.21(4) . ? C73A C75A 1.57(3) . ? C73A C74 2.00(6) . ? N70 C72 1.21(4) . ? C72 C74 1.32(4) . ? C74 C75 1.27(4) . ? C75 C76 1.94(9) . ? C76 C77 1.41(8) . ? C77 C80 1.53(7) . ? C78 C80 1.34(4) . ? C78 C79 1.39(4) . ? C79 N83 1.34(4) . ? C80 C81 1.40(4) . ? C81 C82 1.38(4) . ? C82 N83 1.35(4) . ? N70A C72A 1.47(4) . ? C72A C74A 1.36(4) . ? C74A C75A 1.46(4) . ? C75A C76A 2.02(6) . ? C76A C77A 1.99(6) . ? C77A C80A 1.64(5) . ? C78A C80A 1.35(4) . ? C78A C79A 1.39(4) . ? C79A N83A 1.36(5) . ? C80A C81A 1.38(4) . ? C81A C82A 1.44(4) . ? C82A N83A 1.34(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 O33 W1 O17 90.1(3) . . ? O33 W1 O9 177.8(3) . . ? O17 W1 O9 88.8(3) . . ? O33 W1 O1 91.0(3) . . ? O17 W1 O1 178.9(3) . . ? O9 W1 O1 90.0(3) . . ? O33 W1 O25 90.0(3) . . ? O17 W1 O25 92.3(3) . . ? O9 W1 O25 92.0(3) . . ? O1 W1 O25 87.8(3) . . ? O33 W1 O3 89.5(3) . . ? O17 W1 O3 93.0(3) . . ? O9 W1 O3 88.7(3) . . ? O1 W1 O3 86.9(3) . . ? O25 W1 O3 174.7(3) . . ? C2 O1 W1 143.2(7) . . ? C3 C2 C4 122.6(10) . . ? C3 C2 O1 121.3(10) . . ? C4 C2 O1 116.1(9) . . ? C42A O3 C42B 31.0(10) . . ? C42A O3 W1 144.9(9) . . ? C42B O3 W1 134.6(9) . . ? C2 C3 C5 118.8(11) . . ? C2 C4 C6 116.8(11) . . ? C7 C5 C3 119.0(11) . . ? C7 C6 C4 121.8(12) . . ? C6 C7 O8 123.1(11) . . ? C6 C7 C5 121.0(11) . . ? O8 C7 C5 115.9(10) . . ? C10 O9 W1 136.5(6) . . ? C12 C10 C11 119.7(9) . . ? C12 C10 O9 121.1(9) . . ? C11 C10 O9 119.2(9) . . ? C10 C11 C13 120.8(11) . . ? C10 C12 C14 121.3(10) . . ? C11 C13 C15 119.1(12) . . ? C15 C14 C12 118.4(11) . . ? C14 C15 O16 122.7(10) . . ? C14 C15 C13 120.6(10) . . ? O16 C15 C13 116.8(10) . . ? C18 O17 W1 152.3(6) . . ? C19 C18 O17 122.1(9) . . ? C19 C18 C20 119.6(10) . . ? O17 C18 C20 118.3(9) . . ? C18 C19 C21 121.4(11) . . ? C22 C20 C18 118.9(11) . . ? C19 C21 C23 119.6(11) . . ? C23 C22 C20 121.6(11) . . ? C22 C23 O24 124.9(10) . . ? C22 C23 C21 118.8(11) . . ? O24 C23 C21 116.3(10) . . ? C26 O25 W1 143.9(6) . . ? O25 C26 C28 120.6(9) . . ? O25 C26 C27 119.8(9) . . ? C28 C26 C27 119.5(10) . . ? C29 C27 C26 119.3(11) . . ? C26 C28 C30 120.4(11) . . ? C31 C29 C27 120.1(12) . . ? C31 C30 C28 120.6(12) . . ? C30 C31 O32 120.1(11) . . ? C30 C31 C29 120.1(12) . . ? O32 C31 C29 119.8(12) . . ? C34 O33 W1 145.7(6) . . ? C36 C34 C35 118.6(11) . . ? C36 C34 O33 122.9(10) . . ? C35 C34 O33 118.5(9) . . ? C37 C35 C34 121.7(12) . . ? C34 C36 C38 120.7(12) . . ? C35 C37 C39 119.1(13) . . ? C39 C38 C36 119.8(12) . . ? C38 C39 O40 119.1(10) . . ? C38 C39 C37 119.9(12) . . ? O40 C39 C37 120.9(11) . . ? O3 C42A C43A 123.8(17) . . ? O3 C42A C44A 117.7(17) . . ? C43A C42A C44A 118(2) . . ? C43B C42B C44B 121(2) . . ? C43B C42B O3 118.5(17) . . ? C44B C42B O3 120.1(17) . . ? C46A C43A C42A 123(2) . . ? C42B C43B C46B 118(2) . . ? C45A C44A C42A 118(2) . . ? C45B C44B C42B 121(2) . . ? C47A C45A C44A 123(3) . . ? C44B C45B C47B 119(2) . . ? C43A C46A C47A 119(2) . . ? C47B C46B C43B 122(2) . . ? O48A C47A C45A 118(2) . . ? O48A C47A C46A 123(2) . . ? C45A C47A C46A 119(3) . . ? C46B C47B C45B 119(2) . . ? C46B C47B O48B 123(2) . . ? C45B C47B O48B 118(2) . . ? C51 N50 C52 115.6(12) . . ? N50 C51 C53 122.2(13) . . ? N50 C52 C54 125.4(14) . . ? C55 C53 C51 121.0(14) . . ? C52 C54 C55 118.2(14) . . ? C53 C55 C54 117.6(13) . . ? C53 C55 C56 124.3(15) . . ? C54 C55 C56 115.9(15) . . ? C53 C55 C56A 112.1(17) . . ? C54 C55 C56A 128.1(17) . . ? C56 C55 C56A 31.2(15) . . ? C57 C56 C55 116(2) . . ? C56 C57 C58 117(2) . . ? C60 C58 C59 114(2) . . ? C60 C58 C57 124(2) . . ? C59 C58 C57 121(2) . . ? C58 C59 C61 115(3) . . ? N63 C61 C59 127(3) . . ? N63 C61 C62 30.6(14) . . ? C59 C61 C62 96(2) . . ? C62 N63 C61 116(3) . . ? C57A C56A C55 128(4) . . ? C56A C57A C58A 130(5) . . ? C59A C58A C60 131(3) . . ? C59A C58A C57A 112(3) . . ? C60 C58A C57A 113(3) . . ? C58A C59A C61A 115(4) . . ? C59A C61A N63A 123(3) . . ? C59A C61A C61A 94(3) . 2_684 ? N63A C61A C61A 116(3) . 2_684 ? C61A N63A C62 117(2) . . ? C58 C60 C62 122(2) . . ? C58 C60 C58A 26.9(16) . . ? C62 C60 C58A 108(2) . . ? N63 C62 C60 125(2) . . ? N63 C62 N63A 34.6(15) . . ? C60 C62 N63A 124(2) . . ? N63 C62 C61 33.5(15) . . ? C60 C62 C61 91.8(18) . . ? N63A C62 C61 45.9(14) . . ? N70 C71A N70A 40(2) . . ? N70 C71A C73A 128(4) . . ? N70A C71A C73A 118(3) . . ? N70 C71A C72 38(2) . . ? N70A C71A C72 58(2) . . ? C73A C71A C72 91(3) . . ? C75 C73A C71A 119(4) . . ? C75 C73A C75A 78(3) . . ? C71A C73A C75A 115(3) . . ? C75 C73A C74 37(3) . . ? C71A C73A C74 84(3) . . ? C75A C73A C74 80(2) . . ? C71A N70 C72 108(4) . . ? N70 C72 C74 128(5) . . ? N70 C72 C71A 34(2) . . ? C74 C72 C71A 94(4) . . ? C75 C74 C72 125(5) . . ? C75 C74 C73A 35(3) . . ? C72 C74 C73A 90(4) . . ? C73A C75 C74 107(5) . . ? C73A C75 C76 111(5) . . ? C74 C75 C76 140(5) . . ? C77 C76 C75 83(5) . . ? C76 C77 C80 99(6) . . ? C80 C78 C79 122(5) . . ? N83 C79 C78 121(4) . . ? C78 C80 C81 119(4) . . ? C78 C80 C77 116(4) . . ? C81 C80 C77 125(4) . . ? C82 C81 C80 115(5) . . ? N83 C82 C81 127(5) . . ? C79 N83 C82 116(4) . . ? C71A N70A C72A 113(3) . . ? C74A C72A N70A 136(4) . . ? C72A C74A C75A 104(4) . . ? C74A C75A C73A 128(3) . . ? C74A C75A C76A 94(3) . . ? C73A C75A C76A 135(3) . . ? C77A C76A C75A 74(2) . . ? C80A C77A C76A 101(3) . . ? C80A C78A C79A 113(5) . . ? N83A C79A C78A 129(5) . . ? C78A C80A C81A 122(4) . . ? C78A C80A C77A 117(4) . . ? C81A C80A C77A 121(4) . . ? C80A C81A C82A 122(5) . . ? N83A C82A C81A 117(5) . . ? C82A N83A C79A 118(5) . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 26.15 _diffrn_measured_fraction_theta_full 0.844 _refine_diff_density_max 1.518 _refine_diff_density_min -1.691 _refine_diff_density_rms 0.173 #===END data_os10 _database_code_CSD 156506 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C96 H78 N12 O12 W1' _chemical_formula_weight 1775.56 _chemical_melting_point ? _chemical_compound_source ? 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 27.1402(1) _cell_length_b 27.1402(1) _cell_length_c 9.7013(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6188.52(7) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method ? _exptl_crystal_F_000 2724 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.349149 _exptl_absorpt_correction_T_max 0.693905 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1K CCD' _diffrn_measurement_method '0.3 deg. \w-scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8846 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.1393 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.31 _reflns_number_total 4778 _reflns_number_observed 4306 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.446(12) _refine_ls_number_reflns 4778 _refine_ls_number_parameters 470 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_obs 0.0332 _refine_ls_wR_factor_all 0.0825 _refine_ls_wR_factor_obs 0.0772 _refine_ls_goodness_of_fit_all 0.577 _refine_ls_goodness_of_fit_obs 0.571 _refine_ls_restrained_S_all 0.577 _refine_ls_restrained_S_obs 0.571 _refine_ls_shift/esd_max -5.727 _refine_ls_shift/esd_mean 0.259 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.3333 0.6667 0.69191(14) 0.02407(4) Uani 1 d S . O1 O 0.39728(10) 0.71034(9) 0.8058(3) 0.0236(7) Uani 1 d . . O2 O 0.53911(11) 0.67664(11) 1.1541(3) 0.0400(9) Uani 1 d . . H2B H 0.5495(21) 0.6959(20) 1.2211(57) 0.071(18) Uiso 1 d . . O3 O 0.37770(10) 0.64554(13) 0.5803(3) 0.0259(8) Uani 1 d . . O4 O 0.33946(12) 0.46929(15) 0.2319(3) 0.0428(10) Uani 1 d . . H4B H 0.3673(27) 0.4750(32) 0.1646(81) 0.137(30) Uiso 1 d . . N1 N 0.59409(15) 0.74022(15) 1.3710(4) 0.0413(11) Uani 1 d . . N2 N 0.71556(14) 0.78229(14) 2.0450(4) 0.0375(10) Uani 1 d . . N3 N 0.40267(14) 0.4841(2) -0.0007(4) 0.0372(11) Uani 1 d . . N4 N 0.4573(2) 0.4035(2) -0.6520(4) 0.0479(13) Uani 1 d . . C1 C 0.43371(14) 0.70191(13) 0.8971(4) 0.0200(10) Uani 1 d . . C2 C 0.44796(15) 0.65956(15) 0.8622(4) 0.0267(11) Uani 1 d . . H2 H 0.4299(13) 0.6338(14) 0.8004(39) 0.025(10) Uiso 1 d . . C3 C 0.4841(2) 0.6531(2) 0.9471(4) 0.0306(12) Uani 1 d . . H3 H 0.4864(13) 0.6196(13) 0.9511(38) 0.027(10) Uiso 1 d . . C4 C 0.5023(2) 0.6867(2) 1.0668(4) 0.0315(11) Uani 1 d . . C5 C 0.4899(2) 0.7257(2) 1.1032(4) 0.0310(12) Uani 1 d . . H5 H 0.4978(11) 0.7431(11) 1.1915(31) 0.001(7) Uiso 1 d . . C6 C 0.45273(14) 0.73445(13) 1.0113(4) 0.0206(10) Uani 1 d . . H6 H 0.4486(12) 0.7648(12) 1.0199(34) 0.015(9) Uiso 1 d . . C7 C 0.36775(15) 0.6031(2) 0.4952(4) 0.0211(10) Uani 1 d . . C8 C 0.3282(2) 0.5479(2) 0.5211(5) 0.0260(11) Uani 1 d . . H8 H 0.3087(12) 0.5371(13) 0.6158(37) 0.011(9) Uiso 1 d . . C9 C 0.3186(2) 0.5030(2) 0.4306(5) 0.0299(13) Uani 1 d . . H9 H 0.2955(12) 0.4625(13) 0.4760(33) 0.016(9) Uiso 1 d . . C10 C 0.35070(15) 0.5122(2) 0.3115(5) 0.0227(10) Uani 1 d . . C11 C 0.3927(2) 0.5725(2) 0.2870(4) 0.0263(11) Uani 1 d . . H11 H 0.4208(18) 0.5836(19) 0.2277(50) 0.053(16) Uiso 1 d . . C12 C 0.3999(2) 0.6133(2) 0.3719(5) 0.0330(14) Uani 1 d . . H12 H 0.4261(12) 0.6617(13) 0.3346(35) 0.017(9) Uiso 1 d . . C13 C 0.6510(2) 0.7674(2) 1.3928(5) 0.0400(13) Uani 1 d . . H13 H 0.6645(22) 0.7801(23) 1.3065(61) 0.092(21) Uiso 1 d . . C14 C 0.6713(2) 0.7730(2) 1.5200(5) 0.0369(13) Uani 1 d . . H14 H 0.7232(13) 0.7939(13) 1.5308(36) 0.026(10) Uiso 1 d . . C15 C 0.63763(15) 0.75540(14) 1.6395(4) 0.0249(10) Uani 1 d . . C16 C 0.6669(2) 0.7658(2) 1.7765(5) 0.0313(12) Uani 1 d . . C17 C 0.7201(2) 0.8125(2) 1.8113(5) 0.0325(12) Uani 1 d . . H17 H 0.7470(13) 0.8489(13) 1.7074(36) 0.026(10) Uiso 1 d . . C18 C 0.7413(2) 0.8212(2) 1.9456(5) 0.0344(12) Uani 1 d . . H18 H 0.7886(17) 0.8702(18) 1.9395(47) 0.063(15) Uiso 1 d . . C19 C 0.6674(2) 0.7361(2) 2.0153(5) 0.0401(13) Uani 1 d . . H19 H 0.6536(13) 0.7055(14) 2.0883(36) 0.029(10) Uiso 1 d . . C20 C 0.6398(2) 0.7276(2) 1.8851(5) 0.0384(13) Uani 1 d . . H20 H 0.6148(18) 0.6974(19) 1.8712(52) 0.058(16) Uiso 1 d . . C21 C 0.5790(2) 0.7287(2) 1.6294(5) 0.0343(12) Uani 1 d . . H21 H 0.5541(22) 0.7158(21) 1.7307(57) 0.086(20) Uiso 1 d . . C22 C 0.5622(2) 0.7237(2) 1.4832(5) 0.0406(14) Uani 1 d . . H22 H 0.5109(12) 0.6988(13) 1.4879(34) 0.017(9) Uiso 1 d . . C23 C 0.3884(2) 0.4988(2) -0.1205(5) 0.0343(12) Uani 1 d . . H23 H 0.3842(20) 0.5259(22) -0.1116(59) 0.079(19) Uiso 1 d . . C24 C 0.4000(2) 0.4806(2) -0.2356(5) 0.0319(12) Uani 1 d . . H24 H 0.3874(11) 0.4941(12) -0.3132(34) 0.000(7) Uiso 1 d . . C25 C 0.4258(2) 0.4468(2) -0.2514(5) 0.0314(12) Uani 1 d . . C26 C 0.4345(2) 0.4313(2) -0.3907(5) 0.0304(12) Uani 1 d . . C27 C 0.3958(2) 0.4190(2) -0.4988(5) 0.0342(13) Uani 1 d . . H27 H 0.3581(14) 0.4268(15) -0.4886(41) 0.025(11) Uiso 1 d . . C28 C 0.4104(2) 0.4090(2) -0.6233(6) 0.0423(15) Uani 1 d . . H28 H 0.3883(14) 0.4052(14) -0.6957(39) 0.020(10) Uiso 1 d . . C29 C 0.4901(2) 0.4115(2) -0.5412(6) 0.0409(13) Uani 1 d . . H29 H 0.5184(12) 0.4091(12) -0.5819(32) 0.003(7) Uiso 1 d . . C30 C 0.4833(2) 0.4281(2) -0.4118(6) 0.0359(13) Uani 1 d . . H30 H 0.5065(13) 0.4379(14) -0.3705(37) 0.014(9) Uiso 1 d . . C31 C 0.4414(2) 0.4331(2) -0.1300(6) 0.0381(14) Uani 1 d . . H31 H 0.4538(13) 0.4182(13) -0.1315(37) 0.005(10) Uiso 1 d . . C32 C 0.4258(2) 0.4511(2) -0.0057(5) 0.0373(13) Uani 1 d . . H32 H 0.4395(13) 0.4396(15) 0.0716(41) 0.015(10) Uiso 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 0.02571(5) 0.02571(5) 0.02080(9) 0.000 0.000 0.01285(3) O1 0.0294(10) 0.0251(9) 0.0221(14) -0.0002(9) -0.0017(11) 0.0178(8) O2 0.0436(12) 0.0434(12) 0.043(2) -0.0016(12) -0.0124(14) 0.0295(10) O3 0.0278(11) 0.0305(15) 0.016(2) 0.0018(13) 0.0003(11) 0.0123(10) O4 0.0434(14) 0.040(2) 0.035(2) -0.014(2) 0.0141(14) 0.0133(12) N1 0.043(2) 0.043(2) 0.036(2) 0.0032(15) -0.003(2) 0.0194(13) N2 0.0389(15) 0.045(2) 0.029(2) -0.0045(14) -0.002(2) 0.0218(12) N3 0.038(2) 0.040(2) 0.029(2) -0.012(2) 0.005(2) 0.0167(14) N4 0.061(2) 0.047(2) 0.035(3) -0.005(2) 0.014(2) 0.026(2) C1 0.0178(13) 0.0232(13) 0.016(2) 0.0030(13) -0.0021(14) 0.0083(11) C2 0.028(2) 0.0289(15) 0.024(2) -0.0067(14) 0.002(2) 0.0157(12) C3 0.033(2) 0.033(2) 0.031(2) -0.006(2) 0.000(2) 0.0195(13) C4 0.030(2) 0.035(2) 0.030(2) 0.006(2) -0.011(2) 0.0165(13) C5 0.038(2) 0.034(2) 0.023(2) 0.001(2) -0.007(2) 0.0194(13) C6 0.0240(14) 0.0178(13) 0.019(2) 0.0009(13) -0.0023(15) 0.0098(11) C7 0.0247(14) 0.025(2) 0.014(2) -0.001(2) -0.0004(15) 0.0127(13) C8 0.029(2) 0.028(2) 0.020(2) -0.001(2) 0.005(2) 0.0134(14) C9 0.034(2) 0.023(2) 0.030(3) 0.001(2) 0.003(2) 0.0124(15) C10 0.0247(15) 0.021(2) 0.021(2) 0.001(2) 0.0003(15) 0.0102(12) C11 0.023(2) 0.034(2) 0.016(2) 0.003(2) 0.0106(15) 0.0094(14) C12 0.030(2) 0.036(3) 0.023(3) -0.001(2) -0.001(2) 0.009(2) C13 0.039(2) 0.041(2) 0.035(3) 0.001(2) -0.006(2) 0.016(2) C14 0.035(2) 0.041(2) 0.031(2) 0.000(2) -0.004(2) 0.0160(15) C15 0.0258(14) 0.0248(14) 0.025(2) -0.0020(14) -0.0025(15) 0.0131(11) C16 0.028(2) 0.034(2) 0.033(2) -0.008(2) 0.001(2) 0.0171(13) C17 0.032(2) 0.034(2) 0.031(2) 0.002(2) -0.001(2) 0.0169(13) C18 0.034(2) 0.044(2) 0.031(2) -0.012(2) -0.005(2) 0.0233(13) C19 0.042(2) 0.048(2) 0.033(3) 0.001(2) -0.003(2) 0.024(2) C20 0.038(2) 0.045(2) 0.032(3) 0.000(2) -0.002(2) 0.020(2) C21 0.031(2) 0.033(2) 0.034(2) 0.002(2) -0.002(2) 0.0127(14) C22 0.036(2) 0.041(2) 0.038(3) -0.004(2) -0.012(2) 0.014(2) C23 0.035(2) 0.037(2) 0.035(3) -0.004(2) 0.000(2) 0.0217(15) C24 0.032(2) 0.036(2) 0.035(3) -0.002(2) -0.001(2) 0.0219(14) C25 0.034(2) 0.027(2) 0.036(3) -0.001(2) 0.004(2) 0.0176(14) C26 0.039(2) 0.027(2) 0.026(3) -0.001(2) 0.005(2) 0.0170(15) C27 0.041(2) 0.035(2) 0.027(3) 0.004(2) 0.008(2) 0.020(2) C28 0.053(2) 0.041(2) 0.026(3) -0.002(2) -0.003(2) 0.019(2) C29 0.045(2) 0.042(2) 0.040(3) 0.002(2) 0.015(2) 0.025(2) C30 0.037(2) 0.037(2) 0.035(3) -0.002(2) 0.004(2) 0.019(2) C31 0.050(2) 0.041(2) 0.034(3) 0.001(2) 0.001(2) 0.031(2) C32 0.040(2) 0.043(2) 0.029(3) 0.000(2) 0.002(2) 0.021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.893(2) 2_665 ? W1 O1 1.893(2) . ? W1 O1 1.893(2) 3_565 ? W1 O3 1.908(3) 3_565 ? W1 O3 1.908(3) 2_665 ? W1 O3 1.908(3) . ? O1 C1 1.428(5) . ? O2 C4 1.435(5) . ? O3 C7 1.331(5) . ? O4 C10 1.301(6) . ? N1 C22 1.322(6) . ? N1 C13 1.355(6) . ? N2 C19 1.313(5) . ? N2 C18 1.340(5) . ? N3 C32 1.326(7) . ? N3 C23 1.347(7) . ? N4 C29 1.342(7) . ? N4 C28 1.383(7) . ? C1 C6 1.348(5) . ? C1 C2 1.425(6) . ? C2 C3 1.357(6) . ? C3 C4 1.405(6) . ? C4 C5 1.309(7) . ? C5 C6 1.452(6) . ? C7 C8 1.360(6) . ? C7 C12 1.423(6) . ? C8 C9 1.418(7) . ? C9 C10 1.391(6) . ? C10 C11 1.472(6) . ? C11 C12 1.314(7) . ? C13 C14 1.329(7) . ? C14 C15 1.404(6) . ? C15 C21 1.383(5) . ? C15 C16 1.501(6) . ? C16 C20 1.401(6) . ? C16 C17 1.405(5) . ? C17 C18 1.396(6) . ? C19 C20 1.428(7) . ? C21 C22 1.474(7) . ? C23 C24 1.320(7) . ? C24 C25 1.413(7) . ? C25 C31 1.366(7) . ? C25 C26 1.469(7) . ? C26 C30 1.386(7) . ? C26 C27 1.402(7) . ? C27 C28 1.341(7) . ? C29 C30 1.377(8) . ? C31 C32 1.443(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O1 89.33(11) 2_665 . ? O1 W1 O1 89.33(11) 2_665 3_565 ? O1 W1 O1 89.33(11) . 3_565 ? O1 W1 O3 89.63(12) 2_665 3_565 ? O1 W1 O3 178.8(2) . 3_565 ? O1 W1 O3 90.04(11) 3_565 3_565 ? O1 W1 O3 90.03(11) 2_665 2_665 ? O1 W1 O3 89.63(12) . 2_665 ? O1 W1 O3 178.8(2) 3_565 2_665 ? O3 W1 O3 90.98(13) 3_565 2_665 ? O1 W1 O3 178.8(2) 2_665 . ? O1 W1 O3 90.03(11) . . ? O1 W1 O3 89.63(12) 3_565 . ? O3 W1 O3 90.99(13) 3_565 . ? O3 W1 O3 90.99(13) 2_665 . ? C1 O1 W1 138.9(2) . . ? C7 O3 W1 136.6(2) . . ? C22 N1 C13 115.5(4) . . ? C19 N2 C18 118.3(4) . . ? C32 N3 C23 118.1(4) . . ? C29 N4 C28 113.2(4) . . ? C6 C1 C2 123.7(4) . . ? C6 C1 O1 118.3(4) . . ? C2 C1 O1 118.1(3) . . ? C3 C2 C1 117.7(4) . . ? C2 C3 C4 117.5(4) . . ? C5 C4 C3 126.7(4) . . ? C5 C4 O2 118.7(4) . . ? C3 C4 O2 114.6(4) . . ? C4 C5 C6 116.6(4) . . ? C1 C6 C5 117.8(4) . . ? O3 C7 C8 123.0(4) . . ? O3 C7 C12 120.9(4) . . ? C8 C7 C12 116.1(4) . . ? C7 C8 C9 122.4(4) . . ? C10 C9 C8 122.0(4) . . ? O4 C10 C9 119.1(4) . . ? O4 C10 C11 127.1(4) . . ? C9 C10 C11 113.7(4) . . ? C12 C11 C10 122.7(4) . . ? C11 C12 C7 123.0(4) . . ? C14 C13 N1 120.1(4) . . ? C13 C14 C15 124.5(4) . . ? C21 C15 C14 120.2(4) . . ? C21 C15 C16 121.6(4) . . ? C14 C15 C16 118.3(3) . . ? C20 C16 C17 114.1(4) . . ? C20 C16 C15 119.6(3) . . ? C17 C16 C15 126.2(4) . . ? C18 C17 C16 121.9(4) . . ? N2 C18 C17 122.0(3) . . ? N2 C19 C20 122.6(4) . . ? C16 C20 C19 120.5(3) . . ? C15 C21 C22 109.8(4) . . ? N1 C22 C21 129.9(4) . . ? C24 C23 N3 117.5(5) . . ? C23 C24 C25 128.5(5) . . ? C31 C25 C24 114.0(5) . . ? C31 C25 C26 126.7(5) . . ? C24 C25 C26 119.3(5) . . ? C30 C26 C27 120.1(5) . . ? C30 C26 C25 116.7(4) . . ? C27 C26 C25 123.2(4) . . ? C28 C27 C26 117.4(5) . . ? C27 C28 N4 125.8(5) . . ? N4 C29 C30 126.6(5) . . ? C29 C30 C26 116.3(5) . . ? C25 C31 C32 116.3(5) . . ? N3 C32 C31 125.4(5) . . ? _refine_diff_density_max 0.659 _refine_diff_density_min -1.350 _refine_diff_density_rms 0.072 #===END data_final4 _database_code_CSD 156507 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H74 N6 O13 W' _chemical_formula_weight 1463.26 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 25.132(3) _cell_length_b 11.6991(18) _cell_length_c 25.988(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.724(3) _cell_angle_gamma 90.00 _cell_volume 7389.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 1.627 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.535269 _exptl_absorpt_correction_T_max 0.927875 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker 1K CCD' _diffrn_measurement_method '0.3 degree omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6046 _diffrn_reflns_av_R_equivalents 0.0731 _diffrn_reflns_av_sigmaI/netI 0.1181 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 15.86 _reflns_number_total 3445 _reflns_number_gt 2166 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1784P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3445 _refine_ls_number_parameters 434 _refine_ls_number_restraints 168 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.2940 _refine_ls_wR_factor_gt 0.2575 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 1.510 _refine_ls_shift/su_mean 0.069 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 0.24037(6) 0.01103(11) 0.49089(5) 0.0758(10) Uani 1 1 d . . . O1 O 0.1708(12) 0.011(2) 0.4413(11) 0.147(10) Uiso 1 1 d . . . C2 C 0.1189(13) -0.010(3) 0.4133(10) 0.086(10) Uiso 1 1 d D . . C3 C 0.0974(12) -0.110(3) 0.4021(10) 0.094(11) Uiso 1 1 d D . . H3 H 0.1175 -0.1764 0.4128 0.112 Uiso 1 1 calc R . . C4 C 0.0929(12) 0.090(3) 0.3990(10) 0.101(11) Uiso 1 1 d D . . H4 H 0.1105 0.1589 0.4095 0.121 Uiso 1 1 calc R . . C5 C 0.0441(14) -0.114(3) 0.3743(12) 0.131(14) Uiso 1 1 d D . . H5 H 0.0266 -0.1841 0.3664 0.157 Uiso 1 1 calc R . . C6 C 0.0397(12) 0.087(3) 0.3685(10) 0.084(10) Uiso 1 1 d D . . H6 H 0.0208 0.1540 0.3560 0.101 Uiso 1 1 calc R . . C7 C 0.0159(14) -0.015(3) 0.3575(13) 0.097(11) Uiso 1 1 d D . . O8 O -0.0353(10) -0.033(2) 0.3285(10) 0.136(9) Uiso 1 1 d . . . H8A H -0.0504 0.0285 0.3194 0.203 Uiso 1 1 calc R . . O9 O 0.3056(10) 0.0128(17) 0.5370(9) 0.111(8) Uiso 1 1 d . . . C10 C 0.3585(12) -0.001(3) 0.5669(10) 0.069(9) Uiso 1 1 d D . . C11 C 0.3881(11) 0.093(3) 0.5865(10) 0.079(10) Uiso 1 1 d D . . H11 H 0.3723 0.1653 0.5788 0.095 Uiso 1 1 calc R . . C12 C 0.3846(12) -0.101(3) 0.5804(10) 0.089(10) Uiso 1 1 d D . . H12 H 0.3659 -0.1681 0.5686 0.107 Uiso 1 1 calc R . . C13 C 0.4399(12) 0.085(3) 0.6169(11) 0.085(11) Uiso 1 1 d D . . H13 H 0.4585 0.1513 0.6300 0.103 Uiso 1 1 calc R . . C14 C 0.4362(12) -0.107(3) 0.6101(11) 0.094(11) Uiso 1 1 d D . . H14 H 0.4523 -0.1790 0.6180 0.113 Uiso 1 1 calc R . . C15 C 0.4659(13) -0.014(3) 0.6290(12) 0.086(10) Uiso 1 1 d D . . O16 O 0.5186(9) -0.0328(18) 0.6587(9) 0.117(8) Uiso 1 1 d . . . H16A H 0.5334 0.0287 0.6685 0.176 Uiso 1 1 calc R . . O17 O 0.2238(7) -0.1286(17) 0.5178(8) 0.092(6) Uiso 1 1 d . . . C18 C 0.2409(8) -0.192(3) 0.5662(13) 0.085(10) Uiso 1 1 d D . . C19 C 0.2481(9) -0.306(3) 0.5605(13) 0.109(12) Uiso 1 1 d D . . H19 H 0.2445 -0.3373 0.5269 0.131 Uiso 1 1 calc R . . C20 C 0.2444(9) -0.139(3) 0.6124(13) 0.103(11) Uiso 1 1 d D . . H20 H 0.2405 -0.0604 0.6154 0.124 Uiso 1 1 calc R . . C21 C 0.2609(12) -0.374(3) 0.6052(15) 0.141(14) Uiso 1 1 d D . . H21 H 0.2662 -0.4522 0.6027 0.169 Uiso 1 1 calc R . . C22 C 0.2543(12) -0.212(3) 0.6547(15) 0.150(15) Uiso 1 1 d D . . H22 H 0.2531 -0.1817 0.6875 0.180 Uiso 1 1 calc R . . C23 C 0.2655(14) -0.323(4) 0.6528(17) 0.142(15) Uiso 1 1 d D . . O24 O 0.2740(8) -0.391(2) 0.6964(9) 0.135(9) Uiso 1 1 d . . . H24A H 0.2751 -0.4584 0.6875 0.162 Uiso 1 1 calc R . . O25 O 0.2551(9) 0.153(2) 0.4664(9) 0.123(8) Uiso 1 1 d . . . C26 C 0.2973(11) 0.223(3) 0.4552(9) 0.096(11) Uiso 1 1 d D . . C27 C 0.2973(13) 0.338(3) 0.4660(11) 0.125(13) Uiso 1 1 d D . . H27 H 0.2714 0.3727 0.4809 0.150 Uiso 1 1 calc R . . C28 C 0.3334(10) 0.175(2) 0.4320(9) 0.071(9) Uiso 1 1 d D . . H28 H 0.3327 0.0961 0.4264 0.085 Uiso 1 1 calc R . . C29 C 0.3387(12) 0.397(3) 0.4530(11) 0.113(12) Uiso 1 1 d D . . H29 H 0.3418 0.4738 0.4626 0.136 Uiso 1 1 calc R . . C30 C 0.3719(11) 0.242(3) 0.4164(11) 0.099(11) Uiso 1 1 d D . . H30 H 0.3955 0.2100 0.3979 0.118 Uiso 1 1 calc R . . C31 C 0.3751(12) 0.358(3) 0.4284(11) 0.080(10) Uiso 1 1 d D . . O32 O 0.4142(8) 0.417(2) 0.4127(8) 0.126(8) Uiso 1 1 d . . . H32A H 0.4132 0.4843 0.4213 0.188 Uiso 1 1 calc R . . O33 O 0.2048(11) 0.090(3) 0.5349(11) 0.167(10) Uiso 1 1 d . . . C34 C 0.1759(11) 0.175(3) 0.5497(11) 0.110(12) Uiso 1 1 d D . . C35 C 0.1513(10) 0.153(3) 0.5886(11) 0.095(11) Uiso 1 1 d D . . H35 H 0.1548 0.0823 0.6053 0.114 Uiso 1 1 calc R . . C36 C 0.1727(10) 0.278(3) 0.5248(11) 0.101(11) Uiso 1 1 d D . . H36 H 0.1907 0.2907 0.4981 0.121 Uiso 1 1 calc R . . C37 C 0.1204(12) 0.239(3) 0.6032(13) 0.122(13) Uiso 1 1 d D . . H37 H 0.1010 0.2251 0.6287 0.146 Uiso 1 1 calc R . . C38 C 0.1423(10) 0.363(3) 0.5399(11) 0.091(11) Uiso 1 1 d D . . H38 H 0.1382 0.4336 0.5225 0.110 Uiso 1 1 calc R . . C39 C 0.1185(11) 0.345(3) 0.5800(11) 0.079(10) Uiso 1 1 d D . . O40 O 0.0835(8) 0.422(2) 0.5946(9) 0.132(8) Uiso 1 1 d . . . H40A H 0.0845 0.4830 0.5793 0.197 Uiso 1 1 calc R . . O41 O 0.2735(9) -0.064(2) 0.4419(10) 0.126(8) Uiso 1 1 d . . . C42 C 0.2557(9) -0.147(3) 0.3988(12) 0.092(11) Uiso 1 1 d D . . C43 C 0.2711(11) -0.112(3) 0.3562(13) 0.125(13) Uiso 1 1 d D . . H43 H 0.2831 -0.0384 0.3524 0.150 Uiso 1 1 calc R . . C44 C 0.2371(10) -0.249(3) 0.4075(12) 0.109(12) Uiso 1 1 d D . . H44 H 0.2267 -0.2641 0.4387 0.131 Uiso 1 1 calc R . . C45 C 0.2679(11) -0.196(3) 0.3176(13) 0.124(13) Uiso 1 1 d D . . H45 H 0.2811 -0.1825 0.2879 0.149 Uiso 1 1 calc R . . C46 C 0.2333(10) -0.335(3) 0.3687(11) 0.081(10) Uiso 1 1 d D . . H46 H 0.2236 -0.4097 0.3739 0.097 Uiso 1 1 calc R . . C47 C 0.2448(11) -0.300(3) 0.3241(13) 0.095(11) Uiso 1 1 d D . . O48 O 0.2434(8) -0.3794(19) 0.2824(8) 0.117(8) Uiso 1 1 d . . . H48A H 0.2292 -0.4392 0.2888 0.176 Uiso 1 1 calc R . . N49 N -0.0854(12) 0.171(3) 0.2893(11) 0.140(12) Uiso 1 1 d D . . C50 C -0.1217(14) 0.210(4) 0.3100(13) 0.159(16) Uiso 1 1 d D . . H50 H -0.1381 0.1604 0.3295 0.191 Uiso 1 1 calc R . . C51 C -0.0638(16) 0.230(4) 0.2591(16) 0.22(2) Uiso 1 1 d D . . H51 H -0.0365 0.1996 0.2448 0.266 Uiso 1 1 calc R . . C52 C -0.1381(16) 0.322(4) 0.3050(17) 0.20(2) Uiso 1 1 d D . . H52 H -0.1569 0.3554 0.3278 0.245 Uiso 1 1 calc R . . C53 C -0.0823(17) 0.342(4) 0.2481(17) 0.20(2) Uiso 1 1 d D . . H53 H -0.0651 0.3902 0.2289 0.240 Uiso 1 1 calc R . . C54 C -0.1256(14) 0.381(3) 0.2657(14) 0.121(13) Uiso 1 1 d D . . C55 C -0.1507(16) 0.512(3) 0.2662(17) 0.155(16) Uiso 1 1 d . . . H55A H -0.1905 0.5105 0.2592 0.186 Uiso 1 1 calc R . . H55B H -0.1356 0.5489 0.3003 0.186 Uiso 1 1 calc R . . C56 C -0.1345(17) 0.568(4) 0.2264(17) 0.165(17) Uiso 1 1 d . . . H56B H -0.1468 0.5259 0.1933 0.198 Uiso 1 1 calc R . . H56A H -0.0947 0.5731 0.2351 0.198 Uiso 1 1 calc R . . C57 C -0.1596(15) 0.687(3) 0.2204(13) 0.124(13) Uiso 1 1 d D . . C58 C -0.2080(17) 0.720(4) 0.1849(16) 0.183(18) Uiso 1 1 d D . . H58 H -0.2257 0.6649 0.1606 0.220 Uiso 1 1 calc R . . C59 C -0.1366(14) 0.781(3) 0.2510(14) 0.147(15) Uiso 1 1 d D . . H59 H -0.1040 0.7733 0.2773 0.176 Uiso 1 1 calc R . . C60 C -0.2332(15) 0.827(3) 0.1818(14) 0.129(14) Uiso 1 1 d D . . H60 H -0.2687 0.8375 0.1605 0.155 Uiso 1 1 calc R . . C61 C -0.1629(15) 0.887(3) 0.2419(14) 0.137(14) Uiso 1 1 d D . . H61 H -0.1455 0.9466 0.2633 0.164 Uiso 1 1 calc R . . N62 N -0.2072(12) 0.913(3) 0.2083(11) 0.106(9) Uiso 1 1 d D . . N63 N 0.5613(13) 0.161(3) 0.7056(11) 0.138(11) Uiso 1 1 d D . . C64 C 0.5400(13) 0.215(4) 0.7342(13) 0.160(15) Uiso 1 1 d D . . H64 H 0.5118 0.1798 0.7455 0.192 Uiso 1 1 calc R . . C65 C 0.5986(16) 0.209(4) 0.6934(14) 0.180(18) Uiso 1 1 d D . . H65 H 0.6166 0.1674 0.6723 0.216 Uiso 1 1 calc R . . C66 C 0.5534(19) 0.328(4) 0.7523(18) 0.24(2) Uiso 1 1 d D . . H66 H 0.5306 0.3671 0.7693 0.283 Uiso 1 1 calc R . . C67 C 0.6180(19) 0.319(4) 0.7074(19) 0.24(2) Uiso 1 1 d D . . H67 H 0.6432 0.3524 0.6911 0.286 Uiso 1 1 calc R . . C68 C 0.5999(18) 0.380(4) 0.7450(18) 0.173(17) Uiso 1 1 d D . . C69 C 0.386(2) -0.988(5) 0.736(2) 0.24(3) Uiso 1 1 d . . . H69A H 0.4193 -0.9454 0.7390 0.282 Uiso 1 1 calc R . . H69B H 0.3647 -0.9868 0.6989 0.282 Uiso 1 1 calc R . . C70 C 0.361(3) -0.949(6) 0.762(3) 0.30(4) Uiso 1 1 d . . . H70B H 0.3835 -0.9336 0.7974 0.362 Uiso 1 1 calc R . . H70A H 0.3307 -0.9991 0.7648 0.362 Uiso 1 1 calc R . . C71 C 0.3361(18) -0.825(4) 0.7297(17) 0.164(17) Uiso 1 1 d D . . C72 C 0.292(2) -0.804(5) 0.688(2) 0.27(3) Uiso 1 1 d D . . H72 H 0.2737 -0.8644 0.6683 0.321 Uiso 1 1 calc R . . C73 C 0.3637(15) -0.731(4) 0.7594(15) 0.155(15) Uiso 1 1 d D . . H73 H 0.3939 -0.7390 0.7885 0.186 Uiso 1 1 calc R . . C74 C 0.2745(17) -0.691(5) 0.6748(18) 0.189(19) Uiso 1 1 d D . . H74 H 0.2451 -0.6782 0.6454 0.227 Uiso 1 1 calc R . . C75 C 0.3407(16) -0.623(4) 0.7407(16) 0.150(15) Uiso 1 1 d D . . H75 H 0.3579 -0.5579 0.7577 0.180 Uiso 1 1 calc R . . N76 N 0.2976(14) -0.609(3) 0.7017(14) 0.131(11) Uiso 1 1 d D . . N77 N 0.4278(12) -0.366(3) 0.4510(8) 0.119(10) Uiso 1 1 d D . . C78 C 0.3932(15) -0.282(3) 0.4439(11) 0.140(14) Uiso 1 1 d D . . H78 H 0.3562 -0.3001 0.4307 0.168 Uiso 1 1 calc R . . C79 C 0.4768(14) -0.330(3) 0.4700(11) 0.120(13) Uiso 1 1 d D . . H79 H 0.5035 -0.3871 0.4758 0.144 Uiso 1 1 calc R . . C80 C 0.4052(14) -0.168(3) 0.4537(12) 0.134(14) Uiso 1 1 d D . . H80 H 0.3770 -0.1136 0.4471 0.161 Uiso 1 1 calc R . . C81 C 0.4971(13) -0.220(3) 0.4836(11) 0.109(12) Uiso 1 1 d D . . H81 H 0.5342 -0.2056 0.4985 0.131 Uiso 1 1 calc R . . C82 C 0.4588(12) -0.134(3) 0.4735(10) 0.073(9) Uiso 1 1 d D . . C83 C 0.4722(9) -0.015(2) 0.4841(11) 0.073(10) Uiso 1 1 d . . . H83A H 0.4459 0.0164 0.5019 0.087 Uiso 1 1 calc R . . H83B H 0.4663 0.0237 0.4501 0.087 Uiso 1 1 calc R . . C84 C 0.0277(11) 0.984(3) 0.5141(13) 0.099(12) Uiso 1 1 d . . . H84A H 0.0357 1.0176 0.5495 0.119 Uiso 1 1 calc R . . H84B H 0.0532 1.0167 0.4957 0.119 Uiso 1 1 calc R . . C85 C 0.0369(13) 0.859(3) 0.5192(9) 0.093(10) Uiso 1 1 d D . . C86 C 0.0909(14) 0.821(3) 0.5374(10) 0.128(13) Uiso 1 1 d D . . H86 H 0.1199 0.8728 0.5433 0.153 Uiso 1 1 calc R . . C87 C 0.0000(13) 0.773(3) 0.5147(10) 0.123(14) Uiso 1 1 d D . . H87 H -0.0371 0.7904 0.5020 0.147 Uiso 1 1 calc R . . C88 C 0.1016(15) 0.703(3) 0.5470(12) 0.135(14) Uiso 1 1 d D . . H88 H 0.1381 0.6793 0.5562 0.162 Uiso 1 1 calc R . . C89 C 0.0137(14) 0.659(3) 0.5275(12) 0.116(12) Uiso 1 1 d D . . H89 H -0.0141 0.6052 0.5243 0.139 Uiso 1 1 calc R . . N90 N 0.0641(12) 0.628(2) 0.5438(10) 0.104(9) Uiso 1 1 d D . . O200 O 0.0303 0.5012 0.3365 0.222 Uiso 0.50 1 d P . . C201 C 0.0546 0.5707 0.3738 0.232 Uiso 0.50 1 d P . . H20A H 0.0287 0.5854 0.3945 0.279 Uiso 0.50 1 d P . . H20B H 0.0588 0.6413 0.3565 0.279 Uiso 0.50 1 d P . . C202 C 0.1043 0.5510 0.4100 0.283 Uiso 0.50 1 d P . . H20C H 0.1009 0.5415 0.4460 0.340 Uiso 0.50 1 calc PR . . H20D H 0.1317 0.6089 0.4088 0.340 Uiso 0.50 1 calc PR . . C203 C 0.1141 0.4435 0.3854 0.264 Uiso 0.50 1 d P . . H20E H 0.1343 0.4549 0.3586 0.316 Uiso 0.50 1 calc PR . . H20F H 0.1334 0.3888 0.4116 0.316 Uiso 0.50 1 calc PR . . C204 C 0.0576 0.4084 0.3619 0.246 Uiso 0.50 1 d P . . H20G H 0.0567 0.3471 0.3371 0.295 Uiso 0.50 1 d P . . H20H H 0.0407 0.3825 0.3890 0.295 Uiso 0.50 1 d P . . O210 O 0.4814 0.5181 0.6706 0.240 Uiso 0.50 1 d P . . C211 C 0.4497 0.4212 0.6413 0.256 Uiso 0.50 1 d P . . H21F H 0.4402 0.3753 0.6683 0.307 Uiso 0.50 1 d P . . H21H H 0.4762 0.3774 0.6288 0.307 Uiso 0.50 1 d P . . C212 C 0.4020 0.4204 0.5985 0.229 Uiso 0.50 1 d P . . H21B H 0.3690 0.3998 0.6093 0.274 Uiso 0.50 1 calc PR . . H21C H 0.4058 0.3726 0.5691 0.274 Uiso 0.50 1 calc PR . . C213 C 0.4052 0.5516 0.5867 0.247 Uiso 0.50 1 d P . . H21D H 0.3748 0.5949 0.5934 0.297 Uiso 0.50 1 calc PR . . H21E H 0.4094 0.5673 0.5513 0.297 Uiso 0.50 1 calc PR . . C214 C 0.4641 0.5674 0.6347 0.244 Uiso 0.50 1 d P . . H21A H 0.4924 0.5674 0.6159 0.292 Uiso 0.50 1 d P . . H21G H 0.4625 0.6443 0.6471 0.292 Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.1058(16) 0.0566(14) 0.0659(13) 0.0063(10) 0.0234(11) -0.0008(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 O9 1.77(3) . ? W1 O25 1.85(2) . ? W1 O17 1.87(2) . ? W1 O33 1.87(3) . ? W1 O1 1.89(3) . ? W1 O41 1.91(2) . ? O1 C2 1.34(3) . ? C2 C3 1.29(2) . ? C2 C4 1.35(2) . ? C3 C5 1.35(2) . ? C4 C6 1.37(2) . ? C5 C7 1.37(3) . ? C6 C7 1.34(2) . ? C7 O8 1.33(3) . ? O9 C10 1.37(3) . ? C10 C12 1.34(2) . ? C10 C11 1.36(2) . ? C11 C13 1.34(2) . ? C12 C14 1.33(2) . ? C13 C15 1.32(2) . ? C14 C15 1.34(2) . ? C15 O16 1.37(3) . ? O17 C18 1.43(3) . ? C18 C20 1.33(2) . ? C18 C19 1.36(2) . ? C19 C21 1.38(3) . ? C20 C22 1.36(3) . ? C21 C23 1.35(3) . ? C22 C23 1.34(3) . ? C23 O24 1.36(4) . ? O25 C26 1.43(3) . ? C26 C28 1.33(2) . ? C26 C27 1.38(2) . ? C27 C29 1.36(2) . ? C28 C30 1.39(2) . ? C29 C31 1.32(2) . ? C30 C31 1.39(2) . ? C31 O32 1.35(3) . ? O33 C34 1.34(3) . ? C34 C35 1.34(2) . ? C34 C36 1.37(2) . ? C35 C37 1.38(2) . ? C36 C38 1.37(2) . ? C37 C39 1.38(2) . ? C38 C39 1.34(2) . ? C39 O40 1.38(3) . ? O41 C42 1.46(3) . ? C42 C44 1.32(2) . ? C42 C43 1.33(2) . ? C43 C45 1.39(3) . ? C44 C46 1.41(2) . ? C45 C47 1.37(2) . ? C46 C47 1.33(2) . ? C47 O48 1.42(3) . ? N49 C50 1.26(3) . ? N49 C51 1.27(4) . ? C50 C52 1.38(3) . ? C51 C53 1.40(3) . ? C52 C54 1.34(3) . ? C53 C54 1.36(3) . ? C54 C55 1.66(4) . ? C55 C56 1.37(4) . ? C56 C57 1.52(4) . ? C57 C58 1.38(3) . ? C57 C59 1.39(3) . ? C58 C60 1.40(3) . ? C59 C61 1.40(3) . ? C60 N62 1.29(3) . ? C61 N62 1.26(3) . ? N63 C65 1.20(3) . ? N63 C64 1.20(3) . ? C64 C66 1.41(3) . ? C64 C65 2.03(5) . ? C65 C67 1.40(3) . ? C66 C68 1.37(3) . ? C67 C68 1.37(3) . ? C68 C69 1.64(6) 2_666 ? C69 C70 1.13(7) . ? C69 C68 1.64(6) 2_636 ? C70 C71 1.71(7) . ? C71 C72 1.35(3) . ? C71 C73 1.42(3) . ? C72 C74 1.41(3) . ? C73 C75 1.42(3) . ? C74 N76 1.25(4) . ? C75 N76 1.29(3) . ? N77 C79 1.27(3) . ? N77 C78 1.30(3) . ? C78 C80 1.38(3) . ? C79 C81 1.40(3) . ? C80 C82 1.37(2) . ? C81 C82 1.37(2) . ? C82 C83 1.44(3) . ? C83 C83 1.48(5) 3_656 ? C84 C84 1.44(5) 3_576 ? C84 C85 1.49(4) . ? C85 C87 1.36(3) . ? C85 C86 1.39(2) . ? C86 C88 1.41(3) . ? C87 C89 1.39(3) . ? C88 N90 1.28(3) . ? C89 N90 1.28(3) . ? O200 C201 1.2949 . ? O200 C204 1.3622 . ? C201 C202 1.3785 . ? C201 C204 1.9284 . ? C202 C203 1.4595 . ? C203 C204 1.4545 . ? O210 C214 1.0893 . ? O210 C211 1.4816 . ? C211 C212 1.4124 . ? C211 C214 1.7651 . ? C212 C213 1.5706 . ? C213 C214 1.6850 . ? 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 O9 W1 O25 89.5(9) . . ? O9 W1 O17 90.8(9) . . ? O25 W1 O17 177.2(8) . . ? O9 W1 O33 94.9(11) . . ? O25 W1 O33 86.3(11) . . ? O17 W1 O33 91.0(10) . . ? O9 W1 O1 179.4(10) . . ? O25 W1 O1 89.9(9) . . ? O17 W1 O1 89.8(9) . . ? O33 W1 O1 85.1(11) . . ? O9 W1 O41 88.3(9) . . ? O25 W1 O41 91.4(9) . . ? O17 W1 O41 91.3(9) . . ? O33 W1 O41 176.0(11) . . ? O1 W1 O41 91.7(10) . . ? C2 O1 W1 166(2) . . ? C3 C2 O1 126(3) . . ? C3 C2 C4 125(4) . . ? O1 C2 C4 109(3) . . ? C2 C3 C5 117(4) . . ? C2 C4 C6 118(3) . . ? C3 C5 C7 120(4) . . ? C7 C6 C4 117(3) . . ? C6 C7 O8 125(3) . . ? C6 C7 C5 121(4) . . ? O8 C7 C5 113(3) . . ? C10 O9 W1 169.5(19) . . ? C12 C10 C11 115(3) . . ? C12 C10 O9 126(3) . . ? C11 C10 O9 119(3) . . ? C13 C11 C10 121(3) . . ? C14 C12 C10 123(3) . . ? C15 C13 C11 124(3) . . ? C12 C14 C15 122(3) . . ? C13 C15 C14 115(3) . . ? C13 C15 O16 128(3) . . ? C14 C15 O16 116(3) . . ? C18 O17 W1 137.6(17) . . ? C20 C18 C19 125(3) . . ? C20 C18 O17 119(3) . . ? C19 C18 O17 116(3) . . ? C18 C19 C21 119(4) . . ? C18 C20 C22 113(4) . . ? C23 C21 C19 118(4) . . ? C23 C22 C20 125(4) . . ? C22 C23 C21 119(4) . . ? C22 C23 O24 122(4) . . ? C21 C23 O24 118(4) . . ? C26 O25 W1 144.1(18) . . ? C28 C26 C27 123(3) . . ? C28 C26 O25 118(3) . . ? C27 C26 O25 119(3) . . ? C29 C27 C26 114(3) . . ? C26 C28 C30 120(3) . . ? C31 C29 C27 128(4) . . ? C31 C30 C28 120(3) . . ? C29 C31 O32 128(3) . . ? C29 C31 C30 116(3) . . ? O32 C31 C30 116(3) . . ? C34 O33 W1 157(3) . . ? O33 C34 C35 118(3) . . ? O33 C34 C36 119(3) . . ? C35 C34 C36 123(4) . . ? C34 C35 C37 118(3) . . ? C34 C36 C38 119(3) . . ? C39 C37 C35 120(3) . . ? C39 C38 C36 120(3) . . ? C38 C39 O40 123(3) . . ? C38 C39 C37 121(3) . . ? O40 C39 C37 115(3) . . ? C42 O41 W1 135.8(18) . . ? C44 C42 C43 128(4) . . ? C44 C42 O41 121(3) . . ? C43 C42 O41 110(3) . . ? C42 C43 C45 114(4) . . ? C42 C44 C46 119(3) . . ? C47 C45 C43 119(3) . . ? C47 C46 C44 115(3) . . ? C46 C47 C45 125(3) . . ? C46 C47 O48 119(3) . . ? C45 C47 O48 114(3) . . ? C50 N49 C51 123(4) . . ? N49 C50 C52 123(4) . . ? N49 C51 C53 118(5) . . ? C54 C52 C50 116(4) . . ? C54 C53 C51 120(5) . . ? C52 C54 C53 117(4) . . ? C52 C54 C55 108(4) . . ? C53 C54 C55 131(4) . . ? C56 C55 C54 104(3) . . ? C55 C56 C57 109(4) . . ? C58 C57 C59 109(4) . . ? C58 C57 C56 126(4) . . ? C59 C57 C56 124(4) . . ? C57 C58 C60 127(4) . . ? C57 C59 C61 120(4) . . ? N62 C60 C58 120(4) . . ? N62 C61 C59 129(4) . . ? C61 N62 C60 115(4) . . ? C65 N63 C64 115(4) . . ? N63 C64 C66 126(4) . . ? N63 C64 C65 33(2) . . ? C66 C64 C65 94(3) . . ? N63 C65 C67 127(5) . . ? N63 C65 C64 33(2) . . ? C67 C65 C64 95(4) . . ? C68 C66 C64 120(5) . . ? C68 C67 C65 120(5) . . ? C67 C68 C66 109(5) . . ? C67 C68 C69 128(5) . 2_666 ? C66 C68 C69 120(5) . 2_666 ? C70 C69 C68 108(7) . 2_636 ? C69 C70 C71 104(7) . . ? C72 C71 C73 118(5) . . ? C72 C71 C70 132(5) . . ? C73 C71 C70 109(5) . . ? C71 C72 C74 121(6) . . ? C75 C73 C71 114(4) . . ? N76 C74 C72 121(5) . . ? N76 C75 C73 125(4) . . ? C74 N76 C75 121(4) . . ? C79 N77 C78 111(4) . . ? N77 C78 C80 127(4) . . ? N77 C79 C81 131(4) . . ? C82 C80 C78 120(4) . . ? C82 C81 C79 116(3) . . ? C81 C82 C80 116(3) . . ? C81 C82 C83 124(3) . . ? C80 C82 C83 120(3) . . ? C82 C83 C83 119(3) . 3_656 ? C84 C84 C85 114(3) 3_576 . ? C87 C85 C86 112(3) . . ? C87 C85 C84 130(3) . . ? C86 C85 C84 117(3) . . ? C85 C86 C88 120(4) . . ? C85 C87 C89 125(3) . . ? N90 C88 C86 124(4) . . ? N90 C89 C87 121(3) . . ? C88 N90 C89 118(3) . . ? C201 O200 C204 93.0 . . ? O200 C201 C202 125.4 . . ? O200 C201 C204 44.9 . . ? C202 C201 C204 83.1 . . ? C201 C202 C203 94.0 . . ? C204 C203 C202 99.9 . . ? O200 C204 C203 107.3 . . ? O200 C204 C201 42.1 . . ? C203 C204 C201 74.3 . . ? C214 O210 C211 85.3 . . ? C212 C211 O210 130.4 . . ? C212 C211 C214 94.8 . . ? O210 C211 C214 38.0 . . ? C211 C212 C213 94.1 . . ? C212 C213 C214 92.4 . . ? O210 C214 C213 131.4 . . ? O210 C214 C211 56.8 . . ? C213 C214 C211 78.6 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 15.86 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.992 _refine_diff_density_min -1.430 _refine_diff_density_rms 0.177 #===END