# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gerard Parkin' _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_section_title ; p-tert-Butyltetrathiatetramercaptocalix[4]arene as a Sulfur-Rich Platform for Molybdenum, Tungsten and Nickel ; loop_ _publ_author_name 'Gerard Parkin' 'Daniela Buccella' # Attachment 'S8NIS10_new.CIF' data_s8nis10 _database_code_depnum_ccdc_archive 'CCDC 702274' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H74 Ni2 P2 S8' _chemical_formula_weight 1207.01 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0009(7) _cell_length_b 16.9077(11) _cell_length_c 17.2253(12) _cell_angle_alpha 107.1050(10) _cell_angle_beta 103.4440(10) _cell_angle_gamma 103.6220(10) _cell_volume 3070.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 2768 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 22.48 _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9263 _exptl_absorpt_correction_T_max 0.9808 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13738 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.1498 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10181 _reflns_number_gt 5309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00105(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10181 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1536 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.09934(7) 0.33033(5) 0.36689(5) 0.0343(2) Uani 1 1 d . . . S1 S -0.13301(13) 0.41212(10) 0.29593(10) 0.0314(4) Uani 1 1 d . . . S2 S 0.35910(13) 0.52793(11) 0.45974(10) 0.0365(4) Uani 1 1 d . . . S10 S -0.24349(14) 0.34424(10) 0.41908(11) 0.0379(4) Uani 1 1 d . . . S20 S 0.09173(14) 0.37031(10) 0.38075(11) 0.0361(4) Uani 1 1 d . . . P1 P -0.08583(15) 0.22370(11) 0.40912(11) 0.0382(5) Uani 1 1 d . . . C10 C -0.2575(5) 0.4413(4) 0.4076(4) 0.0261(14) Uani 1 1 d . . . C11 C -0.2164(5) 0.4712(4) 0.3488(3) 0.0253(14) Uani 1 1 d . . . C12 C -0.2499(5) 0.5358(4) 0.3254(4) 0.0302(15) Uani 1 1 d . . . H12A H -0.2263 0.5499 0.2815 0.036 Uiso 1 1 calc R . . C13 C -0.3176(5) 0.5805(4) 0.3649(4) 0.0272(14) Uani 1 1 d . . . C14 C -0.3441(5) 0.5587(4) 0.4318(4) 0.0298(15) Uani 1 1 d . . . H14A H -0.3835 0.5908 0.4635 0.036 Uiso 1 1 calc R . . C15 C -0.3154(5) 0.4921(4) 0.4541(4) 0.0293(15) Uani 1 1 d . . . C16 C -0.3640(6) 0.6461(4) 0.3343(4) 0.0396(17) Uani 1 1 d . . . C17 C -0.2960(6) 0.6807(4) 0.2806(4) 0.057(2) Uani 1 1 d . . . H17A H -0.2122 0.7133 0.3155 0.086 Uiso 1 1 calc R . . H17B H -0.3332 0.7189 0.2599 0.086 Uiso 1 1 calc R . . H17C H -0.2993 0.6320 0.2321 0.086 Uiso 1 1 calc R . . C18 C -0.4980(6) 0.5960(5) 0.2764(4) 0.064(2) Uani 1 1 d . . . H18A H -0.5322 0.6354 0.2556 0.095 Uiso 1 1 calc R . . H18B H -0.5441 0.5743 0.3095 0.095 Uiso 1 1 calc R . . H18C H -0.5014 0.5472 0.2281 0.095 Uiso 1 1 calc R . . C19 C -0.3623(7) 0.7223(4) 0.4088(4) 0.067(2) Uani 1 1 d . . . H19A H -0.2793 0.7551 0.4455 0.100 Uiso 1 1 calc R . . H19B H -0.4083 0.7001 0.4418 0.100 Uiso 1 1 calc R . . H19C H -0.3983 0.7603 0.3868 0.100 Uiso 1 1 calc R . . C20 C 0.1123(5) 0.4707(4) 0.3663(3) 0.0282(15) Uani 1 1 d . . . C21 C 0.2245(5) 0.5349(4) 0.3939(4) 0.0291(15) Uani 1 1 d . . . C22 C 0.2372(5) 0.6075(4) 0.3693(4) 0.0365(16) Uani 1 1 d . . . H22A H 0.3141 0.6502 0.3897 0.044 Uiso 1 1 calc R . . C23 C 0.1421(6) 0.6190(4) 0.3168(4) 0.0371(16) Uani 1 1 d . . . C24 C 0.0293(5) 0.5602(4) 0.2967(4) 0.0349(16) Uani 1 1 d . . . H24A H -0.0387 0.5679 0.2638 0.042 Uiso 1 1 calc R . . C25 C 0.0128(5) 0.4899(4) 0.3235(3) 0.0281(15) Uani 1 1 d . . . C26 C 0.1628(6) 0.6932(5) 0.2819(5) 0.0499(19) Uani 1 1 d . . . C27 C 0.1910(8) 0.6591(6) 0.1986(6) 0.116(4) Uani 1 1 d . . . H27A H 0.2036 0.7045 0.1748 0.173 Uiso 1 1 calc R . . H27B H 0.1236 0.6082 0.1577 0.173 Uiso 1 1 calc R . . H27C H 0.2637 0.6429 0.2105 0.173 Uiso 1 1 calc R . . C28 C 0.0499(7) 0.7179(5) 0.2572(5) 0.078(3) Uani 1 1 d . . . H28A H 0.0670 0.7645 0.2353 0.117 Uiso 1 1 calc R . . H28B H 0.0252 0.7377 0.3073 0.117 Uiso 1 1 calc R . . H28C H -0.0148 0.6672 0.2133 0.117 Uiso 1 1 calc R . . C29 C 0.2630(8) 0.7732(6) 0.3444(6) 0.151(5) Uani 1 1 d . . . H29A H 0.2726 0.8183 0.3200 0.227 Uiso 1 1 calc R . . H29B H 0.3377 0.7596 0.3570 0.227 Uiso 1 1 calc R . . H29C H 0.2439 0.7940 0.3969 0.227 Uiso 1 1 calc R . . C31 C -0.2257(5) 0.1485(4) 0.4009(4) 0.053(2) Uani 1 1 d . . . H31A H -0.2088 0.1035 0.4214 0.079 Uiso 1 1 calc R . . H31B H -0.2776 0.1216 0.3414 0.079 Uiso 1 1 calc R . . H31C H -0.2661 0.1799 0.4355 0.079 Uiso 1 1 calc R . . C32 C 0.0035(6) 0.2636(4) 0.5210(4) 0.064(2) Uani 1 1 d . . . H32A H 0.0080 0.2144 0.5382 0.096 Uiso 1 1 calc R . . H32B H -0.0340 0.2982 0.5554 0.096 Uiso 1 1 calc R . . H32C H 0.0846 0.2996 0.5296 0.096 Uiso 1 1 calc R . . C33 C -0.0137(6) 0.1520(4) 0.3543(4) 0.061(2) Uani 1 1 d . . . H33A H -0.0121 0.1064 0.3776 0.092 Uiso 1 1 calc R . . H33B H 0.0685 0.1858 0.3627 0.092 Uiso 1 1 calc R . . H33C H -0.0592 0.1256 0.2934 0.092 Uiso 1 1 calc R . . Ni2 Ni 0.27442(7) -0.02161(5) -0.11202(5) 0.0395(2) Uani 1 1 d . . . P2 P 0.20396(17) 0.08651(12) -0.08611(12) 0.0496(5) Uani 1 1 d . . . S21 S 0.29743(14) -0.14606(10) -0.16601(10) 0.0331(4) Uani 1 1 d . . . S22 S 0.31624(17) -0.10293(11) 0.16692(11) 0.0475(5) Uani 1 1 d . . . S210 S 0.39930(15) 0.03964(10) -0.16589(11) 0.0435(5) Uani 1 1 d . . . S220 S 0.23453(16) -0.05262(11) -0.00645(11) 0.0477(5) Uani 1 1 d . . . C210 C 0.4849(5) -0.0321(4) -0.1805(3) 0.0311(15) Uani 1 1 d . . . C211 C 0.4388(5) -0.1180(4) -0.1866(3) 0.0272(15) Uani 1 1 d . . . C212 C 0.4901(5) -0.1808(4) -0.2164(3) 0.0338(16) Uani 1 1 d . . . H21A H 0.4505 -0.2395 -0.2258 0.041 Uiso 1 1 calc R . . C213 C 0.5998(6) -0.1588(4) -0.2328(3) 0.0332(16) Uani 1 1 d . . . C214 C 0.6528(6) -0.0703(4) -0.2153(4) 0.0385(17) Uani 1 1 d . . . H21B H 0.7293 -0.0523 -0.2218 0.046 Uiso 1 1 calc R . . C215 C 0.6003(6) -0.0070(4) -0.1888(4) 0.0330(16) Uani 1 1 d . . . C216 C 0.6559(6) -0.2267(4) -0.2709(4) 0.0415(17) Uani 1 1 d . . . C217 C 0.5985(6) -0.3157(4) -0.2686(5) 0.063(2) Uani 1 1 d . . . H21C H 0.6094 -0.3105 -0.2095 0.094 Uiso 1 1 calc R . . H21D H 0.6368 -0.3563 -0.2941 0.094 Uiso 1 1 calc R . . H21E H 0.5126 -0.3372 -0.3007 0.094 Uiso 1 1 calc R . . C218 C 0.7919(6) -0.1967(4) -0.2234(5) 0.067(2) Uani 1 1 d . . . H21F H 0.8052 -0.1895 -0.1637 0.100 Uiso 1 1 calc R . . H21G H 0.8310 -0.1413 -0.2269 0.100 Uiso 1 1 calc R . . H21H H 0.8258 -0.2402 -0.2495 0.100 Uiso 1 1 calc R . . C219 C 0.6383(7) -0.2367(5) -0.3647(4) 0.075(3) Uani 1 1 d . . . H21I H 0.6755 -0.1804 -0.3672 0.113 Uiso 1 1 calc R . . H21J H 0.5523 -0.2580 -0.3966 0.113 Uiso 1 1 calc R . . H21K H 0.6759 -0.2781 -0.3897 0.113 Uiso 1 1 calc R . . C220 C 0.3004(5) -0.1349(4) -0.0049(4) 0.0317(15) Uani 1 1 d . . . C221 C 0.3253(5) -0.1605(4) 0.0650(4) 0.0343(16) Uani 1 1 d . . . C222 C 0.3580(5) -0.2351(4) 0.0579(4) 0.0353(16) Uani 1 1 d . . . H22B H 0.3739 -0.2511 0.1061 0.042 Uiso 1 1 calc R . . C223 C 0.3683(5) -0.2872(4) -0.0177(4) 0.0356(16) Uani 1 1 d . . . C224 C 0.3518(5) -0.2581(4) -0.0849(4) 0.0327(15) Uani 1 1 d . . . H22C H 0.3605 -0.2901 -0.1366 0.039 Uiso 1 1 calc R . . C225 C 0.3226(5) -0.1820(4) -0.0774(4) 0.0283(15) Uani 1 1 d . . . C226 C 0.3877(7) -0.3758(4) -0.0279(4) 0.0454(18) Uani 1 1 d . . . C227 C 0.4535(7) -0.4000(5) -0.0925(5) 0.082(3) Uani 1 1 d . . . H22D H 0.5339 -0.3573 -0.0718 0.123 Uiso 1 1 calc R . . H22E H 0.4083 -0.4006 -0.1473 0.123 Uiso 1 1 calc R . . H22F H 0.4601 -0.4576 -0.0994 0.123 Uiso 1 1 calc R . . C228 C 0.4575(9) -0.3775(5) 0.0565(5) 0.120(4) Uani 1 1 d . . . H22G H 0.5372 -0.3335 0.0790 0.181 Uiso 1 1 calc R . . H22H H 0.4660 -0.4349 0.0475 0.181 Uiso 1 1 calc R . . H22I H 0.4140 -0.3653 0.0972 0.181 Uiso 1 1 calc R . . C229 C 0.2619(8) -0.4456(5) -0.0636(6) 0.097(3) Uani 1 1 d . . . H22J H 0.2174 -0.4325 -0.0238 0.146 Uiso 1 1 calc R . . H22K H 0.2707 -0.5026 -0.0710 0.146 Uiso 1 1 calc R . . H22L H 0.2180 -0.4457 -0.1186 0.146 Uiso 1 1 calc R . . C231 C 0.2962(8) 0.1754(5) 0.0095(5) 0.100(3) Uani 1 1 d . . . H23A H 0.2601 0.2217 0.0179 0.151 Uiso 1 1 calc R . . H23B H 0.3761 0.1973 0.0055 0.151 Uiso 1 1 calc R . . H23C H 0.3030 0.1562 0.0577 0.151 Uiso 1 1 calc R . . C232 C 0.1880(8) 0.1351(6) -0.1659(5) 0.112(4) Uani 1 1 d . . . H23D H 0.1555 0.1824 -0.1488 0.168 Uiso 1 1 calc R . . H23E H 0.1333 0.0912 -0.2205 0.168 Uiso 1 1 calc R . . H23F H 0.2666 0.1579 -0.1714 0.168 Uiso 1 1 calc R . . C233 C 0.0564(7) 0.0608(6) -0.0756(7) 0.141(5) Uani 1 1 d . . . H23G H 0.0320 0.1128 -0.0644 0.211 Uiso 1 1 calc R . . H23H H 0.0580 0.0405 -0.0283 0.211 Uiso 1 1 calc R . . H23I H -0.0010 0.0153 -0.1283 0.211 Uiso 1 1 calc R . . C300 C -0.018(3) -0.0540(10) 0.4208(11) 0.179(9) Uani 1 1 d . . . H30A H -0.0271 -0.0929 0.3662 0.215 Uiso 1 1 calc R . . C301 C -0.1179(18) -0.0476(15) 0.4409(18) 0.198(12) Uani 1 1 d . . . H30B H -0.1970 -0.0774 0.4021 0.238 Uiso 1 1 calc R . . C302 C -0.092(2) 0.0082(15) 0.5258(18) 0.155(7) Uani 1 1 d . . . H30C H -0.1573 0.0132 0.5457 0.186 Uiso 1 1 calc R . . C400 C 0.4650(13) 0.0341(14) 0.5678(11) 0.121(5) Uani 1 1 d . . . H40A H 0.4397 0.0574 0.6148 0.145 Uiso 1 1 calc R . . C401 C 0.5164(14) -0.0271(14) 0.5656(12) 0.110(5) Uani 1 1 d . . . H40B H 0.5294 -0.0462 0.6119 0.132 Uiso 1 1 calc R . . C402 C 0.5509(12) -0.0628(8) 0.4971(19) 0.137(5) Uani 1 1 d . . . H40C H 0.5857 -0.1073 0.4955 0.164 Uiso 1 1 calc R . . C500 C 0.1983(12) 0.4131(9) 0.0782(13) 0.144(5) Uani 1 1 d . . . H50A H 0.2695 0.4555 0.0839 0.172 Uiso 1 1 calc R . . C501 C 0.1235(17) 0.3602(10) 0.0001(9) 0.135(5) Uani 1 1 d . . . H50B H 0.1409 0.3652 -0.0490 0.162 Uiso 1 1 calc R . . C502 C 0.0233(13) 0.3000(8) -0.0070(8) 0.128(5) Uani 1 1 d . . . H50C H -0.0297 0.2613 -0.0617 0.154 Uiso 1 1 calc R . . C503 C -0.0026(9) 0.2943(8) 0.0631(12) 0.119(4) Uani 1 1 d . . . H50D H -0.0742 0.2527 0.0578 0.143 Uiso 1 1 calc R . . C504 C 0.0752(15) 0.3488(9) 0.1414(8) 0.101(4) Uani 1 1 d . . . H50E H 0.0579 0.3446 0.1908 0.122 Uiso 1 1 calc R . . C505 C 0.1743(13) 0.4074(7) 0.1493(8) 0.116(4) Uani 1 1 d . . . H50F H 0.2283 0.4451 0.2040 0.139 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0335(5) 0.0323(5) 0.0401(5) 0.0142(4) 0.0143(4) 0.0127(4) S1 0.0292(9) 0.0311(9) 0.0339(10) 0.0099(8) 0.0114(8) 0.0114(8) S2 0.0268(9) 0.0507(11) 0.0438(11) 0.0254(9) 0.0181(8) 0.0164(8) S10 0.0389(10) 0.0345(10) 0.0523(11) 0.0221(9) 0.0245(9) 0.0160(8) S20 0.0311(10) 0.0322(10) 0.0522(11) 0.0203(9) 0.0159(8) 0.0145(8) P1 0.0377(11) 0.0345(11) 0.0418(11) 0.0153(9) 0.0108(9) 0.0115(9) C10 0.015(3) 0.031(4) 0.029(4) 0.010(3) 0.004(3) 0.005(3) C11 0.017(3) 0.029(4) 0.026(4) 0.010(3) 0.004(3) 0.004(3) C12 0.023(4) 0.037(4) 0.026(4) 0.012(3) 0.003(3) 0.006(3) C13 0.027(4) 0.028(4) 0.028(4) 0.007(3) 0.008(3) 0.014(3) C14 0.023(4) 0.033(4) 0.033(4) 0.011(3) 0.008(3) 0.011(3) C15 0.017(3) 0.032(4) 0.036(4) 0.012(3) 0.006(3) 0.005(3) C16 0.048(4) 0.047(4) 0.039(4) 0.022(4) 0.017(4) 0.033(4) C17 0.065(5) 0.071(5) 0.072(5) 0.049(5) 0.033(4) 0.044(4) C18 0.053(5) 0.086(6) 0.059(5) 0.032(5) 0.009(4) 0.037(5) C19 0.099(6) 0.065(5) 0.054(5) 0.024(4) 0.027(5) 0.051(5) C20 0.036(4) 0.033(4) 0.027(4) 0.015(3) 0.023(3) 0.013(3) C21 0.030(4) 0.038(4) 0.031(4) 0.017(3) 0.017(3) 0.020(3) C22 0.030(4) 0.039(4) 0.043(4) 0.017(3) 0.018(3) 0.006(3) C23 0.034(4) 0.047(4) 0.036(4) 0.021(3) 0.014(3) 0.013(4) C24 0.033(4) 0.047(4) 0.035(4) 0.022(3) 0.015(3) 0.020(4) C25 0.029(4) 0.033(4) 0.025(4) 0.008(3) 0.015(3) 0.011(3) C26 0.047(5) 0.053(5) 0.064(5) 0.043(4) 0.020(4) 0.012(4) C27 0.155(9) 0.163(10) 0.152(9) 0.131(9) 0.124(8) 0.104(8) C28 0.087(6) 0.089(6) 0.117(7) 0.080(6) 0.054(6) 0.058(5) C29 0.131(9) 0.093(8) 0.167(11) 0.103(8) -0.051(8) -0.047(7) C31 0.056(5) 0.042(4) 0.059(5) 0.027(4) 0.019(4) 0.003(4) C32 0.068(5) 0.060(5) 0.053(5) 0.024(4) 0.003(4) 0.015(4) C33 0.072(5) 0.041(5) 0.091(6) 0.029(4) 0.039(5) 0.035(4) Ni2 0.0419(5) 0.0369(5) 0.0411(6) 0.0143(4) 0.0136(4) 0.0156(4) P2 0.0507(13) 0.0466(12) 0.0559(13) 0.0193(11) 0.0161(10) 0.0242(10) S21 0.0353(10) 0.0305(10) 0.0323(10) 0.0119(8) 0.0097(8) 0.0096(8) S22 0.0724(13) 0.0318(10) 0.0460(12) 0.0148(9) 0.0392(10) 0.0102(10) S210 0.0562(12) 0.0338(10) 0.0529(12) 0.0207(9) 0.0266(10) 0.0221(9) S220 0.0611(12) 0.0459(11) 0.0548(12) 0.0239(10) 0.0328(10) 0.0298(10) C210 0.042(4) 0.028(4) 0.024(4) 0.010(3) 0.010(3) 0.013(3) C211 0.035(4) 0.023(4) 0.017(3) 0.004(3) 0.006(3) 0.005(3) C212 0.045(4) 0.022(4) 0.025(4) 0.005(3) 0.007(3) 0.004(3) C213 0.046(4) 0.030(4) 0.020(4) 0.007(3) 0.012(3) 0.009(3) C214 0.049(4) 0.033(4) 0.031(4) 0.007(3) 0.020(3) 0.008(4) C215 0.049(4) 0.027(4) 0.028(4) 0.014(3) 0.019(3) 0.012(3) C216 0.055(5) 0.032(4) 0.044(5) 0.011(3) 0.026(4) 0.020(4) C217 0.065(5) 0.042(5) 0.093(6) 0.019(4) 0.040(5) 0.031(4) C218 0.052(5) 0.055(5) 0.089(6) 0.010(5) 0.028(5) 0.028(4) C219 0.108(7) 0.074(6) 0.058(6) 0.011(5) 0.044(5) 0.055(5) C220 0.038(4) 0.025(4) 0.034(4) 0.010(3) 0.019(3) 0.006(3) C221 0.044(4) 0.028(4) 0.034(4) 0.011(3) 0.022(3) 0.008(3) C222 0.047(4) 0.029(4) 0.030(4) 0.015(3) 0.014(3) 0.006(3) C223 0.039(4) 0.022(4) 0.040(4) 0.010(3) 0.010(3) 0.002(3) C224 0.046(4) 0.026(4) 0.025(4) 0.009(3) 0.014(3) 0.008(3) C225 0.030(4) 0.020(4) 0.029(4) 0.009(3) 0.005(3) 0.003(3) C226 0.077(5) 0.032(4) 0.036(4) 0.017(3) 0.018(4) 0.027(4) C227 0.129(8) 0.046(5) 0.101(7) 0.030(5) 0.054(6) 0.060(5) C228 0.241(12) 0.093(7) 0.042(6) 0.022(5) 0.017(7) 0.114(8) C229 0.123(8) 0.031(5) 0.139(9) 0.031(5) 0.054(7) 0.017(5) C231 0.138(8) 0.049(5) 0.078(7) -0.011(5) 0.002(6) 0.043(6) C232 0.187(10) 0.136(9) 0.093(7) 0.077(7) 0.067(7) 0.127(8) C233 0.065(6) 0.100(8) 0.301(15) 0.084(9) 0.094(8) 0.058(6) C300 0.209(18) 0.092(10) 0.147(14) 0.034(9) -0.084(17) 0.046(15) C301 0.125(15) 0.146(17) 0.27(3) 0.15(2) -0.066(19) -0.011(14) C302 0.126(16) 0.182(18) 0.194(17) 0.130(15) 0.024(14) 0.070(14) C400 0.096(10) 0.131(15) 0.094(12) 0.007(9) 0.030(8) 0.009(10) C401 0.080(8) 0.106(11) 0.121(15) 0.060(11) -0.003(8) 0.000(7) C402 0.127(10) 0.094(10) 0.169(15) 0.012(13) 0.038(13) 0.055(8) C500 0.123(11) 0.110(11) 0.168(14) 0.067(12) 0.036(12) -0.024(8) C501 0.211(16) 0.101(11) 0.086(10) 0.048(9) 0.048(10) 0.022(10) C502 0.125(11) 0.094(10) 0.095(11) 0.028(8) -0.039(8) -0.008(8) C503 0.056(7) 0.145(12) 0.164(13) 0.090(12) 0.039(9) 0.001(7) C504 0.152(12) 0.101(10) 0.069(9) 0.029(7) 0.056(9) 0.058(9) C505 0.136(12) 0.068(8) 0.074(9) 0.005(6) -0.022(8) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 S1 2.1443(17) . ? Ni1 S10 2.1556(17) . ? Ni1 P1 2.1587(18) . ? Ni1 S20 2.1661(17) . ? S1 C25 1.784(6) . ? S1 C11 1.785(6) . ? S2 C15 1.779(6) 2_566 ? S2 C21 1.796(6) . ? S10 C10 1.752(6) . ? S20 C20 1.756(6) . ? P1 C31 1.798(6) . ? P1 C32 1.804(6) . ? P1 C33 1.819(6) . ? C10 C11 1.393(7) . ? C10 C15 1.414(7) . ? C11 C12 1.380(7) . ? C12 C13 1.392(7) . ? C13 C14 1.391(7) . ? C13 C16 1.521(7) . ? C14 C15 1.381(7) . ? C15 S2 1.779(6) 2_566 ? C16 C17 1.518(8) . ? C16 C19 1.521(8) . ? C16 C18 1.554(8) . ? C20 C21 1.388(7) . ? C20 C25 1.410(7) . ? C21 C22 1.399(7) . ? C22 C23 1.374(7) . ? C23 C24 1.374(7) . ? C23 C26 1.536(8) . ? C24 C25 1.385(7) . ? C26 C29 1.487(9) . ? C26 C28 1.514(8) . ? C26 C27 1.529(10) . ? Ni2 S21 2.1472(17) . ? Ni2 S220 2.1585(19) . ? Ni2 S210 2.1587(18) . ? Ni2 P2 2.1633(19) . ? P2 C231 1.763(7) . ? P2 C233 1.786(7) . ? P2 C232 1.792(7) . ? S21 C225 1.792(6) . ? S21 C211 1.797(6) . ? S22 C215 1.771(6) 2_655 ? S22 C221 1.781(6) . ? S210 C210 1.766(6) . ? S220 C220 1.758(6) . ? C210 C211 1.388(7) . ? C210 C215 1.403(7) . ? C211 C212 1.381(7) . ? C212 C213 1.398(7) . ? C213 C214 1.390(7) . ? C213 C216 1.526(8) . ? C214 C215 1.385(7) . ? C215 S22 1.771(6) 2_655 ? C216 C217 1.516(8) . ? C216 C218 1.528(8) . ? C216 C219 1.532(8) . ? C220 C221 1.388(7) . ? C220 C225 1.391(7) . ? C221 C222 1.387(7) . ? C222 C223 1.392(8) . ? C223 C224 1.377(7) . ? C223 C226 1.536(8) . ? C224 C225 1.388(7) . ? C226 C228 1.513(8) . ? C226 C227 1.523(9) . ? C226 C229 1.533(9) . ? C300 C302 1.311(17) 2_556 ? C300 C301 1.34(2) . ? C301 C302 1.40(2) . ? C302 C300 1.311(17) 2_556 ? C400 C401 1.318(14) . ? C400 C402 1.336(15) 2_656 ? C401 C402 1.362(15) . ? C402 C400 1.336(15) 2_656 ? C500 C501 1.330(14) . ? C500 C505 1.345(14) . ? C501 C502 1.333(14) . ? C502 C503 1.340(13) . ? C503 C504 1.348(13) . ? C504 C505 1.306(13) . ? 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 S1 Ni1 S10 92.19(6) . . ? S1 Ni1 P1 166.55(7) . . ? S10 Ni1 P1 91.34(7) . . ? S1 Ni1 S20 91.80(6) . . ? S10 Ni1 S20 149.50(7) . . ? P1 Ni1 S20 91.72(7) . . ? C25 S1 C11 105.6(3) . . ? C25 S1 Ni1 103.7(2) . . ? C11 S1 Ni1 103.4(2) . . ? C15 S2 C21 103.3(3) 2_566 . ? C10 S10 Ni1 100.9(2) . . ? C20 S20 Ni1 101.3(2) . . ? C31 P1 C32 104.4(3) . . ? C31 P1 C33 103.1(3) . . ? C32 P1 C33 104.5(3) . . ? C31 P1 Ni1 116.6(2) . . ? C32 P1 Ni1 111.3(2) . . ? C33 P1 Ni1 115.7(2) . . ? C11 C10 C15 115.8(5) . . ? C11 C10 S10 121.6(5) . . ? C15 C10 S10 122.6(4) . . ? C12 C11 C10 121.9(5) . . ? C12 C11 S1 121.8(4) . . ? C10 C11 S1 115.9(4) . . ? C11 C12 C13 122.1(5) . . ? C14 C13 C12 115.5(5) . . ? C14 C13 C16 122.2(5) . . ? C12 C13 C16 122.2(5) . . ? C15 C14 C13 123.3(6) . . ? C14 C15 C10 120.3(5) . . ? C14 C15 S2 117.0(5) . 2_566 ? C10 C15 S2 122.6(4) . 2_566 ? C17 C16 C13 113.4(5) . . ? C17 C16 C19 109.7(6) . . ? C13 C16 C19 111.7(5) . . ? C17 C16 C18 107.7(5) . . ? C13 C16 C18 106.2(5) . . ? C19 C16 C18 107.9(5) . . ? C21 C20 C25 115.7(5) . . ? C21 C20 S20 123.5(4) . . ? C25 C20 S20 120.7(4) . . ? C20 C21 C22 120.5(5) . . ? C20 C21 S2 122.3(4) . . ? C22 C21 S2 117.1(5) . . ? C23 C22 C21 122.9(6) . . ? C24 C23 C22 116.3(6) . . ? C24 C23 C26 122.5(6) . . ? C22 C23 C26 121.2(6) . . ? C23 C24 C25 122.0(6) . . ? C24 C25 C20 121.4(5) . . ? C24 C25 S1 122.2(5) . . ? C20 C25 S1 116.0(4) . . ? C29 C26 C28 108.5(7) . . ? C29 C26 C27 110.4(7) . . ? C28 C26 C27 105.6(6) . . ? C29 C26 C23 112.2(6) . . ? C28 C26 C23 112.4(6) . . ? C27 C26 C23 107.7(6) . . ? S21 Ni2 S220 92.00(7) . . ? S21 Ni2 S210 91.66(7) . . ? S220 Ni2 S210 151.12(8) . . ? S21 Ni2 P2 164.14(7) . . ? S220 Ni2 P2 91.74(7) . . ? S210 Ni2 P2 92.49(7) . . ? C231 P2 C233 104.9(5) . . ? C231 P2 C232 103.7(4) . . ? C233 P2 C232 103.0(4) . . ? C231 P2 Ni2 113.1(3) . . ? C233 P2 Ni2 115.1(3) . . ? C232 P2 Ni2 115.6(3) . . ? C225 S21 C211 107.4(3) . . ? C225 S21 Ni2 103.2(2) . . ? C211 S21 Ni2 103.61(19) . . ? C215 S22 C221 103.1(3) 2_655 . ? C210 S210 Ni2 101.3(2) . . ? C220 S220 Ni2 101.5(2) . . ? C211 C210 C215 116.6(5) . . ? C211 C210 S210 120.9(5) . . ? C215 C210 S210 122.5(5) . . ? C212 C211 C210 122.3(6) . . ? C212 C211 S21 121.4(5) . . ? C210 C211 S21 115.9(5) . . ? C211 C212 C213 121.3(6) . . ? C214 C213 C212 115.3(6) . . ? C214 C213 C216 121.6(6) . . ? C212 C213 C216 123.1(5) . . ? C215 C214 C213 124.2(6) . . ? C214 C215 C210 119.2(5) . . ? C214 C215 S22 117.6(5) . 2_655 ? C210 C215 S22 123.2(5) . 2_655 ? C217 C216 C213 112.9(5) . . ? C217 C216 C218 108.2(6) . . ? C213 C216 C218 111.0(5) . . ? C217 C216 C219 108.5(6) . . ? C213 C216 C219 108.0(5) . . ? C218 C216 C219 108.1(6) . . ? C221 C220 C225 116.4(5) . . ? C221 C220 S220 122.8(5) . . ? C225 C220 S220 120.6(5) . . ? C222 C221 C220 120.4(5) . . ? C222 C221 S22 116.1(5) . . ? C220 C221 S22 123.5(5) . . ? C221 C222 C223 122.8(6) . . ? C224 C223 C222 116.5(6) . . ? C224 C223 C226 121.5(6) . . ? C222 C223 C226 121.8(6) . . ? C223 C224 C225 120.9(6) . . ? C224 C225 C220 122.4(5) . . ? C224 C225 S21 120.7(5) . . ? C220 C225 S21 116.7(4) . . ? C228 C226 C227 108.8(6) . . ? C228 C226 C229 109.4(6) . . ? C227 C226 C229 107.1(6) . . ? C228 C226 C223 112.1(5) . . ? C227 C226 C223 112.0(5) . . ? C229 C226 C223 107.2(5) . . ? C302 C300 C301 123(2) 2_556 . ? C300 C301 C302 112.9(19) . . ? C300 C302 C301 124.4(19) 2_556 . ? C401 C400 C402 119.6(14) . 2_656 ? C400 C401 C402 120.8(12) . . ? C400 C402 C401 119.6(13) 2_656 . ? C501 C500 C505 121.4(12) . . ? C500 C501 C502 118.7(12) . . ? C501 C502 C503 120.5(11) . . ? C502 C503 C504 119.3(11) . . ? C505 C504 C503 120.7(11) . . ? C504 C505 C500 119.3(11) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.431 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.093 # Attachment 'SCWS10_new.CIF' data_scws10 _database_code_depnum_ccdc_archive 'CCDC 702275' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H81 P3 S8 W' _chemical_formula_weight 1275.44 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 14.3750(6) _cell_length_b 14.9573(7) _cell_length_c 15.3607(8) _cell_angle_alpha 89.2720(10) _cell_angle_beta 75.8420(10) _cell_angle_gamma 76.8000(10) _cell_volume 3114.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5251 _cell_measurement_theta_min 2.279 _cell_measurement_theta_max 25.769 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 2.233 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7306 _exptl_absorpt_correction_T_max 0.9780 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22269 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.28 _reflns_number_total 14001 _reflns_number_gt 8973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0090P)^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 14001 _refine_ls_number_parameters 636 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.163065(16) 0.139395(16) 0.114969(17) 0.02907(7) Uani 1 1 d . . . H1 H 0.115(3) 0.088(3) 0.058(3) 0.035(12) Uiso 1 1 d . . . H2 H 0.150(2) 0.041(2) 0.136(2) 0.016(10) Uiso 1 1 d . . . P1 P 0.28529(10) 0.00718(10) 0.02837(11) 0.0419(4) Uani 1 1 d . . . P2 P 0.09961(10) 0.22589(10) -0.00407(10) 0.0405(4) Uani 1 1 d . . . P3 P -0.00120(11) 0.13139(12) 0.20737(12) 0.0508(5) Uani 1 1 d . . . S1 S 0.31073(9) 0.20308(10) 0.04562(9) 0.0354(4) Uani 1 1 d . . . S2 S 0.10758(10) 0.29612(9) 0.19855(9) 0.0393(4) Uani 1 1 d . . . S3 S 0.07534(11) 0.54644(11) 0.16009(10) 0.0447(4) Uani 1 1 d . . . H3 H 0.042(5) 0.483(5) 0.196(5) 0.18(3) Uiso 1 1 d . . . S4 S 0.43573(11) 0.46715(11) 0.15716(11) 0.0492(4) Uani 1 1 d . . . H4 H 0.508(4) 0.393(4) 0.120(4) 0.10(2) Uiso 1 1 d . . . S5 S 0.24223(9) 0.11037(9) 0.23973(9) 0.0302(3) Uani 1 1 d . . . S6 S 0.01016(9) 0.45435(9) 0.35821(9) 0.0344(3) Uani 1 1 d . . . S7 S 0.26169(10) 0.63619(10) 0.12422(10) 0.0416(4) Uani 1 1 d . . . S8 S 0.50767(9) 0.28748(10) 0.01409(9) 0.0376(4) Uani 1 1 d . . . C10 C 0.3750(3) 0.1998(3) 0.1293(3) 0.0287(12) Uani 1 1 d . . . C11 C 0.4588(3) 0.2379(3) 0.1161(3) 0.0300(13) Uani 1 1 d . . . C12 C 0.5136(3) 0.2295(3) 0.1816(4) 0.0351(14) Uani 1 1 d . . . H12A H 0.5685 0.2560 0.1716 0.042 Uiso 1 1 calc R . . C13 C 0.4897(4) 0.1834(4) 0.2610(4) 0.0385(14) Uani 1 1 d . A . C14 C 0.4077(3) 0.1477(3) 0.2722(3) 0.0353(14) Uani 1 1 d . . . H14A H 0.3898 0.1154 0.3242 0.042 Uiso 1 1 calc R . . C15 C 0.3500(3) 0.1568(3) 0.2109(3) 0.0275(12) Uani 1 1 d . . . C16 C 0.5482(4) 0.1750(5) 0.3331(4) 0.0478(17) Uani 1 1 d . . . C17 C 0.4909(14) 0.2384(16) 0.4100(13) 0.124(13) Uani 0.65(3) 1 d P A 1 H17A H 0.4812 0.3011 0.3907 0.186 Uiso 0.65(3) 1 calc PR A 1 H17B H 0.5265 0.2321 0.4567 0.186 Uiso 0.65(3) 1 calc PR A 1 H17C H 0.4273 0.2238 0.4334 0.186 Uiso 0.65(3) 1 calc PR A 1 C18 C 0.5610(15) 0.0769(11) 0.3651(14) 0.094(9) Uani 0.65(3) 1 d P A 1 H18A H 0.5978 0.0701 0.4110 0.141 Uiso 0.65(3) 1 calc PR A 1 H18B H 0.5968 0.0340 0.3148 0.141 Uiso 0.65(3) 1 calc PR A 1 H18C H 0.4968 0.0642 0.3900 0.141 Uiso 0.65(3) 1 calc PR A 1 C19 C 0.6505(11) 0.1894(19) 0.2942(12) 0.123(14) Uani 0.65(3) 1 d P A 1 H19A H 0.6459 0.2516 0.2741 0.184 Uiso 0.65(3) 1 calc PR A 1 H19B H 0.6838 0.1461 0.2437 0.184 Uiso 0.65(3) 1 calc PR A 1 H19C H 0.6875 0.1797 0.3399 0.184 Uiso 0.65(3) 1 calc PR A 1 C17A C 0.490(2) 0.154(3) 0.4241(18) 0.10(2) Uani 0.35(3) 1 d P A 2 H17D H 0.4467 0.2111 0.4539 0.147 Uiso 0.35(3) 1 calc PR A 2 H17E H 0.5348 0.1276 0.4603 0.147 Uiso 0.35(3) 1 calc PR A 2 H17F H 0.4506 0.1117 0.4165 0.147 Uiso 0.35(3) 1 calc PR A 2 C18A C 0.640(2) 0.103(3) 0.308(2) 0.12(2) Uani 0.35(3) 1 d P A 2 H18D H 0.6909 0.1278 0.2686 0.180 Uiso 0.35(3) 1 calc PR A 2 H18E H 0.6286 0.0520 0.2766 0.180 Uiso 0.35(3) 1 calc PR A 2 H18F H 0.6606 0.0816 0.3614 0.180 Uiso 0.35(3) 1 calc PR A 2 C19A C 0.568(4) 0.2686(19) 0.350(2) 0.11(2) Uani 0.35(3) 1 d P A 2 H19D H 0.5382 0.3136 0.3134 0.163 Uiso 0.35(3) 1 calc PR A 2 H19E H 0.6389 0.2637 0.3356 0.163 Uiso 0.35(3) 1 calc PR A 2 H19F H 0.5405 0.2878 0.4133 0.163 Uiso 0.35(3) 1 calc PR A 2 C20 C 0.1188(3) 0.2758(3) 0.3068(3) 0.0257(12) Uani 1 1 d . . . C21 C 0.1735(3) 0.1921(3) 0.3294(3) 0.0276(12) Uani 1 1 d . . . C22 C 0.1767(3) 0.1714(4) 0.4169(3) 0.0336(13) Uani 1 1 d . . . H22A H 0.2131 0.1138 0.4285 0.040 Uiso 1 1 calc R . . C23 C 0.1266(4) 0.2347(4) 0.4882(4) 0.0385(14) Uani 1 1 d . . . C24 C 0.0767(3) 0.3201(4) 0.4667(4) 0.0388(14) Uani 1 1 d . . . H24A H 0.0439 0.3644 0.5136 0.047 Uiso 1 1 calc R . . C25 C 0.0729(3) 0.3431(3) 0.3796(4) 0.0299(12) Uani 1 1 d . . . C26 C 0.1273(5) 0.2136(5) 0.5867(4) 0.0589(18) Uani 1 1 d . . . C27 C 0.1885(6) 0.1217(5) 0.5969(4) 0.140(4) Uani 1 1 d . . . H27A H 0.2560 0.1260 0.5911 0.210 Uiso 1 1 calc R . . H27B H 0.1867 0.0790 0.5507 0.210 Uiso 1 1 calc R . . H27C H 0.1629 0.0999 0.6557 0.210 Uiso 1 1 calc R . . C28 C 0.1601(7) 0.2869(5) 0.6289(5) 0.133(4) Uani 1 1 d . . . H28A H 0.1835 0.3274 0.5832 0.200 Uiso 1 1 calc R . . H28B H 0.2130 0.2586 0.6563 0.200 Uiso 1 1 calc R . . H28C H 0.1051 0.3220 0.6745 0.200 Uiso 1 1 calc R . . C29 C 0.0230(6) 0.2173(6) 0.6409(5) 0.140(4) Uani 1 1 d . . . H29A H -0.0096 0.2803 0.6616 0.210 Uiso 1 1 calc R . . H29B H 0.0250 0.1791 0.6922 0.210 Uiso 1 1 calc R . . H29C H -0.0131 0.1950 0.6035 0.210 Uiso 1 1 calc R . . C30 C 0.1372(3) 0.5480(3) 0.2451(3) 0.0313(13) Uani 1 1 d . . . C31 C 0.1102(3) 0.5099(3) 0.3297(4) 0.0301(13) Uani 1 1 d . . . C32 C 0.1603(3) 0.5197(3) 0.3954(3) 0.0344(13) Uani 1 1 d . . . H32A H 0.1412 0.4941 0.4514 0.041 Uiso 1 1 calc R . . C33 C 0.2363(4) 0.5649(3) 0.3825(4) 0.0338(13) Uani 1 1 d . . . C34 C 0.2629(4) 0.5994(3) 0.2987(4) 0.0361(14) Uani 1 1 d . . . H34A H 0.3144 0.6303 0.2872 0.043 Uiso 1 1 calc R . . C35 C 0.2168(4) 0.5906(3) 0.2303(3) 0.0319(13) Uani 1 1 d . . . C36 C 0.2876(4) 0.5740(4) 0.4574(4) 0.0461(16) Uani 1 1 d . . . C37 C 0.3032(6) 0.4862(5) 0.5064(5) 0.101(3) Uani 1 1 d . . . H37A H 0.3362 0.4931 0.5531 0.151 Uiso 1 1 calc R . . H37B H 0.3435 0.4363 0.4644 0.151 Uiso 1 1 calc R . . H37C H 0.2398 0.4725 0.5334 0.151 Uiso 1 1 calc R . . C38 C 0.2213(5) 0.6494(5) 0.5242(4) 0.093(3) Uani 1 1 d . . . H38A H 0.2526 0.6563 0.5722 0.139 Uiso 1 1 calc R . . H38B H 0.1587 0.6335 0.5492 0.139 Uiso 1 1 calc R . . H38C H 0.2102 0.7068 0.4940 0.139 Uiso 1 1 calc R . . C39 C 0.3858(4) 0.5984(6) 0.4221(4) 0.099(3) Uani 1 1 d . . . H39A H 0.4158 0.6029 0.4715 0.149 Uiso 1 1 calc R . . H39B H 0.3760 0.6568 0.3936 0.149 Uiso 1 1 calc R . . H39C H 0.4287 0.5510 0.3785 0.149 Uiso 1 1 calc R . . C40 C 0.3827(3) 0.4624(4) 0.0659(3) 0.0343(13) Uani 1 1 d . . . C41 C 0.4151(3) 0.3860(3) 0.0044(3) 0.0321(13) Uani 1 1 d . . . C42 C 0.3826(4) 0.3900(4) -0.0749(4) 0.0372(14) Uani 1 1 d . . . H42A H 0.4050 0.3388 -0.1157 0.045 Uiso 1 1 calc R . . C43 C 0.3183(3) 0.4673(4) -0.0949(3) 0.0333(13) Uani 1 1 d . . . C44 C 0.2794(4) 0.5388(4) -0.0284(4) 0.0423(15) Uani 1 1 d . . . H44A H 0.2306 0.5892 -0.0373 0.051 Uiso 1 1 calc R . . C45 C 0.3109(3) 0.5369(4) 0.0501(3) 0.0339(13) Uani 1 1 d . . . C46 C 0.2928(4) 0.4774(4) -0.1869(4) 0.0412(15) Uani 1 1 d . . . C47 C 0.3387(5) 0.3902(5) -0.2473(4) 0.087(2) Uani 1 1 d . . . H47A H 0.3211 0.3993 -0.3044 0.130 Uiso 1 1 calc R . . H47B H 0.3144 0.3392 -0.2184 0.130 Uiso 1 1 calc R . . H47C H 0.4099 0.3769 -0.2576 0.130 Uiso 1 1 calc R . . C48 C 0.1803(4) 0.4998(5) -0.1749(4) 0.076(2) Uani 1 1 d . . . H48A H 0.1656 0.5061 -0.2333 0.114 Uiso 1 1 calc R . . H48B H 0.1506 0.5569 -0.1393 0.114 Uiso 1 1 calc R . . H48C H 0.1538 0.4505 -0.1444 0.114 Uiso 1 1 calc R . . C49 C 0.3323(4) 0.5564(4) -0.2331(4) 0.068(2) Uani 1 1 d . . . H49A H 0.3166 0.5639 -0.2911 0.102 Uiso 1 1 calc R . . H49B H 0.4032 0.5432 -0.2415 0.102 Uiso 1 1 calc R . . H49C H 0.3021 0.6125 -0.1961 0.102 Uiso 1 1 calc R . . C51 C 0.3928(3) -0.0358(4) 0.0731(4) 0.0488(16) Uani 1 1 d . . . H51A H 0.4366 -0.0874 0.0352 0.073 Uiso 1 1 calc R . . H51B H 0.3716 -0.0555 0.1336 0.073 Uiso 1 1 calc R . . H51C H 0.4272 0.0127 0.0741 0.073 Uiso 1 1 calc R . . C52 C 0.2429(4) -0.0978(4) 0.0241(4) 0.067(2) Uani 1 1 d . . . H52A H 0.2961 -0.1452 -0.0112 0.101 Uiso 1 1 calc R . . H52B H 0.1876 -0.0863 -0.0034 0.101 Uiso 1 1 calc R . . H52C H 0.2225 -0.1180 0.0846 0.101 Uiso 1 1 calc R . . C53 C 0.3437(4) 0.0150(4) -0.0913(4) 0.065(2) Uani 1 1 d . . . H53A H 0.3893 -0.0430 -0.1140 0.098 Uiso 1 1 calc R . . H53B H 0.3792 0.0636 -0.0982 0.098 Uiso 1 1 calc R . . H53C H 0.2934 0.0285 -0.1247 0.098 Uiso 1 1 calc R . . C61 C 0.1772(5) 0.2081(5) -0.1189(4) 0.100(3) Uani 1 1 d . . . H61A H 0.1434 0.2461 -0.1586 0.150 Uiso 1 1 calc R . . H61B H 0.1903 0.1439 -0.1381 0.150 Uiso 1 1 calc R . . H61C H 0.2389 0.2249 -0.1209 0.150 Uiso 1 1 calc R . . C62 C 0.0746(4) 0.3490(4) 0.0076(4) 0.0619(19) Uani 1 1 d . . . H62A H 0.0502 0.3758 -0.0427 0.093 Uiso 1 1 calc R . . H62B H 0.1348 0.3675 0.0085 0.093 Uiso 1 1 calc R . . H62C H 0.0253 0.3701 0.0633 0.093 Uiso 1 1 calc R . . C63 C -0.0155(4) 0.2121(5) -0.0247(5) 0.090(3) Uani 1 1 d . . . H63A H -0.0306 0.2504 -0.0732 0.135 Uiso 1 1 calc R . . H63B H -0.0682 0.2302 0.0293 0.135 Uiso 1 1 calc R . . H63C H -0.0093 0.1482 -0.0413 0.135 Uiso 1 1 calc R . . C71 C -0.0101(5) 0.0966(5) 0.3232(4) 0.101(3) Uani 1 1 d . . . H71A H -0.0780 0.0961 0.3521 0.151 Uiso 1 1 calc R . . H71B H 0.0117 0.1397 0.3558 0.151 Uiso 1 1 calc R . . H71C H 0.0314 0.0355 0.3231 0.151 Uiso 1 1 calc R . . C72 C -0.1056(4) 0.2315(5) 0.2269(5) 0.105(3) Uani 1 1 d . . . H72A H -0.1635 0.2151 0.2646 0.157 Uiso 1 1 calc R . . H72B H -0.1187 0.2514 0.1699 0.157 Uiso 1 1 calc R . . H72C H -0.0900 0.2809 0.2567 0.157 Uiso 1 1 calc R . . C73 C -0.0561(4) 0.0449(4) 0.1697(4) 0.072(2) Uani 1 1 d . . . H73A H -0.1201 0.0471 0.2102 0.108 Uiso 1 1 calc R . . H73B H -0.0135 -0.0156 0.1696 0.108 Uiso 1 1 calc R . . H73C H -0.0639 0.0574 0.1095 0.108 Uiso 1 1 calc R . . C80 C 0.5801(9) 0.1197(7) 0.6412(10) 0.208(8) Uani 1 1 d G . . H80A H 0.5260 0.1068 0.6238 0.249 Uiso 1 1 calc R . . C81 C 0.6744(12) 0.0925(4) 0.5851(5) 0.190(8) Uani 1 1 d G . . H81A H 0.6841 0.0612 0.5298 0.228 Uiso 1 1 calc R . . C82 C 0.7543(6) 0.1116(6) 0.6108(8) 0.163(5) Uani 1 1 d G . . H82A H 0.8181 0.0932 0.5729 0.195 Uiso 1 1 calc R . . C83 C 0.7399(8) 0.1579(6) 0.6927(9) 0.144(5) Uani 1 1 d G . . H83A H 0.7939 0.1708 0.7101 0.173 Uiso 1 1 calc R . . C84 C 0.6456(12) 0.1851(4) 0.7488(4) 0.147(5) Uani 1 1 d G . . H84A H 0.6358 0.2164 0.8042 0.176 Uiso 1 1 calc R . . C85 C 0.5657(6) 0.1660(6) 0.7231(8) 0.164(6) Uani 1 1 d G . . H85A H 0.5019 0.1844 0.7610 0.197 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.02799(11) 0.02971(13) 0.02994(14) -0.00172(10) -0.00951(10) -0.00490(9) P1 0.0385(8) 0.0394(10) 0.0453(11) -0.0098(8) -0.0103(8) -0.0039(7) P2 0.0470(9) 0.0413(10) 0.0393(10) 0.0001(8) -0.0236(8) -0.0087(8) P3 0.0372(9) 0.0599(12) 0.0551(12) -0.0059(9) -0.0057(8) -0.0169(8) S1 0.0365(7) 0.0441(9) 0.0294(9) 0.0038(7) -0.0125(7) -0.0125(7) S2 0.0527(9) 0.0326(9) 0.0309(9) -0.0017(7) -0.0157(7) -0.0002(7) S3 0.0548(9) 0.0515(10) 0.0358(10) 0.0088(8) -0.0229(8) -0.0163(8) S4 0.0518(9) 0.0611(12) 0.0416(10) 0.0023(9) -0.0232(8) -0.0146(9) S5 0.0313(7) 0.0301(8) 0.0297(8) 0.0014(6) -0.0089(6) -0.0064(6) S6 0.0321(7) 0.0337(9) 0.0345(9) -0.0007(7) -0.0055(6) -0.0047(6) S7 0.0580(9) 0.0338(9) 0.0317(9) 0.0055(7) -0.0071(8) -0.0127(7) S8 0.0309(7) 0.0433(9) 0.0339(9) 0.0064(7) -0.0030(7) -0.0049(7) C10 0.034(3) 0.023(3) 0.026(3) -0.001(2) -0.011(3) 0.002(2) C11 0.026(3) 0.026(3) 0.033(3) -0.001(3) -0.004(2) 0.000(2) C12 0.025(3) 0.044(4) 0.038(4) -0.001(3) -0.010(3) -0.008(3) C13 0.029(3) 0.043(4) 0.041(4) 0.002(3) -0.010(3) -0.003(3) C14 0.036(3) 0.041(4) 0.027(3) 0.005(3) -0.008(3) -0.006(3) C15 0.021(2) 0.030(3) 0.031(3) -0.004(3) -0.009(2) -0.002(2) C16 0.041(4) 0.063(5) 0.049(5) 0.010(4) -0.024(3) -0.019(3) C17 0.134(17) 0.15(2) 0.086(19) -0.063(18) -0.069(16) 0.019(18) C18 0.103(17) 0.111(13) 0.115(17) 0.068(12) -0.097(16) -0.047(12) C19 0.084(12) 0.26(4) 0.087(13) 0.10(2) -0.066(11) -0.116(19) C17A 0.07(2) 0.21(6) 0.041(17) 0.05(3) -0.037(17) -0.07(3) C18A 0.08(3) 0.18(4) 0.10(3) -0.02(3) -0.08(3) 0.02(3) C19A 0.24(6) 0.09(2) 0.05(2) 0.012(17) -0.09(3) -0.09(3) C20 0.026(3) 0.027(3) 0.025(3) 0.008(2) -0.008(2) -0.008(2) C21 0.030(3) 0.032(3) 0.022(3) -0.001(3) -0.005(2) -0.009(2) C22 0.032(3) 0.034(3) 0.033(4) 0.005(3) -0.009(3) -0.003(3) C23 0.049(3) 0.033(4) 0.032(4) 0.005(3) -0.009(3) -0.007(3) C24 0.042(3) 0.040(4) 0.027(3) -0.006(3) 0.004(3) -0.008(3) C25 0.026(3) 0.030(3) 0.030(3) 0.006(3) -0.003(2) -0.004(2) C26 0.079(5) 0.055(5) 0.033(4) 0.008(3) -0.011(4) -0.001(4) C27 0.228(10) 0.098(7) 0.032(5) 0.010(5) -0.030(6) 0.083(7) C28 0.274(12) 0.099(7) 0.062(6) 0.013(5) -0.099(7) -0.053(8) C29 0.125(8) 0.193(11) 0.063(6) 0.053(6) 0.020(6) -0.006(7) C30 0.037(3) 0.025(3) 0.029(3) -0.007(3) -0.008(3) -0.003(2) C31 0.028(3) 0.025(3) 0.031(3) -0.001(3) -0.004(3) 0.002(2) C32 0.040(3) 0.036(3) 0.025(3) 0.001(3) -0.005(3) -0.007(3) C33 0.036(3) 0.033(3) 0.032(4) -0.003(3) -0.010(3) -0.005(3) C34 0.037(3) 0.036(3) 0.037(4) -0.001(3) -0.008(3) -0.012(3) C35 0.040(3) 0.022(3) 0.029(3) 0.005(2) -0.001(3) -0.004(2) C36 0.054(4) 0.062(5) 0.029(4) 0.003(3) -0.015(3) -0.023(3) C37 0.158(7) 0.098(7) 0.092(6) 0.037(5) -0.100(6) -0.047(6) C38 0.097(5) 0.128(7) 0.061(5) -0.037(5) -0.036(5) -0.023(5) C39 0.055(4) 0.213(10) 0.051(5) 0.024(6) -0.023(4) -0.066(5) C40 0.038(3) 0.039(4) 0.030(3) 0.014(3) -0.010(3) -0.015(3) C41 0.038(3) 0.035(3) 0.023(3) 0.007(3) -0.006(3) -0.012(3) C42 0.045(3) 0.036(4) 0.031(3) 0.002(3) -0.002(3) -0.018(3) C43 0.032(3) 0.044(4) 0.026(3) 0.006(3) -0.011(3) -0.008(3) C44 0.038(3) 0.051(4) 0.041(4) 0.013(3) -0.009(3) -0.019(3) C45 0.034(3) 0.039(4) 0.027(3) 0.011(3) -0.004(3) -0.009(3) C46 0.046(3) 0.053(4) 0.030(4) 0.010(3) -0.015(3) -0.018(3) C47 0.137(6) 0.084(6) 0.049(5) 0.001(4) -0.055(5) -0.011(5) C48 0.062(4) 0.123(7) 0.060(5) 0.024(5) -0.034(4) -0.036(4) C49 0.090(5) 0.095(6) 0.036(4) 0.022(4) -0.031(4) -0.041(4) C51 0.044(3) 0.049(4) 0.050(4) -0.011(3) -0.013(3) -0.001(3) C52 0.064(4) 0.037(4) 0.100(6) -0.027(4) -0.027(4) 0.000(3) C53 0.065(4) 0.072(5) 0.043(4) -0.017(4) -0.005(3) 0.010(4) C61 0.117(6) 0.125(7) 0.031(4) 0.001(5) -0.020(4) 0.025(5) C62 0.090(5) 0.057(5) 0.050(4) 0.015(4) -0.041(4) -0.015(4) C63 0.091(5) 0.098(6) 0.128(7) 0.055(5) -0.084(5) -0.059(5) C71 0.094(5) 0.182(9) 0.050(5) 0.014(5) -0.006(4) -0.093(6) C72 0.031(4) 0.091(6) 0.170(9) -0.031(6) 0.006(4) 0.001(4) C73 0.055(4) 0.097(6) 0.081(6) -0.005(4) -0.021(4) -0.044(4) C80 0.39(2) 0.067(10) 0.217(18) 0.013(10) -0.195(18) -0.017(11) C81 0.38(2) 0.061(7) 0.161(13) 0.015(7) -0.168(18) -0.001(13) C82 0.263(16) 0.089(10) 0.119(12) 0.029(9) -0.061(10) 0.006(10) C83 0.265(17) 0.094(9) 0.114(10) 0.035(8) -0.092(12) -0.078(10) C84 0.267(15) 0.072(7) 0.100(9) 0.018(6) -0.026(12) -0.057(11) C85 0.251(14) 0.087(9) 0.201(17) 0.045(9) -0.120(13) -0.066(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 W H2 1.55(4) . ? W H1 1.55(4) . ? W S5 2.4446(12) . ? W P2 2.4629(14) . ? W P3 2.4679(16) . ? W P1 2.4706(14) . ? W S1 2.5178(14) . ? W S2 2.5498(14) . ? P1 C52 1.817(5) . ? P1 C51 1.823(4) . ? P1 C53 1.839(6) . ? P2 C62 1.796(6) . ? P2 C63 1.816(5) . ? P2 C61 1.827(6) . ? P3 C73 1.827(5) . ? P3 C72 1.830(6) . ? P3 C71 1.830(6) . ? S1 C10 1.752(5) . ? S2 C20 1.726(5) . ? S3 H3 1.23(8) . ? S3 C30 1.753(5) . ? S4 H4 1.36(5) . ? S4 C40 1.760(5) . ? S5 C21 1.787(5) . ? S5 C15 1.796(5) . ? S6 C25 1.771(5) . ? S6 C31 1.783(5) . ? S7 C45 1.781(5) . ? S7 C35 1.788(5) . ? S8 C41 1.778(5) . ? S8 C11 1.780(5) . ? C10 C15 1.407(6) . ? C10 C11 1.417(6) . ? C11 C12 1.410(6) . ? C12 C13 1.401(7) . ? C13 C14 1.375(6) . ? C13 C16 1.534(7) . ? C14 C15 1.385(6) . ? C16 C18A 1.47(2) . ? C16 C17 1.473(15) . ? C16 C19 1.510(13) . ? C16 C17A 1.51(2) . ? C16 C18 1.527(13) . ? C16 C19A 1.53(2) . ? C20 C21 1.407(6) . ? C20 C25 1.437(6) . ? C21 C22 1.385(6) . ? C22 C23 1.393(6) . ? C23 C24 1.394(6) . ? C23 C26 1.544(7) . ? C24 C25 1.387(6) . ? C26 C27 1.483(8) . ? C26 C28 1.499(8) . ? C26 C29 1.515(8) . ? C30 C35 1.403(6) . ? C30 C31 1.414(6) . ? C31 C32 1.402(6) . ? C32 C33 1.385(6) . ? C33 C34 1.379(7) . ? C33 C36 1.534(7) . ? C34 C35 1.395(6) . ? C36 C37 1.505(8) . ? C36 C39 1.508(7) . ? C36 C38 1.515(7) . ? C40 C45 1.399(6) . ? C40 C41 1.409(7) . ? C41 C42 1.404(6) . ? C42 C43 1.388(6) . ? C43 C44 1.405(7) . ? C43 C46 1.542(7) . ? C44 C45 1.386(6) . ? C46 C49 1.518(7) . ? C46 C47 1.528(7) . ? C46 C48 1.539(7) . ? C80 C81 1.3900 . ? C80 C85 1.3900 . ? C81 C82 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? 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 H2 W H1 58.8(17) . . ? H2 W S5 80.1(12) . . ? H1 W S5 138.8(15) . . ? H2 W P2 122.1(12) . . ? H1 W P2 63.5(15) . . ? S5 W P2 157.74(5) . . ? H2 W P3 65.1(12) . . ? H1 W P3 72.1(14) . . ? S5 W P3 94.13(5) . . ? P2 W P3 94.75(5) . . ? H2 W P1 61.0(13) . . ? H1 W P1 69.2(14) . . ? S5 W P1 89.69(5) . . ? P2 W P1 101.98(5) . . ? P3 W P1 124.31(5) . . ? H2 W S1 133.2(12) . . ? H1 W S1 122.1(15) . . ? S5 W S1 83.23(4) . . ? P2 W S1 81.46(5) . . ? P3 W S1 160.01(5) . . ? P1 W S1 75.59(5) . . ? H2 W S2 136.3(13) . . ? H1 W S2 133.0(14) . . ? S5 W S2 78.37(4) . . ? P2 W S2 83.37(5) . . ? P3 W S2 78.96(5) . . ? P1 W S2 154.91(5) . . ? S1 W S2 81.10(5) . . ? C52 P1 C51 100.1(3) . . ? C52 P1 C53 100.2(3) . . ? C51 P1 C53 101.3(2) . . ? C52 P1 W 115.98(19) . . ? C51 P1 W 114.98(17) . . ? C53 P1 W 120.97(19) . . ? C62 P2 C63 100.1(3) . . ? C62 P2 C61 99.7(3) . . ? C63 P2 C61 99.5(3) . . ? C62 P2 W 116.49(18) . . ? C63 P2 W 119.3(2) . . ? C61 P2 W 118.1(2) . . ? C73 P3 C72 100.6(3) . . ? C73 P3 C71 98.2(3) . . ? C72 P3 C71 99.4(4) . . ? C73 P3 W 115.7(2) . . ? C72 P3 W 121.5(2) . . ? C71 P3 W 117.5(2) . . ? C10 S1 W 105.33(18) . . ? C20 S2 W 105.93(17) . . ? H3 S3 C30 89(3) . . ? H4 S4 C40 89(2) . . ? C21 S5 C15 96.8(2) . . ? C21 S5 W 107.91(15) . . ? C15 S5 W 106.72(17) . . ? C25 S6 C31 100.5(2) . . ? C45 S7 C35 103.6(2) . . ? C41 S8 C11 105.7(2) . . ? C15 C10 C11 116.2(4) . . ? C15 C10 S1 122.9(4) . . ? C11 C10 S1 120.9(4) . . ? C12 C11 C10 120.2(5) . . ? C12 C11 S8 116.5(4) . . ? C10 C11 S8 123.0(4) . . ? C13 C12 C11 122.7(5) . . ? C14 C13 C12 115.7(5) . . ? C14 C13 C16 121.2(5) . . ? C12 C13 C16 123.1(5) . . ? C13 C14 C15 123.4(5) . . ? C14 C15 C10 121.6(4) . . ? C14 C15 S5 117.1(4) . . ? C10 C15 S5 121.3(3) . . ? C18A C16 C17 139.3(11) . . ? C18A C16 C19 53.6(15) . . ? C17 C16 C19 113.7(11) . . ? C18A C16 C17A 108.2(17) . . ? C17 C16 C17A 50.5(13) . . ? C19 C16 C17A 136.2(10) . . ? C18A C16 C18 55.0(16) . . ? C17 C16 C18 108.4(11) . . ? C19 C16 C18 106.6(9) . . ? C17A C16 C18 59.1(14) . . ? C18A C16 C19A 111.7(17) . . ? C17 C16 C19A 56.1(13) . . ? C19 C16 C19A 61.7(14) . . ? C17A C16 C19A 103.0(16) . . ? C18 C16 C19A 142.6(11) . . ? C18A C16 C13 111.6(10) . . ? C17 C16 C13 109.0(7) . . ? C19 C16 C13 110.9(7) . . ? C17A C16 C13 112.9(9) . . ? C18 C16 C13 108.1(6) . . ? C19A C16 C13 109.2(11) . . ? C21 C20 C25 115.6(4) . . ? C21 C20 S2 122.1(4) . . ? C25 C20 S2 122.3(4) . . ? C22 C21 C20 123.0(5) . . ? C22 C21 S5 119.5(4) . . ? C20 C21 S5 117.5(4) . . ? C21 C22 C23 121.0(5) . . ? C22 C23 C24 116.9(5) . . ? C22 C23 C26 122.4(5) . . ? C24 C23 C26 120.6(5) . . ? C25 C24 C23 123.3(5) . . ? C24 C25 C20 119.8(4) . . ? C24 C25 S6 120.3(4) . . ? C20 C25 S6 119.9(4) . . ? C27 C26 C28 110.2(6) . . ? C27 C26 C29 107.5(7) . . ? C28 C26 C29 105.4(7) . . ? C27 C26 C23 113.5(5) . . ? C28 C26 C23 110.3(5) . . ? C29 C26 C23 109.5(5) . . ? C35 C30 C31 117.3(4) . . ? C35 C30 S3 119.1(4) . . ? C31 C30 S3 123.6(4) . . ? C32 C31 C30 119.4(5) . . ? C32 C31 S6 118.3(4) . . ? C30 C31 S6 122.2(4) . . ? C33 C32 C31 123.6(5) . . ? C34 C33 C32 116.0(5) . . ? C34 C33 C36 122.9(5) . . ? C32 C33 C36 121.2(5) . . ? C33 C34 C35 123.0(5) . . ? C34 C35 C30 120.7(5) . . ? C34 C35 S7 117.8(4) . . ? C30 C35 S7 121.4(4) . . ? C37 C36 C39 108.9(5) . . ? C37 C36 C38 108.0(6) . . ? C39 C36 C38 108.6(6) . . ? C37 C36 C33 110.7(5) . . ? C39 C36 C33 112.2(5) . . ? C38 C36 C33 108.2(4) . . ? C45 C40 C41 118.3(5) . . ? C45 C40 S4 120.5(4) . . ? C41 C40 S4 121.1(4) . . ? C42 C41 C40 119.7(5) . . ? C42 C41 S8 116.3(4) . . ? C40 C41 S8 123.5(4) . . ? C43 C42 C41 122.0(5) . . ? C42 C43 C44 117.0(5) . . ? C42 C43 C46 122.3(5) . . ? C44 C43 C46 120.6(5) . . ? C45 C44 C43 121.9(5) . . ? C44 C45 C40 120.5(5) . . ? C44 C45 S7 116.7(4) . . ? C40 C45 S7 122.7(4) . . ? C49 C46 C47 108.7(5) . . ? C49 C46 C48 108.4(5) . . ? C47 C46 C48 108.7(5) . . ? C49 C46 C43 108.4(4) . . ? C47 C46 C43 112.0(4) . . ? C48 C46 C43 110.6(5) . . ? C81 C80 C85 120.0 . . ? C80 C81 C82 120.0 . . ? C83 C82 C81 120.0 . . ? C82 C83 C84 120.0 . . ? C85 C84 C83 120.0 . . ? C84 C85 C80 120.0 . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.882 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.126 # Attachment 'WSCS10_new.CIF' data_wscs10 _database_code_depnum_ccdc_archive 'CCDC 702276' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H114 P6 S8 W2' _chemical_formula_weight 1765.61 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5194(9) _cell_length_b 12.5419(9) _cell_length_c 15.1273(10) _cell_angle_alpha 67.232(2) _cell_angle_beta 77.1440(10) _cell_angle_gamma 79.1250(10) _cell_volume 2121.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5428 _cell_measurement_theta_min 2.416 _cell_measurement_theta_max 26.713 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 3.054 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_T_max 0.7499 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14705 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9434 _reflns_number_gt 7078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^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 9434 _refine_ls_number_parameters 412 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W -0.252253(17) 0.202507(19) 0.076115(15) 0.03755(7) Uani 1 1 d . . . H1 H -0.344(4) 0.224(4) 0.162(4) 0.074(17) Uiso 1 1 d . . . H2 H -0.346(4) 0.303(4) 0.035(3) 0.045(13) Uiso 1 1 d . . . S1 S -0.22225(13) 0.00532(11) 0.06589(9) 0.0502(4) Uani 1 1 d . . . S2 S -0.04939(11) 0.17577(13) 0.06867(9) 0.0505(3) Uani 1 1 d . . . S3 S -0.19840(10) 0.25997(10) -0.10012(9) 0.0374(3) Uani 1 1 d . . . S4 S -0.21114(11) -0.21276(11) -0.00384(9) 0.0425(3) Uani 1 1 d . . . P1 P -0.24311(14) 0.08805(15) 0.24595(11) 0.0603(4) Uani 1 1 d . . . P2 P -0.43917(12) 0.17639(16) 0.06664(12) 0.0610(4) Uani 1 1 d . . . P3 P -0.21948(14) 0.39514(14) 0.06732(12) 0.0601(4) Uani 1 1 d . . . C10 C -0.2027(4) 0.0254(4) -0.0561(3) 0.0340(11) Uani 1 1 d . . . C11 C -0.1974(4) -0.0686(4) -0.0864(3) 0.0351(11) Uani 1 1 d . . . C12 C -0.1916(4) -0.0509(5) -0.1833(3) 0.0422(12) Uani 1 1 d . . . H12A H -0.1864 -0.1161 -0.2009 0.051 Uiso 1 1 calc R . . C13 C -0.1930(4) 0.0575(5) -0.2551(3) 0.0466(13) Uani 1 1 d . A . C14 C -0.1926(4) 0.1513(4) -0.2277(3) 0.0403(12) Uani 1 1 d . . . H14A H -0.1898 0.2266 -0.2750 0.048 Uiso 1 1 calc R . . C15 C -0.1964(4) 0.1340(4) -0.1300(3) 0.0353(11) Uani 1 1 d . . . C16 C -0.1953(5) 0.0775(6) -0.3621(4) 0.0605(16) Uani 1 1 d . . . C17 C -0.2924(10) 0.1639(15) -0.3950(8) 0.111(7) Uani 0.72(2) 1 d PD A 1 H17A H -0.3143 0.2110 -0.3547 0.167 Uiso 0.72(2) 1 calc PR A 1 H17B H -0.3533 0.1228 -0.3895 0.167 Uiso 0.72(2) 1 calc PR A 1 H17C H -0.2722 0.2137 -0.4622 0.167 Uiso 0.72(2) 1 calc PR A 1 C18 C -0.0916(11) 0.1359(16) -0.4248(10) 0.109(6) Uani 0.72(2) 1 d PD A 1 H18A H -0.1041 0.2183 -0.4355 0.163 Uiso 0.72(2) 1 calc PR A 1 H18B H -0.0769 0.1255 -0.4869 0.163 Uiso 0.72(2) 1 calc PR A 1 H18C H -0.0289 0.1003 -0.3914 0.163 Uiso 0.72(2) 1 calc PR A 1 C19 C -0.1959(19) -0.0336(11) -0.3771(9) 0.135(10) Uani 0.72(2) 1 d PD A 1 H19A H -0.2714 -0.0465 -0.3720 0.202 Uiso 0.72(2) 1 calc PR A 1 H19B H -0.1610 -0.0978 -0.3279 0.202 Uiso 0.72(2) 1 calc PR A 1 H19C H -0.1557 -0.0284 -0.4411 0.202 Uiso 0.72(2) 1 calc PR A 1 C17A C -0.307(2) 0.047(3) -0.3638(16) 0.087(13) Uani 0.28(2) 1 d PD A 2 H17D H -0.3647 0.1052 -0.3513 0.131 Uiso 0.28(2) 1 calc PR A 2 H17E H -0.3196 -0.0288 -0.3140 0.131 Uiso 0.28(2) 1 calc PR A 2 H17F H -0.3075 0.0444 -0.4270 0.131 Uiso 0.28(2) 1 calc PR A 2 C18A C -0.168(4) 0.185(3) -0.429(3) 0.19(4) Uani 0.28(2) 1 d PD A 2 H18D H -0.2204 0.2458 -0.4137 0.291 Uiso 0.28(2) 1 calc PR A 2 H18E H -0.1716 0.1893 -0.4937 0.291 Uiso 0.28(2) 1 calc PR A 2 H18F H -0.0945 0.1947 -0.4258 0.291 Uiso 0.28(2) 1 calc PR A 2 C19A C -0.108(3) -0.027(3) -0.384(2) 0.103(14) Uani 0.28(2) 1 d PD A 2 H19D H -0.1399 -0.1002 -0.3518 0.155 Uiso 0.28(2) 1 calc PR A 2 H19E H -0.0407 -0.0338 -0.3588 0.155 Uiso 0.28(2) 1 calc PR A 2 H19F H -0.0902 -0.0105 -0.4531 0.155 Uiso 0.28(2) 1 calc PR A 2 C20 C 0.0080(4) 0.2351(4) -0.0525(3) 0.0345(11) Uani 1 1 d . . . C21 C -0.0537(4) 0.2755(4) -0.1282(3) 0.0343(10) Uani 1 1 d . . . C22 C -0.0096(4) 0.3335(4) -0.2233(3) 0.0442(13) Uani 1 1 d . . . H22A H -0.0552 0.3620 -0.2711 0.053 Uiso 1 1 calc R . . C23 C 0.1024(5) 0.3508(4) -0.2501(4) 0.0477(13) Uani 1 1 d . . . C24 C 0.1640(4) 0.3052(4) -0.1766(3) 0.0427(12) Uani 1 1 d . . . H24A H 0.2399 0.3123 -0.1925 0.051 Uiso 1 1 calc R . . C25 C 0.1205(4) 0.2495(4) -0.0807(3) 0.0343(11) Uani 1 1 d . . . C26 C 0.1496(6) 0.4200(6) -0.3558(4) 0.0708(19) Uani 1 1 d . . . C27 C 0.1181(8) 0.3798(9) -0.4246(5) 0.140(4) Uani 1 1 d . . . H27A H 0.1500 0.2999 -0.4136 0.210 Uiso 1 1 calc R . . H27B H 0.1450 0.4288 -0.4905 0.210 Uiso 1 1 calc R . . H27C H 0.0384 0.3842 -0.4150 0.210 Uiso 1 1 calc R . . C28 C 0.0991(13) 0.5429(8) -0.3798(7) 0.221(8) Uani 1 1 d . . . H28A H 0.1277 0.5880 -0.4465 0.332 Uiso 1 1 calc R . . H28B H 0.1170 0.5749 -0.3366 0.332 Uiso 1 1 calc R . . H28C H 0.0197 0.5460 -0.3720 0.332 Uiso 1 1 calc R . . C29 C 0.2682(8) 0.4178(15) -0.3714(6) 0.276(11) Uani 1 1 d . . . H29A H 0.3023 0.3380 -0.3564 0.414 Uiso 1 1 calc R . . H29B H 0.2878 0.4508 -0.3296 0.414 Uiso 1 1 calc R . . H29C H 0.2940 0.4630 -0.4388 0.414 Uiso 1 1 calc R . . C31 C -0.2072(9) 0.1605(7) 0.3169(5) 0.141(4) Uani 1 1 d . . . H31A H -0.2063 0.1067 0.3832 0.211 Uiso 1 1 calc R . . H31B H -0.2613 0.2271 0.3166 0.211 Uiso 1 1 calc R . . H31C H -0.1349 0.1865 0.2887 0.211 Uiso 1 1 calc R . . C32 C -0.3655(7) 0.0224(9) 0.3212(6) 0.152(5) Uani 1 1 d . . . H32A H -0.3514 -0.0207 0.3870 0.228 Uiso 1 1 calc R . . H32B H -0.3840 -0.0301 0.2952 0.228 Uiso 1 1 calc R . . H32C H -0.4264 0.0829 0.3215 0.228 Uiso 1 1 calc R . . C33 C -0.1392(6) -0.0364(6) 0.2721(5) 0.091(2) Uani 1 1 d . . . H33A H -0.1436 -0.0748 0.3419 0.136 Uiso 1 1 calc R . . H33B H -0.0667 -0.0107 0.2438 0.136 Uiso 1 1 calc R . . H33C H -0.1514 -0.0903 0.2445 0.136 Uiso 1 1 calc R . . C41 C -0.5516(5) 0.2625(8) 0.1163(6) 0.102(3) Uani 1 1 d . . . H41A H -0.6213 0.2463 0.1090 0.154 Uiso 1 1 calc R . . H41B H -0.5437 0.3445 0.0816 0.154 Uiso 1 1 calc R . . H41C H -0.5498 0.2426 0.1846 0.154 Uiso 1 1 calc R . . C42 C -0.4688(5) 0.2168(7) -0.0552(5) 0.087(2) Uani 1 1 d . . . H42A H -0.5438 0.2033 -0.0512 0.131 Uiso 1 1 calc R . . H42B H -0.4180 0.1700 -0.0881 0.131 Uiso 1 1 calc R . . H42C H -0.4605 0.2985 -0.0912 0.131 Uiso 1 1 calc R . . C43 C -0.4903(7) 0.0342(7) 0.1217(6) 0.118(3) Uani 1 1 d . . . H43A H -0.5649 0.0417 0.1100 0.177 Uiso 1 1 calc R . . H43B H -0.4900 0.0043 0.1911 0.177 Uiso 1 1 calc R . . H43C H -0.4431 -0.0191 0.0932 0.177 Uiso 1 1 calc R . . C51 C -0.1078(7) 0.4139(7) 0.1181(6) 0.109(3) Uani 1 1 d . . . H51A H -0.1092 0.4957 0.1070 0.163 Uiso 1 1 calc R . . H51B H -0.0376 0.3865 0.0869 0.163 Uiso 1 1 calc R . . H51C H -0.1174 0.3695 0.1874 0.163 Uiso 1 1 calc R . . C52 C -0.1892(6) 0.5001(5) -0.0550(5) 0.085(2) Uani 1 1 d . . . H52A H -0.1774 0.5727 -0.0520 0.127 Uiso 1 1 calc R . . H52B H -0.2507 0.5134 -0.0887 0.127 Uiso 1 1 calc R . . H52C H -0.1233 0.4701 -0.0897 0.127 Uiso 1 1 calc R . . C53 C -0.3344(6) 0.4748(6) 0.1209(6) 0.099(3) Uani 1 1 d . . . H53A H -0.3133 0.5486 0.1138 0.149 Uiso 1 1 calc R . . H53B H -0.3545 0.4295 0.1894 0.149 Uiso 1 1 calc R . . H53C H -0.3969 0.4888 0.0882 0.149 Uiso 1 1 calc R . . C61 C 0.4409(15) 0.4934(13) 0.3450(12) 0.211(8) Uani 1 1 d G . . H61A H 0.4680 0.5639 0.3318 0.253 Uiso 1 1 calc R . . C62 C 0.4884(6) 0.390(2) 0.4068(10) 0.178(6) Uani 1 1 d G . . H62A H 0.5477 0.3902 0.4354 0.213 Uiso 1 1 calc R . . C63 C 0.4483(15) 0.2855(13) 0.4264(7) 0.182(6) Uani 1 1 d G . . H63A H 0.4804 0.2154 0.4682 0.218 Uiso 1 1 calc R . . C64 C 0.3606(16) 0.2848(13) 0.3842(13) 0.205(8) Uani 1 1 d G . . H64A H 0.3335 0.2143 0.3975 0.246 Uiso 1 1 calc R . . C65 C 0.3131(7) 0.388(2) 0.3224(10) 0.246(12) Uani 1 1 d G . . H65A H 0.2538 0.3879 0.2939 0.295 Uiso 1 1 calc R . . C66 C 0.3532(14) 0.4927(14) 0.3028(6) 0.233(12) Uani 1 1 d G . . H66A H 0.3210 0.5627 0.2610 0.279 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.03645(12) 0.04011(12) 0.04221(12) -0.02140(9) -0.00671(8) -0.00419(9) S1 0.0759(10) 0.0384(7) 0.0392(7) -0.0190(6) -0.0132(7) 0.0018(7) S2 0.0371(7) 0.0675(10) 0.0393(7) -0.0126(7) -0.0070(6) -0.0021(7) S3 0.0389(7) 0.0335(7) 0.0430(7) -0.0152(6) -0.0133(6) -0.0007(6) S4 0.0431(7) 0.0383(7) 0.0529(8) -0.0174(6) -0.0158(6) -0.0088(6) P1 0.0714(11) 0.0692(11) 0.0432(9) -0.0216(8) -0.0069(8) -0.0152(9) P2 0.0396(8) 0.0829(12) 0.0742(11) -0.0440(10) -0.0072(8) -0.0071(8) P3 0.0668(11) 0.0522(9) 0.0720(11) -0.0379(8) -0.0024(9) -0.0087(8) C10 0.027(2) 0.041(3) 0.037(3) -0.017(2) -0.011(2) 0.003(2) C11 0.030(3) 0.039(3) 0.042(3) -0.018(2) -0.010(2) -0.002(2) C12 0.045(3) 0.050(3) 0.043(3) -0.025(3) -0.009(2) -0.009(3) C13 0.050(3) 0.061(4) 0.036(3) -0.022(3) -0.011(2) -0.008(3) C14 0.045(3) 0.039(3) 0.035(3) -0.008(2) -0.011(2) -0.007(2) C15 0.033(3) 0.036(3) 0.039(3) -0.015(2) -0.012(2) 0.000(2) C16 0.076(4) 0.078(4) 0.039(3) -0.028(3) -0.015(3) -0.014(4) C17 0.115(11) 0.165(17) 0.069(8) -0.057(10) -0.056(8) 0.026(11) C18 0.117(11) 0.179(15) 0.038(6) -0.035(8) -0.006(7) -0.050(11) C19 0.28(3) 0.092(10) 0.066(8) -0.035(7) -0.069(13) -0.039(15) C17A 0.12(3) 0.11(3) 0.043(14) -0.005(15) -0.049(15) -0.04(2) C18A 0.33(9) 0.23(6) 0.049(19) 0.05(3) -0.08(4) -0.25(6) C19A 0.10(2) 0.18(4) 0.054(16) -0.09(2) 0.001(18) 0.00(3) C20 0.036(3) 0.026(2) 0.041(3) -0.013(2) -0.005(2) -0.003(2) C21 0.036(3) 0.029(2) 0.038(3) -0.012(2) -0.007(2) -0.004(2) C22 0.060(4) 0.038(3) 0.037(3) -0.007(2) -0.017(3) -0.010(3) C23 0.059(4) 0.040(3) 0.039(3) -0.008(2) -0.003(3) -0.015(3) C24 0.045(3) 0.042(3) 0.042(3) -0.014(2) -0.003(2) -0.013(2) C25 0.040(3) 0.027(2) 0.039(3) -0.013(2) -0.011(2) -0.002(2) C26 0.087(5) 0.077(5) 0.039(3) -0.002(3) -0.004(3) -0.036(4) C27 0.176(10) 0.206(11) 0.041(4) -0.029(5) 0.017(5) -0.103(8) C28 0.43(2) 0.078(7) 0.083(7) 0.015(5) 0.054(10) -0.074(10) C29 0.105(8) 0.54(3) 0.064(6) 0.073(10) -0.006(6) -0.161(13) C31 0.279(13) 0.101(6) 0.071(5) -0.038(5) -0.064(7) -0.029(8) C32 0.083(6) 0.228(12) 0.073(6) 0.027(6) 0.008(5) -0.049(7) C33 0.109(6) 0.087(5) 0.061(4) -0.009(4) -0.031(4) 0.004(5) C41 0.039(4) 0.167(8) 0.134(7) -0.099(6) -0.018(4) 0.012(4) C42 0.047(4) 0.150(7) 0.089(5) -0.065(5) -0.021(4) -0.009(4) C43 0.092(6) 0.119(7) 0.145(8) -0.034(6) -0.018(6) -0.051(6) C51 0.126(7) 0.094(6) 0.143(7) -0.058(5) -0.050(6) -0.033(5) C52 0.125(6) 0.044(4) 0.084(5) -0.030(3) 0.012(4) -0.024(4) C53 0.109(6) 0.071(5) 0.124(6) -0.069(5) 0.032(5) -0.013(4) C61 0.185(17) 0.175(16) 0.173(17) -0.022(13) 0.075(12) 0.002(13) C62 0.107(9) 0.215(16) 0.171(15) -0.049(14) 0.005(9) -0.005(13) C63 0.217(19) 0.154(15) 0.132(11) -0.045(10) -0.002(13) 0.032(12) C64 0.22(2) 0.26(2) 0.186(19) -0.158(19) 0.003(12) -0.008(15) C65 0.231(18) 0.40(3) 0.094(13) -0.120(17) -0.027(13) 0.06(2) C66 0.170(17) 0.30(3) 0.092(10) 0.001(12) 0.019(11) 0.092(16) _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 W H2 1.59(4) . ? W H1 1.61(5) . ? W P1 2.4267(15) . ? W S3 2.4449(12) . ? W P2 2.4655(15) . ? W P3 2.4747(15) . ? W S2 2.4811(13) . ? W S1 2.4902(13) . ? S1 C10 1.730(4) . ? S2 C20 1.728(5) . ? S3 C21 1.796(5) . ? S3 C15 1.798(4) . ? S4 C25 1.769(4) 2 ? S4 C11 1.770(5) . ? P1 C33 1.808(7) . ? P1 C32 1.815(7) . ? P1 C31 1.817(7) . ? P2 C41 1.815(6) . ? P2 C42 1.817(6) . ? P2 C43 1.824(8) . ? P3 C52 1.814(6) . ? P3 C53 1.814(6) . ? P3 C51 1.828(7) . ? C10 C15 1.391(6) . ? C10 C11 1.406(6) . ? C11 C12 1.382(6) . ? C12 C13 1.372(7) . ? C13 C14 1.391(6) . ? C13 C16 1.546(6) . ? C14 C15 1.399(6) . ? C16 C18A 1.38(3) . ? C16 C19 1.497(12) . ? C16 C17 1.500(12) . ? C16 C17A 1.53(2) . ? C16 C18 1.547(14) . ? C16 C19A 1.63(3) . ? C20 C21 1.401(6) . ? C20 C25 1.403(6) . ? C21 C22 1.375(6) . ? C22 C23 1.404(7) . ? C23 C24 1.371(7) . ? C23 C26 1.535(7) . ? C24 C25 1.377(6) . ? C25 S4 1.769(4) 2 ? C26 C29 1.447(11) . ? C26 C27 1.469(9) . ? C26 C28 1.486(12) . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? 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 H2 W H1 68(2) . . ? H2 W P1 126.2(15) . . ? H1 W P1 57.9(18) . . ? H2 W S3 76.7(15) . . ? H1 W S3 145.0(18) . . ? P1 W S3 156.93(5) . . ? H2 W P2 53.7(15) . . ? H1 W P2 67.3(18) . . ? P1 W P2 100.85(6) . . ? S3 W P2 91.21(5) . . ? H2 W P3 66.9(15) . . ? H1 W P3 77.3(18) . . ? P1 W P3 100.70(5) . . ? S3 W P3 90.54(5) . . ? P2 W P3 118.22(6) . . ? H2 W S2 138.8(16) . . ? H1 W S2 126.2(18) . . ? P1 W S2 80.77(5) . . ? S3 W S2 81.80(4) . . ? P2 W S2 161.93(5) . . ? P3 W S2 78.68(5) . . ? H2 W S1 125.9(15) . . ? H1 W S1 117.9(18) . . ? P1 W S1 81.64(5) . . ? S3 W S1 81.67(4) . . ? P2 W S1 78.28(5) . . ? P3 W S1 162.07(5) . . ? S2 W S1 84.21(5) . . ? C10 S1 W 106.84(16) . . ? C20 S2 W 106.85(16) . . ? C21 S3 C15 100.1(2) . . ? C21 S3 W 107.32(15) . . ? C15 S3 W 107.29(16) . . ? C25 S4 C11 108.8(2) 2 . ? C33 P1 C32 101.0(4) . . ? C33 P1 C31 98.4(4) . . ? C32 P1 C31 103.0(5) . . ? C33 P1 W 117.1(2) . . ? C32 P1 W 117.4(3) . . ? C31 P1 W 116.9(3) . . ? C41 P2 C42 101.1(3) . . ? C41 P2 C43 100.4(4) . . ? C42 P2 C43 98.8(4) . . ? C41 P2 W 115.7(2) . . ? C42 P2 W 115.7(2) . . ? C43 P2 W 121.8(3) . . ? C52 P3 C53 101.5(3) . . ? C52 P3 C51 98.8(4) . . ? C53 P3 C51 100.0(4) . . ? C52 P3 W 114.7(2) . . ? C53 P3 W 115.9(2) . . ? C51 P3 W 122.5(3) . . ? C15 C10 C11 115.7(4) . . ? C15 C10 S1 123.1(3) . . ? C11 C10 S1 121.2(4) . . ? C12 C11 C10 121.0(4) . . ? C12 C11 S4 115.8(3) . . ? C10 C11 S4 122.9(3) . . ? C13 C12 C11 123.0(4) . . ? C12 C13 C14 117.0(4) . . ? C12 C13 C16 122.8(5) . . ? C14 C13 C16 120.2(5) . . ? C13 C14 C15 120.3(4) . . ? C10 C15 C14 122.8(4) . . ? C10 C15 S3 119.5(3) . . ? C14 C15 S3 117.6(4) . . ? C18A C16 C19 130(2) . . ? C18A C16 C17 65(2) . . ? C19 C16 C17 111.8(9) . . ? C18A C16 C17A 115.1(19) . . ? C19 C16 C17A 63.0(13) . . ? C17 C16 C17A 54.8(12) . . ? C18A C16 C13 115.3(15) . . ? C19 C16 C13 112.3(6) . . ? C17 C16 C13 109.2(5) . . ? C17A C16 C13 106.3(9) . . ? C18A C16 C18 41(2) . . ? C19 C16 C18 109.5(10) . . ? C17 C16 C18 106.0(9) . . ? C17A C16 C18 145.2(10) . . ? C13 C16 C18 107.7(6) . . ? C18A C16 C19A 111(2) . . ? C19 C16 C19A 40.9(11) . . ? C17 C16 C19A 144.1(11) . . ? C17A C16 C19A 103.8(16) . . ? C13 C16 C19A 104.3(10) . . ? C18 C16 C19A 74.7(16) . . ? C21 C20 C25 115.6(4) . . ? C21 C20 S2 123.2(4) . . ? C25 C20 S2 121.2(4) . . ? C22 C21 C20 122.6(4) . . ? C22 C21 S3 118.1(4) . . ? C20 C21 S3 119.2(3) . . ? C21 C22 C23 121.1(5) . . ? C24 C23 C22 116.0(5) . . ? C24 C23 C26 123.3(5) . . ? C22 C23 C26 120.6(5) . . ? C23 C24 C25 123.5(5) . . ? C24 C25 C20 120.9(4) . . ? C24 C25 S4 115.9(4) . 2 ? C20 C25 S4 122.8(4) . 2 ? C29 C26 C27 110.1(8) . . ? C29 C26 C28 108.6(9) . . ? C27 C26 C28 105.3(8) . . ? C29 C26 C23 112.5(6) . . ? C27 C26 C23 111.8(5) . . ? C28 C26 C23 108.3(6) . . ? C62 C61 C66 120.0 . . ? C61 C62 C63 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 1.268 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.108 # Attachment 'S8SW2_new.CIF' data_s8sw2 _database_code_depnum_ccdc_archive 'CCDC 702277' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H108 P6 S8 W2' _chemical_formula_weight 1687.50 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.5666(18) _cell_length_b 19.595(2) _cell_length_c 23.604(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.152(2) _cell_angle_gamma 90.00 _cell_volume 7618.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 9881 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 30.17 _exptl_crystal_description PLATE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 3.398 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.5799 _exptl_absorpt_correction_T_max 0.9668 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90702 _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.37 _reflns_number_total 15575 _reflns_number_gt 11412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+77.9834P] 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 15575 _refine_ls_number_parameters 733 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 1.10053(2) 0.21363(2) 0.039518(16) 0.02666(12) Uani 1 1 d D . . H1 H 1.198(2) 0.196(5) 0.060(4) 0.032 Uiso 1 1 d D . . H2 H 1.155(5) 0.200(5) -0.015(3) 0.032 Uiso 1 1 d D . . W2 W 0.74869(3) 0.35517(3) 0.229215(18) 0.03741(14) Uani 1 1 d D . . H4 H 0.655(3) 0.356(6) 0.249(4) 0.045 Uiso 1 1 d D . . H3 H 0.752(7) 0.391(5) 0.294(2) 0.045 Uiso 1 1 d D . . P1 P 1.13347(15) 0.09494(15) 0.01662(12) 0.0307(6) Uani 1 1 d . . . P2 P 1.14153(17) 0.2170(2) 0.14295(12) 0.0462(8) Uani 1 1 d . . . P3 P 1.18127(15) 0.31558(16) 0.02188(12) 0.0336(6) Uani 1 1 d . . . P4 P 0.6989(3) 0.4717(2) 0.23940(15) 0.0651(12) Uani 1 1 d . . . P5 P 0.8838(2) 0.3630(3) 0.28352(15) 0.0830(17) Uani 1 1 d . . . P6 P 0.71202(18) 0.26170(17) 0.28913(12) 0.0396(7) Uani 1 1 d . . . S1 S 0.98935(14) 0.14568(16) 0.07519(10) 0.0330(6) Uani 1 1 d . . . S2 S 1.00388(15) 0.31126(16) 0.05910(10) 0.0328(6) Uani 1 1 d . . . S3 S 0.8200(2) 0.4183(2) 0.15830(13) 0.0628(11) Uani 1 1 d . . . S4 S 0.80410(15) 0.2517(2) 0.17821(11) 0.0462(8) Uani 1 1 d . . . S5 S 0.64349(14) 0.34044(15) 0.15015(10) 0.0313(6) Uani 1 1 d . . . S6 S 0.81263(15) 0.10869(16) 0.10551(11) 0.0352(7) Uani 1 1 d . . . S7 S 1.00772(13) 0.21736(14) -0.04830(9) 0.0254(5) Uani 1 1 d . . . S8 S 0.89417(15) 0.45036(15) 0.04355(11) 0.0331(6) Uani 1 1 d . . . C10 C 0.9065(5) 0.1566(5) 0.0235(4) 0.022(2) Uani 1 1 d . . . C11 C 0.9126(5) 0.1832(6) -0.0308(4) 0.027(2) Uani 1 1 d . . . C12 C 0.8475(6) 0.1840(6) -0.0729(4) 0.030(2) Uani 1 1 d . . . H12A H 0.8553 0.2003 -0.1098 0.036 Uiso 1 1 calc R . . C13 C 0.7715(6) 0.1618(6) -0.0622(4) 0.032(2) Uani 1 1 d . . . C14 C 0.7639(6) 0.1379(6) -0.0077(4) 0.035(3) Uani 1 1 d . . . H14A H 0.7124 0.1219 0.0007 0.042 Uiso 1 1 calc R . . C15 C 0.8281(6) 0.1363(6) 0.0350(4) 0.029(2) Uani 1 1 d . . . C16 C 0.6978(7) 0.1638(8) -0.1067(5) 0.054(4) Uani 1 1 d . . . C17 C 0.6291(7) 0.1997(10) -0.0811(6) 0.080(6) Uani 1 1 d . . . H17A H 0.6453 0.2466 -0.0711 0.119 Uiso 1 1 calc R . . H17B H 0.6169 0.1754 -0.0468 0.119 Uiso 1 1 calc R . . H17C H 0.5807 0.2002 -0.1089 0.119 Uiso 1 1 calc R . . C18 C 0.7150(7) 0.2009(8) -0.1608(5) 0.060(4) Uani 1 1 d . . . H18A H 0.7286 0.2486 -0.1518 0.091 Uiso 1 1 calc R . . H18B H 0.6668 0.1990 -0.1887 0.091 Uiso 1 1 calc R . . H18C H 0.7607 0.1789 -0.1767 0.091 Uiso 1 1 calc R . . C19 C 0.6756(10) 0.0898(9) -0.1232(7) 0.092(6) Uani 1 1 d . . . H19A H 0.6636 0.0645 -0.0893 0.138 Uiso 1 1 calc R . . H19B H 0.7213 0.0681 -0.1395 0.138 Uiso 1 1 calc R . . H19C H 0.6277 0.0894 -0.1515 0.138 Uiso 1 1 calc R . . C20 C 0.9644(5) 0.3412(5) -0.0081(4) 0.021(2) Uani 1 1 d . . . C21 C 0.9240(5) 0.4045(5) -0.0159(4) 0.029(2) Uani 1 1 d . . . C22 C 0.9066(6) 0.4326(6) -0.0698(4) 0.035(2) Uani 1 1 d . . . H22A H 0.8856 0.4777 -0.0735 0.042 Uiso 1 1 calc R . . C23 C 0.9195(5) 0.3953(5) -0.1194(4) 0.025(2) Uani 1 1 d . . . C24 C 0.9502(6) 0.3299(6) -0.1114(4) 0.030(2) Uani 1 1 d . . . H24A H 0.9566 0.3022 -0.1436 0.036 Uiso 1 1 calc R . . C25 C 0.9721(5) 0.3039(5) -0.0571(4) 0.025(2) Uani 1 1 d . . . C26 C 0.9013(7) 0.4256(6) -0.1800(5) 0.038(3) Uani 1 1 d . . . C27 C 0.8737(18) 0.4943(11) -0.1799(7) 0.160(13) Uani 1 1 d . . . H27A H 0.8631 0.5108 -0.2192 0.240 Uiso 1 1 calc R . . H27B H 0.9153 0.5229 -0.1590 0.240 Uiso 1 1 calc R . . H27C H 0.8236 0.4966 -0.1614 0.240 Uiso 1 1 calc R . . C28 C 0.8366(12) 0.3818(10) -0.2140(7) 0.093(6) Uani 1 1 d . . . H28A H 0.8247 0.4007 -0.2524 0.140 Uiso 1 1 calc R . . H28B H 0.7870 0.3818 -0.1948 0.140 Uiso 1 1 calc R . . H28C H 0.8567 0.3350 -0.2165 0.140 Uiso 1 1 calc R . . C29 C 0.9743(12) 0.4166(12) -0.2119(7) 0.110(8) Uani 1 1 d . . . H29A H 0.9630 0.4358 -0.2503 0.165 Uiso 1 1 calc R . . H29B H 0.9867 0.3679 -0.2146 0.165 Uiso 1 1 calc R . . H29C H 1.0208 0.4403 -0.1916 0.165 Uiso 1 1 calc R . . C30 C 0.7618(6) 0.4026(6) 0.0934(4) 0.032(2) Uani 1 1 d . . . C31 C 0.6829(6) 0.3770(6) 0.0887(4) 0.030(2) Uani 1 1 d . . . C32 C 0.6305(6) 0.3788(6) 0.0385(4) 0.029(2) Uani 1 1 d . . . H32A H 0.5767 0.3618 0.0380 0.035 Uiso 1 1 calc R . . C33 C 0.6567(6) 0.4052(5) -0.0106(4) 0.027(2) Uani 1 1 d . . . C34 C 0.7378(6) 0.4259(6) -0.0078(4) 0.031(2) Uani 1 1 d . . . H34A H 0.7576 0.4423 -0.0416 0.037 Uiso 1 1 calc R . . C35 C 0.7908(6) 0.4237(6) 0.0417(4) 0.028(2) Uani 1 1 d . . . C36 C 0.5990(6) 0.4189(6) -0.0651(5) 0.039(3) Uani 1 1 d . . . C37 C 0.6376(8) 0.3975(8) -0.1190(5) 0.055(4) Uani 1 1 d . . . H37A H 0.6882 0.4228 -0.1209 0.082 Uiso 1 1 calc R . . H37B H 0.5999 0.4076 -0.1528 0.082 Uiso 1 1 calc R . . H37C H 0.6492 0.3485 -0.1174 0.082 Uiso 1 1 calc R . . C38 C 0.5788(7) 0.4943(7) -0.0680(5) 0.048(3) Uani 1 1 d . . . H38A H 0.5535 0.5075 -0.0340 0.072 Uiso 1 1 calc R . . H38B H 0.5411 0.5035 -0.1020 0.072 Uiso 1 1 calc R . . H38C H 0.6286 0.5207 -0.0698 0.072 Uiso 1 1 calc R . . C39 C 0.5193(7) 0.3784(7) -0.0643(5) 0.052(3) Uani 1 1 d . . . H39A H 0.4931 0.3912 -0.0306 0.078 Uiso 1 1 calc R . . H39B H 0.5313 0.3294 -0.0631 0.078 Uiso 1 1 calc R . . H39C H 0.4829 0.3888 -0.0987 0.078 Uiso 1 1 calc R . . C40 C 0.7200(5) 0.2169(6) 0.1378(4) 0.033(3) Uani 1 1 d . . . C41 C 0.7195(6) 0.1519(6) 0.1129(4) 0.030(2) Uani 1 1 d . . . C42 C 0.6461(6) 0.1202(6) 0.0943(5) 0.034(2) Uani 1 1 d . . . H42A H 0.6473 0.0743 0.0816 0.041 Uiso 1 1 calc R . . C43 C 0.5711(6) 0.1527(6) 0.0935(5) 0.034(2) Uani 1 1 d . . . C44 C 0.5741(6) 0.2218(6) 0.1082(4) 0.033(2) Uani 1 1 d . . . H44A H 0.5256 0.2480 0.1032 0.039 Uiso 1 1 calc R . . C45 C 0.6454(5) 0.2532(5) 0.1296(4) 0.026(2) Uani 1 1 d . . . C46 C 0.4906(6) 0.1184(6) 0.0739(6) 0.048(3) Uani 1 1 d . . . C47 C 0.4280(7) 0.1355(9) 0.1127(5) 0.068(5) Uani 1 1 d . . . H47A H 0.4198 0.1850 0.1130 0.102 Uiso 1 1 calc R . . H47B H 0.4464 0.1198 0.1514 0.102 Uiso 1 1 calc R . . H47C H 0.3767 0.1129 0.0992 0.102 Uiso 1 1 calc R . . C48 C 0.5003(10) 0.0406(10) 0.0735(16) 0.200(18) Uani 1 1 d . . . H48A H 0.5197 0.0247 0.1120 0.300 Uiso 1 1 calc R . . H48B H 0.5395 0.0279 0.0471 0.300 Uiso 1 1 calc R . . H48C H 0.4477 0.0194 0.0612 0.300 Uiso 1 1 calc R . . C49 C 0.4608(8) 0.1423(11) 0.0150(6) 0.097(7) Uani 1 1 d . . . H49A H 0.4552 0.1920 0.0149 0.145 Uiso 1 1 calc R . . H49B H 0.4079 0.1214 0.0030 0.145 Uiso 1 1 calc R . . H49C H 0.4997 0.1289 -0.0115 0.145 Uiso 1 1 calc R . . C51 C 1.1399(7) 0.0271(8) 0.0710(5) 0.054(4) Uani 1 1 d . . . H51A H 1.1537 -0.0162 0.0537 0.081 Uiso 1 1 calc R . . H51B H 1.0875 0.0227 0.0864 0.081 Uiso 1 1 calc R . . H51C H 1.1820 0.0388 0.1019 0.081 Uiso 1 1 calc R . . C52 C 1.2313(6) 0.0803(7) -0.0109(6) 0.047(3) Uani 1 1 d . . . H52A H 1.2377 0.0315 -0.0184 0.070 Uiso 1 1 calc R . . H52B H 1.2753 0.0955 0.0173 0.070 Uiso 1 1 calc R . . H52C H 1.2332 0.1060 -0.0464 0.070 Uiso 1 1 calc R . . C53 C 1.0662(6) 0.0560(6) -0.0405(5) 0.035(2) Uani 1 1 d . . . H53A H 1.0839 0.0091 -0.0466 0.052 Uiso 1 1 calc R . . H53B H 1.0680 0.0823 -0.0756 0.052 Uiso 1 1 calc R . . H53C H 1.0106 0.0555 -0.0299 0.052 Uiso 1 1 calc R . . C61 C 1.2468(7) 0.2324(8) 0.1684(5) 0.052(3) Uani 1 1 d . . . H61A H 1.2534 0.2322 0.2101 0.078 Uiso 1 1 calc R . . H61B H 1.2633 0.2769 0.1546 0.078 Uiso 1 1 calc R . . H61C H 1.2806 0.1965 0.1542 0.078 Uiso 1 1 calc R . . C62 C 1.1282(12) 0.1405(12) 0.1857(6) 0.120(9) Uani 1 1 d . . . H62A H 1.1470 0.1499 0.2257 0.180 Uiso 1 1 calc R . . H62B H 1.1599 0.1029 0.1720 0.180 Uiso 1 1 calc R . . H62C H 1.0707 0.1279 0.1822 0.180 Uiso 1 1 calc R . . C63 C 1.0907(11) 0.2800(13) 0.1820(6) 0.120(9) Uani 1 1 d . . . H63A H 1.1110 0.2774 0.2225 0.180 Uiso 1 1 calc R . . H63B H 1.0321 0.2713 0.1773 0.180 Uiso 1 1 calc R . . H63C H 1.1015 0.3256 0.1675 0.180 Uiso 1 1 calc R . . C71 C 1.2876(7) 0.2978(7) 0.0130(6) 0.051(3) Uani 1 1 d . . . H71A H 1.3155 0.3407 0.0061 0.076 Uiso 1 1 calc R . . H71B H 1.2904 0.2672 -0.0196 0.076 Uiso 1 1 calc R . . H71C H 1.3139 0.2761 0.0476 0.076 Uiso 1 1 calc R . . C72 C 1.1547(7) 0.3666(6) -0.0425(5) 0.042(3) Uani 1 1 d . . . H72A H 1.1925 0.4051 -0.0431 0.063 Uiso 1 1 calc R . . H72B H 1.0992 0.3840 -0.0426 0.063 Uiso 1 1 calc R . . H72C H 1.1582 0.3381 -0.0763 0.063 Uiso 1 1 calc R . . C73 C 1.1926(8) 0.3861(7) 0.0735(5) 0.051(3) Uani 1 1 d . . . H73A H 1.2266 0.4219 0.0593 0.076 Uiso 1 1 calc R . . H73B H 1.2182 0.3691 0.1101 0.076 Uiso 1 1 calc R . . H73C H 1.1390 0.4049 0.0785 0.076 Uiso 1 1 calc R . . C81 C 0.7662(12) 0.5405(6) 0.2629(6) 0.092(7) Uani 1 1 d . . . H81A H 0.7351 0.5829 0.2642 0.138 Uiso 1 1 calc R . . H81B H 0.8073 0.5460 0.2362 0.138 Uiso 1 1 calc R . . H81C H 0.7931 0.5302 0.3010 0.138 Uiso 1 1 calc R . . C82 C 0.6248(12) 0.4808(8) 0.2907(6) 0.082(5) Uani 1 1 d . . . H82A H 0.6079 0.5287 0.2923 0.123 Uiso 1 1 calc R . . H82B H 0.6493 0.4664 0.3285 0.123 Uiso 1 1 calc R . . H82C H 0.5774 0.4523 0.2790 0.123 Uiso 1 1 calc R . . C83 C 0.6419(11) 0.5093(8) 0.1768(6) 0.074(5) Uani 1 1 d . . . H83A H 0.6252 0.5557 0.1857 0.111 Uiso 1 1 calc R . . H83B H 0.5937 0.4815 0.1654 0.111 Uiso 1 1 calc R . . H83C H 0.6762 0.5109 0.1455 0.111 Uiso 1 1 calc R . . C91 C 0.8910(8) 0.3713(8) 0.3603(5) 0.061(4) Uani 1 1 d . . . H91A H 0.9483 0.3739 0.3757 0.091 Uiso 1 1 calc R . . H91B H 0.8657 0.3316 0.3764 0.091 Uiso 1 1 calc R . . H91C H 0.8630 0.4129 0.3702 0.091 Uiso 1 1 calc R . . C92 C 0.9481(14) 0.4332(17) 0.2700(10) 0.23(2) Uani 1 1 d . . . H92A H 0.9995 0.4296 0.2946 0.347 Uiso 1 1 calc R . . H92B H 0.9212 0.4761 0.2780 0.347 Uiso 1 1 calc R . . H92C H 0.9590 0.4324 0.2300 0.347 Uiso 1 1 calc R . . C93 C 0.9521(8) 0.2928(17) 0.2783(9) 0.186(17) Uani 1 1 d . . . H93A H 1.0035 0.3023 0.3015 0.279 Uiso 1 1 calc R . . H93B H 0.9621 0.2867 0.2384 0.279 Uiso 1 1 calc R . . H93C H 0.9279 0.2512 0.2921 0.279 Uiso 1 1 calc R . . C101 C 0.6336(7) 0.2016(7) 0.2611(5) 0.047(3) Uani 1 1 d . . . H10A H 0.6258 0.1672 0.2901 0.071 Uiso 1 1 calc R . . H10B H 0.6504 0.1791 0.2272 0.071 Uiso 1 1 calc R . . H10C H 0.5826 0.2261 0.2509 0.071 Uiso 1 1 calc R . . C102 C 0.6691(12) 0.2899(9) 0.3537(6) 0.088(6) Uani 1 1 d . . . H10D H 0.6556 0.2500 0.3758 0.132 Uiso 1 1 calc R . . H10E H 0.6198 0.3167 0.3429 0.132 Uiso 1 1 calc R . . H10F H 0.7089 0.3182 0.3767 0.132 Uiso 1 1 calc R . . C103 C 0.7859(9) 0.1999(7) 0.3200(6) 0.063(4) Uani 1 1 d . . . H10G H 0.7589 0.1667 0.3425 0.095 Uiso 1 1 calc R . . H10H H 0.8284 0.2236 0.3446 0.095 Uiso 1 1 calc R . . H10I H 0.8103 0.1763 0.2894 0.095 Uiso 1 1 calc R . . C201 C 0.4448(9) 0.3466(10) 0.2856(8) 0.074(5) Uani 1 1 d . . . H20A H 0.4726 0.3168 0.3128 0.089 Uiso 1 1 calc R . . C202 C 0.4431(8) 0.3326(7) 0.2293(7) 0.063(4) Uani 1 1 d . . . H20B H 0.4680 0.2923 0.2170 0.075 Uiso 1 1 calc R . . C203 C 0.4058(9) 0.3761(9) 0.1908(6) 0.066(4) Uani 1 1 d . . . H20C H 0.4068 0.3672 0.1514 0.079 Uiso 1 1 calc R . . C204 C 0.3672(9) 0.4319(9) 0.2072(7) 0.073(5) Uani 1 1 d . . . H20D H 0.3382 0.4608 0.1799 0.088 Uiso 1 1 calc R . . C205 C 0.3708(12) 0.4463(8) 0.2647(9) 0.086(6) Uani 1 1 d . . . H20E H 0.3475 0.4871 0.2774 0.104 Uiso 1 1 calc R . . C206 C 0.4078(12) 0.4017(11) 0.3030(7) 0.089(6) Uani 1 1 d . . . H20F H 0.4073 0.4099 0.3426 0.106 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01340(18) 0.0483(3) 0.01856(19) -0.00241(18) 0.00289(13) -0.00339(18) W2 0.0221(2) 0.0654(3) 0.0235(2) 0.0038(2) -0.00334(16) -0.0131(2) P1 0.0146(12) 0.0428(17) 0.0348(14) 0.0056(12) 0.0032(10) -0.0024(11) P2 0.0247(14) 0.092(3) 0.0206(13) -0.0033(15) -0.0019(11) -0.0024(16) P3 0.0182(12) 0.0465(18) 0.0368(15) -0.0113(13) 0.0067(11) -0.0027(12) P4 0.100(3) 0.049(2) 0.0405(19) -0.0038(16) -0.0223(19) -0.024(2) P5 0.0313(18) 0.183(5) 0.0320(18) 0.006(2) -0.0086(14) -0.035(2) P6 0.0386(16) 0.057(2) 0.0251(14) 0.0072(13) 0.0123(12) 0.0158(14) S1 0.0158(11) 0.0607(19) 0.0223(12) 0.0061(12) 0.0014(9) -0.0042(12) S2 0.0222(12) 0.0566(18) 0.0198(12) -0.0026(11) 0.0039(9) 0.0056(12) S3 0.0414(17) 0.117(3) 0.0280(15) 0.0127(18) -0.0063(13) -0.039(2) S4 0.0122(11) 0.103(3) 0.0225(13) -0.0138(15) -0.0013(10) 0.0034(14) S5 0.0183(11) 0.0545(18) 0.0208(12) -0.0030(11) 0.0012(9) -0.0024(11) S6 0.0191(12) 0.0590(19) 0.0286(13) 0.0211(13) 0.0083(10) 0.0095(12) S7 0.0145(10) 0.0445(15) 0.0179(11) -0.0009(11) 0.0044(8) -0.0047(10) S8 0.0197(12) 0.0494(17) 0.0302(13) -0.0094(12) 0.0023(10) -0.0035(11) C10 0.017(4) 0.025(5) 0.025(5) 0.007(4) -0.001(4) -0.001(4) C11 0.015(4) 0.042(6) 0.024(5) 0.005(4) 0.002(4) -0.005(4) C12 0.020(5) 0.047(7) 0.026(5) 0.008(5) 0.005(4) -0.005(5) C13 0.018(5) 0.049(7) 0.028(5) 0.018(5) -0.004(4) -0.005(4) C14 0.014(5) 0.053(7) 0.037(6) 0.015(5) 0.005(4) -0.005(5) C15 0.017(5) 0.044(7) 0.027(5) 0.014(5) 0.002(4) 0.004(4) C16 0.025(6) 0.090(11) 0.043(7) 0.030(7) -0.012(5) -0.019(6) C17 0.023(6) 0.154(17) 0.061(9) 0.051(10) 0.001(6) 0.018(8) C18 0.027(6) 0.115(13) 0.036(6) 0.040(7) -0.013(5) -0.018(7) C19 0.075(11) 0.126(16) 0.064(10) 0.034(10) -0.040(8) -0.057(11) C20 0.012(4) 0.027(5) 0.025(5) 0.002(4) 0.001(3) -0.006(4) C21 0.015(4) 0.041(6) 0.031(5) 0.009(5) 0.002(4) -0.018(4) C22 0.025(5) 0.043(7) 0.038(6) -0.010(5) 0.007(4) -0.007(5) C23 0.009(4) 0.043(6) 0.024(5) -0.001(4) 0.003(3) -0.001(4) C24 0.020(5) 0.048(7) 0.023(5) -0.007(5) 0.004(4) 0.001(5) C25 0.015(4) 0.039(6) 0.023(5) 0.001(4) 0.008(4) -0.004(4) C26 0.033(6) 0.050(7) 0.032(6) 0.012(5) 0.004(5) 0.008(5) C27 0.31(4) 0.139(19) 0.033(8) 0.038(11) 0.047(14) 0.15(2) C28 0.118(16) 0.102(15) 0.054(10) 0.004(10) -0.019(10) 0.004(12) C29 0.124(16) 0.16(2) 0.053(10) 0.047(11) 0.048(10) 0.068(15) C30 0.022(5) 0.052(7) 0.022(5) -0.001(5) -0.003(4) -0.009(5) C31 0.025(5) 0.046(7) 0.018(5) -0.001(4) -0.002(4) -0.005(5) C32 0.024(5) 0.042(6) 0.022(5) 0.000(4) -0.005(4) 0.002(4) C33 0.023(5) 0.032(6) 0.024(5) -0.004(4) -0.004(4) 0.005(4) C34 0.028(5) 0.042(7) 0.023(5) -0.006(5) 0.004(4) 0.001(5) C35 0.020(5) 0.043(6) 0.022(5) -0.003(4) 0.000(4) 0.000(4) C36 0.029(6) 0.056(8) 0.032(6) -0.003(5) -0.006(4) -0.006(5) C37 0.051(8) 0.082(10) 0.028(6) 0.000(6) -0.008(5) 0.011(7) C38 0.037(6) 0.059(9) 0.045(7) 0.011(6) -0.002(5) -0.005(6) C39 0.036(7) 0.081(10) 0.033(6) 0.001(6) -0.018(5) -0.006(6) C40 0.011(4) 0.068(8) 0.021(5) 0.015(5) 0.003(4) -0.004(5) C41 0.021(5) 0.044(7) 0.025(5) 0.019(5) 0.004(4) 0.000(5) C42 0.023(5) 0.042(7) 0.038(6) 0.012(5) 0.008(4) 0.000(5) C43 0.025(5) 0.032(6) 0.044(6) 0.016(5) -0.001(4) -0.003(4) C44 0.015(5) 0.049(7) 0.033(5) 0.004(5) 0.000(4) 0.000(5) C45 0.020(5) 0.043(6) 0.013(4) 0.003(4) 0.001(4) -0.002(4) C46 0.020(5) 0.038(7) 0.086(10) -0.012(7) 0.009(6) -0.018(5) C47 0.027(6) 0.135(15) 0.044(7) 0.003(8) 0.007(5) -0.035(8) C48 0.030(9) 0.066(14) 0.50(6) -0.03(2) -0.016(18) -0.025(9) C49 0.033(7) 0.22(2) 0.039(8) -0.022(10) 0.002(6) -0.065(11) C51 0.021(6) 0.089(11) 0.049(7) 0.009(7) -0.007(5) 0.001(6) C52 0.017(5) 0.058(8) 0.066(8) -0.007(7) 0.005(5) 0.004(5) C53 0.023(5) 0.041(7) 0.041(6) -0.005(5) 0.004(4) 0.001(5) C61 0.036(6) 0.083(10) 0.034(6) 0.007(6) -0.009(5) -0.004(6) C62 0.111(15) 0.20(2) 0.043(9) 0.053(12) -0.036(9) -0.087(16) C63 0.084(12) 0.24(3) 0.030(7) -0.059(12) -0.012(8) 0.075(15) C71 0.026(6) 0.049(8) 0.078(9) -0.007(7) 0.008(6) -0.004(5) C72 0.041(6) 0.043(7) 0.044(7) -0.007(5) 0.019(5) -0.014(5) C73 0.044(7) 0.053(8) 0.053(8) -0.022(6) -0.002(6) 0.001(6) C81 0.20(2) 0.022(7) 0.045(8) -0.006(6) -0.040(10) -0.041(10) C82 0.139(16) 0.056(10) 0.050(9) -0.029(8) 0.013(9) 0.000(10) C83 0.105(13) 0.063(10) 0.050(8) -0.027(7) -0.015(8) 0.011(9) C91 0.052(8) 0.100(12) 0.029(6) -0.009(7) -0.005(6) -0.005(8) C92 0.14(2) 0.39(5) 0.129(19) 0.18(3) -0.105(16) -0.21(3) C93 0.013(7) 0.41(5) 0.130(18) -0.17(2) -0.008(9) 0.019(14) C101 0.028(6) 0.066(9) 0.051(7) 0.019(6) 0.017(5) 0.000(6) C102 0.139(16) 0.093(13) 0.041(8) 0.018(8) 0.051(10) 0.030(12) C103 0.066(9) 0.062(10) 0.055(8) -0.016(7) -0.023(7) 0.025(7) C201 0.048(9) 0.092(13) 0.080(12) 0.045(10) 0.001(8) 0.011(8) C202 0.048(8) 0.051(9) 0.091(12) 0.007(8) 0.022(8) 0.019(7) C203 0.052(8) 0.097(13) 0.047(8) 0.002(8) -0.003(7) 0.002(8) C204 0.064(10) 0.095(13) 0.060(9) 0.034(9) 0.001(8) 0.033(9) C205 0.117(15) 0.049(10) 0.102(14) -0.009(10) 0.052(12) 0.016(10) C206 0.110(15) 0.122(17) 0.036(8) -0.005(10) 0.013(9) -0.006(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 S7 2.446(2) . ? W1 P1 2.462(3) . ? W1 P2 2.464(3) . ? W1 P3 2.464(3) . ? W1 S1 2.491(3) . ? W1 S2 2.568(3) . ? W2 S5 2.430(2) . ? W2 P6 2.431(3) . ? W2 P4 2.449(4) . ? W2 P5 2.463(3) . ? W2 S3 2.480(3) . ? W2 S4 2.577(3) . ? P1 C53 1.821(10) . ? P1 C52 1.832(11) . ? P1 C51 1.843(13) . ? P2 C63 1.804(16) . ? P2 C61 1.807(12) . ? P2 C62 1.832(18) . ? P3 C71 1.830(11) . ? P3 C72 1.834(12) . ? P3 C73 1.839(12) . ? P4 C81 1.799(13) . ? P4 C83 1.822(15) . ? P4 C82 1.824(17) . ? P5 C92 1.790(19) . ? P5 C93 1.79(2) . ? P5 C91 1.810(12) . ? P6 C103 1.817(13) . ? P6 C101 1.825(13) . ? P6 C102 1.834(13) . ? S1 C10 1.749(9) . ? S2 C20 1.752(9) . ? S3 C30 1.747(10) . ? S4 C40 1.741(10) . ? S5 C45 1.777(11) . ? S5 C31 1.801(10) . ? S6 C41 1.785(10) . ? S6 C15 1.794(10) . ? S7 C11 1.800(9) . ? S7 C25 1.801(11) . ? S8 C21 1.780(11) . ? S8 C35 1.787(10) . ? C10 C11 1.398(13) . ? C10 C15 1.411(13) . ? C11 C12 1.386(13) . ? C12 C13 1.380(13) . ? C13 C14 1.389(14) . ? C13 C16 1.524(14) . ? C14 C15 1.386(13) . ? C16 C17 1.52(2) . ? C16 C18 1.522(15) . ? C16 C19 1.54(2) . ? C20 C25 1.385(13) . ? C20 C21 1.411(14) . ? C21 C22 1.388(14) . ? C22 C23 1.417(14) . ? C23 C24 1.385(15) . ? C23 C26 1.548(14) . ? C24 C25 1.390(13) . ? C26 C27 1.42(2) . ? C26 C29 1.500(18) . ? C26 C28 1.53(2) . ? C30 C31 1.395(13) . ? C30 C35 1.418(13) . ? C31 C32 1.394(13) . ? C32 C33 1.381(14) . ? C33 C34 1.399(14) . ? C33 C36 1.541(13) . ? C34 C35 1.386(13) . ? C36 C38 1.515(17) . ? C36 C37 1.541(16) . ? C36 C39 1.543(16) . ? C40 C41 1.402(16) . ? C40 C45 1.421(14) . ? C41 C42 1.393(14) . ? C42 C43 1.395(14) . ? C43 C44 1.397(15) . ? C43 C46 1.520(14) . ? C44 C45 1.379(13) . ? C46 C47 1.494(17) . ? C46 C49 1.50(2) . ? C46 C48 1.53(2) . ? C201 C206 1.33(2) . ? C201 C202 1.35(2) . ? C202 C203 1.35(2) . ? C203 C204 1.34(2) . ? C204 C205 1.38(2) . ? C205 C206 1.35(2) . ? 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 S7 W1 P1 88.63(9) . . ? S7 W1 P2 156.99(9) . . ? P1 W1 P2 101.45(11) . . ? S7 W1 P3 97.81(9) . . ? P1 W1 P3 126.27(9) . . ? P2 W1 P3 92.81(11) . . ? S7 W1 S1 83.22(8) . . ? P1 W1 S1 76.03(9) . . ? P2 W1 S1 79.31(9) . . ? P3 W1 S1 157.62(10) . . ? S7 W1 S2 77.46(8) . . ? P1 W1 S2 154.19(9) . . ? P2 W1 S2 85.01(10) . . ? P3 W1 S2 77.69(9) . . ? S1 W1 S2 80.76(10) . . ? S5 W2 P6 98.85(10) . . ? S5 W2 P4 87.99(11) . . ? P6 W2 P4 122.54(13) . . ? S5 W2 P5 160.78(11) . . ? P6 W2 P5 90.81(14) . . ? P4 W2 P5 100.82(17) . . ? S5 W2 S3 83.97(9) . . ? P6 W2 S3 159.29(13) . . ? P4 W2 S3 77.92(15) . . ? P5 W2 S3 81.27(12) . . ? S5 W2 S4 79.04(9) . . ? P6 W2 S4 78.62(10) . . ? P4 W2 S4 156.97(12) . . ? P5 W2 S4 86.72(15) . . ? S3 W2 S4 81.82(13) . . ? C53 P1 C52 99.5(5) . . ? C53 P1 C51 101.4(6) . . ? C52 P1 C51 98.5(6) . . ? C53 P1 W1 115.2(4) . . ? C52 P1 W1 116.8(4) . . ? C51 P1 W1 121.7(5) . . ? C63 P2 C61 101.7(8) . . ? C63 P2 C62 100.8(11) . . ? C61 P2 C62 97.1(7) . . ? C63 P2 W1 115.5(5) . . ? C61 P2 W1 119.1(4) . . ? C62 P2 W1 119.1(6) . . ? C71 P3 C72 99.0(6) . . ? C71 P3 C73 100.8(6) . . ? C72 P3 C73 97.9(6) . . ? C71 P3 W1 114.3(4) . . ? C72 P3 W1 119.7(4) . . ? C73 P3 W1 121.1(5) . . ? C81 P4 C83 101.4(7) . . ? C81 P4 C82 99.3(8) . . ? C83 P4 C82 99.9(8) . . ? C81 P4 W2 121.7(7) . . ? C83 P4 W2 116.6(5) . . ? C82 P4 W2 114.4(5) . . ? C92 P5 C93 100.7(14) . . ? C92 P5 C91 97.6(10) . . ? C93 P5 C91 99.4(9) . . ? C92 P5 W2 118.7(7) . . ? C93 P5 W2 117.5(6) . . ? C91 P5 W2 119.0(5) . . ? C103 P6 C101 97.9(6) . . ? C103 P6 C102 100.0(7) . . ? C101 P6 C102 99.9(8) . . ? C103 P6 W2 122.4(6) . . ? C101 P6 W2 119.2(4) . . ? C102 P6 W2 113.5(6) . . ? C10 S1 W1 104.6(3) . . ? C20 S2 W1 105.5(3) . . ? C30 S3 W2 104.3(4) . . ? C40 S4 W2 105.1(4) . . ? C45 S5 C31 98.3(5) . . ? C45 S5 W2 106.9(3) . . ? C31 S5 W2 106.2(3) . . ? C41 S6 C15 99.1(4) . . ? C11 S7 C25 95.3(4) . . ? C11 S7 W1 106.3(3) . . ? C25 S7 W1 107.1(3) . . ? C21 S8 C35 100.4(4) . . ? C11 C10 C15 116.1(8) . . ? C11 C10 S1 123.8(7) . . ? C15 C10 S1 120.1(7) . . ? C12 C11 C10 122.3(8) . . ? C12 C11 S7 117.7(7) . . ? C10 C11 S7 120.0(7) . . ? C13 C12 C11 121.4(9) . . ? C12 C13 C14 116.8(9) . . ? C12 C13 C16 123.1(9) . . ? C14 C13 C16 120.1(9) . . ? C15 C14 C13 122.9(9) . . ? C14 C15 C10 120.3(9) . . ? C14 C15 S6 120.4(7) . . ? C10 C15 S6 119.3(7) . . ? C17 C16 C18 109.2(12) . . ? C17 C16 C13 108.5(11) . . ? C18 C16 C13 112.5(9) . . ? C17 C16 C19 111.7(12) . . ? C18 C16 C19 107.4(12) . . ? C13 C16 C19 107.6(11) . . ? C25 C20 C21 116.1(9) . . ? C25 C20 S2 121.3(7) . . ? C21 C20 S2 122.6(7) . . ? C22 C21 C20 121.1(10) . . ? C22 C21 S8 118.3(8) . . ? C20 C21 S8 120.6(7) . . ? C21 C22 C23 121.2(11) . . ? C24 C23 C22 116.8(9) . . ? C24 C23 C26 120.9(9) . . ? C22 C23 C26 122.3(10) . . ? C23 C24 C25 121.4(9) . . ? C20 C25 C24 122.5(9) . . ? C20 C25 S7 117.4(7) . . ? C24 C25 S7 120.1(8) . . ? C27 C26 C29 112.9(15) . . ? C27 C26 C28 108.9(16) . . ? C29 C26 C28 103.2(14) . . ? C27 C26 C23 113.0(11) . . ? C29 C26 C23 109.3(10) . . ? C28 C26 C23 108.9(10) . . ? C31 C30 C35 116.0(8) . . ? C31 C30 S3 123.8(8) . . ? C35 C30 S3 119.8(7) . . ? C32 C31 C30 123.5(9) . . ? C32 C31 S5 116.7(8) . . ? C30 C31 S5 119.9(7) . . ? C33 C32 C31 120.1(9) . . ? C32 C33 C34 117.1(9) . . ? C32 C33 C36 122.9(9) . . ? C34 C33 C36 119.7(9) . . ? C35 C34 C33 123.3(9) . . ? C34 C35 C30 119.6(9) . . ? C34 C35 S8 122.0(8) . . ? C30 C35 S8 118.4(7) . . ? C38 C36 C37 109.8(10) . . ? C38 C36 C33 108.8(9) . . ? C37 C36 C33 111.5(9) . . ? C38 C36 C39 108.5(10) . . ? C37 C36 C39 107.5(10) . . ? C33 C36 C39 110.8(9) . . ? C41 C40 C45 115.6(9) . . ? C41 C40 S4 123.6(8) . . ? C45 C40 S4 120.8(9) . . ? C42 C41 C40 120.2(9) . . ? C42 C41 S6 119.4(9) . . ? C40 C41 S6 120.4(7) . . ? C41 C42 C43 123.2(11) . . ? C42 C43 C44 115.5(9) . . ? C42 C43 C46 123.6(11) . . ? C44 C43 C46 120.8(9) . . ? C45 C44 C43 122.0(10) . . ? C44 C45 C40 121.6(10) . . ? C44 C45 S5 119.3(8) . . ? C40 C45 S5 119.0(8) . . ? C47 C46 C49 108.5(11) . . ? C47 C46 C43 111.0(11) . . ? C49 C46 C43 109.6(10) . . ? C47 C46 C48 107.9(15) . . ? C49 C46 C48 109.2(18) . . ? C43 C46 C48 110.7(11) . . ? C206 C201 C202 120.4(14) . . ? C203 C202 C201 119.5(14) . . ? C204 C203 C202 121.3(14) . . ? C203 C204 C205 118.5(14) . . ? C206 C205 C204 119.4(15) . . ? C201 C206 C205 120.6(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.593 _refine_diff_density_min -1.412 _refine_diff_density_rms 0.163