# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 # CCDC Number: 440/236 data_[WO2(L3)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H94 N4 O11 W2' _chemical_formula_weight 1367.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 20.712(4) _cell_length_b 14.805(3) _cell_length_c 21.362(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.50(3) _cell_angle_gamma 90.00 _cell_volume 6095(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 3.829 _exptl_absorpt_correction_type 'abscor' _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 1.075 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9327 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9327 _reflns_number_gt 8590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.1049P)^2^+0.2639P] 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 0.00000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9327 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _refine_ls_shift/su_max 1.360 _refine_ls_shift/su_mean 0.034 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.420511(4) 0.218703(7) 0.292546(4) 0.05605(3) Uani 1 1 d . . . W2 W 0.787760(4) 0.171532(7) 0.045816(4) 0.05861(3) Uani 1 1 d . . . N1 N 0.49011(10) 0.15165(14) 0.39051(8) 0.0634(6) Uani 1 1 d . . . N2 N 0.34317(9) 0.33635(13) 0.25183(9) 0.0611(6) Uani 1 1 d . . . N1' N 0.89957(9) 0.12842(15) 0.10877(9) 0.0664(6) Uani 1 1 d . . . N2' N 0.71363(10) 0.22463(15) -0.05673(9) 0.0665(7) Uani 1 1 d . . . O1 O 0.47240(7) 0.12249(11) 0.27362(7) 0.0622(5) Uani 1 1 d . . . O1' O 0.79147(7) 0.11522(12) 0.12845(8) 0.0670(5) Uani 1 1 d . . . O2 O 0.35971(8) 0.18893(13) 0.32858(8) 0.0714(5) Uani 1 1 d . . . O2' O 0.83096(9) 0.27264(12) 0.04498(9) 0.0761(6) Uani 1 1 d . . . O3 O 0.38192(8) 0.21620(11) 0.19635(7) 0.0613(5) Uani 1 1 d . . . O3' O 0.69870(8) 0.20154(12) 0.04932(7) 0.0643(5) Uani 1 1 d . . . O4 O 0.47364(8) 0.31101(13) 0.32930(8) 0.0691(5) Uani 1 1 d . . . O4' O 0.79789(8) 0.08985(13) -0.00818(8) 0.0709(6) Uani 1 1 d . . . O5 O 0.33128(13) 0.10299(17) 0.43922(11) 0.1170(9) Uani 1 1 d . . . O6 O 0.50140(11) 0.39958(16) 0.45203(10) 0.1000(8) Uani 1 1 d . . . O7 O 0.89012(9) -0.00774(16) -0.04828(9) 0.0893(7) Uani 1 1 d . . . C1 C 0.52927(11) 0.08211(18) 0.38731(11) 0.0648(7) Uani 1 1 d . . . C1' C 0.90998(12) 0.08018(18) 0.16397(12) 0.0682(8) Uani 1 1 d . . . C2 C 0.57253(13) 0.0384(2) 0.44505(12) 0.0766(9) Uani 1 1 d . . . H2 H 0.5987 -0.0115 0.4424 0.092 Uiso 1 1 calc R . . C2' C 0.97571(14) 0.0473(2) 0.19917(15) 0.0902(11) Uani 1 1 d . . . H2' H 0.9836 0.0135 0.2380 0.108 Uiso 1 1 calc R . . C3 C 0.57545(14) 0.0721(2) 0.50749(13) 0.0863(10) Uani 1 1 d . . . H3 H 0.6042 0.0446 0.5471 0.104 Uiso 1 1 calc R . . C3' C 1.02867(14) 0.0633(2) 0.17810(15) 0.1010(12) Uani 1 1 d . . . H3' H 1.0726 0.0402 0.2020 0.121 Uiso 1 1 calc R . . C4 C 0.53685(14) 0.1440(2) 0.51028(12) 0.0824(9) Uani 1 1 d . . . H4 H 0.5392 0.1669 0.5516 0.099 Uiso 1 1 calc R . . C4' C 1.01734(13) 0.1136(2) 0.12169(14) 0.0882(10) Uani 1 1 d . . . H4' H 1.0533 0.1259 0.1067 0.106 Uiso 1 1 calc R . . C5 C 0.49377(14) 0.1836(2) 0.45131(12) 0.0772(9) Uani 1 1 d . . . H5 H 0.4668 0.2329 0.4532 0.093 Uiso 1 1 calc R . . C5' C 0.95259(12) 0.1450(2) 0.08812(13) 0.0782(9) Uani 1 1 d . . . H5' H 0.9443 0.1792 0.0495 0.094 Uiso 1 1 calc R . . C6 C 0.31384(11) 0.34638(17) 0.18512(12) 0.0614(7) Uani 1 1 d . . . C6' C 0.65054(12) 0.24980(18) -0.06297(11) 0.0641(7) Uani 1 1 d . . . C7 C 0.27029(13) 0.41981(19) 0.15945(14) 0.0783(9) Uani 1 1 d . . . H7 H 0.2507 0.4291 0.1132 0.094 Uiso 1 1 calc R . . C7' C 0.60522(15) 0.2829(2) -0.12385(14) 0.0840(10) Uani 1 1 d . . . H7' H 0.5607 0.3005 -0.1281 0.101 Uiso 1 1 calc R . . C8' C 0.62589(17) 0.2901(2) -0.17888(15) 0.0988(12) Uani 1 1 d . . . H8' H 0.5957 0.3119 -0.2200 0.119 Uiso 1 1 calc R . . C8 C 0.25615(14) 0.4794(2) 0.20334(15) 0.0907(10) Uani 1 1 d . . . H8 H 0.2270 0.5285 0.1862 0.109 Uiso 1 1 calc R . . C9' C 0.69158(18) 0.2642(3) -0.17050(15) 0.1020(13) Uani 1 1 d . . . C9 C 0.28518(13) 0.4660(2) 0.27235(14) 0.0827(10) Uani 1 1 d . . . C10' C 0.73641(15) 0.2297(2) -0.10986(13) 0.0847(10) Uani 1 1 d . . . C10 C 0.33065(13) 0.39414(19) 0.29502(14) 0.0769(9) Uani 1 1 d . . . C11 C 0.52133(11) 0.05790(17) 0.31483(10) 0.0616(7) Uani 1 1 d . . . C11' C 0.84562(12) 0.07197(18) 0.18188(12) 0.0683(8) Uani 1 1 d . . . C12 C 0.48466(13) -0.03782(18) 0.29416(12) 0.0718(8) Uani 1 1 d . . . C12' C 0.82196(14) -0.0327(2) 0.17754(14) 0.0825(10) Uani 1 1 d . . . C13 C 0.4698(2) -0.0584(2) 0.22004(15) 0.1204(15) Uani 1 1 d . . . H13A H 0.4451 -0.0087 0.1929 0.181 Uiso 1 1 calc R . . H13B H 0.4422 -0.1122 0.2072 0.181 Uiso 1 1 calc R . . H13C H 0.5128 -0.0671 0.2135 0.181 Uiso 1 1 calc R . . C13' C 0.7501(2) -0.0423(3) 0.1789(3) 0.171(2) Uani 1 1 d . . . H13D H 0.7493 -0.0177 0.2202 0.256 Uiso 1 1 calc R . . H13E H 0.7376 -0.1050 0.1758 0.256 Uiso 1 1 calc R . . H13F H 0.7177 -0.0102 0.1415 0.256 Uiso 1 1 calc R . . C14 C 0.41368(14) -0.0331(2) 0.30261(16) 0.0959(11) Uani 1 1 d . . . H14A H 0.3872 0.0163 0.2766 0.144 Uiso 1 1 calc R . . H14B H 0.4209 -0.0242 0.3492 0.144 Uiso 1 1 calc R . . H14C H 0.3889 -0.0886 0.2872 0.144 Uiso 1 1 calc R . . C14' C 0.8706(2) -0.0959(2) 0.22998(17) 0.1268(17) Uani 1 1 d . . . H14D H 0.9165 -0.0912 0.2290 0.190 Uiso 1 1 calc R . . H14E H 0.8544 -0.1569 0.2202 0.190 Uiso 1 1 calc R . . H14F H 0.8717 -0.0794 0.2738 0.190 Uiso 1 1 calc R . . C15 C 0.52336(17) -0.1181(2) 0.33624(15) 0.0977(11) Uani 1 1 d . . . H15A H 0.5683 -0.1231 0.3332 0.147 Uiso 1 1 calc R . . H15B H 0.4975 -0.1724 0.3196 0.147 Uiso 1 1 calc R . . H15C H 0.5286 -0.1091 0.3823 0.147 Uiso 1 1 calc R . . C15' C 0.8185(2) -0.0716(2) 0.11084(16) 0.1313(18) Uani 1 1 d . . . H15D H 0.8633 -0.0668 0.1072 0.197 Uiso 1 1 calc R . . H15E H 0.7850 -0.0386 0.0748 0.197 Uiso 1 1 calc R . . H15F H 0.8051 -0.1339 0.1082 0.197 Uiso 1 1 calc R . . C16 C 0.58084(15) 0.0972(3) 0.22944(13) 0.1069(13) Uani 1 1 d . . . H16A H 0.5463 0.1434 0.2121 0.160 Uiso 1 1 calc R . . H16B H 0.5652 0.0425 0.2042 0.160 Uiso 1 1 calc R . . H16C H 0.6235 0.1165 0.2255 0.160 Uiso 1 1 calc R . . C16' C 0.8797(2) 0.2239(2) 0.23847(17) 0.1128(14) Uani 1 1 d . . . H16D H 0.8490 0.2497 0.1970 0.169 Uiso 1 1 calc R . . H16E H 0.9256 0.2195 0.2376 0.169 Uiso 1 1 calc R . . H16F H 0.8805 0.2617 0.2753 0.169 Uiso 1 1 calc R . . C17 C 0.62241(16) 0.1677(2) 0.34126(17) 0.1059(12) Uani 1 1 d . . . H17A H 0.5882 0.2146 0.3256 0.159 Uiso 1 1 calc R . . H17B H 0.6631 0.1845 0.3325 0.159 Uiso 1 1 calc R . . H17C H 0.6344 0.1593 0.3888 0.159 Uiso 1 1 calc R . . C17' C 0.90379(18) 0.0921(3) 0.31322(16) 0.1117(15) Uani 1 1 d . . . H17D H 0.9482 0.0819 0.3098 0.168 Uiso 1 1 calc R . . H17E H 0.8860 0.0361 0.3229 0.168 Uiso 1 1 calc R . . H17F H 0.9088 0.1345 0.3487 0.168 Uiso 1 1 calc R . . C18 C 0.64855(14) 0.0073(3) 0.33145(15) 0.1053(11) Uani 1 1 d . . . H18A H 0.6318 -0.0487 0.3086 0.158 Uiso 1 1 calc R . . H18B H 0.6592 -0.0005 0.3788 0.158 Uiso 1 1 calc R . . H18C H 0.6896 0.0254 0.3239 0.158 Uiso 1 1 calc R . . C18' C 0.78463(16) 0.1465(3) 0.25568(16) 0.1245(15) Uani 1 1 d . . . H18D H 0.7518 0.1705 0.2146 0.187 Uiso 1 1 calc R . . H18E H 0.7913 0.1889 0.2915 0.187 Uiso 1 1 calc R . . H18F H 0.7674 0.0906 0.2662 0.187 Uiso 1 1 calc R . . C19 C 0.59303(12) 0.0798(2) 0.30452(12) 0.0752(8) Uani 1 1 d . . . C19' C 0.85387(13) 0.1297(2) 0.24727(13) 0.0773(9) Uani 1 1 d . . . C20 C 0.33378(12) 0.27224(17) 0.14550(11) 0.0625(7) Uani 1 1 d . . . C20' C 0.63627(11) 0.23556(18) 0.00166(11) 0.0640(7) Uani 1 1 d . . . C21 C 0.26782(13) 0.21006(18) 0.10916(13) 0.0685(8) Uani 1 1 d . . . C21' C 0.62481(15) 0.3295(2) 0.03181(14) 0.0828(10) Uani 1 1 d . . . C22 C 0.22884(15) 0.1961(2) 0.15767(15) 0.0906(11) Uani 1 1 d . . . H22A H 0.2136 0.2535 0.1681 0.136 Uiso 1 1 calc R . . H22B H 0.2593 0.1683 0.1984 0.136 Uiso 1 1 calc R . . H22C H 0.1893 0.1579 0.1368 0.136 Uiso 1 1 calc R . . C22' C 0.68408(19) 0.3918(2) 0.03197(18) 0.1113(14) Uani 1 1 d . . . H22D H 0.7278 0.3633 0.0560 0.167 Uiso 1 1 calc R . . H22E H 0.6814 0.4479 0.0535 0.167 Uiso 1 1 calc R . . H22F H 0.6801 0.4034 -0.0135 0.167 Uiso 1 1 calc R . . C23 C 0.21622(16) 0.2473(3) 0.04315(15) 0.0972(12) Uani 1 1 d . . . H23A H 0.2025 0.3071 0.0503 0.146 Uiso 1 1 calc R . . H23B H 0.1761 0.2089 0.0274 0.146 Uiso 1 1 calc R . . H23C H 0.2376 0.2491 0.0102 0.146 Uiso 1 1 calc R . . C23' C 0.6310(2) 0.3192(3) 0.10521(16) 0.1408(17) Uani 1 1 d . . . H23D H 0.6742 0.2902 0.1306 0.211 Uiso 1 1 calc R . . H23E H 0.5932 0.2832 0.1070 0.211 Uiso 1 1 calc R . . H23F H 0.6295 0.3777 0.1240 0.211 Uiso 1 1 calc R . . C24 C 0.28945(16) 0.1150(2) 0.09602(16) 0.0988(12) Uani 1 1 d . . . H24A H 0.3222 0.0906 0.1370 0.148 Uiso 1 1 calc R . . H24B H 0.3104 0.1181 0.0628 0.148 Uiso 1 1 calc R . . H24C H 0.2493 0.0767 0.0800 0.148 Uiso 1 1 calc R . . C24' C 0.55579(18) 0.3772(3) -0.0083(2) 0.1396(17) Uani 1 1 d . . . H24D H 0.5177 0.3400 -0.0088 0.209 Uiso 1 1 calc R . . H24E H 0.5530 0.3873 -0.0537 0.209 Uiso 1 1 calc R . . H24F H 0.5537 0.4341 0.0124 0.209 Uiso 1 1 calc R . . C25' C 0.60881(15) 0.0725(2) -0.03496(15) 0.0889(11) Uani 1 1 d . . . H25A H 0.6552 0.0595 -0.0047 0.133 Uiso 1 1 calc R . . H25B H 0.6090 0.0839 -0.0791 0.133 Uiso 1 1 calc R . . H25C H 0.5793 0.0219 -0.0366 0.133 Uiso 1 1 calc R . . C25 C 0.40419(17) 0.2391(3) 0.07188(16) 0.1174(13) Uani 1 1 d . . . H25D H 0.3658 0.2061 0.0411 0.176 Uiso 1 1 calc R . . H25E H 0.4334 0.1988 0.1056 0.176 Uiso 1 1 calc R . . H25F H 0.4304 0.2659 0.0478 0.176 Uiso 1 1 calc R . . C26' C 0.50793(14) 0.1741(3) -0.06099(16) 0.0989(13) Uani 1 1 d . . . H26A H 0.4887 0.2263 -0.0476 0.148 Uiso 1 1 calc R . . H26B H 0.4793 0.1225 -0.0627 0.148 Uiso 1 1 calc R . . H26C H 0.5099 0.1843 -0.1046 0.148 Uiso 1 1 calc R . . C26 C 0.33847(17) 0.3808(3) 0.04899(16) 0.1172(13) Uani 1 1 d . . . H26D H 0.3199 0.4287 0.0676 0.176 Uiso 1 1 calc R . . H26E H 0.3013 0.3505 0.0145 0.176 Uiso 1 1 calc R . . H26F H 0.3701 0.4054 0.0300 0.176 Uiso 1 1 calc R . . C27' C 0.57437(15) 0.1282(3) 0.05773(14) 0.1070(13) Uani 1 1 d . . . H27A H 0.5570 0.1781 0.0756 0.161 Uiso 1 1 calc R . . H27B H 0.6190 0.1105 0.0894 0.161 Uiso 1 1 calc R . . H27C H 0.5428 0.0782 0.0497 0.161 Uiso 1 1 calc R . . C27 C 0.44059(16) 0.3606(3) 0.15336(16) 0.1247(14) Uani 1 1 d . . . H27D H 0.4261 0.4088 0.1753 0.187 Uiso 1 1 calc R . . H27E H 0.4673 0.3848 0.1288 0.187 Uiso 1 1 calc R . . H27F H 0.4685 0.3186 0.1865 0.187 Uiso 1 1 calc R . . C28' C 0.58136(12) 0.1569(2) -0.00987(12) 0.0731(9) Uani 1 1 d . . . C28 C 0.37736(14) 0.3125(2) 0.10523(14) 0.0817(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.05391(4) 0.05881(6) 0.05907(4) -0.00179(3) 0.02499(3) 0.00296(4) W2 0.05294(4) 0.06270(6) 0.06290(4) 0.00360(4) 0.02443(3) 0.00076(4) N1 0.0686(10) 0.0659(11) 0.0582(9) -0.0075(8) 0.0261(7) -0.0003(10) N2 0.0542(8) 0.0563(11) 0.0780(10) -0.0020(8) 0.0304(7) 0.0032(8) N1' 0.0509(8) 0.0794(13) 0.0709(10) -0.0089(9) 0.0247(7) -0.0059(9) N2' 0.0644(10) 0.0758(14) 0.0621(9) 0.0046(9) 0.0264(7) 0.0014(9) O1 0.0651(7) 0.0637(9) 0.0590(7) 0.0006(7) 0.0242(6) 0.0141(7) O1' 0.0510(7) 0.0728(10) 0.0814(8) 0.0170(8) 0.0294(6) 0.0072(7) O2 0.0661(8) 0.0725(10) 0.0851(9) 0.0002(8) 0.0388(6) 0.0072(8) O2' 0.0722(9) 0.0742(11) 0.0801(10) 0.0064(8) 0.0258(7) -0.0138(8) O3 0.0576(7) 0.0598(9) 0.0666(8) -0.0019(7) 0.0231(6) 0.0096(7) O3' 0.0578(7) 0.0769(10) 0.0602(7) 0.0011(7) 0.0241(6) 0.0057(8) O4 0.0638(8) 0.0730(10) 0.0716(8) -0.0077(8) 0.0261(6) 0.0003(8) O4' 0.0602(8) 0.0801(11) 0.0733(8) -0.0022(8) 0.0254(6) 0.0073(8) O5 0.1531(17) 0.0942(15) 0.1088(13) 0.0051(12) 0.0539(11) 0.0284(14) O6 0.1158(13) 0.0940(14) 0.0987(11) -0.0204(10) 0.0492(9) -0.0110(12) O7 0.0794(9) 0.1042(15) 0.0910(10) -0.0060(10) 0.0393(7) 0.0099(10) C1 0.0576(10) 0.0738(15) 0.0652(11) 0.0028(11) 0.0252(8) -0.0057(11) C1' 0.0556(11) 0.0688(15) 0.0765(13) -0.0043(12) 0.0196(10) 0.0025(11) C2 0.0696(13) 0.0852(18) 0.0733(13) 0.0149(12) 0.0244(10) 0.0096(13) C2' 0.0685(14) 0.102(2) 0.0924(17) 0.0089(16) 0.0203(12) 0.0192(15) C3 0.0806(15) 0.109(2) 0.0608(13) 0.0053(14) 0.0160(11) -0.0124(16) C3' 0.0603(14) 0.119(2) 0.1130(19) -0.0359(17) 0.0198(13) 0.0167(15) C4 0.0971(16) 0.0915(19) 0.0630(12) -0.0104(13) 0.0345(11) -0.0104(16) C4' 0.0644(12) 0.102(2) 0.1090(16) -0.0244(15) 0.0440(10) -0.0055(14) C5 0.0880(14) 0.0828(18) 0.0703(12) -0.0043(12) 0.0403(10) -0.0026(14) C5' 0.0555(11) 0.0961(19) 0.0879(14) -0.0156(14) 0.0319(10) -0.0050(13) C6 0.0504(10) 0.0584(13) 0.0752(12) 0.0056(11) 0.0227(9) 0.0006(10) C6' 0.0682(11) 0.0672(14) 0.0594(11) 0.0045(10) 0.0264(8) 0.0041(12) C7 0.0686(13) 0.0714(17) 0.0895(15) 0.0071(13) 0.0227(11) 0.0122(13) C7' 0.0774(15) 0.086(2) 0.0810(16) 0.0192(13) 0.0206(12) 0.0142(14) C8' 0.100(2) 0.116(2) 0.0734(15) 0.0309(14) 0.0233(14) 0.0033(19) C8 0.0803(14) 0.0636(16) 0.135(2) 0.0045(16) 0.0471(13) 0.0179(13) C9' 0.112(2) 0.120(3) 0.0736(15) 0.0119(16) 0.0322(14) -0.010(2) C9 0.0698(13) 0.0752(17) 0.1079(17) -0.0096(14) 0.0384(11) 0.0058(13) C10' 0.0955(16) 0.098(2) 0.0665(12) 0.0091(13) 0.0364(11) -0.0080(16) C10 0.0677(12) 0.0701(16) 0.1001(14) -0.0172(13) 0.0392(10) 0.0025(12) C11 0.0664(11) 0.0646(14) 0.0582(10) 0.0053(10) 0.0280(8) 0.0078(11) C11' 0.0583(11) 0.0696(15) 0.0781(12) 0.0118(11) 0.0263(9) 0.0071(11) C12 0.0794(13) 0.0621(15) 0.0780(13) -0.0041(11) 0.0338(10) 0.0032(12) C12' 0.0775(15) 0.0739(17) 0.0931(15) 0.0135(14) 0.0278(12) -0.0011(14) C13 0.171(3) 0.098(2) 0.0927(18) -0.0251(17) 0.0485(18) -0.013(2) C13' 0.141(2) 0.092(3) 0.308(5) 0.020(3) 0.114(3) -0.028(2) C14 0.0729(14) 0.085(2) 0.133(2) -0.0134(18) 0.0421(14) -0.0136(15) C14' 0.186(4) 0.075(2) 0.093(2) 0.0221(16) 0.019(2) 0.008(2) C15 0.1094(18) 0.0747(19) 0.1174(19) 0.0129(16) 0.0516(14) 0.0195(17) C15' 0.210(4) 0.074(2) 0.090(2) -0.0137(17) 0.033(2) -0.033(2) C16 0.0995(16) 0.154(3) 0.0862(13) 0.0305(17) 0.0560(11) 0.020(2) C16' 0.161(3) 0.086(2) 0.1071(18) -0.0163(16) 0.0677(16) -0.007(2) C17 0.0864(15) 0.114(3) 0.134(2) 0.0139(18) 0.0607(13) -0.0134(17) C17' 0.115(2) 0.106(3) 0.087(2) -0.0077(18) 0.0053(18) 0.005(2) C18 0.0848(14) 0.119(2) 0.1303(18) 0.0412(18) 0.0607(12) 0.0372(16) C18' 0.0937(17) 0.184(4) 0.1138(18) -0.041(2) 0.0586(13) -0.018(2) C19 0.0669(11) 0.0871(18) 0.0820(12) 0.0161(12) 0.0396(9) 0.0106(13) C19' 0.0654(12) 0.095(2) 0.0757(13) 0.0044(13) 0.0311(10) -0.0025(14) C20 0.0602(11) 0.0675(15) 0.0617(11) 0.0022(10) 0.0245(8) 0.0041(11) C20' 0.0551(10) 0.0731(15) 0.0663(11) 0.0081(11) 0.0252(8) 0.0143(11) C21 0.0621(12) 0.0646(15) 0.0746(13) 0.0009(11) 0.0204(10) 0.0045(11) C21' 0.0781(15) 0.0793(18) 0.0861(16) -0.0078(13) 0.0243(12) 0.0153(14) C22 0.0800(15) 0.096(2) 0.0991(17) -0.0067(16) 0.0367(12) -0.0241(15) C22' 0.121(2) 0.074(2) 0.125(2) -0.0148(18) 0.0278(19) 0.009(2) C23 0.0811(18) 0.103(2) 0.0856(19) 0.0019(17) 0.0045(15) -0.0066(19) C23' 0.200(3) 0.140(3) 0.0951(17) -0.0188(19) 0.0702(18) 0.041(3) C24 0.0931(19) 0.086(2) 0.108(2) -0.0291(16) 0.0251(15) -0.0001(17) C24' 0.118(2) 0.118(3) 0.157(3) -0.017(2) 0.020(2) 0.0645(19) C25' 0.0814(16) 0.0802(19) 0.1027(18) -0.0056(16) 0.0308(13) -0.0110(15) C25 0.1234(17) 0.140(3) 0.1249(16) 0.0040(19) 0.0881(12) 0.012(2) C26' 0.0646(15) 0.124(3) 0.0977(19) 0.0109(18) 0.0171(14) 0.0121(17) C26 0.1062(19) 0.135(3) 0.1208(18) 0.0563(17) 0.0538(14) 0.009(2) C27' 0.0979(16) 0.146(3) 0.0925(15) 0.0107(18) 0.0531(12) -0.019(2) C27 0.1081(16) 0.163(3) 0.121(2) -0.020(2) 0.0622(14) -0.0670(19) C28' 0.0532(11) 0.0919(18) 0.0752(13) 0.0107(13) 0.0247(9) 0.0070(12) C28 0.0716(13) 0.097(2) 0.0829(14) 0.0107(14) 0.0361(10) 0.0045(15) _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 O4 1.7498(18) . ? W1 O2 1.756(2) . ? W1 O3 1.9129(16) . ? W1 O1 1.9147(17) . ? W1 N1 2.2873(18) . ? W1 N2 2.3098(19) . ? W2 O4' 1.7363(18) . ? W2 O2' 1.7474(19) . ? W2 O3' 1.9253(17) . ? W2 O1' 1.9281(17) . ? W2 N2' 2.3040(19) . ? W2 N1' 2.3013(18) . ? N1 C1 1.328(3) . ? N1 C5 1.358(3) . ? N2 C6 1.337(3) . ? N2 C10 1.351(4) . ? N1' C1' 1.327(3) . ? N1' C5' 1.348(4) . ? N2' C6' 1.318(3) . ? N2' C10' 1.382(4) . ? O1 C11 1.436(3) . ? O1' C11' 1.426(3) . ? O3 C20 1.438(3) . ? O3' C20' 1.413(3) . ? C1 C2 1.390(3) . ? C1 C11 1.538(3) . ? C1' C2' 1.381(3) . ? C1' C11' 1.520(4) . ? C2 C3 1.405(4) . ? C2' C3' 1.351(5) . ? C3 C4 1.346(5) . ? C3' C4' 1.361(5) . ? C4 C5 1.379(3) . ? C4' C5' 1.351(3) . ? C6 C7 1.391(4) . ? C6 C20 1.532(4) . ? C6' C7' 1.385(3) . ? C6' C20' 1.529(4) . ? C7 C8 1.394(5) . ? C7' C8' 1.395(5) . ? C8' C9' 1.361(5) . ? C8 C9 1.387(4) . ? C9' C10' 1.385(4) . ? C9 C10 1.385(4) . ? C11 C12 1.592(4) . ? C11 C19 1.612(4) . ? C11' C19' 1.592(4) . ? C11' C12' 1.617(4) . ? C12 C15 1.528(4) . ? C12 C13 1.529(4) . ? C12 C14 1.547(4) . ? C12' C13' 1.506(5) . ? C12' C15' 1.514(5) . ? C12' C14' 1.523(4) . ? C16 C19 1.551(4) . ? C16' C19' 1.530(5) . ? C17 C19 1.526(4) . ? C17' C19' 1.515(4) . ? C18 C19 1.523(4) . ? C18' C19' 1.530(4) . ? C20 C28 1.574(4) . ? C20 C21 1.593(3) . ? C20' C28' 1.583(4) . ? C20' C21' 1.587(4) . ? C21 C23 1.526(4) . ? C21 C22 1.543(5) . ? C21 C24 1.534(4) . ? C21' C22' 1.534(5) . ? C21' C23' 1.533(5) . ? C21' C24' 1.542(4) . ? C25' C28' 1.547(4) . ? C25 C28 1.512(5) . ? C26' C28' 1.534(3) . ? C26 C28 1.551(4) . ? C27' C28' 1.562(4) . ? C27 C28 1.514(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 W1 O2 115.69(9) . . ? O4 W1 O3 116.34(8) . . ? O2 W1 O3 112.44(7) . . ? O4 W1 O1 111.49(8) . . ? O2 W1 O1 117.01(8) . . ? O3 W1 O1 78.73(6) . . ? O4 W1 N1 81.17(8) . . ? O2 W1 N1 78.62(8) . . ? O3 W1 N1 148.16(7) . . ? O1 W1 N1 69.88(7) . . ? O4 W1 N2 79.36(7) . . ? O2 W1 N2 81.06(8) . . ? O3 W1 N2 69.58(7) . . ? O1 W1 N2 147.88(7) . . ? N1 W1 N2 142.13(7) . . ? O4' W2 O2' 113.76(9) . . ? O4' W2 O3' 122.50(7) . . ? O2' W2 O3' 107.71(8) . . ? O4' W2 O1' 109.46(8) . . ? O2' W2 O1' 122.07(8) . . ? O3' W2 O1' 77.37(7) . . ? O4' W2 N2' 78.85(8) . . ? O2' W2 N2' 82.15(8) . . ? O3' W2 N2' 69.15(8) . . ? O1' W2 N2' 143.80(7) . . ? O4' W2 N1' 81.62(7) . . ? O2' W2 N1' 80.46(8) . . ? O3' W2 N1' 144.54(7) . . ? O1' W2 N1' 69.59(7) . . ? N2' W2 N1' 145.84(8) . . ? C1 N1 C5 119.86(19) . . ? C1 N1 W1 118.79(15) . . ? C5 N1 W1 121.31(17) . . ? C6 N2 C10 122.1(2) . . ? C6 N2 W1 117.81(16) . . ? C10 N2 W1 120.04(15) . . ? C1' N1' C5' 120.2(2) . . ? C1' N1' W2 118.00(16) . . ? C5' N1' W2 121.63(16) . . ? C6' N2' C10' 121.7(2) . . ? C6' N2' W2 118.90(17) . . ? C10' N2' W2 119.35(16) . . ? C11 O1 W1 133.67(14) . . ? C11' O1' W2 133.06(16) . . ? C20 O3 W1 134.52(15) . . ? C20' O3' W2 133.70(15) . . ? N1 C1 C2 121.5(2) . . ? N1 C1 C11 112.98(18) . . ? C2 C1 C11 125.5(2) . . ? N1' C1' C2' 118.7(3) . . ? N1' C1' C11' 113.25(19) . . ? C2' C1' C11' 128.0(3) . . ? C1 C2 C3 117.8(3) . . ? C3' C2' C1' 121.0(3) . . ? C4 C3 C2 120.2(2) . . ? C2' C3' C4' 119.6(3) . . ? C3 C4 C5 119.4(3) . . ? C3' C4' C5' 118.3(3) . . ? N1 C5 C4 121.1(3) . . ? N1' C5' C4' 122.2(3) . . ? N2 C6 C7 118.9(2) . . ? N2 C6 C20 113.6(2) . . ? C7 C6 C20 127.5(2) . . ? N2' C6' C7' 120.1(3) . . ? N2' C6' C20' 112.48(19) . . ? C7' C6' C20' 127.4(2) . . ? C8 C7 C6 119.7(3) . . ? C6' C7' C8' 120.4(3) . . ? C9' C8' C7' 117.9(3) . . ? C9 C8 C7 120.5(3) . . ? C8' C9' C10' 121.5(3) . . ? C10 C9 C8 117.1(3) . . ? N2' C10' C9' 118.3(3) . . ? N2 C10 C9 121.6(2) . . ? O1 C11 C1 104.65(19) . . ? O1 C11 C12 105.37(16) . . ? C1 C11 C12 110.5(2) . . ? O1 C11 C19 105.13(19) . . ? C1 C11 C19 109.07(17) . . ? C12 C11 C19 120.7(2) . . ? O1' C11' C1' 105.5(2) . . ? O1' C11' C19' 105.1(2) . . ? C1' C11' C19' 110.8(2) . . ? O1' C11' C12' 104.56(17) . . ? C1' C11' C12' 109.7(2) . . ? C19' C11' C12' 119.8(2) . . ? C15 C12 C13 108.5(3) . . ? C15 C12 C14 106.4(3) . . ? C13 C12 C14 106.9(2) . . ? C15 C12 C11 115.79(19) . . ? C13 C12 C11 111.0(2) . . ? C14 C12 C11 107.8(2) . . ? C13' C12' C15' 106.0(3) . . ? C13' C12' C14' 108.7(3) . . ? C15' C12' C14' 104.4(3) . . ? C13' C12' C11' 111.7(3) . . ? C15' C12' C11' 109.1(3) . . ? C14' C12' C11' 116.2(2) . . ? C18 C19 C17 107.6(2) . . ? C18 C19 C16 108.8(3) . . ? C17 C19 C16 105.8(3) . . ? C18 C19 C11 114.4(2) . . ? C17 C19 C11 108.3(2) . . ? C16 C19 C11 111.46(18) . . ? C17' C19' C18' 107.5(3) . . ? C17' C19' C16' 107.4(2) . . ? C18' C19' C16' 104.5(3) . . ? C17' C19' C11' 115.8(3) . . ? C18' C19' C11' 112.7(2) . . ? C16' C19' C11' 108.1(2) . . ? O3 C20 C6 104.40(18) . . ? O3 C20 C28 104.68(19) . . ? C6 C20 C28 110.8(2) . . ? O3 C20 C21 105.54(19) . . ? C6 C20 C21 109.1(2) . . ? C28 C20 C21 120.9(2) . . ? O3' C20' C6' 105.73(19) . . ? O3' C20' C28' 105.4(2) . . ? C6' C20' C28' 109.06(19) . . ? O3' C20' C21' 104.69(18) . . ? C6' C20' C21' 110.7(2) . . ? C28' C20' C21' 120.2(2) . . ? C23 C21 C22 107.9(2) . . ? C23 C21 C24 108.3(2) . . ? C22 C21 C24 105.1(3) . . ? C23 C21 C20 115.3(2) . . ? C22 C21 C20 108.4(2) . . ? C24 C21 C20 111.3(2) . . ? C22' C21' C23' 106.9(3) . . ? C22' C21' C24' 107.7(3) . . ? C23' C21' C24' 109.1(3) . . ? C22' C21' C20' 106.8(3) . . ? C23' C21' C20' 111.0(3) . . ? C24' C21' C20' 114.9(2) . . ? C26' C28' C25' 106.4(2) . . ? C26' C28' C27' 107.4(2) . . ? C25' C28' C27' 105.7(3) . . ? C26' C28' C20' 117.2(2) . . ? C25' C28' C20' 108.3(2) . . ? C27' C28' C20' 111.2(2) . . ? C25 C28 C27 106.4(3) . . ? C25 C28 C26 106.2(3) . . ? C27 C28 C26 107.1(3) . . ? C25 C28 C20 111.6(3) . . ? C27 C28 C20 109.5(2) . . ? C26 C28 C20 115.5(2) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 1.166 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.117 #===END data_[WO2(L4)2] _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H42 N4 O6 W' _chemical_formula_weight 882.65 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.467(3) _cell_length_b 24.756(5) _cell_length_c 11.723(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.04(3) _cell_angle_gamma 90.00 _cell_volume 3848.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used IP _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description PRISM _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method ? _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 3.054 _exptl_absorpt_correction_type SEMI-EMPIRICAL _exptl_absorpt_correction_T_min 0.814 _exptl_absorpt_correction_T_max 1.114 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device RAX-IIC _diffrn_measurement_method IP _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6301 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.58 _reflns_number_total 6301 _reflns_number_observed 5295 _reflns_observed_criterion >2sigma(I) _computing_data_collection BIOTEX _computing_cell_refinement BIOTEX _computing_data_reduction BIOTEX _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXT _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6301 _refine_ls_number_parameters 461 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_obs 0.0531 _refine_ls_wR_factor_all 0.1639 _refine_ls_wR_factor_obs 0.1487 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.058 _refine_ls_shift/esd_max -0.019 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.166313(8) 0.398484(4) 0.820040(9) 0.05267(3) Uani 1 d . . O1 O 0.2653(2) 0.37571(9) 0.7565(2) 0.0688(6) Uani 1 d . . O2 O 0.1446(2) 0.46431(7) 0.7718(2) 0.0685(7) Uani 1 d . . O3 O 0.06690(14) 0.35561(7) 0.71950(14) 0.0541(5) Uani 1 d . . O4 O 0.22799(14) 0.41974(7) 0.97462(15) 0.0572(6) Uani 1 d . . N1 N 0.0152(2) 0.40235(7) 0.8926(2) 0.0513(6) Uani 1 d . . N2 N 0.1894(2) 0.32010(8) 0.9357(2) 0.0540(7) Uani 1 d . . C1 C -0.0388(2) 0.35263(10) 0.7183(2) 0.0546(8) Uani 1 d . . C2 C -0.0657(2) 0.29223(10) 0.7176(2) 0.0522(8) Uani 1 d . . C3 C -0.0420(2) 0.26090(11) 0.6256(2) 0.0647(9) Uani 1 d . . H3A H -0.0137(2) 0.27704(11) 0.5672(2) 0.078 Uiso 1 calc R . C4 C -0.0614(3) 0.20558(12) 0.6226(3) 0.0791(11) Uani 1 d . . H4A H -0.0470(3) 0.18513(12) 0.5610(3) 0.095 Uiso 1 calc R . C5 C -0.1019(3) 0.18030(11) 0.7107(3) 0.0755(11) Uani 1 d . . H5A H -0.1137(3) 0.14327(11) 0.7083(3) 0.091 Uiso 1 calc R . C6 C -0.1241(3) 0.21068(12) 0.8003(3) 0.0808(12) Uani 1 d . . H6A H -0.1510(3) 0.19415(12) 0.8594(3) 0.097 Uiso 1 calc R . C7 C -0.1069(2) 0.26635(12) 0.8039(2) 0.0690(10) Uani 1 d . . H7A H -0.1232(2) 0.28648(12) 0.8650(2) 0.083 Uiso 1 calc R . C8 C -0.0952(2) 0.37946(11) 0.6050(2) 0.0537(8) Uani 1 d . . C9 C -0.1966(2) 0.36794(12) 0.5660(2) 0.0679(10) Uani 1 d . . H9A H -0.2295(2) 0.34280(12) 0.6053(2) 0.081 Uiso 1 calc R . C10 C -0.2490(3) 0.39399(12) 0.4684(3) 0.0772(11) Uani 1 d . . H10A H -0.3175(3) 0.38747(12) 0.4444(3) 0.093 Uiso 1 calc R . C11 C -0.1989(3) 0.42955(12) 0.4076(2) 0.0725(10) Uani 1 d . . H11A H -0.2335(3) 0.44641(12) 0.3415(2) 0.087 Uiso 1 calc R . C12 C -0.0991(2) 0.44004(12) 0.4437(2) 0.0664(9) Uani 1 d . . H12A H -0.0654(2) 0.46372(12) 0.4021(2) 0.080 Uiso 1 calc R . C13 C -0.0480(2) 0.41509(11) 0.5432(2) 0.0598(9) Uani 1 d . . H13A H 0.0198(2) 0.42286(11) 0.5682(2) 0.072 Uiso 1 calc R . C14 C -0.0655(2) 0.38290(10) 0.8221(2) 0.0502(7) Uani 1 d . . C15 C -0.1622(2) 0.39128(11) 0.8431(2) 0.0613(9) Uani 1 d . . H15A H -0.2177(2) 0.37801(11) 0.7925(2) 0.074 Uiso 1 calc R . C16 C -0.1746(2) 0.41970(12) 0.9408(2) 0.0650(9) Uani 1 d . . H16A H -0.2389(2) 0.42525(12) 0.9571(2) 0.078 Uiso 1 calc R . C17 C -0.0933(2) 0.43959(11) 1.0131(2) 0.0637(9) Uani 1 d . . H17A H -0.1012(2) 0.45901(11) 1.0789(2) 0.076 Uiso 1 calc R . C18 C 0.0012(2) 0.43049(10) 0.9875(2) 0.0601(9) Uani 1 d . . H18A H 0.0571(2) 0.44411(10) 1.0369(2) 0.072 Uiso 1 calc R . C19 C 0.2714(2) 0.38570(11) 1.0721(2) 0.0606(9) Uani 1 d . . C20 C 0.2306(2) 0.40767(10) 1.1758(2) 0.0572(8) Uani 1 d . . C21 C 0.1599(2) 0.38255(12) 1.2250(2) 0.0670(10) Uani 1 d . . H21A H 0.1379(2) 0.34831(12) 1.1994(2) 0.080 Uiso 1 calc R . C22 C 0.1193(3) 0.40678(13) 1.3130(3) 0.0817(12) Uani 1 d . . H22A H 0.0688(3) 0.38920(13) 1.3435(3) 0.098 Uiso 1 calc R . C23 C 0.1524(3) 0.45589(13) 1.3553(3) 0.0774(11) Uani 1 d . . H23A H 0.1275(3) 0.47102(13) 1.4173(3) 0.093 Uiso 1 calc R . C24 C 0.2234(3) 0.48309(13) 1.3052(3) 0.0845(12) Uani 1 d . . H24A H 0.2446(3) 0.51739(13) 1.3311(3) 0.101 Uiso 1 calc R . C25 C 0.2631(3) 0.45899(12) 1.2156(3) 0.0734(11) Uani 1 d . . H25A H 0.3114(3) 0.47708(12) 1.1823(3) 0.088 Uiso 1 calc R . C26 C 0.3867(2) 0.39054(13) 1.0865(3) 0.0748(11) Uani 1 d . . C27 C 0.4313(3) 0.4152(2) 1.0019(4) 0.126(2) Uani 1 d . . H27A H 0.3921(3) 0.4292(2) 0.9352(4) 0.151 Uiso 1 calc R . C28 C 0.5365(4) 0.4186(3) 1.0193(4) 0.174(3) Uani 1 d . . H28A H 0.5670(4) 0.4356(3) 0.9636(4) 0.208 Uiso 1 calc R . C29 C 0.5984(3) 0.3969(2) 1.1195(4) 0.154(3) Uani 1 d . . H29A H 0.6683(3) 0.3986(2) 1.1283(4) 0.185 Uiso 1 calc R . C30 C 0.5525(3) 0.3736(2) 1.2030(4) 0.134(2) Uani 1 d . . H30A H 0.5915(3) 0.3597(2) 1.2698(4) 0.161 Uiso 1 calc R . C31 C 0.4462(3) 0.3705(2) 1.1878(3) 0.1012(15) Uani 1 d . . H31A H 0.4156(3) 0.3552(2) 1.2453(3) 0.121 Uiso 1 calc R . C32 C 0.2407(2) 0.32819(11) 1.0446(2) 0.0581(8) Uani 1 d . . C33 C 0.2628(3) 0.28439(12) 1.1181(2) 0.0719(10) Uani 1 d . . H33A H 0.2967(3) 0.29023(12) 1.1932(2) 0.086 Uiso 1 calc R . C34 C 0.2362(3) 0.23225(13) 1.0832(3) 0.0807(12) Uani 1 d . . H34A H 0.2514(3) 0.20296(13) 1.1329(3) 0.097 Uiso 1 calc R . C35 C 0.1861(3) 0.22591(11) 0.9712(3) 0.0766(11) Uani 1 d . . H35A H 0.1680(3) 0.19133(11) 0.9442(3) 0.092 Uiso 1 calc R . C36 C 0.1620(2) 0.26891(10) 0.8982(3) 0.0611(9) Uani 1 d . . H36A H 0.1271(2) 0.26342(10) 0.8234(3) 0.073 Uiso 1 calc R . O5 O -0.3942(2) 0.42200(12) 0.7490(2) 0.163(2) Uani 1 d D . N3 N -0.54042(11) 0.43416(6) 0.62300(14) 0.1219(15) Uani 1 d D . C37 C -0.45068(12) 0.40303(9) 0.6648(2) 0.1604(13) Uani 1 d D . C38 C -0.6019(2) 0.40464(12) 0.5297(2) 0.177(2) Uani 1 d D . C39 C -0.5697(3) 0.48188(8) 0.6805(3) 0.1795(15) Uani 1 d D . O6 O 0.58805(15) 0.28071(14) 1.5577(2) 0.1903(4) Uani 1 d D . N4 N 0.53898(9) 0.23149(8) 1.40225(15) 0.156(2) Uani 1 d D . C40 C 0.51200(13) 0.26588(9) 1.4908(2) 0.1783(5) Uani 1 d D . C41 C 0.64664(11) 0.2248(2) 1.4148(4) 0.203(3) Uani 1 d D . C42 C 0.4550(2) 0.20575(14) 1.3287(3) 0.1878(6) Uani 1 d D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.05585(6) 0.05212(5) 0.04969(5) 0.00075(5) 0.00826(5) -0.00360(5) O1 0.0588(11) 0.0839(12) 0.0664(10) -0.0026(10) 0.0183(9) -0.0049(10) O2 0.0847(14) 0.0570(10) 0.0622(10) 0.0089(9) 0.0082(10) -0.0142(10) O3 0.0558(10) 0.0538(9) 0.0510(9) -0.0067(8) 0.0047(8) 0.0038(8) O4 0.0624(11) 0.0503(8) 0.0579(9) 0.0003(8) 0.0081(9) -0.0056(9) N1 0.0554(12) 0.0451(10) 0.0517(11) -0.0034(9) 0.0047(10) 0.0021(9) N2 0.0586(13) 0.0519(11) 0.0504(10) -0.0015(10) 0.0060(10) 0.0041(10) C1 0.058(2) 0.0521(13) 0.0532(13) 0.0084(12) 0.0079(12) 0.0053(12) C2 0.0537(15) 0.0484(13) 0.0539(13) -0.0030(11) 0.0079(12) -0.0011(11) C3 0.078(2) 0.0563(14) 0.0614(15) 0.0056(13) 0.0160(14) 0.0072(14) C4 0.107(3) 0.057(2) 0.069(2) -0.0154(15) 0.003(2) 0.003(2) C5 0.096(2) 0.0520(15) 0.078(2) 0.0000(15) 0.014(2) -0.005(2) C6 0.095(2) 0.071(2) 0.080(2) 0.005(2) 0.023(2) -0.016(2) C7 0.080(2) 0.068(2) 0.0614(14) -0.0135(14) 0.0197(14) -0.013(2) C8 0.059(2) 0.0580(13) 0.0432(11) 0.0008(12) 0.0070(11) -0.0002(13) C9 0.062(2) 0.074(2) 0.062(2) 0.008(2) -0.0048(15) 0.0022(15) C10 0.074(2) 0.091(2) 0.063(2) -0.013(2) -0.001(2) 0.008(2) C11 0.085(2) 0.074(2) 0.0516(14) 0.0017(15) -0.0081(15) 0.026(2) C12 0.072(2) 0.066(2) 0.0606(15) 0.0024(14) 0.0097(14) 0.0088(15) C13 0.067(2) 0.0608(14) 0.0508(13) 0.0049(12) 0.0071(13) 0.0023(13) C14 0.063(2) 0.0438(11) 0.0442(11) 0.0038(11) 0.0099(11) 0.0006(11) C15 0.053(2) 0.069(2) 0.0613(15) -0.0028(13) 0.0076(13) 0.0028(13) C16 0.069(2) 0.0637(14) 0.0641(15) 0.0069(14) 0.0167(14) 0.0060(14) C17 0.074(2) 0.0529(13) 0.0675(15) 0.0014(13) 0.0229(14) 0.0078(13) C18 0.082(2) 0.0404(12) 0.0572(14) 0.0004(12) 0.0089(14) 0.0018(13) C19 0.064(2) 0.067(2) 0.0471(12) -0.0039(13) 0.0009(13) 0.0048(14) C20 0.069(2) 0.0565(14) 0.0433(12) -0.0018(11) 0.0037(12) 0.0063(13) C21 0.083(2) 0.0603(14) 0.0617(15) -0.0007(14) 0.0222(14) 0.0039(15) C22 0.095(2) 0.083(2) 0.071(2) 0.002(2) 0.028(2) 0.007(2) C23 0.100(2) 0.071(2) 0.065(2) -0.0064(15) 0.024(2) -0.001(2) C24 0.112(3) 0.063(2) 0.078(2) -0.023(2) 0.016(2) 0.013(2) C25 0.084(2) 0.068(2) 0.067(2) -0.0040(15) 0.011(2) -0.005(2) C26 0.051(2) 0.102(2) 0.068(2) -0.026(2) 0.0016(14) -0.005(2) C27 0.070(2) 0.227(5) 0.081(2) 0.000(3) 0.015(2) -0.036(3) C28 0.092(3) 0.333(7) 0.096(3) 0.003(4) 0.015(3) -0.072(4) C29 0.053(2) 0.293(7) 0.112(3) -0.033(4) 0.004(2) 0.022(3) C30 0.082(3) 0.186(4) 0.115(3) -0.024(3) -0.038(2) 0.025(3) C31 0.061(2) 0.133(3) 0.101(2) 0.002(3) -0.012(2) 0.014(2) C32 0.055(2) 0.0624(14) 0.0547(14) -0.0039(13) 0.0030(12) 0.0027(13) C33 0.085(2) 0.071(2) 0.0541(15) 0.0064(14) -0.004(2) 0.008(2) C34 0.092(2) 0.074(2) 0.076(2) 0.005(2) 0.015(2) 0.018(2) C35 0.101(2) 0.0433(13) 0.087(2) -0.0008(14) 0.019(2) -0.0016(15) C36 0.062(2) 0.0529(13) 0.069(2) -0.0119(13) 0.0124(13) -0.0073(13) O5 0.131(3) 0.172(3) 0.180(3) 0.013(3) 0.012(3) -0.018(3) N3 0.097(2) 0.145(3) 0.127(2) 0.030(2) 0.026(2) -0.004(2) C37 0.101(4) 0.190(4) 0.190(4) 0.025(4) 0.025(4) -0.029(3) C38 0.172(4) 0.188(4) 0.144(4) -0.006(4) -0.048(4) -0.023(4) C39 0.189(4) 0.155(4) 0.198(4) -0.006(4) 0.046(4) 0.053(4) O6 0.159(4) 0.199(3) 0.200(3) -0.024(3) -0.003(3) -0.020(3) N4 0.184(4) 0.107(3) 0.184(4) -0.018(3) 0.053(3) -0.022(3) C40 0.153(4) 0.179(4) 0.184(4) -0.025(4) -0.024(4) -0.041(4) C41 0.231(8) 0.196(7) 0.181(8) 0.013(5) 0.031(6) -0.017(6) C42 0.181(6) 0.174(7) 0.185(7) 0.007(5) -0.033(5) -0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.731(2) . ? W1 O2 1.733(2) . ? W1 O4 1.930(2) . ? W1 O3 1.938(2) . ? W1 N1 2.341(3) . ? W1 N2 2.357(2) . ? O3 C1 1.423(3) . ? O4 C19 1.458(3) . ? N1 C14 1.336(3) . ? N1 C18 1.353(3) . ? N2 C32 1.356(3) . ? N2 C36 1.371(3) . ? C1 C14 1.524(4) . ? C1 C2 1.538(3) . ? C1 C8 1.559(3) . ? C2 C7 1.392(4) . ? C2 C3 1.409(4) . ? C3 C4 1.393(4) . ? C4 C5 1.397(5) . ? C5 C6 1.367(5) . ? C6 C7 1.397(4) . ? C8 C13 1.366(4) . ? C8 C9 1.392(4) . ? C9 C10 1.393(4) . ? C10 C11 1.381(5) . ? C11 C12 1.361(4) . ? C12 C13 1.392(4) . ? C14 C15 1.383(4) . ? C15 C16 1.378(4) . ? C16 C17 1.356(4) . ? C17 C18 1.375(5) . ? C19 C32 1.502(4) . ? C19 C20 1.519(4) . ? C19 C26 1.536(5) . ? C20 C21 1.348(5) . ? C20 C25 1.397(4) . ? C21 C22 1.385(5) . ? C22 C23 1.358(5) . ? C23 C24 1.382(5) . ? C24 C25 1.393(5) . ? C26 C27 1.388(6) . ? C26 C31 1.403(5) . ? C27 C28 1.399(6) . ? C28 C29 1.422(7) . ? C29 C30 1.373(7) . ? C30 C31 1.413(6) . ? C32 C33 1.384(4) . ? C33 C34 1.382(4) . ? C34 C35 1.377(4) . ? C35 C36 1.369(4) . ? O5 C37 1.230(3) . ? N3 C37 1.445(2) . ? N3 C39 1.449(3) . ? N3 C38 1.449(3) . ? O6 C40 1.233(3) . ? N4 C40 1.438(2) . ? N4 C41 1.441(2) . ? N4 C42 1.445(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O2 105.35(10) . . ? O1 W1 O4 104.78(9) . . ? O2 W1 O4 94.05(8) . . ? O1 W1 O3 93.57(9) . . ? O2 W1 O3 104.88(8) . . ? O4 W1 O3 149.16(8) . . ? O1 W1 N1 162.45(8) . . ? O2 W1 N1 88.40(9) . . ? O4 W1 N1 84.65(8) . . ? O3 W1 N1 72.02(8) . . ? O1 W1 N2 86.85(9) . . ? O2 W1 N2 163.72(8) . . ? O4 W1 N2 72.08(7) . . ? O3 W1 N2 84.66(7) . . ? N1 W1 N2 81.98(8) . . ? C1 O3 W1 128.18(15) . . ? C19 O4 W1 128.80(15) . . ? C14 N1 C18 118.6(3) . . ? C14 N1 W1 115.2(2) . . ? C18 N1 W1 125.1(2) . . ? C32 N2 C36 120.2(2) . . ? C32 N2 W1 114.5(2) . . ? C36 N2 W1 125.1(2) . . ? O3 C1 C14 109.9(2) . . ? O3 C1 C2 106.5(2) . . ? C14 C1 C2 113.2(2) . . ? O3 C1 C8 108.9(2) . . ? C14 C1 C8 108.9(2) . . ? C2 C1 C8 109.3(2) . . ? C7 C2 C3 118.3(2) . . ? C7 C2 C1 124.5(2) . . ? C3 C2 C1 117.1(2) . . ? C4 C3 C2 119.6(3) . . ? C5 C4 C3 121.1(3) . . ? C6 C5 C4 119.2(3) . . ? C5 C6 C7 120.5(3) . . ? C6 C7 C2 121.2(3) . . ? C13 C8 C9 118.6(2) . . ? C13 C8 C1 121.6(2) . . ? C9 C8 C1 119.8(2) . . ? C10 C9 C8 120.1(3) . . ? C11 C10 C9 119.7(3) . . ? C12 C11 C10 120.4(3) . . ? C11 C12 C13 119.6(3) . . ? C8 C13 C12 121.5(3) . . ? N1 C14 C15 121.7(2) . . ? N1 C14 C1 113.1(2) . . ? C15 C14 C1 125.2(2) . . ? C16 C15 C14 118.6(3) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 118.7(3) . . ? N1 C18 C17 122.1(3) . . ? O4 C19 C32 108.7(2) . . ? O4 C19 C20 105.6(2) . . ? C32 C19 C20 112.7(2) . . ? O4 C19 C26 107.5(2) . . ? C32 C19 C26 109.5(2) . . ? C20 C19 C26 112.6(2) . . ? C21 C20 C25 118.7(3) . . ? C21 C20 C19 124.0(2) . . ? C25 C20 C19 117.2(3) . . ? C20 C21 C22 121.3(3) . . ? C23 C22 C21 120.8(4) . . ? C22 C23 C24 119.2(3) . . ? C25 C24 C23 119.8(3) . . ? C24 C25 C20 120.1(3) . . ? C27 C26 C31 120.4(3) . . ? C27 C26 C19 120.7(3) . . ? C31 C26 C19 118.9(3) . . ? C26 C27 C28 118.4(4) . . ? C29 C28 C27 122.1(5) . . ? C30 C29 C28 118.4(4) . . ? C29 C30 C31 120.3(4) . . ? C26 C31 C30 120.3(4) . . ? N2 C32 C33 119.3(2) . . ? N2 C32 C19 114.7(2) . . ? C33 C32 C19 126.0(2) . . ? C32 C33 C34 122.1(3) . . ? C33 C34 C35 116.5(3) . . ? C36 C35 C34 122.1(3) . . ? C35 C36 N2 119.8(3) . . ? C37 N3 C39 123.8(2) . . ? C37 N3 C38 108.7(2) . . ? C39 N3 C38 126.6(2) . . ? O5 C37 N3 115.6(2) . . ? C40 N4 C41 111.7(2) . . ? C40 N4 C42 115.0(2) . . ? C41 N4 C42 132.8(3) . . ? O6 C40 N4 110.5(2) . . ? _refine_diff_density_max 0.664 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.086 #===END data_[WO2(L5)2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53.50 H63.50 N2.50 O4.50 W' _chemical_formula_weight 997.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 17.660(3) _cell_length_b 16.118(1) _cell_length_c 19.974(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.760(3) _cell_angle_gamma 90.00 _cell_volume 5444(1) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 2.164 _exptl_absorpt_correction_type 'abscor' _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 1.118 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7249 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.55 _reflns_number_total 7249 _reflns_number_gt 5316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0607P)^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 0.00015(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7249 _refine_ls_number_parameters 550 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1285 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1741 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.133 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.633093(12) 0.097964(13) 0.202859(11) 0.07882(6) Uani 1 1 d . . . O1 O 0.70942(18) 0.09971(17) 0.14903(15) 0.0823(11) Uani 1 1 d . . . O2 O 0.5736(2) 0.01443(19) 0.16824(17) 0.1004(13) Uani 1 1 d . . . O3 O 0.58704(18) 0.1845(2) 0.16280(15) 0.0895(12) Uani 1 1 d . . . O4 O 0.60922(19) 0.09698(18) 0.29139(15) 0.0847(11) Uani 1 1 d . . . N1 N 0.7314(2) -0.0005(2) 0.25092(19) 0.0870(14) Uani 1 1 d . . . N2 N 0.7244(2) 0.1824(2) 0.2800(2) 0.0763(13) Uani 1 1 d . . . C1 C 0.7828(3) -0.0143(3) 0.2152(2) 0.0853(17) Uani 1 1 d . . . C2 C 0.8377(3) -0.0770(3) 0.2325(3) 0.0852(18) Uani 1 1 d . . . H2 H 0.8704 -0.0878 0.2044 0.102 Uiso 1 1 calc R . . C3 C 0.8439(4) -0.1224(3) 0.2899(3) 0.104(2) Uani 1 1 d . . . H3 H 0.8827 -0.1631 0.3029 0.124 Uiso 1 1 calc R . . C4 C 0.7918(4) -0.1090(3) 0.3309(3) 0.111(2) Uani 1 1 d . . . H4 H 0.7933 -0.1410 0.3700 0.133 Uiso 1 1 calc R . . C5 C 0.7398(4) -0.0465(3) 0.3093(3) 0.108(2) Uani 1 1 d . . . H5 H 0.7070 -0.0339 0.3368 0.129 Uiso 1 1 calc R . . C6 C 0.7110(3) 0.1957(3) 0.3420(2) 0.0800(16) Uani 1 1 d . . . C7 C 0.7560(3) 0.2513(3) 0.3911(3) 0.098(2) Uani 1 1 d . . . H7 H 0.7440 0.2605 0.4329 0.118 Uiso 1 1 calc R . . C8 C 0.8193(3) 0.2934(3) 0.3772(3) 0.103(2) Uani 1 1 d . . . H8 H 0.8516 0.3287 0.4100 0.123 Uiso 1 1 calc R . . C9 C 0.8322(3) 0.2804(3) 0.3123(3) 0.108(2) Uani 1 1 d . . . H9 H 0.8727 0.3085 0.3007 0.130 Uiso 1 1 calc R . . C10 C 0.7852(3) 0.2265(3) 0.2658(3) 0.0952(19) Uani 1 1 d . . . H10 H 0.7945 0.2190 0.2226 0.114 Uiso 1 1 calc R . . C11 C 0.8461(3) 0.0978(3) 0.1587(2) 0.0807(16) Uani 1 1 d . . . C12 C 0.9098(3) 0.0997(3) 0.2162(3) 0.0924(19) Uani 1 1 d . . . H12 H 0.9135 0.0635 0.2533 0.111 Uiso 1 1 calc R . . C13 C 0.9711(3) 0.1584(3) 0.2188(3) 0.0899(19) Uani 1 1 d . . . H13 H 1.0171 0.1555 0.2560 0.108 Uiso 1 1 calc R . . C14 C 0.9658(3) 0.2184(3) 0.1696(3) 0.0982(19) Uani 1 1 d . . . C15 C 0.8988(3) 0.2170(4) 0.1109(3) 0.112(2) Uani 1 1 d . . . H15 H 0.8932 0.2563 0.0757 0.134 Uiso 1 1 calc R . . C16 C 0.8412(3) 0.1574(3) 0.1054(3) 0.106(2) Uani 1 1 d . . . H16 H 0.7980 0.1562 0.0656 0.128 Uiso 1 1 calc R . . C17 C 0.9966(4) 0.3662(4) 0.1954(4) 0.158(3) Uani 1 1 d . . . H17A H 1.0363 0.4081 0.1999 0.237 Uiso 1 1 calc R . . H17B H 0.9851 0.3597 0.2393 0.237 Uiso 1 1 calc R . . H17C H 0.9494 0.3825 0.1602 0.237 Uiso 1 1 calc R . . C18 C 1.0487(4) 0.2974(5) 0.1061(3) 0.163(3) Uani 1 1 d . . . H18A H 1.0888 0.3394 0.1133 0.244 Uiso 1 1 calc R . . H18B H 1.0027 0.3149 0.0701 0.244 Uiso 1 1 calc R . . H18C H 1.0684 0.2466 0.0922 0.244 Uiso 1 1 calc R . . C19 C 1.1048(4) 0.2634(4) 0.2295(4) 0.158(3) Uani 1 1 d . . . H19A H 1.1419 0.3074 0.2311 0.237 Uiso 1 1 calc R . . H19B H 1.1258 0.2123 0.2177 0.237 Uiso 1 1 calc R . . H19C H 1.0958 0.2580 0.2745 0.237 Uiso 1 1 calc R . . C20 C 1.0269(3) 0.2832(4) 0.1745(3) 0.109(2) Uani 1 1 d . . . C21 C 0.7509(3) -0.0043(3) 0.0832(2) 0.0815(16) Uani 1 1 d . . . C22 C 0.8038(3) -0.0428(3) 0.0560(2) 0.0860(18) Uani 1 1 d . . . H22 H 0.8572 -0.0389 0.0803 0.103 Uiso 1 1 calc R . . C23 C 0.7833(3) -0.0864(3) -0.0045(3) 0.0936(18) Uani 1 1 d . . . H23 H 0.8232 -0.1112 -0.0194 0.112 Uiso 1 1 calc R . . C24 C 0.7056(3) -0.0959(3) -0.0454(3) 0.0897(17) Uani 1 1 d . . . C25 C 0.6493(3) -0.0562(4) -0.0206(3) 0.108(2) Uani 1 1 d . . . H25 H 0.5959 -0.0599 -0.0452 0.129 Uiso 1 1 calc R . . C26 C 0.6735(3) -0.0105(3) 0.0418(3) 0.106(2) Uani 1 1 d . . . H26 H 0.6349 0.0174 0.0562 0.127 Uiso 1 1 calc R . . C27 C 0.6259(4) -0.2124(4) -0.1063(3) 0.144(3) Uani 1 1 d . . . H27A H 0.5832 -0.1896 -0.0914 0.217 Uiso 1 1 calc R . . H27B H 0.6540 -0.2524 -0.0726 0.217 Uiso 1 1 calc R . . H27C H 0.6051 -0.2391 -0.1508 0.217 Uiso 1 1 calc R . . C28 C 0.6340(5) -0.0903(4) -0.1708(3) 0.160(3) Uani 1 1 d . . . H28A H 0.5887 -0.0686 -0.1592 0.240 Uiso 1 1 calc R . . H28B H 0.6169 -0.1219 -0.2133 0.240 Uiso 1 1 calc R . . H28C H 0.6668 -0.0452 -0.1772 0.240 Uiso 1 1 calc R . . C29 C 0.7461(4) -0.1753(5) -0.1375(4) 0.206(4) Uani 1 1 d . . . H29A H 0.7254 -0.2055 -0.1803 0.310 Uiso 1 1 calc R . . H29B H 0.7793 -0.2111 -0.1028 0.310 Uiso 1 1 calc R . . H29C H 0.7765 -0.1290 -0.1455 0.310 Uiso 1 1 calc R . . C30 C 0.6804(3) -0.1451(3) -0.1126(3) 0.102(2) Uani 1 1 d . . . C31 C 0.6598(3) 0.0910(3) 0.4158(2) 0.0905(17) Uani 1 1 d . . . C32 C 0.7341(3) 0.0775(4) 0.4590(3) 0.114(2) Uani 1 1 d . . . H32 H 0.7767 0.1041 0.4497 0.137 Uiso 1 1 calc R . . C33 C 0.7479(3) 0.0252(4) 0.5163(3) 0.128(3) Uani 1 1 d . . . H33 H 0.7995 0.0187 0.5447 0.153 Uiso 1 1 calc R . . C34 C 0.6889(4) -0.0168(4) 0.5325(3) 0.114(2) Uani 1 1 d . . . C35 C 0.6135(3) -0.0072(4) 0.4859(3) 0.122(2) Uani 1 1 d . . . H35 H 0.5716 -0.0371 0.4934 0.146 Uiso 1 1 calc R . . C36 C 0.5990(3) 0.0466(3) 0.4276(3) 0.099(2) Uani 1 1 d . . . H36 H 0.5481 0.0517 0.3973 0.118 Uiso 1 1 calc R . . C37 C 0.7810(5) -0.0643(10) 0.6470(7) 0.184(7) Uiso 0.50 1 d PD . . H37A H 0.8061 -0.0163 0.6345 0.276 Uiso 0.50 1 calc PR . . H37B H 0.8115 -0.1129 0.6441 0.276 Uiso 0.50 1 calc PR . . H37C H 0.7777 -0.0582 0.6939 0.276 Uiso 0.50 1 calc PR . . C37' C 0.7818(5) -0.1071(10) 0.6093(14) 0.295(13) Uiso 0.50 1 d PD . . H37D H 0.8197 -0.0645 0.6285 0.443 Uiso 0.50 1 calc PR . . H37E H 0.7882 -0.1256 0.5656 0.443 Uiso 0.50 1 calc PR . . H37F H 0.7898 -0.1530 0.6413 0.443 Uiso 0.50 1 calc PR . . C38' C 0.7176(9) -0.0160(6) 0.6600(5) 0.173(6) Uiso 0.50 1 d PD . . H38A H 0.7367 0.0360 0.6480 0.260 Uiso 0.50 1 calc PR . . H38B H 0.7574 -0.0409 0.6980 0.260 Uiso 0.50 1 calc PR . . H38C H 0.6706 -0.0069 0.6739 0.260 Uiso 0.50 1 calc PR . . C38 C 0.6553(6) -0.0345(7) 0.6439(5) 0.170(6) Uiso 0.50 1 d PD . . H38D H 0.6771 0.0193 0.6589 0.255 Uiso 0.50 1 calc PR . . H38E H 0.6604 -0.0692 0.6841 0.255 Uiso 0.50 1 calc PR . . H38F H 0.6004 -0.0290 0.6185 0.255 Uiso 0.50 1 calc PR . . C39 C 0.6817(9) -0.1597(5) 0.5735(7) 0.163(6) Uiso 0.50 1 d PD . . H39A H 0.6719 -0.1922 0.6104 0.245 Uiso 0.50 1 calc PR . . H39B H 0.7260 -0.1823 0.5610 0.245 Uiso 0.50 1 calc PR . . H39C H 0.6357 -0.1607 0.5336 0.245 Uiso 0.50 1 calc PR . . C39' C 0.6297(5) -0.1243(6) 0.6013(7) 0.134(5) Uiso 0.50 1 d PD . . H39D H 0.6029 -0.0970 0.6307 0.202 Uiso 0.50 1 calc PR . . H39E H 0.6477 -0.1778 0.6205 0.202 Uiso 0.50 1 calc PR . . H39F H 0.5940 -0.1309 0.5552 0.202 Uiso 0.50 1 calc PR . . C40 C 0.6992(3) -0.0731(3) 0.5975(3) 0.130(3) Uani 1 1 d D . . C41 C 0.5759(2) 0.2122(3) 0.3560(2) 0.0720(15) Uani 1 1 d . . . C42 C 0.5261(3) 0.2472(3) 0.2972(3) 0.0920(18) Uani 1 1 d . . . H42 H 0.5287 0.2296 0.2536 0.110 Uiso 1 1 calc R . . C43 C 0.4733(3) 0.3065(3) 0.3009(3) 0.095(2) Uani 1 1 d . . . H43 H 0.4398 0.3273 0.2594 0.114 Uiso 1 1 calc R . . C44 C 0.4668(3) 0.3375(3) 0.3633(2) 0.0808(17) Uani 1 1 d . . . C45 C 0.5172(3) 0.3048(3) 0.4219(3) 0.1024(19) Uani 1 1 d . . . H45 H 0.5143 0.3231 0.4653 0.123 Uiso 1 1 calc R . . C46 C 0.5733(3) 0.2450(3) 0.4197(3) 0.0891(18) Uani 1 1 d . . . H46 H 0.6091 0.2268 0.4610 0.107 Uiso 1 1 calc R . . C47 C 0.3803(4) 0.4011(4) 0.4289(3) 0.200(4) Uani 1 1 d D . . H47A H 0.3625 0.3462 0.4354 0.300 Uiso 1 1 calc R . . H47B H 0.3380 0.4399 0.4250 0.300 Uiso 1 1 calc R . . H47C H 0.4242 0.4156 0.4681 0.300 Uiso 1 1 calc R . . C48 C 0.3270(4) 0.3837(5) 0.3106(5) 0.234(5) Uani 1 1 d D . . H48A H 0.3094 0.3298 0.3201 0.351 Uiso 1 1 calc R . . H48B H 0.3334 0.3843 0.2645 0.351 Uiso 1 1 calc R . . H48C H 0.2885 0.4245 0.3136 0.351 Uiso 1 1 calc R . . C49 C 0.4468(7) 0.4854(5) 0.3877(7) 0.144(5) Uiso 0.50 1 d PD . . H49A H 0.4595 0.5116 0.3492 0.216 Uiso 0.50 1 calc PR . . H49B H 0.4945 0.4754 0.4246 0.216 Uiso 0.50 1 calc PR . . H49C H 0.4126 0.5209 0.4045 0.216 Uiso 0.50 1 calc PR . . C49' C 0.4187(6) 0.4796(5) 0.3265(5) 0.112(4) Uiso 0.50 1 d PD . . H49D H 0.4342 0.4643 0.2859 0.169 Uiso 0.50 1 calc PR . . H49E H 0.4597 0.5123 0.3572 0.169 Uiso 0.50 1 calc PR . . H49F H 0.3707 0.5115 0.3124 0.169 Uiso 0.50 1 calc PR . . C50 C 0.4053(3) 0.4034(3) 0.3637(2) 0.105(2) Uani 1 1 d D . . C61 C 0.7715(2) 0.0434(3) 0.1509(2) 0.0749(15) Uani 1 1 d . . . C62 C 0.6388(3) 0.1478(3) 0.3505(3) 0.0801(17) Uani 1 1 d . . . O5 O 0.8171(6) -0.2251(7) 0.4812(6) 0.187(4) Uiso 0.50 1 d P . . N3 N 0.9089(6) -0.3089(6) 0.5343(6) 0.136(4) Uiso 0.50 1 d P . . C73 C 0.8802(7) -0.2629(7) 0.4862(7) 0.122(4) Uiso 0.50 1 d P . . H73 H 0.9057 -0.2552 0.4519 0.147 Uiso 0.50 1 calc PR . . C72 C 0.9724(9) -0.3620(9) 0.5351(8) 0.167(6) Uiso 0.50 1 d P . . H72A H 0.9851 -0.3950 0.5769 0.250 Uiso 0.50 1 calc PR . . H72B H 1.0176 -0.3295 0.5341 0.250 Uiso 0.50 1 calc PR . . H72C H 0.9578 -0.3977 0.4950 0.250 Uiso 0.50 1 calc PR . . C71 C 0.8603(12) -0.3459(11) 0.5717(10) 0.222(9) Uiso 0.50 1 d P . . H71A H 0.8916 -0.3824 0.6068 0.333 Uiso 0.50 1 calc PR . . H71B H 0.8187 -0.3769 0.5400 0.333 Uiso 0.50 1 calc PR . . H71C H 0.8377 -0.3033 0.5936 0.333 Uiso 0.50 1 calc PR . . 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 0.07979(10) 0.08648(12) 0.07666(10) -0.00948(11) 0.03288(8) 0.00071(12) O1 0.0919(19) 0.0829(18) 0.0747(18) -0.0060(16) 0.0282(15) 0.0087(18) O2 0.111(2) 0.0872(19) 0.107(2) -0.0431(17) 0.0386(19) -0.0329(18) O3 0.0926(19) 0.111(2) 0.0732(18) 0.0105(17) 0.0370(15) 0.0048(19) O4 0.1009(19) 0.0856(18) 0.0729(17) -0.0227(16) 0.0337(15) -0.0043(18) N1 0.128(3) 0.064(2) 0.078(2) -0.0081(18) 0.045(2) -0.002(2) N2 0.068(2) 0.070(2) 0.098(2) -0.0010(19) 0.0345(18) 0.0014(18) C1 0.110(3) 0.074(3) 0.084(3) 0.001(2) 0.046(2) 0.008(3) C2 0.081(3) 0.083(3) 0.086(3) 0.000(2) 0.016(3) 0.022(2) C3 0.128(5) 0.070(3) 0.100(4) 0.019(3) 0.012(4) 0.017(3) C4 0.176(5) 0.068(3) 0.096(3) 0.021(3) 0.049(3) 0.030(3) C5 0.155(4) 0.088(3) 0.095(3) -0.014(3) 0.061(3) -0.005(3) C6 0.071(2) 0.089(3) 0.086(3) -0.020(3) 0.033(2) -0.002(2) C7 0.095(3) 0.107(4) 0.089(3) -0.003(3) 0.020(3) 0.000(3) C8 0.083(3) 0.106(3) 0.116(4) -0.032(3) 0.026(3) -0.003(3) C9 0.099(3) 0.084(3) 0.150(4) -0.028(3) 0.050(3) -0.017(3) C10 0.094(3) 0.090(3) 0.107(4) -0.020(3) 0.037(3) 0.002(3) C11 0.092(3) 0.082(3) 0.074(3) -0.004(2) 0.034(2) 0.010(3) C12 0.082(3) 0.104(3) 0.092(3) -0.002(3) 0.027(3) -0.003(3) C13 0.069(3) 0.121(4) 0.073(3) 0.003(3) 0.010(3) 0.013(3) C14 0.108(3) 0.104(4) 0.095(3) -0.006(3) 0.050(3) -0.005(3) C15 0.108(4) 0.137(4) 0.094(4) 0.021(4) 0.034(3) -0.002(4) C16 0.097(3) 0.137(4) 0.085(3) 0.001(3) 0.027(3) -0.033(3) C17 0.144(4) 0.143(5) 0.219(6) -0.020(5) 0.103(4) -0.046(4) C18 0.118(4) 0.232(7) 0.140(5) 0.013(6) 0.040(4) -0.038(5) C19 0.093(4) 0.192(6) 0.171(7) 0.019(5) 0.010(5) -0.033(5) C20 0.108(4) 0.116(4) 0.111(4) 0.000(3) 0.047(3) 0.001(4) C21 0.067(2) 0.106(3) 0.077(3) 0.004(3) 0.030(2) 0.015(3) C22 0.079(3) 0.109(3) 0.072(3) 0.000(3) 0.024(2) -0.006(3) C23 0.085(3) 0.101(3) 0.108(3) -0.015(3) 0.049(2) -0.004(3) C24 0.084(3) 0.110(3) 0.083(3) -0.010(3) 0.036(2) -0.001(3) C25 0.084(3) 0.167(5) 0.068(3) -0.031(3) 0.015(3) 0.010(4) C26 0.112(3) 0.132(4) 0.090(3) 0.008(3) 0.056(2) 0.029(3) C27 0.154(5) 0.180(5) 0.112(4) -0.042(4) 0.059(4) -0.038(5) C28 0.181(6) 0.205(7) 0.096(4) -0.027(5) 0.042(4) 0.017(6) C29 0.112(5) 0.315(8) 0.199(6) -0.158(5) 0.055(4) -0.019(6) C30 0.100(3) 0.127(4) 0.087(3) -0.019(3) 0.040(3) 0.000(3) C31 0.124(3) 0.078(3) 0.086(3) -0.004(2) 0.058(2) 0.006(3) C32 0.088(3) 0.157(5) 0.098(4) 0.043(3) 0.029(3) 0.004(4) C33 0.110(4) 0.163(5) 0.121(4) 0.021(4) 0.049(3) -0.020(4) C34 0.130(4) 0.123(4) 0.090(4) 0.020(3) 0.032(3) 0.022(4) C35 0.125(4) 0.127(4) 0.133(4) 0.008(4) 0.068(3) -0.006(4) C36 0.094(4) 0.113(4) 0.078(3) 0.018(3) 0.005(3) 0.005(3) C40 0.163(5) 0.133(5) 0.105(4) 0.002(4) 0.055(4) -0.012(4) C41 0.069(3) 0.081(3) 0.066(3) -0.004(2) 0.021(2) 0.002(2) C42 0.085(3) 0.111(3) 0.081(3) -0.023(3) 0.027(2) 0.013(3) C43 0.086(3) 0.121(4) 0.073(3) 0.004(3) 0.015(3) 0.027(3) C44 0.078(3) 0.086(3) 0.085(3) 0.011(2) 0.035(2) 0.019(2) C45 0.119(3) 0.123(4) 0.083(3) -0.021(3) 0.057(2) 0.010(3) C46 0.092(3) 0.104(3) 0.072(3) -0.001(3) 0.025(3) 0.012(3) C47 0.229(6) 0.191(6) 0.223(7) 0.035(5) 0.133(5) 0.098(5) C48 0.118(5) 0.221(7) 0.352(13) -0.052(7) 0.050(7) 0.077(5) C50 0.106(3) 0.108(4) 0.118(4) 0.009(3) 0.059(3) 0.027(3) C61 0.072(2) 0.077(3) 0.084(3) -0.025(2) 0.035(2) 0.004(2) C62 0.073(3) 0.083(3) 0.090(3) -0.004(3) 0.033(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 1.695(3) . ? W1 O2 1.725(3) . ? W1 O4 1.933(3) . ? W1 O1 1.952(3) . ? W1 N2 2.322(3) . ? W1 N1 2.343(4) . ? O1 C61 1.416(5) . ? O4 C62 1.408(5) . ? N1 C1 1.326(7) . ? N1 C5 1.353(6) . ? N2 C6 1.343(6) . ? N2 C10 1.384(6) . ? C1 C2 1.373(6) . ? C1 C61 1.552(6) . ? C2 C3 1.338(7) . ? C3 C4 1.412(9) . ? C4 C5 1.347(7) . ? C6 C7 1.396(6) . ? C6 C62 1.542(7) . ? C7 C8 1.403(8) . ? C8 C9 1.395(8) . ? C9 C10 1.365(7) . ? C11 C12 1.358(6) . ? C11 C16 1.418(7) . ? C11 C61 1.551(6) . ? C12 C13 1.427(7) . ? C13 C14 1.363(7) . ? C14 C15 1.405(7) . ? C14 C20 1.486(8) . ? C15 C16 1.380(8) . ? C17 C20 1.543(9) . ? C18 C20 1.540(9) . ? C19 C20 1.528(8) . ? C21 C22 1.361(7) . ? C21 C26 1.381(6) . ? C21 C61 1.504(6) . ? C22 C23 1.353(7) . ? C23 C24 1.388(6) . ? C24 C25 1.388(8) . ? C24 C30 1.512(7) . ? C25 C26 1.404(7) . ? C27 C30 1.480(9) . ? C28 C30 1.502(8) . ? C29 C30 1.470(9) . ? C31 C32 1.364(7) . ? C31 C36 1.367(8) . ? C31 C62 1.547(7) . ? C32 C33 1.385(8) . ? C33 C34 1.359(9) . ? C34 C35 1.395(8) . ? C34 C40 1.552(8) . ? C35 C36 1.416(8) . ? C37 C40 1.504(9) . ? C37' C40 1.512(11) . ? C37' C39 1.904(17) . ? C38' C40 1.509(10) . ? C38 C40 1.504(11) . ? C39 C40 1.479(9) . ? C39' C40 1.499(10) . ? C41 C42 1.368(6) . ? C41 C46 1.391(7) . ? C41 C62 1.547(6) . ? C42 C43 1.353(7) . ? C43 C44 1.378(7) . ? C44 C45 1.358(6) . ? C44 C50 1.520(6) . ? C45 C46 1.392(7) . ? C47 C50 1.490(8) . ? C48 C50 1.514(7) . ? C49 C50 1.521(9) . ? C49' C50 1.491(9) . ? O5 C73 1.249(16) . ? N3 C73 1.204(15) . ? N3 C72 1.406(18) . ? N3 C71 1.42(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 O3 W1 O2 107.41(14) . . ? O3 W1 O4 103.72(14) . . ? O2 W1 O4 95.27(15) . . ? O3 W1 O1 92.39(14) . . ? O2 W1 O1 103.19(15) . . ? O4 W1 O1 150.66(12) . . ? O3 W1 N2 88.70(13) . . ? O2 W1 N2 161.72(14) . . ? O4 W1 N2 71.98(13) . . ? O1 W1 N2 84.23(13) . . ? O3 W1 N1 161.57(15) . . ? O2 W1 N1 85.96(13) . . ? O4 W1 N1 87.18(13) . . ? O1 W1 N1 71.81(13) . . ? N2 W1 N1 80.49(11) . . ? C61 O1 W1 129.0(3) . . ? C62 O4 W1 129.6(3) . . ? C1 N1 C5 116.7(4) . . ? C1 N1 W1 115.8(3) . . ? C5 N1 W1 127.5(4) . . ? C6 N2 C10 117.4(4) . . ? C6 N2 W1 115.6(3) . . ? C10 N2 W1 126.6(3) . . ? N1 C1 C2 122.1(5) . . ? N1 C1 C61 113.6(4) . . ? C2 C1 C61 124.2(5) . . ? C3 C2 C1 119.7(5) . . ? C2 C3 C4 120.5(5) . . ? C5 C4 C3 115.2(5) . . ? C4 C5 N1 125.5(6) . . ? N2 C6 C7 122.3(5) . . ? N2 C6 C62 113.1(4) . . ? C7 C6 C62 124.4(5) . . ? C6 C7 C8 119.7(5) . . ? C9 C8 C7 117.7(5) . . ? C10 C9 C8 119.9(5) . . ? C9 C10 N2 122.9(5) . . ? C12 C11 C16 118.4(5) . . ? C12 C11 C61 124.8(4) . . ? C16 C11 C61 116.2(4) . . ? C11 C12 C13 118.8(5) . . ? C14 C13 C12 123.3(4) . . ? C13 C14 C15 117.2(5) . . ? C13 C14 C20 123.7(4) . . ? C15 C14 C20 119.1(5) . . ? C16 C15 C14 120.0(5) . . ? C15 C16 C11 121.9(5) . . ? C14 C20 C19 112.7(5) . . ? C14 C20 C18 114.2(5) . . ? C19 C20 C18 105.4(5) . . ? C14 C20 C17 109.0(5) . . ? C19 C20 C17 107.3(5) . . ? C18 C20 C17 107.9(5) . . ? C22 C21 C26 113.7(4) . . ? C22 C21 C61 125.1(4) . . ? C26 C21 C61 121.2(4) . . ? C23 C22 C21 123.8(4) . . ? C22 C23 C24 123.2(5) . . ? C23 C24 C25 115.3(5) . . ? C23 C24 C30 124.6(5) . . ? C25 C24 C30 120.0(4) . . ? C24 C25 C26 119.4(5) . . ? C21 C26 C25 124.5(5) . . ? C29 C30 C27 112.5(6) . . ? C29 C30 C28 103.9(6) . . ? C27 C30 C28 105.9(5) . . ? C29 C30 C24 114.5(5) . . ? C27 C30 C24 110.0(5) . . ? C28 C30 C24 109.5(5) . . ? C32 C31 C36 117.9(5) . . ? C32 C31 C62 125.5(5) . . ? C36 C31 C62 116.4(4) . . ? C31 C32 C33 121.9(6) . . ? C34 C33 C32 122.4(5) . . ? C33 C34 C35 115.9(5) . . ? C33 C34 C40 125.3(5) . . ? C35 C34 C40 118.8(5) . . ? C34 C35 C36 121.9(6) . . ? C31 C36 C35 119.8(5) . . ? C40 C37' C39 49.7(5) . . ? C40 C39 C37' 51.2(6) . . ? C39 C40 C39' 53.1(8) . . ? C39 C40 C38 119.6(9) . . ? C39' C40 C38 67.7(7) . . ? C39 C40 C37 111.9(9) . . ? C39' C40 C37 131.6(8) . . ? C38 C40 C37 97.2(7) . . ? C39 C40 C38' 144.9(8) . . ? C39' C40 C38' 106.1(8) . . ? C38 C40 C38' 42.6(7) . . ? C37 C40 C38' 57.4(8) . . ? C39 C40 C37' 79.1(9) . . ? C39' C40 C37' 124.0(8) . . ? C38 C40 C37' 134.4(11) . . ? C37 C40 C37' 39.7(10) . . ? C38' C40 C37' 97.1(11) . . ? C39 C40 C34 108.5(6) . . ? C39' C40 C34 117.7(6) . . ? C38 C40 C34 108.5(6) . . ? C37 C40 C34 110.7(7) . . ? C38' C40 C34 106.4(5) . . ? C37' C40 C34 102.6(11) . . ? C42 C41 C46 116.5(4) . . ? C42 C41 C62 120.9(4) . . ? C46 C41 C62 122.2(4) . . ? C43 C42 C41 121.8(5) . . ? C42 C43 C44 123.0(4) . . ? C45 C44 C43 115.7(4) . . ? C45 C44 C50 123.9(5) . . ? C43 C44 C50 120.3(4) . . ? C44 C45 C46 122.5(5) . . ? C45 C46 C41 120.3(4) . . ? C47 C50 C49' 125.8(6) . . ? C47 C50 C48 99.6(5) . . ? C49' C50 C48 93.9(5) . . ? C47 C50 C44 112.3(4) . . ? C49' C50 C44 110.9(6) . . ? C48 C50 C44 111.1(4) . . ? C47 C50 C49 89.1(7) . . ? C49' C50 C49 46.3(6) . . ? C48 C50 C49 131.5(6) . . ? C44 C50 C49 109.1(5) . . ? O1 C61 C21 108.6(3) . . ? O1 C61 C11 105.6(3) . . ? C21 C61 C11 111.0(4) . . ? O1 C61 C1 108.6(4) . . ? C21 C61 C1 112.1(4) . . ? C11 C61 C1 110.6(3) . . ? O4 C62 C6 108.5(4) . . ? O4 C62 C41 110.4(3) . . ? C6 C62 C41 107.7(4) . . ? O4 C62 C31 107.7(3) . . ? C6 C62 C31 112.6(4) . . ? C41 C62 C31 109.9(4) . . ? C73 N3 C72 122.4(14) . . ? C73 N3 C71 119.9(13) . . ? C72 N3 C71 109.8(12) . . ? N3 C73 O5 121.7(15) . . ? _diffrn_measured_fraction_theta_max 0.712 _diffrn_reflns_theta_full 25.55 _diffrn_measured_fraction_theta_full 0.712 _refine_diff_density_max 0.634 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.090