# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl5 _database_code_depnum_ccdc_archive 'CCDC 876657' #TrackingRef 'Compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H96 N8 O16 W4' _chemical_formula_sum 'C40 H96 N8 O16 W4' _chemical_formula_weight 1680.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 27.4610(3) _cell_length_b 14.6920(2) _cell_length_c 30.7850(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.243(4) _cell_angle_gamma 90.00 _cell_volume 11924.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 81557 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 21.71 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6528 _exptl_absorpt_coefficient_mu 7.755 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1722 _exptl_absorpt_correction_T_max 0.3892 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 81557 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 21.71 _reflns_number_total 14039 _reflns_number_gt 12145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0250P)^2^+183.5796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14039 _refine_ls_number_parameters 1272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1071 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.339450(17) -0.03556(3) 0.522413(16) 0.02761(14) Uani 1 1 d . . . W2 W 0.401304(19) -0.10664(4) 0.644636(17) 0.03459(15) Uani 1 1 d . . . W3 W 0.353509(19) 0.13018(4) 0.659726(17) 0.03359(15) Uani 1 1 d . . . W4 W 0.423584(17) 0.16841(3) 0.569830(16) 0.02804(14) Uani 1 1 d . . . W5 W 0.332724(17) -0.03600(3) 0.010793(16) 0.02514(13) Uani 1 1 d . . . W6 W 0.395584(19) -0.10801(3) 0.132520(17) 0.03317(15) Uani 1 1 d . . . W7 W 0.346816(18) 0.12913(4) 0.148609(16) 0.03172(14) Uani 1 1 d . . . W8 W 0.416066(17) 0.16914(3) 0.058598(16) 0.02586(14) Uani 1 1 d . . . O1 O 0.3746(3) -0.0791(5) 0.5855(3) 0.035(2) Uani 1 1 d . . . O2 O 0.2819(3) -0.0132(5) 0.5321(3) 0.036(2) Uani 1 1 d . . . O3 O 0.3197(3) -0.0061(5) 0.4593(3) 0.0311(19) Uani 1 1 d . . . O4 O 0.3262(3) -0.1636(5) 0.5092(3) 0.0315(19) Uani 1 1 d . . . O5 O 0.3772(3) 0.0670(5) 0.5376(2) 0.0277(18) Uani 1 1 d . . . O6 O 0.4787(3) 0.1078(6) 0.5870(3) 0.037(2) Uani 1 1 d . . . O7 O 0.4284(3) 0.1933(5) 0.5091(3) 0.035(2) Uani 1 1 d . . . O8 O 0.4532(3) 0.2828(5) 0.5919(3) 0.034(2) Uani 1 1 d . . . O9 O 0.3933(3) 0.1566(6) 0.6154(3) 0.037(2) Uani 1 1 d . . . O10 O 0.2952(3) 0.1383(6) 0.6220(3) 0.042(2) Uani 1 1 d . . . O11 O 0.3280(3) 0.1092(7) 0.7103(3) 0.049(2) Uani 1 1 d . . . O12 O 0.3618(3) 0.2587(5) 0.6723(3) 0.038(2) Uani 1 1 d . . . O13 O 0.3733(3) 0.0110(6) 0.6589(3) 0.039(2) Uani 1 1 d . . . O14 O 0.4637(3) -0.0752(7) 0.6568(3) 0.049(2) Uani 1 1 d . . . O15 O 0.4085(3) -0.2325(5) 0.6307(3) 0.042(2) Uani 1 1 d . . . O16 O 0.4039(3) -0.1409(6) 0.7060(3) 0.047(2) Uani 1 1 d . . . O17 O 0.3675(3) -0.0865(5) 0.0726(2) 0.0305(19) Uani 1 1 d . . . O18 O 0.2750(3) -0.0134(5) 0.0198(3) 0.036(2) Uani 1 1 d . . . O19 O 0.3137(3) -0.0071(6) -0.0519(3) 0.038(2) Uani 1 1 d . . . O20 O 0.3194(3) -0.1626(5) -0.0032(3) 0.0309(19) Uani 1 1 d . . . O21 O 0.3703(3) 0.0683(5) 0.0277(2) 0.0295(19) Uani 1 1 d . . . O22 O 0.4713(3) 0.1075(5) 0.0764(3) 0.0336(19) Uani 1 1 d . . . O23 O 0.4450(3) 0.2840(5) 0.0792(3) 0.034(2) Uani 1 1 d . . . O24 O 0.4212(3) 0.1917(5) -0.0017(3) 0.0314(19) Uani 1 1 d . . . O25 O 0.3866(3) 0.1589(5) 0.1051(2) 0.0261(18) Uani 1 1 d . . . O26 O 0.2877(3) 0.1376(6) 0.1116(3) 0.039(2) Uani 1 1 d . . . O27 O 0.3231(3) 0.1051(6) 0.2005(3) 0.040(2) Uani 1 1 d . . . O28 O 0.3545(3) 0.2569(6) 0.1634(3) 0.043(2) Uani 1 1 d . . . O29 O 0.3671(3) 0.0113(5) 0.1461(3) 0.035(2) Uani 1 1 d . . . O30 O 0.4573(3) -0.0759(5) 0.1437(3) 0.037(2) Uani 1 1 d . . . O31 O 0.4045(3) -0.2331(6) 0.1210(3) 0.049(2) Uani 1 1 d . . . O32 O 0.3989(3) -0.1372(6) 0.1948(3) 0.047(2) Uani 1 1 d . . . N1 N 0.4150(3) -0.0943(6) 0.5037(3) 0.029(2) Uani 1 1 d . . . N2 N 0.3684(4) -0.3767(8) 0.4690(4) 0.049(3) Uani 1 1 d . . . N3 N 0.3141(4) -0.1581(7) 0.6411(4) 0.041(3) Uani 1 1 d . . . N4 N 0.3568(6) -0.1934(11) 0.8001(5) 0.083(5) Uani 1 1 d . . . N5 N 0.4318(4) 0.1445(7) 0.7202(3) 0.044(3) Uani 1 1 d . . . N6 N 0.4166(7) 0.4287(10) 0.7574(5) 0.081(4) Uani 1 1 d . . . N7 N 0.3509(3) 0.2680(7) 0.5350(3) 0.031(2) Uani 1 1 d . . . N8 N 0.3602(6) 0.2708(12) 0.3956(5) 0.084(5) Uani 1 1 d . . . N9 N 0.4086(3) -0.0947(7) -0.0080(3) 0.031(2) Uani 1 1 d . . . N10 N 0.3626(4) -0.3795(6) -0.0413(4) 0.035(3) Uani 1 1 d . . . N11 N 0.3092(4) -0.1632(8) 0.1300(3) 0.043(3) Uani 1 1 d . . . N12 N 0.3383(7) -0.2042(15) 0.2791(6) 0.113(6) Uani 1 1 d . . . N13 N 0.4290(4) 0.1428(7) 0.2065(3) 0.041(3) Uani 1 1 d . . . N14 N 0.3796(5) 0.4083(9) 0.2387(4) 0.060(3) Uani 1 1 d . . . N15 N 0.3428(3) 0.2656(7) 0.0230(3) 0.033(2) Uani 1 1 d . . . N16 N 0.3543(5) 0.2725(10) -0.1174(4) 0.067(4) Uani 1 1 d . . . C1 C 0.2743(5) -0.0397(12) 0.4269(4) 0.058(4) Uani 1 1 d . . . H1 H 0.2639 -0.0955 0.4405 0.070 Uiso 1 1 calc R . . C2 C 0.2328(6) 0.0251(11) 0.4210(5) 0.066(5) Uani 1 1 d . . . H2A H 0.2416 0.0818 0.4081 0.099 Uiso 1 1 calc R . . H2B H 0.2270 0.0378 0.4504 0.099 Uiso 1 1 calc R . . H2C H 0.2020 -0.0006 0.4005 0.099 Uiso 1 1 calc R . . C3 C 0.2843(7) -0.0678(16) 0.3861(5) 0.109(8) Uani 1 1 d . . . H3A H 0.2910 -0.0143 0.3697 0.164 Uiso 1 1 calc R . . H3B H 0.2549 -0.1007 0.3674 0.164 Uiso 1 1 calc R . . H3C H 0.3141 -0.1079 0.3932 0.164 Uiso 1 1 calc R . . C4 C 0.3628(4) -0.2289(8) 0.5055(5) 0.038(3) Uani 1 1 d . . . H4 H 0.3831 -0.2482 0.5364 0.046 Uiso 1 1 calc R . . C5 C 0.3980(5) -0.1829(8) 0.4809(4) 0.037(3) Uani 1 1 d . . . H5A H 0.4276 -0.2223 0.4822 0.044 Uiso 1 1 calc R . . H5B H 0.3795 -0.1727 0.4487 0.044 Uiso 1 1 calc R . . C6 C 0.4311(5) -0.0339(9) 0.4719(4) 0.039(3) Uani 1 1 d . . . H6A H 0.4602 -0.0610 0.4642 0.059 Uiso 1 1 calc R . . H6B H 0.4408 0.0256 0.4862 0.059 Uiso 1 1 calc R . . H6C H 0.4030 -0.0263 0.4444 0.059 Uiso 1 1 calc R . . C7 C 0.4591(4) -0.1096(8) 0.5437(4) 0.036(3) Uani 1 1 d . . . H7A H 0.4507 -0.1570 0.5628 0.055 Uiso 1 1 calc R . . H7B H 0.4674 -0.0530 0.5610 0.055 Uiso 1 1 calc R . . H7C H 0.4883 -0.1291 0.5336 0.055 Uiso 1 1 calc R . . C8 C 0.3340(5) -0.3104(9) 0.4804(5) 0.047(4) Uani 1 1 d . . . H8A H 0.3150 -0.3401 0.4994 0.057 Uiso 1 1 calc R . . H8B H 0.3092 -0.2893 0.4522 0.057 Uiso 1 1 calc R . . C9 C 0.3998(6) -0.4210(10) 0.5086(6) 0.061(4) Uani 1 1 d . . . H9A H 0.4215 -0.3758 0.5283 0.092 Uiso 1 1 calc R . . H9B H 0.4211 -0.4668 0.4996 0.092 Uiso 1 1 calc R . . H9C H 0.3783 -0.4507 0.5250 0.092 Uiso 1 1 calc R . . C10 C 0.3370(6) -0.4476(11) 0.4392(6) 0.076(5) Uani 1 1 d . . . H10A H 0.3161 -0.4791 0.4556 0.115 Uiso 1 1 calc R . . H10B H 0.3593 -0.4917 0.4304 0.115 Uiso 1 1 calc R . . H10C H 0.3151 -0.4187 0.4121 0.115 Uiso 1 1 calc R . . C11 C 0.4416(6) -0.2989(10) 0.6565(5) 0.058(4) Uani 1 1 d . . . H11 H 0.4445 -0.2896 0.6893 0.070 Uiso 1 1 calc R . . C12 C 0.4931(6) -0.2908(12) 0.6490(6) 0.081(5) Uani 1 1 d . . . H12A H 0.4903 -0.2998 0.6169 0.121 Uiso 1 1 calc R . . H12B H 0.5157 -0.3371 0.6669 0.121 Uiso 1 1 calc R . . H12C H 0.5070 -0.2301 0.6583 0.121 Uiso 1 1 calc R . . C13 C 0.4175(8) -0.3911(11) 0.6416(6) 0.084(6) Uani 1 1 d . . . H13A H 0.3857 -0.3963 0.6501 0.126 Uiso 1 1 calc R . . H13B H 0.4408 -0.4395 0.6564 0.126 Uiso 1 1 calc R . . H13C H 0.4104 -0.3970 0.6087 0.126 Uiso 1 1 calc R . . C14 C 0.3609(5) -0.1585(9) 0.7215(4) 0.047(4) Uani 1 1 d . . . H14 H 0.3456 -0.1005 0.7286 0.056 Uiso 1 1 calc R . . C15 C 0.3228(6) -0.2114(11) 0.6839(4) 0.055(4) Uani 1 1 d . . . H15A H 0.3366 -0.2723 0.6801 0.066 Uiso 1 1 calc R . . H15B H 0.2905 -0.2196 0.6917 0.066 Uiso 1 1 calc R . . C16 C 0.2776(5) -0.0858(9) 0.6385(5) 0.048(4) Uani 1 1 d . . . H16A H 0.2439 -0.1122 0.6350 0.071 Uiso 1 1 calc R . . H16B H 0.2767 -0.0469 0.6124 0.071 Uiso 1 1 calc R . . H16C H 0.2875 -0.0494 0.6663 0.071 Uiso 1 1 calc R . . C17 C 0.2934(5) -0.2214(10) 0.6026(5) 0.055(4) Uani 1 1 d . . . H17A H 0.2603 -0.2441 0.6039 0.083 Uiso 1 1 calc R . . H17B H 0.3167 -0.2726 0.6046 0.083 Uiso 1 1 calc R . . H17C H 0.2896 -0.1890 0.5740 0.083 Uiso 1 1 calc R . . C18 C 0.3768(6) -0.2225(12) 0.7644(5) 0.067(5) Uani 1 1 d . . . H18A H 0.3649 -0.2851 0.7554 0.080 Uiso 1 1 calc R . . H18B H 0.4143 -0.2242 0.7757 0.080 Uiso 1 1 calc R . . C19 C 0.3887(10) -0.1136(16) 0.8230(7) 0.126(9) Uani 1 1 d . . . H19A H 0.4183 -0.1361 0.8463 0.189 Uiso 1 1 calc R . . H19B H 0.3684 -0.0744 0.8370 0.189 Uiso 1 1 calc R . . H19C H 0.4000 -0.0785 0.8005 0.189 Uiso 1 1 calc R . . C20 C 0.3618(7) -0.2654(12) 0.8331(5) 0.075(5) Uani 1 1 d . . . H20A H 0.3470 -0.3215 0.8178 0.113 Uiso 1 1 calc R . . H20B H 0.3441 -0.2481 0.8554 0.113 Uiso 1 1 calc R . . H20C H 0.3978 -0.2754 0.8484 0.113 Uiso 1 1 calc R . . C21 C 0.2774(6) 0.1290(11) 0.7146(5) 0.061(4) Uani 1 1 d . . . H21 H 0.2527 0.1184 0.6843 0.074 Uiso 1 1 calc R . . C22 C 0.2646(7) 0.0668(14) 0.7461(7) 0.098(7) Uani 1 1 d . . . H22A H 0.2695 0.0040 0.7374 0.146 Uiso 1 1 calc R . . H22B H 0.2291 0.0757 0.7456 0.146 Uiso 1 1 calc R . . H22C H 0.2865 0.0785 0.7767 0.146 Uiso 1 1 calc R . . C23 C 0.2734(7) 0.2278(13) 0.7264(6) 0.087(6) Uani 1 1 d . . . H23A H 0.2957 0.2396 0.7569 0.131 Uiso 1 1 calc R . . H23B H 0.2383 0.2418 0.7256 0.131 Uiso 1 1 calc R . . H23C H 0.2838 0.2662 0.7045 0.131 Uiso 1 1 calc R . . C24 C 0.4054(6) 0.2995(10) 0.7014(5) 0.056(4) Uani 1 1 d . . . H24 H 0.4304 0.3146 0.6844 0.068 Uiso 1 1 calc R . . C25 C 0.4280(6) 0.2353(9) 0.7385(5) 0.060(4) Uani 1 1 d . . . H25A H 0.4621 0.2568 0.7556 0.072 Uiso 1 1 calc R . . H25B H 0.4066 0.2325 0.7597 0.072 Uiso 1 1 calc R . . C26 C 0.4383(6) 0.0741(11) 0.7553(5) 0.062(4) Uani 1 1 d . . . H26A H 0.4705 0.0840 0.7786 0.092 Uiso 1 1 calc R . . H26B H 0.4387 0.0139 0.7417 0.092 Uiso 1 1 calc R . . H26C H 0.4102 0.0774 0.7691 0.092 Uiso 1 1 calc R . . C27 C 0.4775(5) 0.1371(10) 0.7033(5) 0.057(4) Uani 1 1 d . . . H27A H 0.4753 0.1822 0.6793 0.086 Uiso 1 1 calc R . . H27B H 0.4792 0.0759 0.6912 0.086 Uiso 1 1 calc R . . H27C H 0.5081 0.1484 0.7282 0.086 Uiso 1 1 calc R . . C28 C 0.3850(8) 0.3915(10) 0.7192(6) 0.089(7) Uani 1 1 d . . . H28A H 0.3787 0.4374 0.6948 0.106 Uiso 1 1 calc R . . H28B H 0.3521 0.3781 0.7251 0.106 Uiso 1 1 calc R . . C29 C 0.4672(9) 0.4564(17) 0.7493(8) 0.133(10) Uani 1 1 d . . . H29A H 0.4615 0.5071 0.7278 0.200 Uiso 1 1 calc R . . H29B H 0.4813 0.4045 0.7369 0.200 Uiso 1 1 calc R . . H29C H 0.4909 0.4752 0.7780 0.200 Uiso 1 1 calc R . . C30 C 0.3956(9) 0.5021(14) 0.7739(6) 0.108(8) Uani 1 1 d . . . H30A H 0.3775 0.5408 0.7486 0.162 Uiso 1 1 calc R . . H30B H 0.4226 0.5373 0.7946 0.162 Uiso 1 1 calc R . . H30C H 0.3718 0.4800 0.7900 0.162 Uiso 1 1 calc R . . C31 C 0.5032(5) 0.3156(10) 0.5964(5) 0.051(4) Uani 1 1 d . . . H31 H 0.5274 0.2631 0.6020 0.062 Uiso 1 1 calc R . . C32 C 0.5174(7) 0.3804(12) 0.6374(6) 0.080(6) Uani 1 1 d . . . H32A H 0.4925 0.4299 0.6327 0.121 Uiso 1 1 calc R . . H32B H 0.5512 0.4059 0.6405 0.121 Uiso 1 1 calc R . . H32C H 0.5175 0.3467 0.6649 0.121 Uiso 1 1 calc R . . C33 C 0.5056(6) 0.3644(11) 0.5542(6) 0.070(5) Uani 1 1 d . . . H33A H 0.4894 0.3271 0.5277 0.105 Uiso 1 1 calc R . . H33B H 0.5411 0.3753 0.5553 0.105 Uiso 1 1 calc R . . H33C H 0.4878 0.4228 0.5522 0.105 Uiso 1 1 calc R . . C34 C 0.3870(5) 0.2257(8) 0.4736(4) 0.035(3) Uani 1 1 d . . . H34 H 0.3622 0.1749 0.4634 0.042 Uiso 1 1 calc R . . C35 C 0.3617(5) 0.3011(9) 0.4942(4) 0.041(3) Uani 1 1 d . . . H35A H 0.3845 0.3546 0.5016 0.049 Uiso 1 1 calc R . . H35B H 0.3298 0.3204 0.4721 0.049 Uiso 1 1 calc R . . C36 C 0.3465(5) 0.3448(9) 0.5649(4) 0.047(4) Uani 1 1 d . . . H36A H 0.3801 0.3718 0.5780 0.070 Uiso 1 1 calc R . . H36B H 0.3330 0.3225 0.5892 0.070 Uiso 1 1 calc R . . H36C H 0.3236 0.3910 0.5473 0.070 Uiso 1 1 calc R . . C37 C 0.3020(4) 0.2186(9) 0.5234(4) 0.041(3) Uani 1 1 d . . . H37A H 0.2740 0.2623 0.5147 0.061 Uiso 1 1 calc R . . H37B H 0.2992 0.1837 0.5498 0.061 Uiso 1 1 calc R . . H37C H 0.3003 0.1770 0.4982 0.061 Uiso 1 1 calc R . . C38 C 0.4044(5) 0.2559(12) 0.4352(4) 0.059(4) Uani 1 1 d . . . H38A H 0.4269 0.2092 0.4279 0.071 Uiso 1 1 calc R . . H38B H 0.4239 0.3131 0.4430 0.071 Uiso 1 1 calc R . . C39 C 0.3722(8) 0.3290(18) 0.3627(6) 0.118(9) Uani 1 1 d . . . H39A H 0.3941 0.3787 0.3781 0.178 Uiso 1 1 calc R . . H39B H 0.3409 0.3542 0.3427 0.178 Uiso 1 1 calc R . . H39C H 0.3899 0.2938 0.3447 0.178 Uiso 1 1 calc R . . C40 C 0.3377(8) 0.1847(19) 0.3735(7) 0.121(9) Uani 1 1 d . . . H40A H 0.3064 0.1983 0.3498 0.182 Uiso 1 1 calc R . . H40B H 0.3300 0.1445 0.3961 0.182 Uiso 1 1 calc R . . H40C H 0.3618 0.1546 0.3600 0.182 Uiso 1 1 calc R . . C41 C 0.2668(5) -0.0371(9) -0.0846(4) 0.041(3) Uani 1 1 d . . . H41 H 0.2555 -0.0936 -0.0721 0.049 Uiso 1 1 calc R . . C42 C 0.2269(6) 0.0322(12) -0.0879(6) 0.072(5) Uani 1 1 d . . . H42A H 0.2239 0.0460 -0.0576 0.107 Uiso 1 1 calc R . . H42B H 0.1944 0.0087 -0.1068 0.107 Uiso 1 1 calc R . . H42C H 0.2358 0.0877 -0.1016 0.107 Uiso 1 1 calc R . . C43 C 0.2769(8) -0.0623(15) -0.1277(6) 0.102(7) Uani 1 1 d . . . H43A H 0.2887 -0.0087 -0.1407 0.153 Uiso 1 1 calc R . . H43B H 0.2456 -0.0852 -0.1488 0.153 Uiso 1 1 calc R . . H43C H 0.3030 -0.1098 -0.1221 0.153 Uiso 1 1 calc R . . C44 C 0.3563(4) -0.2277(8) -0.0076(4) 0.031(3) Uani 1 1 d . . . H44 H 0.3766 -0.2472 0.0233 0.037 Uiso 1 1 calc R . . C45 C 0.3908(5) -0.1813(8) -0.0307(4) 0.037(3) Uani 1 1 d . . . H45A H 0.4202 -0.2210 -0.0298 0.045 Uiso 1 1 calc R . . H45B H 0.3725 -0.1699 -0.0628 0.045 Uiso 1 1 calc R . . C46 C 0.4259(4) -0.0320(9) -0.0383(4) 0.036(3) Uani 1 1 d . . . H46A H 0.4529 -0.0610 -0.0484 0.054 Uiso 1 1 calc R . . H46B H 0.4388 0.0242 -0.0219 0.054 Uiso 1 1 calc R . . H46C H 0.3974 -0.0174 -0.0646 0.054 Uiso 1 1 calc R . . C47 C 0.4527(4) -0.1114(10) 0.0328(4) 0.045(4) Uani 1 1 d . . . H47A H 0.4429 -0.1556 0.0526 0.067 Uiso 1 1 calc R . . H47B H 0.4626 -0.0541 0.0492 0.067 Uiso 1 1 calc R . . H47C H 0.4814 -0.1353 0.0232 0.067 Uiso 1 1 calc R . . C48 C 0.3292(4) -0.3096(8) -0.0330(5) 0.038(3) Uani 1 1 d . . . H48A H 0.3076 -0.3365 -0.0154 0.046 Uiso 1 1 calc R . . H48B H 0.3066 -0.2890 -0.0623 0.046 Uiso 1 1 calc R . . C49 C 0.3895(6) -0.4239(10) 0.0003(6) 0.063(4) Uani 1 1 d . . . H49A H 0.4088 -0.3786 0.0216 0.095 Uiso 1 1 calc R . . H49B H 0.4128 -0.4693 -0.0060 0.095 Uiso 1 1 calc R . . H49C H 0.3651 -0.4540 0.0134 0.095 Uiso 1 1 calc R . . C50 C 0.3329(6) -0.4476(10) -0.0732(5) 0.064(5) Uani 1 1 d . . . H50A H 0.3105 -0.4804 -0.0588 0.096 Uiso 1 1 calc R . . H50B H 0.3560 -0.4908 -0.0814 0.096 Uiso 1 1 calc R . . H50C H 0.3125 -0.4169 -0.1005 0.096 Uiso 1 1 calc R . . C51 C 0.4389(6) -0.2987(10) 0.1471(5) 0.053(4) Uani 1 1 d . . . H51 H 0.4450 -0.2841 0.1799 0.064 Uiso 1 1 calc R . . C52 C 0.4886(6) -0.2940(12) 0.1357(6) 0.077(5) Uani 1 1 d . . . H52A H 0.4850 -0.3224 0.1061 0.116 Uiso 1 1 calc R . . H52B H 0.5147 -0.3264 0.1588 0.116 Uiso 1 1 calc R . . H52C H 0.4986 -0.2302 0.1347 0.116 Uiso 1 1 calc R . . C53 C 0.4157(7) -0.3913(10) 0.1384(6) 0.077(5) Uani 1 1 d . . . H53A H 0.3886 -0.3969 0.1533 0.116 Uiso 1 1 calc R . . H53B H 0.4417 -0.4375 0.1504 0.116 Uiso 1 1 calc R . . H53C H 0.4015 -0.4002 0.1058 0.116 Uiso 1 1 calc R . . C54 C 0.3555(6) -0.1504(11) 0.2093(4) 0.055(4) Uani 1 1 d . . . H54 H 0.3401 -0.0895 0.2115 0.066 Uiso 1 1 calc R . . C55 C 0.3180(6) -0.2053(10) 0.1756(5) 0.052(4) Uani 1 1 d . . . H55A H 0.2857 -0.2081 0.1839 0.063 Uiso 1 1 calc R . . H55B H 0.3308 -0.2682 0.1751 0.063 Uiso 1 1 calc R . . C56 C 0.2715(6) -0.0900(12) 0.1235(6) 0.066(5) Uani 1 1 d . . . H56A H 0.2378 -0.1164 0.1195 0.099 Uiso 1 1 calc R . . H56B H 0.2718 -0.0548 0.0965 0.099 Uiso 1 1 calc R . . H56C H 0.2799 -0.0500 0.1500 0.099 Uiso 1 1 calc R . . C57 C 0.2913(6) -0.2293(10) 0.0940(5) 0.055(4) Uani 1 1 d . . . H57A H 0.2613 -0.2606 0.0980 0.083 Uiso 1 1 calc R . . H57B H 0.3181 -0.2739 0.0949 0.083 Uiso 1 1 calc R . . H57C H 0.2823 -0.1980 0.0647 0.083 Uiso 1 1 calc R . . C58 C 0.3733(7) -0.1905(11) 0.2565(5) 0.069(5) Uani 1 1 d . . . H58A H 0.3897 -0.2498 0.2544 0.083 Uiso 1 1 calc R . . H58B H 0.3998 -0.1499 0.2751 0.083 Uiso 1 1 calc R . . C59 C 0.3141(17) -0.118(3) 0.2854(10) 0.28(3) Uani 1 1 d . . . H59A H 0.3379 -0.0815 0.3084 0.427 Uiso 1 1 calc R . . H59B H 0.2838 -0.1309 0.2953 0.427 Uiso 1 1 calc R . . H59C H 0.3044 -0.0847 0.2567 0.427 Uiso 1 1 calc R . . C60 C 0.3598(9) -0.2430(17) 0.3250(7) 0.119(8) Uani 1 1 d . . . H60A H 0.3700 -0.3063 0.3224 0.179 Uiso 1 1 calc R . . H60B H 0.3342 -0.2410 0.3417 0.179 Uiso 1 1 calc R . . H60C H 0.3895 -0.2074 0.3413 0.179 Uiso 1 1 calc R . . C61 C 0.2799(5) 0.1479(11) 0.2102(5) 0.052(4) Uani 1 1 d . . . H61 H 0.2693 0.2033 0.1909 0.062 Uiso 1 1 calc R . . C62 C 0.2945(8) 0.1725(15) 0.2579(6) 0.103(7) Uani 1 1 d . . . H62A H 0.3050 0.1177 0.2763 0.155 Uiso 1 1 calc R . . H62B H 0.2656 0.2005 0.2656 0.155 Uiso 1 1 calc R . . H62C H 0.3228 0.2158 0.2640 0.155 Uiso 1 1 calc R . . C63 C 0.2382(8) 0.0800(15) 0.2006(8) 0.104(7) Uani 1 1 d . . . H63A H 0.2325 0.0566 0.1698 0.156 Uiso 1 1 calc R . . H63B H 0.2071 0.1090 0.2034 0.156 Uiso 1 1 calc R . . H63C H 0.2474 0.0297 0.2222 0.156 Uiso 1 1 calc R . . C64 C 0.4018(5) 0.2968(9) 0.1859(5) 0.047(4) Uani 1 1 d . . . H64 H 0.4228 0.2971 0.1641 0.056 Uiso 1 1 calc R . . C65 C 0.4282(5) 0.2356(9) 0.2245(4) 0.052(4) Uani 1 1 d . . . H65A H 0.4632 0.2572 0.2383 0.062 Uiso 1 1 calc R . . H65B H 0.4098 0.2359 0.2480 0.062 Uiso 1 1 calc R . . C66 C 0.4344(5) 0.0757(9) 0.2434(4) 0.044(3) Uani 1 1 d . . . H66A H 0.4358 0.0142 0.2315 0.066 Uiso 1 1 calc R . . H66B H 0.4052 0.0804 0.2558 0.066 Uiso 1 1 calc R . . H66C H 0.4656 0.0881 0.2674 0.066 Uiso 1 1 calc R . . C67 C 0.4729(5) 0.1315(10) 0.1881(5) 0.050(4) Uani 1 1 d . . . H67A H 0.5042 0.1285 0.2131 0.076 Uiso 1 1 calc R . . H67B H 0.4747 0.1833 0.1685 0.076 Uiso 1 1 calc R . . H67C H 0.4690 0.0751 0.1704 0.076 Uiso 1 1 calc R . . C68 C 0.3974(6) 0.3930(10) 0.1997(5) 0.058(4) Uani 1 1 d . . . H68A H 0.4313 0.4218 0.2054 0.069 Uiso 1 1 calc R . . H68B H 0.3744 0.4252 0.1738 0.069 Uiso 1 1 calc R . . C69 C 0.3233(8) 0.4076(13) 0.2241(7) 0.092(6) Uani 1 1 d . . . H69A H 0.3105 0.4153 0.2505 0.138 Uiso 1 1 calc R . . H69B H 0.3113 0.3494 0.2094 0.138 Uiso 1 1 calc R . . H69C H 0.3109 0.4575 0.2027 0.138 Uiso 1 1 calc R . . C70 C 0.3976(8) 0.4879(13) 0.2641(6) 0.098(7) Uani 1 1 d . . . H70A H 0.4347 0.4881 0.2732 0.147 Uiso 1 1 calc R . . H70B H 0.3854 0.4887 0.2912 0.147 Uiso 1 1 calc R . . H70C H 0.3849 0.5418 0.2457 0.147 Uiso 1 1 calc R . . C71 C 0.4954(5) 0.3188(8) 0.0834(5) 0.046(4) Uani 1 1 d . . . H71 H 0.5201 0.2675 0.0923 0.055 Uiso 1 1 calc R . . C72 C 0.5056(6) 0.3862(13) 0.1221(7) 0.086(6) Uani 1 1 d . . . H72A H 0.4986 0.3574 0.1484 0.129 Uiso 1 1 calc R . . H72B H 0.4835 0.4394 0.1130 0.129 Uiso 1 1 calc R . . H72C H 0.5412 0.4055 0.1299 0.129 Uiso 1 1 calc R . . C73 C 0.5005(6) 0.3587(12) 0.0401(6) 0.068(5) Uani 1 1 d . . . H73A H 0.4889 0.3144 0.0156 0.101 Uiso 1 1 calc R . . H73B H 0.5361 0.3739 0.0435 0.101 Uiso 1 1 calc R . . H73C H 0.4798 0.4140 0.0330 0.101 Uiso 1 1 calc R . . C74 C 0.3796(5) 0.2259(10) -0.0372(4) 0.048(4) Uani 1 1 d . . . H74 H 0.3546 0.1754 -0.0474 0.057 Uiso 1 1 calc R . . C75 C 0.3546(5) 0.2996(9) -0.0180(4) 0.041(3) Uani 1 1 d . . . H75A H 0.3774 0.3530 -0.0103 0.049 Uiso 1 1 calc R . . H75B H 0.3230 0.3188 -0.0406 0.049 Uiso 1 1 calc R . . C76 C 0.3381(5) 0.3444(8) 0.0523(5) 0.041(3) Uani 1 1 d . . . H76A H 0.3698 0.3792 0.0601 0.062 Uiso 1 1 calc R . . H76B H 0.3313 0.3220 0.0800 0.062 Uiso 1 1 calc R . . H76C H 0.3102 0.3837 0.0359 0.062 Uiso 1 1 calc R . . C77 C 0.2938(4) 0.2173(8) 0.0109(4) 0.037(3) Uani 1 1 d . . . H77A H 0.2665 0.2605 -0.0024 0.056 Uiso 1 1 calc R . . H77B H 0.2881 0.1900 0.0381 0.056 Uiso 1 1 calc R . . H77C H 0.2943 0.1694 -0.0112 0.056 Uiso 1 1 calc R . . C78 C 0.3982(5) 0.2549(11) -0.0771(4) 0.051(4) Uani 1 1 d . . . H78A H 0.4190 0.3108 -0.0692 0.061 Uiso 1 1 calc R . . H78B H 0.4199 0.2065 -0.0842 0.061 Uiso 1 1 calc R . . C79 C 0.3688(7) 0.3332(13) -0.1487(6) 0.081(6) Uani 1 1 d . . . H79A H 0.3858 0.3869 -0.1324 0.122 Uiso 1 1 calc R . . H79B H 0.3385 0.3522 -0.1723 0.122 Uiso 1 1 calc R . . H79C H 0.3920 0.3015 -0.1627 0.122 Uiso 1 1 calc R . . C80 C 0.3337(8) 0.1851(15) -0.1403(6) 0.099(7) Uani 1 1 d . . . H80A H 0.3042 0.1981 -0.1660 0.148 Uiso 1 1 calc R . . H80B H 0.3236 0.1454 -0.1188 0.148 Uiso 1 1 calc R . . H80C H 0.3599 0.1549 -0.1512 0.148 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 0.0195(3) 0.0263(3) 0.0367(3) -0.0027(2) 0.0073(2) -0.0004(2) W2 0.0324(3) 0.0308(3) 0.0371(3) 0.0018(2) 0.0041(2) -0.0023(2) W3 0.0336(3) 0.0345(3) 0.0335(3) -0.0015(2) 0.0107(2) 0.0008(2) W4 0.0227(3) 0.0253(3) 0.0362(3) -0.0023(2) 0.0083(2) 0.0002(2) W5 0.0200(3) 0.0222(3) 0.0342(3) -0.0006(2) 0.0091(2) -0.0007(2) W6 0.0344(3) 0.0256(3) 0.0365(3) 0.0030(2) 0.0050(2) -0.0041(2) W7 0.0285(3) 0.0348(3) 0.0337(3) -0.0008(2) 0.0118(2) -0.0003(2) W8 0.0211(3) 0.0215(3) 0.0367(3) -0.0026(2) 0.0109(2) -0.0009(2) O1 0.031(5) 0.014(4) 0.069(6) 0.000(4) 0.027(4) -0.005(4) O2 0.022(4) 0.032(5) 0.059(6) 0.006(4) 0.017(4) 0.005(4) O3 0.017(4) 0.020(4) 0.056(5) -0.002(4) 0.009(4) -0.006(3) O4 0.023(4) 0.025(5) 0.049(5) -0.007(4) 0.013(4) -0.005(4) O5 0.035(5) 0.011(4) 0.033(4) -0.003(3) 0.003(4) -0.004(3) O6 0.022(4) 0.039(5) 0.047(5) -0.004(4) 0.004(4) 0.008(4) O7 0.040(5) 0.030(5) 0.037(5) -0.001(4) 0.014(4) -0.005(4) O8 0.024(5) 0.027(5) 0.051(5) -0.009(4) 0.008(4) -0.007(4) O9 0.033(5) 0.043(5) 0.031(5) -0.002(4) 0.000(4) 0.003(4) O10 0.029(5) 0.044(6) 0.054(6) 0.002(4) 0.014(4) 0.003(4) O11 0.045(6) 0.064(7) 0.041(5) 0.001(5) 0.017(4) 0.007(5) O12 0.051(6) 0.025(5) 0.039(5) -0.001(4) 0.016(4) 0.001(4) O13 0.036(5) 0.043(6) 0.035(5) 0.006(4) 0.006(4) -0.010(4) O14 0.030(5) 0.064(7) 0.049(6) -0.007(5) 0.003(4) -0.001(5) O15 0.048(5) 0.021(5) 0.050(5) 0.014(4) 0.004(4) 0.007(4) O16 0.048(6) 0.046(6) 0.044(5) 0.006(4) 0.006(4) -0.007(5) O17 0.029(4) 0.025(5) 0.036(5) -0.001(4) 0.007(4) 0.004(4) O18 0.029(5) 0.036(5) 0.045(5) 0.002(4) 0.011(4) 0.007(4) O19 0.025(5) 0.053(6) 0.033(5) -0.006(4) 0.003(4) 0.002(4) O20 0.024(4) 0.029(5) 0.040(5) -0.008(4) 0.010(4) 0.000(4) O21 0.026(4) 0.028(5) 0.036(5) -0.001(4) 0.011(4) 0.005(4) O22 0.025(4) 0.029(5) 0.046(5) -0.004(4) 0.009(4) 0.000(4) O23 0.024(4) 0.021(5) 0.058(5) -0.012(4) 0.012(4) -0.004(4) O24 0.028(5) 0.022(5) 0.051(5) 0.000(4) 0.021(4) 0.005(4) O25 0.026(4) 0.010(4) 0.040(5) -0.005(3) 0.005(4) 0.002(3) O26 0.027(5) 0.051(6) 0.038(5) 0.002(4) 0.006(4) 0.002(4) O27 0.041(5) 0.041(5) 0.041(5) 0.003(4) 0.019(4) -0.003(4) O28 0.039(5) 0.057(6) 0.037(5) -0.003(4) 0.018(4) 0.004(5) O29 0.040(5) 0.029(5) 0.039(5) 0.002(4) 0.015(4) -0.007(4) O30 0.028(5) 0.025(5) 0.053(5) -0.001(4) 0.004(4) -0.008(4) O31 0.042(5) 0.050(6) 0.045(5) 0.007(5) -0.002(4) -0.011(5) O32 0.057(6) 0.041(6) 0.040(5) 0.010(4) 0.009(5) -0.013(5) N1 0.025(5) 0.013(5) 0.050(6) -0.003(4) 0.011(5) -0.006(4) N2 0.039(7) 0.040(7) 0.066(8) -0.015(6) 0.011(6) -0.001(6) N3 0.050(7) 0.026(6) 0.050(7) -0.004(5) 0.018(6) -0.011(5) N4 0.091(11) 0.094(12) 0.076(10) 0.022(9) 0.045(9) 0.007(9) N5 0.046(7) 0.041(7) 0.035(6) -0.002(5) -0.003(5) -0.002(5) N6 0.113(13) 0.053(10) 0.083(11) 0.009(8) 0.039(10) 0.017(9) N7 0.030(6) 0.031(6) 0.036(6) 0.008(5) 0.014(5) 0.005(5) N8 0.077(10) 0.126(14) 0.058(9) 0.020(10) 0.033(8) 0.044(10) N9 0.017(5) 0.036(6) 0.042(6) -0.006(5) 0.012(4) -0.001(5) N10 0.031(6) 0.013(5) 0.062(7) -0.007(5) 0.016(5) -0.001(5) N11 0.048(7) 0.046(7) 0.038(7) 0.000(5) 0.015(5) -0.007(6) N12 0.102(13) 0.147(18) 0.103(14) 0.021(12) 0.048(11) 0.039(13) N13 0.043(7) 0.035(7) 0.043(7) -0.010(5) 0.010(5) 0.002(5) N14 0.063(9) 0.057(9) 0.065(9) -0.006(7) 0.023(7) 0.001(7) N15 0.029(6) 0.029(6) 0.045(6) 0.000(5) 0.019(5) 0.003(5) N16 0.066(9) 0.085(11) 0.053(8) 0.012(7) 0.021(7) 0.011(8) C1 0.026(8) 0.099(13) 0.039(8) -0.029(8) -0.010(6) 0.002(8) C2 0.050(10) 0.068(12) 0.072(11) 0.008(9) 0.003(8) 0.002(9) C3 0.090(14) 0.17(2) 0.040(10) -0.037(12) -0.032(9) 0.042(14) C4 0.028(7) 0.021(7) 0.063(9) -0.006(6) 0.010(6) 0.008(6) C5 0.030(7) 0.022(7) 0.061(9) -0.006(6) 0.017(6) -0.001(6) C6 0.032(7) 0.039(8) 0.050(8) -0.005(6) 0.016(6) 0.006(6) C7 0.023(7) 0.028(7) 0.056(8) -0.004(6) 0.009(6) -0.006(6) C8 0.034(8) 0.044(9) 0.064(9) -0.009(7) 0.013(7) -0.013(7) C9 0.049(9) 0.030(9) 0.102(13) 0.001(8) 0.016(9) 0.018(7) C10 0.063(11) 0.049(11) 0.114(15) -0.036(10) 0.019(10) 0.002(9) C11 0.072(11) 0.053(10) 0.051(9) 0.004(8) 0.019(8) 0.010(9) C12 0.072(12) 0.069(13) 0.100(14) 0.012(10) 0.020(10) 0.025(10) C13 0.123(16) 0.038(10) 0.089(13) 0.014(9) 0.026(12) 0.016(10) C14 0.054(9) 0.037(9) 0.045(8) 0.002(6) 0.007(7) -0.003(7) C15 0.061(10) 0.062(10) 0.049(9) 0.009(8) 0.025(7) -0.024(8) C16 0.033(8) 0.042(9) 0.070(10) 0.010(7) 0.018(7) -0.014(7) C17 0.047(9) 0.052(10) 0.058(9) -0.006(8) 0.002(7) -0.017(8) C18 0.068(11) 0.085(13) 0.051(10) 0.011(9) 0.022(8) 0.012(10) C19 0.18(3) 0.102(18) 0.098(17) -0.022(14) 0.045(16) -0.069(18) C20 0.083(13) 0.089(14) 0.063(11) 0.021(10) 0.034(9) 0.000(10) C21 0.069(11) 0.073(12) 0.054(10) -0.006(8) 0.037(8) 0.014(9) C22 0.092(15) 0.103(16) 0.130(17) -0.019(13) 0.085(14) -0.024(12) C23 0.092(14) 0.089(15) 0.083(13) -0.011(11) 0.030(11) 0.006(12) C24 0.056(10) 0.058(10) 0.042(8) -0.008(7) -0.008(7) -0.013(8) C25 0.078(11) 0.032(9) 0.057(10) -0.002(7) -0.003(8) 0.006(8) C26 0.068(11) 0.065(11) 0.041(9) 0.008(8) -0.004(7) -0.003(9) C27 0.047(9) 0.052(10) 0.060(10) 0.000(8) -0.007(8) -0.011(8) C28 0.125(16) 0.017(8) 0.085(13) -0.007(8) -0.035(12) 0.002(9) C29 0.12(2) 0.12(2) 0.14(2) 0.033(16) 0.007(16) -0.054(17) C30 0.16(2) 0.075(15) 0.069(13) -0.023(11) 0.007(13) 0.010(14) C31 0.039(8) 0.053(10) 0.064(10) -0.010(8) 0.017(7) -0.005(7) C32 0.075(12) 0.072(13) 0.091(13) -0.039(10) 0.019(10) -0.031(10) C33 0.044(9) 0.064(12) 0.109(14) -0.009(10) 0.035(9) -0.018(8) C34 0.046(8) 0.028(7) 0.029(7) 0.004(5) 0.008(6) 0.011(6) C35 0.035(8) 0.043(9) 0.041(8) 0.010(6) 0.006(6) 0.015(6) C36 0.051(9) 0.041(9) 0.050(9) -0.004(7) 0.016(7) 0.016(7) C37 0.031(7) 0.047(9) 0.045(8) 0.007(6) 0.011(6) -0.002(6) C38 0.054(10) 0.088(13) 0.036(8) 0.011(8) 0.015(7) 0.018(9) C39 0.124(19) 0.17(2) 0.064(13) 0.041(14) 0.036(13) 0.063(17) C40 0.094(17) 0.20(3) 0.070(14) -0.031(16) 0.014(12) -0.015(17) C41 0.032(7) 0.040(8) 0.050(9) -0.008(6) 0.010(6) 0.000(6) C42 0.056(10) 0.077(13) 0.075(12) 0.000(9) 0.008(9) 0.001(9) C43 0.097(15) 0.103(16) 0.084(14) -0.038(12) -0.011(11) 0.017(13) C44 0.022(6) 0.021(7) 0.049(8) -0.005(6) 0.008(6) -0.004(5) C45 0.025(7) 0.035(8) 0.055(8) -0.013(6) 0.015(6) -0.003(6) C46 0.028(7) 0.038(8) 0.049(8) 0.003(6) 0.023(6) 0.001(6) C47 0.020(7) 0.061(10) 0.047(8) -0.014(7) 0.001(6) 0.000(6) C48 0.027(7) 0.029(8) 0.062(9) -0.003(6) 0.018(6) 0.003(6) C49 0.055(10) 0.046(10) 0.093(13) 0.010(9) 0.029(9) 0.003(8) C50 0.064(10) 0.040(10) 0.081(11) -0.026(8) 0.009(9) -0.007(8) C51 0.063(10) 0.041(9) 0.045(9) 0.015(7) 0.000(7) 0.021(8) C52 0.066(12) 0.070(12) 0.097(14) 0.013(10) 0.024(10) 0.027(10) C53 0.087(13) 0.029(9) 0.110(14) 0.023(9) 0.015(11) 0.008(9) C54 0.068(11) 0.064(11) 0.034(8) 0.003(7) 0.016(7) -0.001(9) C55 0.064(10) 0.040(9) 0.065(10) -0.005(7) 0.037(8) -0.003(8) C56 0.044(9) 0.084(13) 0.077(11) -0.001(9) 0.028(8) -0.015(9) C57 0.056(9) 0.054(10) 0.056(9) -0.002(8) 0.017(7) -0.028(8) C58 0.105(14) 0.052(11) 0.060(11) 0.009(8) 0.039(10) 0.000(10) C59 0.46(7) 0.31(5) 0.16(3) 0.13(3) 0.21(4) 0.30(5) C60 0.14(2) 0.15(2) 0.071(14) 0.030(14) 0.019(13) 0.043(17) C61 0.048(9) 0.056(10) 0.061(10) 0.006(8) 0.032(8) -0.003(8) C62 0.120(17) 0.125(19) 0.090(15) -0.015(13) 0.069(13) 0.039(14) C63 0.089(15) 0.105(17) 0.140(19) -0.017(14) 0.068(14) -0.003(13) C64 0.060(10) 0.026(8) 0.051(9) -0.015(6) 0.009(7) -0.007(7) C65 0.054(9) 0.045(9) 0.041(8) -0.013(7) -0.011(7) 0.008(7) C66 0.039(8) 0.043(9) 0.042(8) 0.005(7) -0.002(6) 0.010(7) C67 0.032(8) 0.057(10) 0.055(9) 0.006(7) 0.000(7) -0.012(7) C68 0.073(11) 0.042(9) 0.056(10) -0.006(7) 0.015(8) -0.002(8) C69 0.106(17) 0.077(14) 0.095(14) -0.031(11) 0.032(12) 0.006(12) C70 0.132(18) 0.081(14) 0.070(12) -0.045(11) 0.012(12) -0.022(13) C71 0.031(8) 0.018(7) 0.086(11) -0.016(7) 0.014(7) -0.011(6) C72 0.057(11) 0.085(14) 0.122(16) -0.058(12) 0.036(11) -0.041(10) C73 0.049(10) 0.070(12) 0.095(13) 0.003(10) 0.037(9) -0.013(9) C74 0.045(9) 0.058(10) 0.043(8) 0.013(7) 0.017(7) 0.008(7) C75 0.038(8) 0.044(9) 0.043(8) 0.007(6) 0.016(6) -0.005(7) C76 0.044(8) 0.022(7) 0.062(9) -0.003(6) 0.023(7) 0.002(6) C77 0.033(7) 0.026(7) 0.050(8) 0.013(6) 0.008(6) 0.009(6) C78 0.050(9) 0.063(10) 0.046(9) 0.007(7) 0.024(7) 0.008(8) C79 0.105(15) 0.082(14) 0.067(12) 0.009(10) 0.043(11) 0.020(11) C80 0.091(15) 0.117(18) 0.080(14) -0.016(12) 0.012(11) -0.023(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 O2 1.721(7) . ? W1 O5 1.815(7) . ? W1 O3 1.914(8) . ? W1 O4 1.937(7) . ? W1 O1 2.015(8) . ? W1 N1 2.460(9) . ? W2 O14 1.711(8) . ? W2 O1 1.809(8) . ? W2 O15 1.921(8) . ? W2 O16 1.937(9) . ? W2 O13 1.990(9) . ? W2 N3 2.485(10) . ? W3 O10 1.698(8) . ? W3 O13 1.835(9) . ? W3 O11 1.905(8) . ? W3 O12 1.929(8) . ? W3 O9 2.010(8) . ? W3 N5 2.428(10) . ? W4 O6 1.707(7) . ? W4 O9 1.828(8) . ? W4 O8 1.907(7) . ? W4 O7 1.946(8) . ? W4 O5 2.029(7) . ? W4 N7 2.466(9) . ? W5 O18 1.717(8) . ? W5 O21 1.840(8) . ? W5 O19 1.901(8) . ? W5 O20 1.921(8) . ? W5 O17 2.017(7) . ? W5 N9 2.470(9) . ? W6 O30 1.698(7) . ? W6 O17 1.817(7) . ? W6 O31 1.901(9) . ? W6 O32 1.941(8) . ? W6 O29 2.010(8) . ? W6 N11 2.488(11) . ? W7 O26 1.707(8) . ? W7 O29 1.827(8) . ? W7 O27 1.919(8) . ? W7 O28 1.929(9) . ? W7 O25 2.000(7) . ? W7 N13 2.461(10) . ? W8 O22 1.719(7) . ? W8 O25 1.837(7) . ? W8 O23 1.897(7) . ? W8 O24 1.930(8) . ? W8 O21 2.002(7) . ? W8 N15 2.454(9) . ? O3 C1 1.448(14) . ? O4 C4 1.416(13) . ? O7 C34 1.419(14) . ? O8 C31 1.427(15) . ? O11 C21 1.459(17) . ? O12 C24 1.411(15) . ? O15 C11 1.415(16) . ? O16 C14 1.417(16) . ? O19 C41 1.464(14) . ? O20 C44 1.426(13) . ? O23 C71 1.448(14) . ? O24 C74 1.431(15) . ? O27 C61 1.446(16) . ? O28 C64 1.418(15) . ? O31 C51 1.428(15) . ? O32 C54 1.397(17) . ? N1 C6 1.476(15) . ? N1 C7 1.482(15) . ? N1 C5 1.492(14) . ? N2 C9 1.437(18) . ? N2 C8 1.466(17) . ? N2 C10 1.493(18) . ? N3 C16 1.447(16) . ? N3 C17 1.488(16) . ? N3 C15 1.491(17) . ? N4 C18 1.42(2) . ? N4 C20 1.45(2) . ? N4 C19 1.52(2) . ? N5 C25 1.464(17) . ? N5 C26 1.470(17) . ? N5 C27 1.492(18) . ? N6 C28 1.37(2) . ? N6 C30 1.38(2) . ? N6 C29 1.53(3) . ? N7 C35 1.450(15) . ? N7 C37 1.480(15) . ? N7 C36 1.483(15) . ? N8 C39 1.43(2) . ? N8 C38 1.476(19) . ? N8 C40 1.49(3) . ? N9 C45 1.467(15) . ? N9 C46 1.479(15) . ? N9 C47 1.501(15) . ? N10 C49 1.443(17) . ? N10 C48 1.448(15) . ? N10 C50 1.477(16) . ? N11 C57 1.453(17) . ? N11 C56 1.466(19) . ? N11 C55 1.489(17) . ? N12 C58 1.35(2) . ? N12 C59 1.47(3) . ? N12 C60 1.49(2) . ? N13 C65 1.473(16) . ? N13 C67 1.479(17) . ? N13 C66 1.480(16) . ? N14 C70 1.416(19) . ? N14 C68 1.434(18) . ? N14 C69 1.49(2) . ? N15 C77 1.473(15) . ? N15 C75 1.476(15) . ? N15 C76 1.494(15) . ? N16 C79 1.45(2) . ? N16 C78 1.491(18) . ? N16 C80 1.50(2) . ? C1 C3 1.42(2) . ? C1 C2 1.46(2) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C8 1.521(17) . ? C4 C5 1.542(17) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.50(2) . ? C11 C13 1.52(2) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.536(19) . ? C14 C18 1.581(19) . ? C14 H14 1.0000 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.45(2) . ? C21 C23 1.51(2) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.477(19) . ? C24 C28 1.62(2) . ? C24 H24 1.0000 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.50(2) . ? C31 C32 1.54(2) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C38 1.463(18) . ? C34 C35 1.538(17) . ? C34 H34 1.0000 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.48(2) . ? C41 C42 1.478(19) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.499(17) . ? C44 C48 1.512(16) . ? C44 H44 1.0000 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C53 1.49(2) . ? C51 C52 1.50(2) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.48(2) . ? C54 C58 1.52(2) . ? C54 H54 1.0000 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.46(2) . ? C61 C63 1.48(2) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C68 1.491(18) . ? C64 C65 1.503(18) . ? C64 H64 1.0000 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C73 1.50(2) . ? C71 C72 1.514(19) . ? C71 H71 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C75 1.491(18) . ? C74 C78 1.517(18) . ? C74 H74 1.0000 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W1 O5 106.5(4) . . ? O2 W1 O3 96.9(3) . . ? O5 W1 O3 93.0(3) . . ? O2 W1 O4 95.4(3) . . ? O5 W1 O4 157.0(3) . . ? O3 W1 O4 91.4(3) . . ? O2 W1 O1 96.3(3) . . ? O5 W1 O1 86.0(3) . . ? O3 W1 O1 166.6(3) . . ? O4 W1 O1 84.5(3) . . ? O2 W1 N1 169.7(3) . . ? O5 W1 N1 83.8(3) . . ? O3 W1 N1 82.0(3) . . ? O4 W1 N1 74.4(3) . . ? O1 W1 N1 84.6(3) . . ? O14 W2 O1 105.0(4) . . ? O14 W2 O15 98.6(4) . . ? O1 W2 O15 91.6(3) . . ? O14 W2 O16 95.4(4) . . ? O1 W2 O16 159.1(4) . . ? O15 W2 O16 89.4(4) . . ? O14 W2 O13 98.2(4) . . ? O1 W2 O13 87.4(3) . . ? O15 W2 O13 162.8(3) . . ? O16 W2 O13 85.6(4) . . ? O14 W2 N3 170.1(4) . . ? O1 W2 N3 84.9(3) . . ? O15 W2 N3 81.7(4) . . ? O16 W2 N3 74.7(4) . . ? O13 W2 N3 81.2(3) . . ? O10 W3 O13 106.5(4) . . ? O10 W3 O11 94.5(4) . . ? O13 W3 O11 92.0(4) . . ? O10 W3 O12 96.0(4) . . ? O13 W3 O12 156.7(3) . . ? O11 W3 O12 92.5(4) . . ? O10 W3 O9 96.4(4) . . ? O13 W3 O9 87.4(3) . . ? O11 W3 O9 168.9(3) . . ? O12 W3 O9 83.7(3) . . ? O10 W3 N5 168.9(4) . . ? O13 W3 N5 83.8(3) . . ? O11 W3 N5 80.6(4) . . ? O12 W3 N5 74.4(4) . . ? O9 W3 N5 88.3(3) . . ? O6 W4 O9 105.5(4) . . ? O6 W4 O8 95.6(4) . . ? O9 W4 O8 92.8(4) . . ? O6 W4 O7 95.9(4) . . ? O9 W4 O7 157.4(3) . . ? O8 W4 O7 92.3(3) . . ? O6 W4 O5 98.6(3) . . ? O9 W4 O5 87.0(3) . . ? O8 W4 O5 165.4(3) . . ? O7 W4 O5 82.5(3) . . ? O6 W4 N7 169.6(4) . . ? O9 W4 N7 84.5(3) . . ? O8 W4 N7 81.0(3) . . ? O7 W4 N7 74.6(3) . . ? O5 W4 N7 84.4(3) . . ? O18 W5 O21 105.2(4) . . ? O18 W5 O19 96.7(3) . . ? O21 W5 O19 94.3(3) . . ? O18 W5 O20 95.6(3) . . ? O21 W5 O20 157.9(3) . . ? O19 W5 O20 90.4(3) . . ? O18 W5 O17 97.7(3) . . ? O21 W5 O17 87.7(3) . . ? O19 W5 O17 164.3(3) . . ? O20 W5 O17 82.3(3) . . ? O18 W5 N9 169.6(3) . . ? O21 W5 N9 85.1(3) . . ? O19 W5 N9 81.3(3) . . ? O20 W5 N9 74.3(3) . . ? O17 W5 N9 83.4(3) . . ? O30 W6 O17 105.8(4) . . ? O30 W6 O31 97.6(4) . . ? O17 W6 O31 91.1(3) . . ? O30 W6 O32 95.4(4) . . ? O17 W6 O32 158.5(4) . . ? O31 W6 O32 89.8(4) . . ? O30 W6 O29 98.1(3) . . ? O17 W6 O29 88.9(3) . . ? O31 W6 O29 163.7(3) . . ? O32 W6 O29 84.3(3) . . ? O30 W6 N11 170.2(4) . . ? O17 W6 N11 84.0(3) . . ? O31 W6 N11 81.4(4) . . ? O32 W6 N11 74.9(4) . . ? O29 W6 N11 82.4(3) . . ? O26 W7 O29 106.6(4) . . ? O26 W7 O27 95.0(4) . . ? O29 W7 O27 92.3(3) . . ? O26 W7 O28 96.1(4) . . ? O29 W7 O28 156.6(3) . . ? O27 W7 O28 91.3(3) . . ? O26 W7 O25 97.7(3) . . ? O29 W7 O25 87.1(3) . . ? O27 W7 O25 166.9(3) . . ? O28 W7 O25 84.3(3) . . ? O26 W7 N13 170.1(4) . . ? O29 W7 N13 83.1(3) . . ? O27 W7 N13 82.4(4) . . ? O28 W7 N13 74.4(3) . . ? O25 W7 N13 84.6(3) . . ? O22 W8 O25 104.5(3) . . ? O22 W8 O23 96.5(3) . . ? O25 W8 O23 92.7(3) . . ? O22 W8 O24 95.8(3) . . ? O25 W8 O24 158.5(3) . . ? O23 W8 O24 91.8(3) . . ? O22 W8 O21 98.2(3) . . ? O25 W8 O21 87.4(3) . . ? O23 W8 O21 164.8(3) . . ? O24 W8 O21 82.9(3) . . ? O22 W8 N15 170.5(3) . . ? O25 W8 N15 84.8(3) . . ? O23 W8 N15 81.4(3) . . ? O24 W8 N15 75.1(3) . . ? O21 W8 N15 83.5(3) . . ? W2 O1 W1 172.3(5) . . ? C1 O3 W1 124.6(8) . . ? C4 O4 W1 125.4(7) . . ? W1 O5 W4 166.1(4) . . ? C34 O7 W4 123.3(7) . . ? C31 O8 W4 129.4(8) . . ? W4 O9 W3 171.6(5) . . ? C21 O11 W3 128.2(8) . . ? C24 O12 W3 125.1(8) . . ? W3 O13 W2 165.0(5) . . ? C11 O15 W2 128.9(8) . . ? C14 O16 W2 124.6(8) . . ? W6 O17 W5 167.5(4) . . ? C41 O19 W5 124.7(8) . . ? C44 O20 W5 125.1(6) . . ? W5 O21 W8 168.2(4) . . ? C71 O23 W8 130.1(7) . . ? C74 O24 W8 122.5(7) . . ? W8 O25 W7 169.2(4) . . ? C61 O27 W7 125.5(8) . . ? C64 O28 W7 122.8(8) . . ? W7 O29 W6 167.4(4) . . ? C51 O31 W6 130.4(8) . . ? C54 O32 W6 122.5(8) . . ? C6 N1 C7 108.4(9) . . ? C6 N1 C5 108.9(9) . . ? C7 N1 C5 109.5(9) . . ? C6 N1 W1 111.9(7) . . ? C7 N1 W1 113.9(7) . . ? C5 N1 W1 104.0(6) . . ? C9 N2 C8 111.9(12) . . ? C9 N2 C10 108.1(12) . . ? C8 N2 C10 108.1(10) . . ? C16 N3 C17 108.0(11) . . ? C16 N3 C15 111.9(11) . . ? C17 N3 C15 107.8(11) . . ? C16 N3 W2 115.1(7) . . ? C17 N3 W2 111.9(8) . . ? C15 N3 W2 101.9(8) . . ? C18 N4 C20 109.9(14) . . ? C18 N4 C19 107.1(15) . . ? C20 N4 C19 108.0(15) . . ? C25 N5 C26 111.4(11) . . ? C25 N5 C27 111.1(12) . . ? C26 N5 C27 105.3(11) . . ? C25 N5 W3 103.3(8) . . ? C26 N5 W3 113.8(8) . . ? C27 N5 W3 112.1(8) . . ? C28 N6 C30 113.4(16) . . ? C28 N6 C29 110.7(17) . . ? C30 N6 C29 110.0(18) . . ? C35 N7 C37 110.4(10) . . ? C35 N7 C36 110.7(10) . . ? C37 N7 C36 107.3(10) . . ? C35 N7 W4 103.8(7) . . ? C37 N7 W4 112.5(7) . . ? C36 N7 W4 112.2(7) . . ? C39 N8 C38 112.0(16) . . ? C39 N8 C40 109.5(17) . . ? C38 N8 C40 113.1(16) . . ? C45 N9 C46 111.3(9) . . ? C45 N9 C47 109.9(10) . . ? C46 N9 C47 107.7(9) . . ? C45 N9 W5 102.9(6) . . ? C46 N9 W5 111.7(7) . . ? C47 N9 W5 113.3(7) . . ? C49 N10 C48 110.8(11) . . ? C49 N10 C50 109.4(11) . . ? C48 N10 C50 109.8(10) . . ? C57 N11 C56 108.0(11) . . ? C57 N11 C55 111.9(11) . . ? C56 N11 C55 110.9(11) . . ? C57 N11 W6 111.0(8) . . ? C56 N11 W6 113.2(8) . . ? C55 N11 W6 101.7(8) . . ? C58 N12 C59 111(2) . . ? C58 N12 C60 113.3(17) . . ? C59 N12 C60 106.2(19) . . ? C65 N13 C67 110.4(11) . . ? C65 N13 C66 109.7(10) . . ? C67 N13 C66 107.6(10) . . ? C65 N13 W7 103.9(7) . . ? C67 N13 W7 113.2(7) . . ? C66 N13 W7 112.1(8) . . ? C70 N14 C68 116.5(14) . . ? C70 N14 C69 110.2(14) . . ? C68 N14 C69 108.4(13) . . ? C77 N15 C75 110.4(9) . . ? C77 N15 C76 107.5(9) . . ? C75 N15 C76 109.2(10) . . ? C77 N15 W8 114.3(7) . . ? C75 N15 W8 103.2(7) . . ? C76 N15 W8 112.1(7) . . ? C79 N16 C78 110.6(13) . . ? C79 N16 C80 110.5(14) . . ? C78 N16 C80 110.8(14) . . ? C3 C1 O3 111.5(13) . . ? C3 C1 C2 114.8(14) . . ? O3 C1 C2 110.8(12) . . ? C3 C1 H1 106.4 . . ? O3 C1 H1 106.4 . . ? C2 C1 H1 106.4 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O4 C4 C8 107.2(10) . . ? O4 C4 C5 107.4(10) . . ? C8 C4 C5 113.7(11) . . ? O4 C4 H4 109.5 . . ? C8 C4 H4 109.5 . . ? C5 C4 H4 109.5 . . ? N1 C5 C4 107.9(10) . . ? N1 C5 H5A 110.1 . . ? C4 C5 H5A 110.1 . . ? N1 C5 H5B 110.1 . . ? C4 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C4 111.5(10) . . ? N2 C8 H8A 109.3 . . ? C4 C8 H8A 109.3 . . ? N2 C8 H8B 109.3 . . ? C4 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O15 C11 C12 110.1(13) . . ? O15 C11 C13 106.7(12) . . ? C12 C11 C13 112.0(14) . . ? O15 C11 H11 109.3 . . ? C12 C11 H11 109.3 . . ? C13 C11 H11 109.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O16 C14 C15 107.1(11) . . ? O16 C14 C18 109.1(11) . . ? C15 C14 C18 107.5(12) . . ? O16 C14 H14 111.0 . . ? C15 C14 H14 111.0 . . ? C18 C14 H14 111.0 . . ? N3 C15 C14 107.9(11) . . ? N3 C15 H15A 110.1 . . ? C14 C15 H15A 110.1 . . ? N3 C15 H15B 110.1 . . ? C14 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C14 112.9(14) . . ? N4 C18 H18A 109.0 . . ? C14 C18 H18A 109.0 . . ? N4 C18 H18B 109.0 . . ? C14 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 H20A 109.5 . . ? N4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 O11 110.5(14) . . ? C22 C21 C23 113.5(14) . . ? O11 C21 C23 110.4(14) . . ? C22 C21 H21 107.4 . . ? O11 C21 H21 107.4 . . ? C23 C21 H21 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O12 C24 C25 108.6(12) . . ? O12 C24 C28 105.0(12) . . ? C25 C24 C28 112.5(12) . . ? O12 C24 H24 110.2 . . ? C25 C24 H24 110.2 . . ? C28 C24 H24 110.2 . . ? N5 C25 C24 110.2(12) . . ? N5 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? N5 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 C24 115.4(14) . . ? N6 C28 H28A 108.4 . . ? C24 C28 H28A 108.4 . . ? N6 C28 H28B 108.4 . . ? C24 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 H30A 109.5 . . ? N6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O8 C31 C33 110.5(11) . . ? O8 C31 C32 107.7(11) . . ? C33 C31 C32 110.5(14) . . ? O8 C31 H31 109.4 . . ? C33 C31 H31 109.4 . . ? C32 C31 H31 109.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O7 C34 C38 110.7(11) . . ? O7 C34 C35 106.3(9) . . ? C38 C34 C35 113.8(11) . . ? O7 C34 H34 108.7 . . ? C38 C34 H34 108.7 . . ? C35 C34 H34 108.7 . . ? N7 C35 C34 109.9(10) . . ? N7 C35 H35A 109.7 . . ? C34 C35 H35A 109.7 . . ? N7 C35 H35B 109.7 . . ? C34 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? N7 C36 H36A 109.5 . . ? N7 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N7 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N7 C37 H37A 109.5 . . ? N7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 N8 109.6(12) . . ? C34 C38 H38A 109.7 . . ? N8 C38 H38A 109.7 . . ? C34 C38 H38B 109.7 . . ? N8 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? N8 C39 H39A 109.5 . . ? N8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N8 C40 H40A 109.5 . . ? N8 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N8 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O19 C41 C43 110.0(12) . . ? O19 C41 C42 109.5(11) . . ? C43 C41 C42 115.6(13) . . ? O19 C41 H41 107.1 . . ? C43 C41 H41 107.1 . . ? C42 C41 H41 107.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O20 C44 C45 107.5(9) . . ? O20 C44 C48 108.8(9) . . ? C45 C44 C48 113.7(10) . . ? O20 C44 H44 108.9 . . ? C45 C44 H44 108.9 . . ? C48 C44 H44 108.9 . . ? N9 C45 C44 109.8(10) . . ? N9 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? N9 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? N9 C46 H46A 109.5 . . ? N9 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N9 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N9 C47 H47A 109.5 . . ? N9 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N9 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N10 C48 C44 114.3(10) . . ? N10 C48 H48A 108.7 . . ? C44 C48 H48A 108.7 . . ? N10 C48 H48B 108.7 . . ? C44 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? N10 C49 H49A 109.5 . . ? N10 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N10 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N10 C50 H50A 109.5 . . ? N10 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N10 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O31 C51 C53 109.4(12) . . ? O31 C51 C52 109.8(12) . . ? C53 C51 C52 111.7(14) . . ? O31 C51 H51 108.6 . . ? C53 C51 H51 108.6 . . ? C52 C51 H51 108.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O32 C54 C55 109.8(11) . . ? O32 C54 C58 106.6(12) . . ? C55 C54 C58 115.7(14) . . ? O32 C54 H54 108.1 . . ? C55 C54 H54 108.1 . . ? C58 C54 H54 108.1 . . ? C54 C55 N11 109.4(12) . . ? C54 C55 H55A 109.8 . . ? N11 C55 H55A 109.8 . . ? C54 C55 H55B 109.8 . . ? N11 C55 H55B 109.8 . . ? H55A C55 H55B 108.2 . . ? N11 C56 H56A 109.5 . . ? N11 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N11 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N11 C57 H57A 109.5 . . ? N11 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? N11 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N12 C58 C54 117.8(16) . . ? N12 C58 H58A 107.8 . . ? C54 C58 H58A 107.8 . . ? N12 C58 H58B 107.8 . . ? C54 C58 H58B 107.8 . . ? H58A C58 H58B 107.2 . . ? N12 C59 H59A 109.5 . . ? N12 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N12 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N12 C60 H60A 109.5 . . ? N12 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N12 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O27 C61 C62 107.8(13) . . ? O27 C61 C63 107.4(13) . . ? C62 C61 C63 110.3(15) . . ? O27 C61 H61 110.4 . . ? C62 C61 H61 110.4 . . ? C63 C61 H61 110.4 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O28 C64 C68 113.3(12) . . ? O28 C64 C65 108.2(11) . . ? C68 C64 C65 113.7(11) . . ? O28 C64 H64 107.1 . . ? C68 C64 H64 107.1 . . ? C65 C64 H64 107.1 . . ? N13 C65 C64 108.1(10) . . ? N13 C65 H65A 110.1 . . ? C64 C65 H65A 110.1 . . ? N13 C65 H65B 110.1 . . ? C64 C65 H65B 110.1 . . ? H65A C65 H65B 108.4 . . ? N13 C66 H66A 109.5 . . ? N13 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N13 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N13 C67 H67A 109.5 . . ? N13 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N13 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N14 C68 C64 117.4(13) . . ? N14 C68 H68A 108.0 . . ? C64 C68 H68A 108.0 . . ? N14 C68 H68B 108.0 . . ? C64 C68 H68B 108.0 . . ? H68A C68 H68B 107.2 . . ? N14 C69 H69A 109.5 . . ? N14 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N14 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N14 C70 H70A 109.5 . . ? N14 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N14 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O23 C71 C73 112.6(11) . . ? O23 C71 C72 105.2(11) . . ? C73 C71 C72 113.7(13) . . ? O23 C71 H71 108.4 . . ? C73 C71 H71 108.4 . . ? C72 C71 H71 108.4 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? O24 C74 C75 108.0(11) . . ? O24 C74 C78 109.8(11) . . ? C75 C74 C78 114.5(12) . . ? O24 C74 H74 108.1 . . ? C75 C74 H74 108.1 . . ? C78 C74 H74 108.1 . . ? N15 C75 C74 109.3(10) . . ? N15 C75 H75A 109.8 . . ? C74 C75 H75A 109.8 . . ? N15 C75 H75B 109.8 . . ? C74 C75 H75B 109.8 . . ? H75A C75 H75B 108.3 . . ? N15 C76 H76A 109.5 . . ? N15 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N15 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N15 C77 H77A 109.5 . . ? N15 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N15 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N16 C78 C74 110.1(11) . . ? N16 C78 H78A 109.6 . . ? C74 C78 H78A 109.6 . . ? N16 C78 H78B 109.6 . . ? C74 C78 H78B 109.6 . . ? H78A C78 H78B 108.1 . . ? N16 C79 H79A 109.5 . . ? N16 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N16 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N16 C80 H80A 109.5 . . ? N16 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N16 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.71 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.888 _refine_diff_density_min -1.383 _refine_diff_density_rms 0.190 data_h05kcm32 _database_code_depnum_ccdc_archive 'CCDC 876658' #TrackingRef '- Compound 6 new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C42 H97 N12 O21 W6), C3 H8 O, 0.5(C6 H6)' _chemical_formula_sum 'C90 H216 N24 O43 W12' _chemical_formula_weight 4529.07 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.8397(3) _cell_length_b 18.8679(4) _cell_length_c 22.7712(5) _cell_angle_alpha 81.0700(10) _cell_angle_beta 72.2060(10) _cell_angle_gamma 87.8660(10) _cell_volume 7209.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 228865 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4312 _exptl_absorpt_coefficient_mu 9.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2496 _exptl_absorpt_correction_T_max 0.2496 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '316 1.9 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 98234 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _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 3.75 _diffrn_reflns_theta_max 27.56 _reflns_number_total 29500 _reflns_number_gt 19920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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. Distances between C68 C70, C69 C70, C82A C83 and C83 C84 had to be restrained which lead to a sensible angle in the disordered NMe2 groups. ; _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^)+(0.0564P)^2^+37.8803P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 29500 _refine_ls_number_parameters 1572 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1315 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.82296(2) 0.19507(2) 0.625242(18) 0.03995(11) Uani 1 1 d . . . W2 W 0.76955(2) 0.16566(2) 0.802986(18) 0.03992(11) Uani 1 1 d . . . W3 W 0.98594(2) 0.16306(2) 0.704736(19) 0.04080(11) Uani 1 1 d . . . W4 W 0.79222(3) 0.38467(2) 0.65362(2) 0.04312(11) Uani 1 1 d . A . W5 W 0.83355(3) 0.34804(3) 0.81227(2) 0.04924(12) Uani 1 1 d . . . W6 W 1.00393(3) 0.36114(3) 0.65776(2) 0.04852(12) Uani 1 1 d . A . W7 W 0.54746(2) 0.02388(2) 0.200492(18) 0.03758(10) Uani 1 1 d . . . W8 W 0.67959(2) -0.00327(2) 0.308617(18) 0.04040(11) Uani 1 1 d . . . W9 W 0.77241(2) 0.04987(2) 0.133170(18) 0.03749(10) Uani 1 1 d . . . W10 W 0.56448(3) 0.22336(2) 0.17507(2) 0.04508(12) Uani 1 1 d . B . W11 W 0.59727(3) 0.17657(3) 0.335160(19) 0.04401(11) Uani 1 1 d . . . W12 W 0.77334(3) 0.22439(3) 0.18900(2) 0.04567(12) Uani 1 1 d . . . O1 O 0.7692(4) 0.1898(4) 0.7255(3) 0.0381(16) Uani 1 1 d . . . O2 O 0.8015(4) 0.2937(4) 0.6279(3) 0.0417(17) Uani 1 1 d . . . O3 O 0.8458(4) 0.2015(4) 0.5453(3) 0.0497(19) Uani 1 1 d . . . O4 O 0.7933(4) 0.0962(4) 0.6447(3) 0.0444(17) Uani 1 1 d . . . O5 O 0.8986(4) 0.1669(4) 0.7666(3) 0.0411(17) Uani 1 1 d . . . O6 O 0.7909(4) 0.2558(4) 0.8238(3) 0.0467(18) Uani 1 1 d . . . O7 O 0.6710(4) 0.1622(4) 0.8449(3) 0.055(2) Uani 1 1 d . . . O8 O 0.7833(5) 0.0655(4) 0.7987(4) 0.056(2) Uani 1 1 d . . . O9 O 0.9165(4) 0.1869(4) 0.6387(3) 0.0417(17) Uani 1 1 d . . . O10 O 1.0142(4) 0.2617(3) 0.6773(3) 0.0388(16) Uani 1 1 d . . . O11 O 1.0541(4) 0.1447(5) 0.7443(4) 0.056(2) Uani 1 1 d . . . O12 O 0.9692(5) 0.0672(4) 0.6924(4) 0.053(2) Uani 1 1 d . . . O13 O 0.7834(4) 0.3643(4) 0.7335(3) 0.0440(17) Uani 1 1 d . . . O14 O 0.6965(4) 0.3988(4) 0.6517(4) 0.055(2) Uani 1 1 d . . . O15 O 0.8232(5) 0.4826(4) 0.6435(4) 0.056(2) Uani 1 1 d . . . O16 O 0.9253(4) 0.3443(4) 0.7549(3) 0.0506(19) Uani 1 1 d . . . O17 O 0.8599(5) 0.3371(5) 0.8797(3) 0.064(2) Uani 1 1 d . . . O18 O 0.8238(5) 0.4504(4) 0.8039(4) 0.059(2) Uani 1 1 d . . . O19 O 0.9183(4) 0.3682(4) 0.6337(3) 0.0459(18) Uani 1 1 d . . . O20 O 1.0795(5) 0.3716(5) 0.5887(4) 0.073(3) Uani 1 1 d . . . O21 O 1.0008(5) 0.4576(4) 0.6753(5) 0.069(3) Uani 1 1 d . . . O22 O 0.5862(4) 0.0101(4) 0.2639(3) 0.0405(16) Uani 1 1 d . . . O23 O 0.5391(4) 0.1254(4) 0.1826(3) 0.0426(17) Uani 1 1 d . . . O24 O 0.4494(4) 0.0061(4) 0.2368(3) 0.0508(19) Uani 1 1 d . . . O25 O 0.5758(4) -0.0685(4) 0.1747(4) 0.0473(18) Uani 1 1 d . . . O26 O 0.7440(4) 0.0305(4) 0.2344(3) 0.0422(17) Uani 1 1 d . . . O27 O 0.6310(4) 0.0808(4) 0.3393(3) 0.0446(17) Uani 1 1 d . . . O28 O 0.7403(4) -0.0165(5) 0.3549(4) 0.059(2) Uani 1 1 d . . . O29 O 0.6778(5) -0.0995(4) 0.2931(4) 0.056(2) Uani 1 1 d . . . O30 O 0.6704(4) 0.0510(4) 0.1396(3) 0.0385(16) Uani 1 1 d . . . O31 O 0.7921(4) 0.1426(4) 0.1485(3) 0.0407(16) Uani 1 1 d . . . O32 O 0.8176(4) 0.0653(4) 0.0541(3) 0.0476(18) Uani 1 1 d . . . O33 O 0.7830(4) -0.0519(4) 0.1442(3) 0.0428(17) Uani 1 1 d . . . O34 O 0.5559(4) 0.1869(4) 0.2734(3) 0.0455(18) Uani 1 1 d . . . O35 O 0.5503(5) 0.2499(5) 0.1042(3) 0.061(2) Uani 1 1 d . . . O36 O 0.5520(5) 0.3144(4) 0.2030(4) 0.060(2) Uani 1 1 d . B . O37 O 0.7115(4) 0.1917(4) 0.2654(3) 0.0433(17) Uani 1 1 d . . . O38 O 0.5163(5) 0.1630(5) 0.4012(3) 0.060(2) Uani 1 1 d . . . O39 O 0.6085(5) 0.2770(4) 0.3356(4) 0.053(2) Uani 1 1 d . . . O40 O 0.6680(4) 0.2232(4) 0.1579(3) 0.0482(18) Uani 1 1 d . . . O41 O 0.8648(4) 0.2265(5) 0.1994(4) 0.061(2) Uani 1 1 d . . . O42 O 0.7448(5) 0.3217(4) 0.1943(4) 0.064(2) Uani 1 1 d . C . N1 N 0.6841(5) 0.1950(5) 0.6385(4) 0.048(2) Uani 1 1 d . . . N2 N 0.7242(7) -0.0046(6) 0.5734(5) 0.064(3) Uani 1 1 d . . . N3 N 0.8066(5) 0.1174(6) 0.8910(4) 0.055(3) Uani 1 1 d . . . N4 N 0.8483(10) -0.1111(8) 0.8536(9) 0.109(5) Uani 1 1 d . . . N5 N 1.0835(6) 0.1476(6) 0.6104(5) 0.061(3) Uani 1 1 d . . . N6 N 1.0421(9) -0.0857(9) 0.6081(8) 0.105(5) Uani 1 1 d . . . N7 N 0.8414(6) 0.4220(6) 0.5416(5) 0.062(3) Uani 1 1 d . . . N9 N 0.7047(7) 0.3699(6) 0.8722(5) 0.070(3) Uani 1 1 d . . . N10 N 0.7662(11) 0.5785(8) 0.9115(7) 0.103(5) Uani 1 1 d . . . N11 N 1.0955(7) 0.3646(6) 0.7143(5) 0.066(3) Uani 1 1 d D . . N13 N 0.5221(5) 0.0316(5) 0.1029(4) 0.046(2) Uani 1 1 d . . . N14 N 0.5786(10) -0.1847(7) 0.0572(6) 0.101(5) Uani 1 1 d . . . N15 N 0.5695(5) -0.0585(5) 0.3894(4) 0.048(2) Uani 1 1 d . . . N16 N 0.5636(7) -0.2652(6) 0.3202(6) 0.074(3) Uani 1 1 d . . . H16 H 0.5164 -0.2415 0.3346 0.089 Uiso 1 1 calc R . . N17 N 0.9006(5) 0.0304(5) 0.1445(4) 0.051(2) Uani 1 1 d . . . N18 N 0.8934(6) -0.1574(6) 0.0650(6) 0.069(3) Uani 1 1 d . . . N19 N 0.4265(6) 0.2331(6) 0.2250(5) 0.061(3) Uani 1 1 d . . . N20 N 0.4252(12) 0.4386(8) 0.3024(10) 0.131(7) Uani 1 1 d . . . N21 N 0.6759(6) 0.1830(5) 0.3995(4) 0.052(2) Uani 1 1 d . . . N22 N 0.6484(8) 0.4130(6) 0.4213(7) 0.083(4) Uani 1 1 d . . . N23 N 0.8234(6) 0.2848(6) 0.0858(5) 0.064(3) Uani 1 1 d . . . N24 N 0.7540(13) 0.5076(8) 0.1273(9) 0.131(7) Uani 1 1 d D . . C1 C 0.7150(7) 0.0667(7) 0.6591(7) 0.062(3) Uani 1 1 d . . . H1 H 0.6906 0.0602 0.7054 0.074 Uiso 1 1 calc R . . C2 C 0.6689(7) 0.1213(7) 0.6306(6) 0.058(3) Uani 1 1 d . . . H2A H 0.6822 0.1185 0.5856 0.069 Uiso 1 1 calc R . . H2B H 0.6121 0.1100 0.6499 0.069 Uiso 1 1 calc R . . C3 C 0.6653(8) 0.2457(8) 0.5896(6) 0.066(4) Uani 1 1 d . . . H3A H 0.6105 0.2384 0.5914 0.099 Uiso 1 1 calc R . . H3B H 0.7003 0.2377 0.5488 0.099 Uiso 1 1 calc R . . H3C H 0.6725 0.2948 0.5961 0.099 Uiso 1 1 calc R . . C4 C 0.6315(7) 0.2099(8) 0.6984(6) 0.064(4) Uani 1 1 d . . . H4A H 0.6510 0.2520 0.7098 0.097 Uiso 1 1 calc R . . H4B H 0.6297 0.1683 0.7305 0.097 Uiso 1 1 calc R . . H4C H 0.5785 0.2192 0.6950 0.097 Uiso 1 1 calc R . . C5 C 0.7187(8) -0.0058(7) 0.6384(6) 0.062(3) Uani 1 1 d . . . H5A H 0.7648 -0.0316 0.6464 0.074 Uiso 1 1 calc R . . H5B H 0.6710 -0.0336 0.6646 0.074 Uiso 1 1 calc R . . C6 C 0.8032(9) 0.0223(9) 0.5327(7) 0.082(5) Uani 1 1 d . . . H6A H 0.8438 -0.0096 0.5425 0.123 Uiso 1 1 calc R . . H6B H 0.8117 0.0708 0.5398 0.123 Uiso 1 1 calc R . . H6C H 0.8061 0.0233 0.4889 0.123 Uiso 1 1 calc R . . C7 C 0.7082(9) -0.0734(8) 0.5606(8) 0.084(5) Uani 1 1 d . . . H7A H 0.7458 -0.1083 0.5713 0.126 Uiso 1 1 calc R . . H7B H 0.7131 -0.0703 0.5163 0.126 Uiso 1 1 calc R . . H7C H 0.6545 -0.0888 0.5857 0.126 Uiso 1 1 calc R . . C8 C 0.7961(10) 0.0129(8) 0.8433(7) 0.084(5) Uani 1 1 d D . . H8 H 0.7432 -0.0011 0.8736 0.100 Uiso 1 1 calc R . . C9 C 0.8377(10) 0.0435(8) 0.8761(8) 0.086(5) Uani 1 1 d . . . H9A H 0.8940 0.0481 0.8510 0.103 Uiso 1 1 calc R . . H9B H 0.8341 0.0112 0.9155 0.103 Uiso 1 1 calc R . . C10 C 0.7385(9) 0.1139(14) 0.9452(6) 0.139(10) Uani 1 1 d . . . H10A H 0.6954 0.0890 0.9381 0.208 Uiso 1 1 calc R . . H10B H 0.7221 0.1625 0.9531 0.208 Uiso 1 1 calc R . . H10C H 0.7514 0.0875 0.9814 0.208 Uiso 1 1 calc R . . C11 C 0.8710(9) 0.1550(7) 0.9018(6) 0.066(4) Uani 1 1 d . . . H11A H 0.8522 0.2012 0.9150 0.098 Uiso 1 1 calc R . . H11B H 0.9151 0.1631 0.8632 0.098 Uiso 1 1 calc R . . H11C H 0.8886 0.1256 0.9345 0.098 Uiso 1 1 calc R . . C12 C 0.8294(10) -0.0560(9) 0.8125(8) 0.095(5) Uani 1 1 d D . . H12A H 0.7897 -0.0740 0.7960 0.114 Uiso 1 1 calc R . . H12B H 0.8771 -0.0422 0.7769 0.114 Uiso 1 1 calc R . . C13 C 0.897(2) -0.1627(10) 0.8209(11) 0.174(13) Uani 1 1 d . . . H13A H 0.8691 -0.1843 0.7971 0.261 Uiso 1 1 calc R . . H13B H 0.9107 -0.2003 0.8509 0.261 Uiso 1 1 calc R . . H13C H 0.9455 -0.1392 0.7923 0.261 Uiso 1 1 calc R . . C14 C 0.7757(17) -0.1525(14) 0.8923(12) 0.158(10) Uani 1 1 d . . . H14A H 0.7359 -0.1196 0.9126 0.237 Uiso 1 1 calc R . . H14B H 0.7883 -0.1879 0.9242 0.237 Uiso 1 1 calc R . . H14C H 0.7552 -0.1773 0.8656 0.237 Uiso 1 1 calc R . . C15 C 1.0094(10) 0.0336(8) 0.6411(6) 0.083(5) Uani 1 1 d . . . H15 H 0.9780 0.0489 0.6117 0.099 Uiso 1 1 calc R . . C16 C 1.0824(11) 0.0681(11) 0.6087(10) 0.126(9) Uani 1 1 d . . . H16A H 1.0972 0.0603 0.5646 0.152 Uiso 1 1 calc R . . H16B H 1.1228 0.0451 0.6268 0.152 Uiso 1 1 calc R . . C17 C 1.0710(10) 0.1885(14) 0.5555(6) 0.128(9) Uani 1 1 d . . . H17A H 1.0529 0.2366 0.5641 0.192 Uiso 1 1 calc R . . H17B H 1.0311 0.1645 0.5438 0.192 Uiso 1 1 calc R . . H17C H 1.1205 0.1924 0.5212 0.192 Uiso 1 1 calc R . . C18 C 1.1615(7) 0.1629(8) 0.6122(6) 0.063(3) Uani 1 1 d . . . H18A H 1.2009 0.1475 0.5761 0.095 Uiso 1 1 calc R . . H18B H 1.1691 0.1371 0.6507 0.095 Uiso 1 1 calc R . . H18C H 1.1673 0.2146 0.6110 0.095 Uiso 1 1 calc R . . C19 C 0.9940(12) -0.0454(10) 0.6559(10) 0.112(7) Uani 1 1 d . . . H19A H 1.0040 -0.0635 0.6960 0.135 Uiso 1 1 calc R . . H19B H 0.9378 -0.0544 0.6614 0.135 Uiso 1 1 calc R . . C20 C 1.0055(16) -0.0877(14) 0.5623(12) 0.153(10) Uani 1 1 d . . . H20A H 0.9486 -0.0947 0.5820 0.230 Uiso 1 1 calc R . . H20B H 1.0267 -0.1274 0.5392 0.230 Uiso 1 1 calc R . . H20C H 1.0154 -0.0423 0.5334 0.230 Uiso 1 1 calc R . . C21 C 1.0421(12) -0.1600(11) 0.6407(12) 0.134(9) Uani 1 1 d . . . H21A H 0.9885 -0.1740 0.6668 0.202 Uiso 1 1 calc R . . H21B H 1.0769 -0.1626 0.6670 0.202 Uiso 1 1 calc R . . H21C H 1.0610 -0.1927 0.6099 0.202 Uiso 1 1 calc R . . C24 C 0.7778(12) 0.4175(18) 0.5151(8) 0.178(14) Uani 1 1 d . A . H24A H 0.7274 0.4240 0.5464 0.266 Uiso 1 1 calc R . . H24B H 0.7782 0.3704 0.5020 0.266 Uiso 1 1 calc R . . H24C H 0.7847 0.4551 0.4789 0.266 Uiso 1 1 calc R . . C25 C 0.9097(9) 0.3837(9) 0.5081(6) 0.085(5) Uani 1 1 d . A . H25A H 0.9339 0.4111 0.4666 0.128 Uiso 1 1 calc R . . H25B H 0.8931 0.3364 0.5037 0.128 Uiso 1 1 calc R . . H25C H 0.9481 0.3779 0.5314 0.128 Uiso 1 1 calc R . . N8 N 0.8294(16) 0.6504(13) 0.6326(15) 0.095(11) Uani 0.55(3) 1 d PD A 1 C22 C 0.8380(17) 0.5340(12) 0.5911(11) 0.048(6) Uiso 0.55(3) 1 d PD A 1 H22 H 0.7862 0.5492 0.5851 0.058 Uiso 0.55(3) 1 calc PR A 1 C23 C 0.8816(19) 0.4949(13) 0.5378(12) 0.062(7) Uiso 0.55(3) 1 d P A 1 H23A H 0.9364 0.4862 0.5388 0.075 Uiso 0.55(3) 1 calc PR A 1 H23B H 0.8838 0.5253 0.4978 0.075 Uiso 0.55(3) 1 calc PR A 1 C26 C 0.8813(17) 0.6020(14) 0.5945(19) 0.084(10) Uiso 0.55(3) 1 d PD A 1 H26A H 0.9249 0.5875 0.6121 0.100 Uiso 0.55(3) 1 calc PR A 1 H26B H 0.9047 0.6278 0.5517 0.100 Uiso 0.55(3) 1 calc PR A 1 C27 C 0.866(3) 0.717(2) 0.6184(19) 0.106(12) Uiso 0.55(3) 1 d P A 1 H27A H 0.8269 0.7533 0.6335 0.158 Uiso 0.55(3) 1 calc PR A 1 H27B H 0.8892 0.7289 0.5731 0.158 Uiso 0.55(3) 1 calc PR A 1 H27C H 0.9072 0.7160 0.6386 0.158 Uiso 0.55(3) 1 calc PR A 1 C28 C 0.807(3) 0.622(2) 0.7015(18) 0.104(12) Uiso 0.55(3) 1 d P A 1 H28A H 0.8526 0.6248 0.7165 0.156 Uiso 0.55(3) 1 calc PR A 1 H28B H 0.7903 0.5713 0.7083 0.156 Uiso 0.55(3) 1 calc PR A 1 H28C H 0.7638 0.6498 0.7243 0.156 Uiso 0.55(3) 1 calc PR A 1 N8A N 0.889(3) 0.6311(15) 0.6224(12) 0.094(15) Uani 0.45(3) 1 d P A 2 C22A C 0.873(3) 0.5225(18) 0.5777(16) 0.065(9) Uiso 0.45(3) 1 d P A 2 H22A H 0.9302 0.5125 0.5684 0.078 Uiso 0.45(3) 1 calc PR A 2 C23A C 0.840(2) 0.4980(17) 0.5344(15) 0.067(9) Uiso 0.45(3) 1 d P A 2 H23C H 0.7854 0.5148 0.5415 0.080 Uiso 0.45(3) 1 calc PR A 2 H23D H 0.8712 0.5181 0.4913 0.080 Uiso 0.45(3) 1 calc PR A 2 C26A C 0.855(3) 0.5977(19) 0.5822(17) 0.074(11) Uiso 0.45(3) 1 d P A 2 H26C H 0.7975 0.6027 0.5974 0.088 Uiso 0.45(3) 1 calc PR A 2 H26D H 0.8738 0.6253 0.5396 0.088 Uiso 0.45(3) 1 calc PR A 2 C27A C 0.912(3) 0.707(2) 0.602(2) 0.090(12) Uiso 0.45(3) 1 d P A 2 H27D H 0.9695 0.7110 0.5856 0.135 Uiso 0.45(3) 1 calc PR A 2 H27E H 0.8926 0.7333 0.6371 0.135 Uiso 0.45(3) 1 calc PR A 2 H27F H 0.8890 0.7265 0.5688 0.135 Uiso 0.45(3) 1 calc PR A 2 C28A C 0.847(3) 0.616(2) 0.6847(19) 0.084(12) Uiso 0.45(3) 1 d P A 2 H28D H 0.7930 0.6334 0.6907 0.126 Uiso 0.45(3) 1 calc PR A 2 H28E H 0.8718 0.6408 0.7091 0.126 Uiso 0.45(3) 1 calc PR A 2 H28F H 0.8462 0.5645 0.6986 0.126 Uiso 0.45(3) 1 calc PR A 2 C29 C 0.7672(10) 0.4887(8) 0.8437(8) 0.086(5) Uani 1 1 d . . . H29 H 0.7352 0.5166 0.8190 0.103 Uiso 1 1 calc R . . C30 C 0.7147(12) 0.4379(11) 0.8932(9) 0.118(7) Uani 1 1 d . . . H30A H 0.6626 0.4603 0.9081 0.142 Uiso 1 1 calc R . . H30B H 0.7364 0.4278 0.9288 0.142 Uiso 1 1 calc R . . C31 C 0.6736(11) 0.3162(9) 0.9281(7) 0.098(6) Uani 1 1 d . . . H31A H 0.7050 0.3173 0.9565 0.148 Uiso 1 1 calc R . . H31B H 0.6763 0.2684 0.9159 0.148 Uiso 1 1 calc R . . H31C H 0.6187 0.3271 0.9492 0.148 Uiso 1 1 calc R . . C32 C 0.6484(10) 0.3765(13) 0.8375(8) 0.116(7) Uani 1 1 d . . . H32A H 0.5990 0.3957 0.8623 0.174 Uiso 1 1 calc R . . H32B H 0.6384 0.3293 0.8285 0.174 Uiso 1 1 calc R . . H32C H 0.6695 0.4091 0.7982 0.174 Uiso 1 1 calc R . . C33 C 0.8115(15) 0.5420(11) 0.8659(11) 0.159(12) Uani 1 1 d . . . H33A H 0.8521 0.5154 0.8817 0.191 Uiso 1 1 calc R . . H33B H 0.8392 0.5773 0.8295 0.191 Uiso 1 1 calc R . . C34 C 0.720(2) 0.6333(15) 0.8902(16) 0.196(14) Uani 1 1 d . . . H34A H 0.6806 0.6489 0.9260 0.293 Uiso 1 1 calc R . . H34B H 0.6941 0.6149 0.8634 0.293 Uiso 1 1 calc R . . H34C H 0.7544 0.6740 0.8663 0.293 Uiso 1 1 calc R . . C35 C 0.810(2) 0.6169(18) 0.9373(18) 0.220(17) Uani 1 1 d . . . H35A H 0.8326 0.5836 0.9646 0.329 Uiso 1 1 calc R . . H35B H 0.7754 0.6506 0.9617 0.329 Uiso 1 1 calc R . . H35C H 0.8521 0.6436 0.9039 0.329 Uiso 1 1 calc R . . C36 C 1.0582(16) 0.4899(12) 0.6911(15) 0.044(7) Uiso 0.46(4) 1 d PD A 1 H36 H 1.0951 0.4977 0.6476 0.053 Uiso 0.46(4) 1 calc PR A 1 C37 C 1.1064(19) 0.4344(14) 0.7144(17) 0.061(9) Uiso 0.46(4) 1 d PD A 1 H37A H 1.1620 0.4459 0.6901 0.073 Uiso 0.46(4) 1 calc PR A 1 H37B H 1.1007 0.4402 0.7580 0.073 Uiso 0.46(4) 1 calc PR A 1 C40 C 1.049(2) 0.5577(18) 0.6947(18) 0.065(9) Uiso 0.46(4) 1 d P A 1 H40A H 0.9914 0.5664 0.7081 0.077 Uiso 0.46(4) 1 calc PR A 1 H40B H 1.0701 0.5840 0.6519 0.077 Uiso 0.46(4) 1 calc PR A 1 N12 N 1.083(3) 0.592(2) 0.7356(18) 0.060(11) Uani 0.46(4) 1 d PD A 1 C41 C 1.114(4) 0.663(3) 0.703(3) 0.13(2) Uiso 0.46(4) 1 d PD A 1 H41A H 1.1475 0.6583 0.6607 0.196 Uiso 0.46(4) 1 calc PR A 1 H41B H 1.1454 0.6822 0.7257 0.196 Uiso 0.46(4) 1 calc PR A 1 H41C H 1.0705 0.6952 0.7008 0.196 Uiso 0.46(4) 1 calc PR A 1 C42 C 1.040(3) 0.613(4) 0.791(2) 0.100(15) Uiso 0.46(4) 1 d P A 1 H42A H 1.0141 0.5710 0.8199 0.150 Uiso 0.46(4) 1 calc PR A 1 H42B H 1.0005 0.6479 0.7838 0.150 Uiso 0.46(4) 1 calc PR A 1 H42C H 1.0755 0.6352 0.8086 0.150 Uiso 0.46(4) 1 calc PR A 1 C36A C 1.0316(18) 0.4846(14) 0.7224(17) 0.065(8) Uiso 0.54(4) 1 d P A 2 H36A H 0.9847 0.4695 0.7592 0.078 Uiso 0.54(4) 1 calc PR A 2 C37A C 1.079(2) 0.4350(11) 0.7378(15) 0.067(8) Uiso 0.54(4) 1 d PD A 2 H37C H 1.0599 0.4234 0.7838 0.081 Uiso 0.54(4) 1 calc PR A 2 H37D H 1.1310 0.4589 0.7274 0.081 Uiso 0.54(4) 1 calc PR A 2 C40A C 1.0202(19) 0.5568(15) 0.7215(16) 0.067(8) Uiso 0.54(4) 1 d P A 2 H40C H 0.9638 0.5652 0.7421 0.081 Uiso 0.54(4) 1 calc PR A 2 H40D H 1.0331 0.5804 0.6776 0.081 Uiso 0.54(4) 1 calc PR A 2 N12A N 1.066(4) 0.589(3) 0.751(4) 0.17(3) Uani 0.54(4) 1 d PD A 2 C41A C 1.128(4) 0.627(4) 0.707(3) 0.14(2) Uiso 0.54(4) 1 d P A 2 H41D H 1.1620 0.6460 0.7279 0.216 Uiso 0.54(4) 1 calc PR A 2 H41E H 1.1081 0.6670 0.6833 0.216 Uiso 0.54(4) 1 calc PR A 2 H41F H 1.1589 0.5952 0.6786 0.216 Uiso 0.54(4) 1 calc PR A 2 C42A C 1.016(4) 0.646(4) 0.780(3) 0.20(3) Uiso 0.54(4) 1 d PD A 2 H42D H 0.9686 0.6240 0.8115 0.293 Uiso 0.54(4) 1 calc PR A 2 H42E H 1.0016 0.6789 0.7483 0.293 Uiso 0.54(4) 1 calc PR A 2 H42F H 1.0455 0.6715 0.8005 0.293 Uiso 0.54(4) 1 calc PR A 2 C38 C 1.1726(11) 0.3467(15) 0.6800(12) 0.156(11) Uani 1 1 d . A . H38A H 1.1904 0.3805 0.6411 0.235 Uiso 1 1 calc R . . H38B H 1.1725 0.2979 0.6705 0.235 Uiso 1 1 calc R . . H38C H 1.2084 0.3495 0.7049 0.235 Uiso 1 1 calc R . . C39 C 1.0781(14) 0.3172(11) 0.7737(10) 0.149(11) Uani 1 1 d . A . H39A H 1.0822 0.2672 0.7664 0.224 Uiso 1 1 calc R . . H39B H 1.0247 0.3261 0.7996 0.224 Uiso 1 1 calc R . . H39C H 1.1159 0.3264 0.7952 0.224 Uiso 1 1 calc R . . C43 C 0.5676(12) -0.0895(9) 0.1207(8) 0.096(6) Uani 1 1 d . . . H43 H 0.5104 -0.1010 0.1410 0.115 Uiso 1 1 calc R . . C44 C 0.553(2) -0.0358(9) 0.0813(10) 0.174(14) Uani 1 1 d . . . H44A H 0.5148 -0.0538 0.0630 0.208 Uiso 1 1 calc R . . H44B H 0.6023 -0.0243 0.0468 0.208 Uiso 1 1 calc R . . C45 C 0.4390(9) 0.0402(16) 0.1101(7) 0.145(11) Uani 1 1 d . . . H45A H 0.4296 0.0380 0.0702 0.217 Uiso 1 1 calc R . . H45B H 0.4218 0.0867 0.1233 0.217 Uiso 1 1 calc R . . H45C H 0.4092 0.0017 0.1417 0.217 Uiso 1 1 calc R . . C46 C 0.5654(11) 0.0886(10) 0.0561(6) 0.105(6) Uani 1 1 d . . . H46A H 0.5452 0.0947 0.0202 0.158 Uiso 1 1 calc R . . H46B H 0.6213 0.0764 0.0427 0.158 Uiso 1 1 calc R . . H46C H 0.5590 0.1335 0.0738 0.158 Uiso 1 1 calc R . . C47 C 0.5856(13) -0.1601(9) 0.1140(8) 0.110(7) Uani 1 1 d . . . H47A H 0.5509 -0.1909 0.1508 0.132 Uiso 1 1 calc R . . H47B H 0.6404 -0.1684 0.1150 0.132 Uiso 1 1 calc R . . C48 C 0.5071(12) -0.2242(13) 0.0677(12) 0.131(8) Uani 1 1 d . . . H48A H 0.5063 -0.2392 0.0286 0.196 Uiso 1 1 calc R . . H48B H 0.4617 -0.1937 0.0826 0.196 Uiso 1 1 calc R . . H48C H 0.5047 -0.2667 0.0990 0.196 Uiso 1 1 calc R . . C49 C 0.6443(14) -0.229(2) 0.0324(17) 0.26(2) Uani 1 1 d . . . H49A H 0.6251 -0.2743 0.0261 0.395 Uiso 1 1 calc R . . H49B H 0.6751 -0.2387 0.0617 0.395 Uiso 1 1 calc R . . H49C H 0.6776 -0.2040 -0.0076 0.395 Uiso 1 1 calc R . . C50 C 0.6267(10) -0.1536(7) 0.3302(7) 0.087(5) Uani 1 1 d . . . H50 H 0.6544 -0.1764 0.3603 0.104 Uiso 1 1 calc R . . C51 C 0.5572(9) -0.1276(7) 0.3683(7) 0.075(4) Uani 1 1 d . . . H51A H 0.5352 -0.1642 0.4053 0.091 Uiso 1 1 calc R . . H51B H 0.5181 -0.1198 0.3450 0.091 Uiso 1 1 calc R . . C52 C 0.4971(7) -0.0184(8) 0.3985(6) 0.063(4) Uani 1 1 d . . . H52A H 0.4819 -0.0122 0.3601 0.095 Uiso 1 1 calc R . . H52B H 0.5050 0.0288 0.4087 0.095 Uiso 1 1 calc R . . H52C H 0.4553 -0.0446 0.4327 0.095 Uiso 1 1 calc R . . C53 C 0.5895(8) -0.0708(9) 0.4489(5) 0.078(4) Uani 1 1 d . . . H53A H 0.6020 -0.0248 0.4588 0.117 Uiso 1 1 calc R . . H53B H 0.6351 -0.1024 0.4446 0.117 Uiso 1 1 calc R . . H53C H 0.5445 -0.0933 0.4825 0.117 Uiso 1 1 calc R . . C54 C 0.6232(8) -0.2118(8) 0.2932(7) 0.069(4) Uani 1 1 d . . . H54A H 0.6169 -0.1889 0.2528 0.083 Uiso 1 1 calc R . . H54B H 0.6747 -0.2362 0.2838 0.083 Uiso 1 1 calc R . . C55 C 0.5531(13) -0.3097(11) 0.2781(10) 0.118(7) Uani 1 1 d . . . H55A H 0.5345 -0.2806 0.2458 0.178 Uiso 1 1 calc R . . H55B H 0.5142 -0.3474 0.3010 0.178 Uiso 1 1 calc R . . H55C H 0.6034 -0.3317 0.2585 0.178 Uiso 1 1 calc R . . C56 C 0.5758(12) -0.3116(9) 0.3735(8) 0.107(6) Uani 1 1 d . . . H56A H 0.6260 -0.3365 0.3604 0.160 Uiso 1 1 calc R . . H56B H 0.5328 -0.3468 0.3908 0.160 Uiso 1 1 calc R . . H56C H 0.5770 -0.2826 0.4055 0.160 Uiso 1 1 calc R . . C57 C 0.8491(7) -0.0910(7) 0.1559(5) 0.056(3) Uani 1 1 d . . . H57 H 0.8393 -0.1010 0.2021 0.067 Uiso 1 1 calc R . . C58 C 0.9198(7) -0.0437(7) 0.1283(6) 0.058(3) Uani 1 1 d . . . H58A H 0.9377 -0.0416 0.0824 0.069 Uiso 1 1 calc R . . H58B H 0.9630 -0.0637 0.1445 0.069 Uiso 1 1 calc R . . C59 C 0.9595(7) 0.0819(7) 0.1004(6) 0.065(4) Uani 1 1 d . . . H59A H 1.0126 0.0648 0.0987 0.098 Uiso 1 1 calc R . . H59B H 0.9520 0.1289 0.1145 0.098 Uiso 1 1 calc R . . H59C H 0.9530 0.0862 0.0588 0.098 Uiso 1 1 calc R . . C60 C 0.9076(7) 0.0336(8) 0.2081(6) 0.065(4) Uani 1 1 d . . . H60A H 0.9623 0.0249 0.2076 0.097 Uiso 1 1 calc R . . H60B H 0.8733 -0.0031 0.2386 0.097 Uiso 1 1 calc R . . H60C H 0.8918 0.0811 0.2196 0.097 Uiso 1 1 calc R . . C61 C 0.8570(8) -0.1617(7) 0.1319(6) 0.068(4) Uani 1 1 d . . . H61A H 0.8886 -0.1941 0.1534 0.081 Uiso 1 1 calc R . . H61B H 0.8040 -0.1836 0.1431 0.081 Uiso 1 1 calc R . . C62 C 0.8412(9) -0.1228(9) 0.0312(7) 0.090(5) Uani 1 1 d . . . H62A H 0.7921 -0.1506 0.0434 0.135 Uiso 1 1 calc R . . H62B H 0.8668 -0.1205 -0.0138 0.135 Uiso 1 1 calc R . . H62C H 0.8296 -0.0741 0.0412 0.135 Uiso 1 1 calc R . . C63 C 0.9123(13) -0.2286(10) 0.0505(10) 0.129(8) Uani 1 1 d . . . H63A H 0.9457 -0.2517 0.0749 0.194 Uiso 1 1 calc R . . H63B H 0.9404 -0.2261 0.0059 0.194 Uiso 1 1 calc R . . H63C H 0.8637 -0.2567 0.0608 0.194 Uiso 1 1 calc R . . C64 C 0.4828(9) 0.3457(8) 0.2362(9) 0.081(5) Uani 1 1 d . . . H64 H 0.4785 0.3134 0.2763 0.097 Uiso 0.46(8) 1 calc PR B 1 H64A H 0.4647 0.3687 0.2003 0.097 Uiso 0.54(8) 1 calc PR B 2 C65 C 0.418(3) 0.315(2) 0.227(4) 0.090(18) Uani 0.46(8) 1 d P B 1 H65A H 0.4114 0.3389 0.1872 0.108 Uiso 0.46(8) 1 calc PR B 1 H65B H 0.3705 0.3232 0.2610 0.108 Uiso 0.46(8) 1 calc PR B 1 C65A C 0.4195(15) 0.289(2) 0.265(2) 0.067(13) Uani 0.54(8) 1 d P B 2 H65C H 0.4233 0.2665 0.3059 0.081 Uiso 0.54(8) 1 calc PR B 2 H65D H 0.3673 0.3115 0.2710 0.081 Uiso 0.54(8) 1 calc PR B 2 C66 C 0.3824(10) 0.2366(13) 0.1798(10) 0.121(7) Uani 1 1 d . B . H66A H 0.3948 0.1948 0.1579 0.181 Uiso 1 1 calc R . . H66B H 0.3971 0.2806 0.1495 0.181 Uiso 1 1 calc R . . H66C H 0.3258 0.2368 0.2017 0.181 Uiso 1 1 calc R . . C67 C 0.3909(8) 0.1742(12) 0.2736(8) 0.114(7) Uani 1 1 d . B . H67A H 0.3382 0.1879 0.2976 0.171 Uiso 1 1 calc R . . H67B H 0.4236 0.1631 0.3015 0.171 Uiso 1 1 calc R . . H67C H 0.3869 0.1318 0.2547 0.171 Uiso 1 1 calc R . . C68 C 0.4965(10) 0.4076(9) 0.2585(11) 0.120(8) Uani 1 1 d D B . H68A H 0.5193 0.4450 0.2222 0.144 Uiso 1 1 calc R . . H68B H 0.5366 0.3964 0.2804 0.144 Uiso 1 1 calc R . . C69 C 0.446(2) 0.485(2) 0.3382(18) 0.220(15) Uiso 1 1 d . . . H69A H 0.4630 0.4571 0.3718 0.330 Uiso 1 1 calc R . . H69B H 0.4008 0.5145 0.3562 0.330 Uiso 1 1 calc R . . H69C H 0.4896 0.5171 0.3113 0.330 Uiso 1 1 calc R . . C70 C 0.392(2) 0.491(2) 0.257(2) 0.31(2) Uiso 1 1 d D . . H70A H 0.3425 0.5107 0.2807 0.469 Uiso 1 1 calc R . . H70B H 0.3829 0.4649 0.2259 0.469 Uiso 1 1 calc R . . H70C H 0.4302 0.5298 0.2364 0.469 Uiso 1 1 calc R . . C71 C 0.6424(11) 0.3075(9) 0.3733(9) 0.092(5) Uani 1 1 d . . . H71 H 0.6942 0.3215 0.3414 0.111 Uiso 1 1 calc R . . C72 C 0.6697(12) 0.2586(7) 0.4131(8) 0.093(6) Uani 1 1 d . . . H72A H 0.6343 0.2588 0.4561 0.112 Uiso 1 1 calc R . . H72B H 0.7224 0.2747 0.4118 0.112 Uiso 1 1 calc R . . C73 C 0.6488(10) 0.1341(8) 0.4579(6) 0.083(5) Uani 1 1 d . . . H73A H 0.6603 0.0846 0.4499 0.124 Uiso 1 1 calc R . . H73B H 0.5919 0.1392 0.4762 0.124 Uiso 1 1 calc R . . H73C H 0.6758 0.1453 0.4869 0.124 Uiso 1 1 calc R . . C74 C 0.7625(10) 0.1672(14) 0.3728(9) 0.128(9) Uani 1 1 d . . . H74A H 0.7892 0.1698 0.4041 0.193 Uiso 1 1 calc R . . H74B H 0.7859 0.2025 0.3358 0.193 Uiso 1 1 calc R . . H74C H 0.7683 0.1190 0.3611 0.193 Uiso 1 1 calc R . . C75 C 0.6151(12) 0.3766(9) 0.3830(10) 0.102(6) Uani 1 1 d . . . H75A H 0.5573 0.3736 0.4025 0.122 Uiso 1 1 calc R . . H75B H 0.6253 0.4069 0.3417 0.122 Uiso 1 1 calc R . . C76 C 0.5860(15) 0.4378(18) 0.4702(13) 0.179(13) Uani 1 1 d . . . H76A H 0.5537 0.4722 0.4519 0.268 Uiso 1 1 calc R . . H76B H 0.6086 0.4613 0.4965 0.268 Uiso 1 1 calc R . . H76C H 0.5532 0.3969 0.4956 0.268 Uiso 1 1 calc R . . C77 C 0.6930(16) 0.4761(10) 0.3829(13) 0.155(11) Uani 1 1 d . . . H77A H 0.7460 0.4617 0.3603 0.233 Uiso 1 1 calc R . . H77B H 0.6967 0.5108 0.4098 0.233 Uiso 1 1 calc R . . H77C H 0.6661 0.4980 0.3531 0.233 Uiso 1 1 calc R . . C78 C 0.7607(12) 0.3779(8) 0.1436(9) 0.095(5) Uani 1 1 d . . . H78 H 0.7092 0.3777 0.1346 0.114 Uiso 0.50(4) 1 calc PR C 1 H78A H 0.8056 0.3972 0.1542 0.114 Uiso 0.50(4) 1 calc PR C 2 C79 C 0.8066(16) 0.3590(9) 0.0910(10) 0.167(13) Uani 1 1 d . C . H79A H 0.8577 0.3841 0.0810 0.200 Uiso 1 1 calc R . . H79B H 0.7830 0.3784 0.0578 0.200 Uiso 1 1 calc R . . C80 C 0.9063(11) 0.2783(13) 0.0611(9) 0.154(11) Uani 1 1 d . . . H80A H 0.9205 0.2275 0.0656 0.231 Uiso 1 1 calc R . . H80B H 0.9324 0.3040 0.0838 0.231 Uiso 1 1 calc R . . H80C H 0.9233 0.2990 0.0168 0.231 Uiso 1 1 calc R . . C81 C 0.7954(19) 0.2579(16) 0.0403(8) 0.197(15) Uani 1 1 d . . . H81A H 0.8401 0.2412 0.0085 0.296 Uiso 1 1 calc R . . H81B H 0.7686 0.2963 0.0206 0.296 Uiso 1 1 calc R . . H81C H 0.7585 0.2180 0.0610 0.296 Uiso 1 1 calc R . . C82 C 0.7501(17) 0.4459(13) 0.1727(13) 0.057(8) Uiso 0.50(4) 1 d P C 1 H82A H 0.6984 0.4441 0.2055 0.068 Uiso 0.50(4) 1 calc PR C 1 H82B H 0.7916 0.4491 0.1927 0.068 Uiso 0.50(4) 1 calc PR C 1 C83 C 0.690(2) 0.513(3) 0.094(2) 0.136(19) Uiso 0.50(4) 1 d PD C 1 H83A H 0.6414 0.5316 0.1203 0.203 Uiso 0.50(4) 1 calc PR C 1 H83B H 0.6797 0.4654 0.0857 0.203 Uiso 0.50(4) 1 calc PR C 1 H83C H 0.7082 0.5456 0.0542 0.203 Uiso 0.50(4) 1 calc PR C 1 C84 C 0.742(5) 0.579(2) 0.152(3) 0.19(3) Uiso 0.50(4) 1 d PD C 1 H84A H 0.6852 0.5874 0.1695 0.286 Uiso 0.50(4) 1 calc PR C 1 H84B H 0.7649 0.6180 0.1180 0.286 Uiso 0.50(4) 1 calc PR C 1 H84C H 0.7671 0.5781 0.1848 0.286 Uiso 0.50(4) 1 calc PR C 1 C82A C 0.719(3) 0.441(3) 0.149(3) 0.130(18) Uiso 0.50(4) 1 d P C 2 H82C H 0.6914 0.4396 0.1937 0.156 Uiso 0.50(4) 1 calc PR C 2 H82D H 0.6785 0.4380 0.1281 0.156 Uiso 0.50(4) 1 calc PR C 2 C83A C 0.678(2) 0.552(3) 0.133(3) 0.17(2) Uiso 0.50(4) 1 d PD C 2 H83D H 0.6620 0.5708 0.1722 0.251 Uiso 0.50(4) 1 calc PR C 2 H83E H 0.6358 0.5206 0.1313 0.251 Uiso 0.50(4) 1 calc PR C 2 H83F H 0.6875 0.5913 0.0979 0.251 Uiso 0.50(4) 1 calc PR C 2 C84A C 0.803(3) 0.565(3) 0.141(3) 0.15(2) Uiso 0.50(4) 1 d PD C 2 H84D H 0.8048 0.6092 0.1114 0.230 Uiso 0.50(4) 1 calc PR C 2 H84E H 0.8568 0.5476 0.1359 0.230 Uiso 0.50(4) 1 calc PR C 2 H84F H 0.7791 0.5747 0.1835 0.230 Uiso 0.50(4) 1 calc PR C 2 O50 O 0.4298(8) 0.2598(7) 0.4842(6) 0.106(4) Uani 1 1 d . . . H50A H 0.4156 0.2166 0.4912 0.159 Uiso 1 1 calc R . . C91 C 0.3830(14) 0.2993(11) 0.4570(9) 0.115(7) Uani 1 1 d D . . H91 H 0.4165 0.3276 0.4174 0.138 Uiso 1 1 calc R . . C92 C 0.3199(16) 0.2649(14) 0.4435(14) 0.173(13) Uani 1 1 d . . . H92A H 0.3422 0.2304 0.4148 0.259 Uiso 1 1 calc R . . H92B H 0.2906 0.3013 0.4241 0.259 Uiso 1 1 calc R . . H92C H 0.2843 0.2397 0.4823 0.259 Uiso 1 1 calc R . . C93 C 0.336(2) 0.3538(11) 0.5012(11) 0.185(14) Uani 1 1 d D . . H93A H 0.3723 0.3802 0.5144 0.277 Uiso 1 1 calc R . . H93B H 0.2976 0.3271 0.5379 0.277 Uiso 1 1 calc R . . H93C H 0.3074 0.3877 0.4784 0.277 Uiso 1 1 calc R . . C101 C 0.494(4) 0.429(2) 1.024(2) 0.18(2) Uani 1 1 d . . . H101 H 0.4882 0.3797 1.0412 0.222 Uiso 1 1 calc R . . C102 C 0.466(2) 0.455(3) 0.980(3) 0.179(17) Uani 1 1 d . . . H102 H 0.4402 0.4227 0.9639 0.214 Uiso 1 1 calc R . . C103 C 0.4699(19) 0.526(5) 0.9549(17) 0.173(18) Uani 1 1 d . . . H103 H 0.4469 0.5424 0.9228 0.207 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 0.0389(2) 0.0493(3) 0.0320(2) -0.00736(17) -0.01141(17) 0.00633(19) W2 0.0387(2) 0.0455(2) 0.0320(2) -0.00134(17) -0.00740(17) -0.00217(19) W3 0.0366(2) 0.0482(3) 0.0346(2) 0.00026(18) -0.01006(17) 0.00391(19) W4 0.0429(2) 0.0434(2) 0.0394(2) -0.00031(18) -0.01075(18) 0.0051(2) W5 0.0618(3) 0.0470(3) 0.0358(2) -0.00606(19) -0.0099(2) -0.0041(2) W6 0.0425(2) 0.0510(3) 0.0467(2) 0.0133(2) -0.01477(19) -0.0071(2) W7 0.0350(2) 0.0457(2) 0.0312(2) -0.00624(17) -0.00849(16) 0.00007(18) W8 0.0368(2) 0.0496(3) 0.0308(2) 0.00246(17) -0.00836(16) -0.00085(19) W9 0.0346(2) 0.0445(2) 0.02910(19) -0.00227(16) -0.00522(16) 0.00116(18) W10 0.0488(3) 0.0444(3) 0.0412(2) -0.00452(19) -0.01385(19) 0.0055(2) W11 0.0441(2) 0.0547(3) 0.0311(2) -0.00972(18) -0.00642(17) -0.0021(2) W12 0.0457(3) 0.0483(3) 0.0387(2) -0.00637(19) -0.00556(19) -0.0090(2) O1 0.035(4) 0.046(4) 0.032(3) -0.004(3) -0.009(3) 0.004(3) O2 0.048(4) 0.037(4) 0.038(4) -0.007(3) -0.012(3) 0.013(3) O3 0.060(5) 0.062(5) 0.029(3) -0.009(3) -0.015(3) 0.012(4) O4 0.047(4) 0.048(4) 0.040(4) -0.006(3) -0.014(3) -0.004(3) O5 0.037(4) 0.055(4) 0.029(3) -0.006(3) -0.005(3) -0.003(3) O6 0.064(5) 0.037(4) 0.033(4) -0.002(3) -0.008(3) -0.009(4) O7 0.036(4) 0.068(5) 0.047(4) 0.002(4) 0.001(3) -0.005(4) O8 0.058(5) 0.040(4) 0.066(5) -0.002(4) -0.016(4) -0.003(4) O9 0.037(4) 0.049(4) 0.036(4) -0.007(3) -0.006(3) 0.005(3) O10 0.045(4) 0.034(4) 0.036(4) 0.002(3) -0.013(3) -0.007(3) O11 0.041(4) 0.075(6) 0.051(4) 0.001(4) -0.019(4) 0.005(4) O12 0.069(5) 0.039(4) 0.051(4) -0.007(3) -0.016(4) 0.008(4) O13 0.050(4) 0.046(4) 0.033(4) -0.007(3) -0.007(3) 0.000(3) O14 0.050(5) 0.058(5) 0.058(5) -0.006(4) -0.021(4) 0.013(4) O15 0.060(5) 0.037(4) 0.069(5) 0.007(4) -0.022(4) -0.006(4) O16 0.054(5) 0.060(5) 0.039(4) -0.008(3) -0.015(3) 0.003(4) O17 0.089(6) 0.069(6) 0.037(4) -0.003(4) -0.023(4) -0.016(5) O18 0.083(6) 0.039(4) 0.050(5) -0.012(4) -0.011(4) -0.007(4) O19 0.039(4) 0.063(5) 0.033(4) 0.009(3) -0.016(3) -0.004(4) O20 0.042(4) 0.101(7) 0.055(5) 0.032(5) -0.005(4) -0.003(5) O21 0.078(6) 0.039(5) 0.106(7) 0.003(5) -0.056(6) -0.008(4) O22 0.036(4) 0.045(4) 0.038(4) -0.002(3) -0.009(3) -0.002(3) O23 0.048(4) 0.037(4) 0.046(4) -0.013(3) -0.016(3) 0.005(3) O24 0.029(4) 0.060(5) 0.053(4) -0.005(4) 0.002(3) -0.007(3) O25 0.049(4) 0.042(4) 0.055(5) -0.013(3) -0.020(4) -0.001(3) O26 0.036(4) 0.058(5) 0.032(3) 0.005(3) -0.014(3) -0.005(3) O27 0.054(4) 0.046(4) 0.034(4) -0.009(3) -0.012(3) -0.001(4) O28 0.042(4) 0.087(6) 0.045(4) 0.013(4) -0.021(3) -0.003(4) O29 0.063(5) 0.038(4) 0.055(5) -0.004(3) -0.003(4) -0.001(4) O30 0.032(4) 0.049(4) 0.036(4) -0.008(3) -0.013(3) 0.006(3) O31 0.043(4) 0.041(4) 0.037(4) -0.009(3) -0.009(3) -0.004(3) O32 0.050(4) 0.054(5) 0.032(4) -0.005(3) -0.003(3) 0.003(4) O33 0.041(4) 0.035(4) 0.043(4) -0.002(3) -0.003(3) 0.009(3) O34 0.048(4) 0.056(5) 0.033(4) -0.010(3) -0.012(3) 0.003(4) O35 0.076(6) 0.068(5) 0.039(4) 0.005(4) -0.025(4) 0.004(5) O36 0.068(5) 0.042(4) 0.059(5) -0.010(4) -0.004(4) 0.011(4) O37 0.048(4) 0.051(4) 0.032(4) -0.008(3) -0.011(3) -0.006(3) O38 0.059(5) 0.075(6) 0.035(4) -0.010(4) 0.005(4) -0.001(4) O39 0.059(5) 0.051(5) 0.055(5) -0.018(4) -0.021(4) 0.003(4) O40 0.048(4) 0.052(5) 0.041(4) -0.002(3) -0.010(3) 0.000(4) O41 0.040(4) 0.081(6) 0.061(5) -0.017(4) -0.011(4) -0.018(4) O42 0.079(6) 0.037(4) 0.072(6) -0.011(4) -0.015(5) -0.003(4) N1 0.046(5) 0.062(6) 0.041(5) -0.019(4) -0.018(4) 0.006(5) N2 0.067(7) 0.071(7) 0.057(6) -0.021(5) -0.018(5) 0.007(6) N3 0.045(5) 0.072(7) 0.040(5) 0.008(5) -0.008(4) -0.014(5) N4 0.123(13) 0.065(9) 0.137(14) 0.028(9) -0.053(11) -0.019(9) N5 0.047(6) 0.077(7) 0.048(6) -0.002(5) -0.003(4) 0.011(5) N6 0.098(11) 0.105(12) 0.108(12) -0.043(10) -0.008(9) -0.033(9) N7 0.069(7) 0.064(7) 0.047(6) 0.013(5) -0.021(5) -0.001(6) N9 0.082(8) 0.065(7) 0.050(6) -0.022(5) 0.007(6) -0.006(6) N10 0.143(14) 0.088(10) 0.092(10) -0.040(8) -0.045(10) 0.005(10) N11 0.071(7) 0.058(7) 0.065(7) 0.002(5) -0.022(6) 0.004(6) N13 0.038(5) 0.054(6) 0.047(5) -0.009(4) -0.015(4) 0.002(4) N14 0.127(12) 0.079(9) 0.085(9) -0.045(8) 0.003(8) -0.024(9) N15 0.045(5) 0.055(6) 0.040(5) 0.006(4) -0.013(4) -0.009(5) N16 0.062(7) 0.065(7) 0.083(8) -0.008(6) -0.007(6) 0.010(6) N17 0.038(5) 0.061(6) 0.044(5) 0.003(4) -0.004(4) -0.001(4) N18 0.060(7) 0.060(7) 0.078(8) -0.012(6) -0.007(6) 0.011(6) N19 0.051(6) 0.055(6) 0.081(7) -0.026(6) -0.020(5) 0.012(5) N20 0.178(17) 0.067(9) 0.184(18) -0.051(11) -0.097(15) 0.046(10) N21 0.061(6) 0.058(6) 0.037(5) -0.004(4) -0.013(4) -0.006(5) N22 0.096(10) 0.054(7) 0.111(10) -0.022(7) -0.044(8) -0.008(7) N23 0.064(7) 0.064(7) 0.052(6) 0.005(5) -0.005(5) -0.022(6) N24 0.198(19) 0.048(8) 0.172(17) 0.002(9) -0.103(15) 0.001(10) C1 0.044(7) 0.067(8) 0.074(9) -0.011(7) -0.017(6) -0.001(6) C2 0.041(6) 0.071(8) 0.060(7) -0.021(6) -0.007(5) 0.009(6) C3 0.053(7) 0.078(9) 0.070(8) -0.003(7) -0.028(6) 0.003(7) C4 0.045(7) 0.089(10) 0.070(8) -0.041(7) -0.021(6) 0.022(7) C5 0.061(8) 0.054(8) 0.072(8) -0.005(6) -0.024(7) -0.005(6) C6 0.090(11) 0.088(11) 0.064(9) -0.034(8) -0.009(8) 0.013(9) C7 0.082(11) 0.082(11) 0.096(12) -0.034(9) -0.029(9) 0.009(9) C8 0.086(11) 0.068(10) 0.079(10) 0.009(8) -0.008(9) -0.002(9) C9 0.095(11) 0.058(9) 0.107(12) 0.033(8) -0.056(10) -0.007(8) C10 0.054(9) 0.30(3) 0.036(7) 0.038(12) -0.007(6) 0.023(13) C11 0.089(10) 0.065(8) 0.043(7) 0.003(6) -0.027(7) -0.003(7) C12 0.088(12) 0.110(14) 0.089(12) 0.001(10) -0.035(9) -0.017(10) C13 0.35(4) 0.064(12) 0.123(18) -0.013(12) -0.11(2) 0.059(19) C14 0.20(3) 0.13(2) 0.127(19) 0.035(16) -0.061(19) 0.020(19) C15 0.109(12) 0.066(9) 0.054(8) -0.012(7) 0.003(8) 0.023(9) C16 0.102(14) 0.118(16) 0.134(16) -0.088(14) 0.037(12) -0.028(12) C17 0.078(11) 0.26(3) 0.032(7) -0.010(11) -0.011(7) 0.060(14) C18 0.042(7) 0.084(10) 0.059(8) -0.014(7) -0.008(6) 0.004(7) C19 0.111(15) 0.109(15) 0.118(15) -0.061(12) -0.014(12) 0.009(12) C20 0.16(2) 0.15(2) 0.14(2) -0.056(18) -0.021(18) 0.080(18) C21 0.105(15) 0.101(15) 0.18(2) 0.012(15) -0.043(15) 0.029(12) C24 0.109(15) 0.36(4) 0.055(10) 0.058(16) -0.058(11) -0.04(2) C25 0.098(11) 0.097(11) 0.034(6) 0.016(7) 0.004(7) 0.017(9) N8 0.073(18) 0.056(16) 0.16(3) -0.016(16) -0.047(18) 0.003(14) N8A 0.17(4) 0.033(15) 0.053(16) -0.002(11) -0.002(19) -0.03(2) C29 0.091(11) 0.060(9) 0.089(11) -0.040(8) 0.012(9) -0.004(8) C30 0.121(15) 0.110(15) 0.097(13) -0.049(12) 0.023(11) -0.001(12) C31 0.112(13) 0.095(12) 0.066(10) -0.020(9) 0.011(9) -0.016(10) C32 0.071(11) 0.19(2) 0.074(11) -0.043(12) 0.003(9) 0.037(12) C33 0.18(2) 0.094(15) 0.15(2) -0.064(14) 0.059(17) -0.045(15) C34 0.22(3) 0.13(2) 0.23(3) -0.05(2) -0.06(3) 0.06(2) C35 0.24(4) 0.23(3) 0.28(4) -0.19(3) -0.15(3) 0.10(3) N12 0.07(2) 0.05(2) 0.067(18) -0.001(14) -0.032(15) -0.019(18) N12A 0.12(5) 0.06(3) 0.36(10) -0.07(4) -0.11(6) 0.01(3) C38 0.071(12) 0.26(3) 0.19(2) -0.13(2) -0.070(14) 0.072(16) C39 0.19(2) 0.129(16) 0.159(19) 0.100(15) -0.147(18) -0.106(16) C43 0.139(16) 0.085(12) 0.089(11) -0.036(10) -0.061(11) 0.028(11) C44 0.42(4) 0.055(10) 0.118(15) -0.047(10) -0.18(2) 0.062(17) C45 0.058(9) 0.33(3) 0.049(9) -0.018(14) -0.023(7) 0.022(15) C46 0.141(16) 0.132(15) 0.042(8) 0.018(9) -0.035(9) -0.067(13) C47 0.171(19) 0.068(10) 0.093(12) -0.056(9) -0.024(12) 0.008(11) C48 0.098(15) 0.15(2) 0.16(2) -0.033(17) -0.053(14) -0.011(14) C49 0.090(17) 0.46(6) 0.29(4) -0.31(4) -0.02(2) 0.02(3) C50 0.101(12) 0.050(8) 0.082(10) -0.012(7) 0.015(9) -0.012(8) C51 0.071(9) 0.059(9) 0.084(10) -0.010(7) -0.004(8) -0.012(7) C52 0.038(6) 0.090(10) 0.051(7) 0.000(7) -0.002(5) -0.001(6) C53 0.072(9) 0.118(13) 0.031(6) 0.017(7) -0.008(6) -0.023(9) C54 0.052(8) 0.077(10) 0.072(9) -0.001(7) -0.012(6) -0.005(7) C55 0.133(17) 0.125(17) 0.109(15) -0.056(13) -0.037(13) 0.010(13) C56 0.134(16) 0.075(11) 0.089(12) 0.021(9) -0.016(11) 0.000(11) C57 0.050(7) 0.070(8) 0.040(6) 0.004(6) -0.012(5) 0.011(6) C58 0.045(7) 0.072(8) 0.053(7) -0.007(6) -0.014(5) 0.016(6) C59 0.046(7) 0.072(9) 0.064(8) 0.012(7) -0.007(6) -0.001(6) C60 0.043(7) 0.099(11) 0.057(7) -0.017(7) -0.021(6) 0.010(7) C61 0.060(8) 0.050(7) 0.074(9) 0.002(6) 0.000(7) 0.014(6) C62 0.083(11) 0.087(11) 0.083(11) -0.035(9) 0.008(9) 0.015(9) C63 0.133(17) 0.095(14) 0.120(16) -0.039(12) 0.026(13) 0.032(12) C64 0.067(10) 0.057(9) 0.114(13) -0.023(9) -0.017(9) 0.001(8) C65 0.11(3) 0.032(19) 0.10(4) -0.01(2) 0.00(3) 0.027(19) C65A 0.052(15) 0.05(2) 0.08(2) -0.026(18) 0.014(14) 0.019(13) C66 0.059(10) 0.19(2) 0.116(15) -0.051(15) -0.025(10) 0.010(12) C67 0.043(8) 0.172(19) 0.090(12) 0.026(12) 0.009(8) 0.027(10) C68 0.088(12) 0.070(11) 0.21(2) -0.078(13) -0.024(13) 0.020(10) C71 0.117(14) 0.081(11) 0.111(13) -0.050(10) -0.069(11) 0.048(10) C72 0.169(18) 0.053(9) 0.087(11) 0.001(8) -0.083(12) -0.027(10) C73 0.116(13) 0.090(11) 0.044(7) 0.018(7) -0.035(8) -0.042(10) C74 0.072(11) 0.25(3) 0.095(13) -0.090(16) -0.038(10) 0.009(14) C75 0.143(17) 0.070(11) 0.128(15) -0.023(10) -0.091(14) 0.013(11) C76 0.13(2) 0.27(4) 0.18(3) -0.14(3) -0.068(19) 0.04(2) C77 0.20(3) 0.068(12) 0.22(3) 0.024(15) -0.12(2) -0.055(15) C78 0.119(14) 0.052(9) 0.118(14) -0.013(9) -0.040(12) 0.010(9) C79 0.22(3) 0.059(11) 0.115(16) 0.039(10) 0.070(17) 0.038(14) C80 0.086(13) 0.20(2) 0.097(14) 0.078(15) 0.035(11) 0.034(14) C81 0.30(4) 0.23(3) 0.051(10) 0.081(14) -0.071(16) -0.17(3) O50 0.119(10) 0.103(9) 0.091(8) -0.016(7) -0.026(7) 0.028(8) C91 0.123(17) 0.111(16) 0.107(15) 0.007(12) -0.041(13) 0.005(14) C92 0.14(2) 0.14(2) 0.19(3) -0.06(2) 0.043(19) -0.061(17) C93 0.36(4) 0.086(15) 0.122(19) -0.048(14) -0.09(2) 0.06(2) C101 0.20(4) 0.20(4) 0.10(2) -0.04(3) 0.05(2) 0.05(4) C102 0.18(3) 0.15(4) 0.17(4) -0.04(3) 0.02(3) -0.03(3) C103 0.10(2) 0.24(6) 0.16(3) -0.08(5) 0.00(2) 0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O3 1.726(7) . ? W1 O9 1.784(7) . ? W1 O2 1.892(6) . ? W1 O4 1.905(7) . ? W1 O1 2.178(6) . ? W1 N1 2.402(9) . ? W2 O7 1.723(7) . ? W2 O1 1.754(6) . ? W2 O8 1.910(8) . ? W2 O6 1.916(7) . ? W2 O5 2.196(7) . ? W2 N3 2.341(10) . ? W3 O11 1.718(7) . ? W3 O5 1.760(6) . ? W3 O10 1.903(6) . ? W3 O12 1.920(8) . ? W3 O9 2.210(7) . ? W3 N5 2.367(9) . ? W4 O14 1.732(7) . ? W4 O13 1.760(7) . ? W4 O2 1.884(7) . ? W4 O15 1.907(8) . ? W4 O19 2.175(7) . ? W4 N7 2.428(10) . ? W5 O17 1.718(8) . ? W5 O16 1.761(7) . ? W5 O6 1.874(7) . ? W5 O18 1.917(8) . ? W5 O13 2.213(7) . ? W5 N9 2.346(11) . ? W6 O20 1.720(8) . ? W6 O19 1.767(7) . ? W6 O10 1.876(6) . ? W6 O21 1.918(9) . ? W6 O16 2.210(7) . ? W6 N11 2.378(12) . ? W7 O24 1.712(7) . ? W7 O22 1.762(7) . ? W7 O23 1.905(7) . ? W7 O25 1.927(7) . ? W7 O30 2.235(6) . ? W7 N13 2.382(9) . ? W8 O28 1.716(7) . ? W8 O26 1.765(6) . ? W8 O27 1.905(7) . ? W8 O29 1.906(8) . ? W8 O22 2.193(7) . ? W8 N15 2.382(8) . ? W9 O32 1.716(7) . ? W9 O30 1.781(6) . ? W9 O31 1.901(7) . ? W9 O33 1.907(7) . ? W9 O26 2.178(6) . ? W9 N17 2.389(9) . ? W10 O35 1.706(7) . ? W10 O40 1.767(7) . ? W10 O23 1.889(7) . ? W10 O36 1.906(8) . ? W10 O34 2.197(7) . ? W10 N19 2.389(10) . ? W11 O38 1.730(7) . ? W11 O34 1.762(7) . ? W11 O27 1.880(7) . ? W11 O39 1.914(8) . ? W11 O37 2.165(7) . ? W11 N21 2.336(10) . ? W12 O41 1.722(8) . ? W12 O37 1.779(7) . ? W12 O31 1.887(7) . ? W12 O42 1.899(8) . ? W12 O40 2.203(8) . ? W12 N23 2.363(10) . ? O4 C1 1.446(14) . ? O8 C8 1.372(17) . ? O12 C15 1.402(14) . ? O15 C22 1.38(2) . ? O15 C22A 1.58(4) . ? O18 C29 1.397(14) . ? O21 C36 1.37(3) . ? O21 C36A 1.50(3) . ? O25 C43 1.397(17) . ? O29 C50 1.385(15) . ? O33 C57 1.440(13) . ? O36 C64 1.399(16) . ? O39 C71 1.390(17) . ? O42 C78 1.407(18) . ? N1 C4 1.461(14) . ? N1 C3 1.463(15) . ? N1 C2 1.475(15) . ? N2 C7 1.432(17) . ? N2 C5 1.450(16) . ? N2 C6 1.486(18) . ? N3 C10 1.439(15) . ? N3 C11 1.474(17) . ? N3 C9 1.532(18) . ? N4 C12 1.39(2) . ? N4 C13 1.42(3) . ? N4 C14 1.49(3) . ? N5 C17 1.437(17) . ? N5 C18 1.447(16) . ? N5 C16 1.51(2) . ? N6 C20 1.40(3) . ? N6 C19 1.46(2) . ? N6 C21 1.48(2) . ? N7 C23A 1.42(3) . ? N7 C24 1.45(2) . ? N7 C25 1.459(16) . ? N7 C23 1.55(3) . ? N9 C32 1.45(2) . ? N9 C31 1.472(18) . ? N9 C30 1.47(2) . ? N10 C33 1.37(2) . ? N10 C35 1.39(3) . ? N10 C34 1.41(3) . ? N11 C37 1.34(3) . ? N11 C38 1.42(2) . ? N11 C39 1.454(18) . ? N11 C37A 1.492(17) . ? N13 C45 1.446(17) . ? N13 C46 1.446(17) . ? N13 C44 1.463(18) . ? N14 C49 1.44(3) . ? N14 C48 1.44(2) . ? N14 C47 1.48(2) . ? N15 C52 1.450(14) . ? N15 C53 1.485(15) . ? N15 C51 1.503(16) . ? N16 C54 1.418(17) . ? N16 C55 1.42(2) . ? N16 C56 1.452(19) . ? N16 H16 0.9300 . ? N17 C59 1.479(14) . ? N17 C60 1.500(15) . ? N17 C58 1.502(15) . ? N18 C63 1.437(19) . ? N18 C61 1.452(17) . ? N18 C62 1.46(2) . ? N19 C67 1.451(19) . ? N19 C66 1.47(2) . ? N19 C65A 1.47(3) . ? N19 C65 1.55(3) . ? N20 C69 1.42(4) . ? N20 C68 1.52(2) . ? N20 C70 1.54(4) . ? N21 C73 1.453(15) . ? N21 C72 1.499(17) . ? N21 C74 1.513(18) . ? N22 C76 1.44(2) . ? N22 C75 1.455(19) . ? N22 C77 1.46(2) . ? N23 C80 1.421(19) . ? N23 C79 1.43(2) . ? N23 C81 1.44(2) . ? N24 C82A 1.38(5) . ? N24 C82 1.42(3) . ? N24 C84 1.53(2) . ? N24 C84A 1.540(19) . ? N24 C83A 1.548(19) . ? N24 C83 1.548(19) . ? C1 C2 1.487(17) . ? C1 C5 1.507(18) . ? C1 H1 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.39(2) . ? C8 C12 1.583(15) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.41(2) . ? C15 C19 1.49(2) . ? C15 H15 1.0000 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? N8 C27 1.38(4) . ? N8 C26 1.463(19) . ? N8 C28 1.51(5) . ? C22 C23 1.51(4) . ? C22 C26 1.546(19) . ? C22 H22 1.0000 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? N8A C28A 1.38(5) . ? N8A C27A 1.46(5) . ? N8A C26A 1.47(5) . ? C22A C23A 1.43(5) . ? C22A C26A 1.45(5) . ? C22A H22A 1.0000 . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27A H27D 0.9800 . ? C27A H27E 0.9800 . ? C27A H27F 0.9800 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29 C30 1.47(2) . ? C29 C33 1.53(3) . ? C29 H29 1.0000 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C40 1.30(4) . ? C36 C37 1.469(18) . ? C36 H36 1.0000 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C40 N12 1.49(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N12 C42 1.36(6) . ? N12 C41 1.46(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C36A C37A 1.32(3) . ? C36A C40A 1.37(4) . ? C36A H36A 1.0000 . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C40A N12A 1.41(8) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? N12A C41A 1.39(7) . ? N12A C42A 1.46(2) . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C43 C44 1.32(2) . ? C43 C47 1.38(2) . ? C43 H43 1.0000 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.400(19) . ? C50 C54 1.50(2) . ? C50 H50 1.0000 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.485(17) . ? C57 C61 1.506(18) . ? C57 H57 1.0000 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.39(6) . ? C64 C68 1.40(2) . ? C64 C65A 1.51(4) . ? C64 H64 1.0000 . ? C64 H64A 1.0000 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C65A H65C 0.9900 . ? C65A H65D 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C72 1.37(2) . ? C71 C75 1.40(2) . ? C71 H71 1.0000 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.32(2) . ? C78 C82A 1.37(5) . ? C78 C82 1.51(3) . ? C78 H78 1.0000 . ? C78 H78A 1.0000 . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C82A H82C 0.9900 . ? C82A H82D 0.9900 . ? C83A H83D 0.9800 . ? C83A H83E 0.9800 . ? C83A H83F 0.9800 . ? C84A H84D 0.9800 . ? C84A H84E 0.9800 . ? C84A H84F 0.9800 . ? O50 C91 1.33(2) . ? O50 H50A 0.8400 . ? C91 C92 1.45(3) . ? C91 C93 1.588(17) . ? C91 H91 1.0000 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C101 C102 1.27(5) . ? C101 C103 1.31(5) 2_667 ? C101 H101 0.9500 . ? C102 C103 1.37(5) . ? C102 H102 0.9500 . ? C103 C101 1.31(5) 2_667 ? C103 H103 0.9500 . ? 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 O9 103.7(3) . . ? O3 W1 O2 95.6(3) . . ? O9 W1 O2 102.1(3) . . ? O3 W1 O4 96.9(3) . . ? O9 W1 O4 98.4(3) . . ? O2 W1 O4 152.7(3) . . ? O3 W1 O1 168.1(3) . . ? O9 W1 O1 88.1(3) . . ? O2 W1 O1 81.2(3) . . ? O4 W1 O1 81.6(3) . . ? O3 W1 N1 92.1(3) . . ? O9 W1 N1 163.7(3) . . ? O2 W1 N1 79.9(3) . . ? O4 W1 N1 75.5(3) . . ? O1 W1 N1 76.1(3) . . ? O7 W2 O1 103.4(3) . . ? O7 W2 O8 97.5(4) . . ? O1 W2 O8 95.2(3) . . ? O7 W2 O6 95.9(4) . . ? O1 W2 O6 102.0(3) . . ? O8 W2 O6 155.1(3) . . ? O7 W2 O5 169.4(3) . . ? O1 W2 O5 87.2(3) . . ? O8 W2 O5 82.5(3) . . ? O6 W2 O5 80.5(3) . . ? O7 W2 N3 92.4(3) . . ? O1 W2 N3 162.3(3) . . ? O8 W2 N3 74.6(4) . . ? O6 W2 N3 83.9(3) . . ? O5 W2 N3 77.3(3) . . ? O11 W3 O5 101.4(3) . . ? O11 W3 O10 95.6(4) . . ? O5 W3 O10 102.4(3) . . ? O11 W3 O12 98.6(4) . . ? O5 W3 O12 96.0(3) . . ? O10 W3 O12 154.0(3) . . ? O11 W3 O9 169.7(3) . . ? O5 W3 O9 88.9(3) . . ? O10 W3 O9 81.8(3) . . ? O12 W3 O9 80.4(3) . . ? O11 W3 N5 90.0(4) . . ? O5 W3 N5 166.6(4) . . ? O10 W3 N5 83.1(3) . . ? O12 W3 N5 75.2(4) . . ? O9 W3 N5 79.9(3) . . ? O14 W4 O13 104.5(4) . . ? O14 W4 O2 95.5(3) . . ? O13 W4 O2 103.2(3) . . ? O14 W4 O15 98.0(4) . . ? O13 W4 O15 96.5(3) . . ? O2 W4 O15 152.4(3) . . ? O14 W4 O19 167.2(3) . . ? O13 W4 O19 88.2(3) . . ? O2 W4 O19 79.5(3) . . ? O15 W4 O19 82.1(3) . . ? O14 W4 N7 90.3(4) . . ? O13 W4 N7 164.0(4) . . ? O2 W4 N7 81.1(3) . . ? O15 W4 N7 74.9(4) . . ? O19 W4 N7 77.3(3) . . ? O17 W5 O16 102.0(4) . . ? O17 W5 O6 96.4(4) . . ? O16 W5 O6 103.7(3) . . ? O17 W5 O18 96.6(4) . . ? O16 W5 O18 98.0(4) . . ? O6 W5 O18 151.7(4) . . ? O17 W5 O13 172.3(3) . . ? O16 W5 O13 85.7(3) . . ? O6 W5 O13 82.2(3) . . ? O18 W5 O13 81.6(3) . . ? O17 W5 N9 88.2(4) . . ? O16 W5 N9 167.9(4) . . ? O6 W5 N9 81.2(4) . . ? O18 W5 N9 74.2(4) . . ? O13 W5 N9 84.1(4) . . ? O20 W6 O19 103.6(4) . . ? O20 W6 O10 96.2(4) . . ? O19 W6 O10 102.8(3) . . ? O20 W6 O21 98.6(5) . . ? O19 W6 O21 95.3(4) . . ? O10 W6 O21 153.1(3) . . ? O20 W6 O16 168.9(4) . . ? O19 W6 O16 87.4(3) . . ? O10 W6 O16 80.5(3) . . ? O21 W6 O16 80.7(4) . . ? O20 W6 N11 90.4(4) . . ? O19 W6 N11 164.1(4) . . ? O10 W6 N11 82.8(3) . . ? O21 W6 N11 74.8(4) . . ? O16 W6 N11 78.7(3) . . ? O24 W7 O22 101.9(3) . . ? O24 W7 O23 96.9(3) . . ? O22 W7 O23 104.6(3) . . ? O24 W7 O25 97.5(3) . . ? O22 W7 O25 96.1(3) . . ? O23 W7 O25 151.7(3) . . ? O24 W7 O30 171.2(3) . . ? O22 W7 O30 86.9(3) . . ? O23 W7 O30 80.3(3) . . ? O25 W7 O30 81.7(3) . . ? O24 W7 N13 88.5(3) . . ? O22 W7 N13 167.3(3) . . ? O23 W7 N13 81.0(3) . . ? O25 W7 N13 75.1(3) . . ? O30 W7 N13 82.8(3) . . ? O28 W8 O26 103.3(3) . . ? O28 W8 O27 96.0(4) . . ? O26 W8 O27 103.3(3) . . ? O28 W8 O29 97.7(4) . . ? O26 W8 O29 95.8(3) . . ? O27 W8 O29 153.2(3) . . ? O28 W8 O22 170.6(3) . . ? O26 W8 O22 85.9(3) . . ? O27 W8 O22 80.1(3) . . ? O29 W8 O22 82.7(3) . . ? O28 W8 N15 93.0(3) . . ? O26 W8 N15 162.3(3) . . ? O27 W8 N15 81.3(3) . . ? O29 W8 N15 75.0(3) . . ? O22 W8 N15 77.9(3) . . ? O32 W9 O30 103.3(3) . . ? O32 W9 O31 96.3(3) . . ? O30 W9 O31 103.8(3) . . ? O32 W9 O33 97.2(3) . . ? O30 W9 O33 96.6(3) . . ? O31 W9 O33 152.1(3) . . ? O32 W9 O26 166.2(3) . . ? O30 W9 O26 90.5(3) . . ? O31 W9 O26 79.6(3) . . ? O33 W9 O26 81.5(3) . . ? O32 W9 N17 87.1(3) . . ? O30 W9 N17 167.8(3) . . ? O31 W9 N17 80.9(3) . . ? O33 W9 N17 75.5(3) . . ? O26 W9 N17 79.2(3) . . ? O35 W10 O40 103.7(4) . . ? O35 W10 O23 97.0(4) . . ? O40 W10 O23 103.2(3) . . ? O35 W10 O36 98.0(4) . . ? O40 W10 O36 94.5(4) . . ? O23 W10 O36 153.3(3) . . ? O35 W10 O34 168.0(4) . . ? O40 W10 O34 88.2(3) . . ? O23 W10 O34 79.3(3) . . ? O36 W10 O34 81.5(3) . . ? O35 W10 N19 90.0(4) . . ? O40 W10 N19 163.8(4) . . ? O23 W10 N19 83.2(3) . . ? O36 W10 N19 74.8(4) . . ? O34 W10 N19 78.3(3) . . ? O38 W11 O34 103.7(4) . . ? O38 W11 O27 96.4(4) . . ? O34 W11 O27 103.2(3) . . ? O38 W11 O39 95.8(4) . . ? O34 W11 O39 95.9(3) . . ? O27 W11 O39 154.2(3) . . ? O38 W11 O37 168.8(3) . . ? O34 W11 O37 87.5(3) . . ? O27 W11 O37 80.9(3) . . ? O39 W11 O37 82.8(3) . . ? O38 W11 N21 88.6(4) . . ? O34 W11 N21 165.6(3) . . ? O27 W11 N21 82.6(3) . . ? O39 W11 N21 75.1(3) . . ? O37 W11 N21 80.2(3) . . ? O41 W12 O37 102.7(4) . . ? O41 W12 O31 95.8(4) . . ? O37 W12 O31 103.9(3) . . ? O41 W12 O42 99.2(4) . . ? O37 W12 O42 94.2(4) . . ? O31 W12 O42 153.2(4) . . ? O41 W12 O40 169.8(3) . . ? O37 W12 O40 87.1(3) . . ? O31 W12 O40 78.9(3) . . ? O42 W12 O40 82.6(3) . . ? O41 W12 N23 90.9(4) . . ? O37 W12 N23 164.1(4) . . ? O31 W12 N23 82.6(3) . . ? O42 W12 N23 75.2(4) . . ? O40 W12 N23 79.8(3) . . ? W2 O1 W1 152.3(4) . . ? W4 O2 W1 161.0(4) . . ? C1 O4 W1 126.9(7) . . ? W3 O5 W2 150.6(4) . . ? W5 O6 W2 158.3(4) . . ? C8 O8 W2 127.4(9) . . ? W1 O9 W3 149.2(4) . . ? W6 O10 W3 160.0(4) . . ? C15 O12 W3 127.0(8) . . ? W4 O13 W5 152.3(4) . . ? C22 O15 W4 129.0(11) . . ? C22A O15 W4 120.7(14) . . ? W5 O16 W6 153.1(4) . . ? C29 O18 W5 126.2(8) . . ? W6 O19 W4 150.6(4) . . ? C36 O21 W6 125.2(11) . . ? C36A O21 W6 127.1(11) . . ? W7 O22 W8 155.5(4) . . ? W10 O23 W7 158.5(4) . . ? C43 O25 W7 125.0(8) . . ? W8 O26 W9 150.4(4) . . ? W11 O27 W8 157.1(4) . . ? C50 O29 W8 126.2(7) . . ? W9 O30 W7 147.0(4) . . ? W12 O31 W9 156.9(4) . . ? C57 O33 W9 126.0(7) . . ? W11 O34 W10 150.6(4) . . ? C64 O36 W10 128.3(9) . . ? W12 O37 W11 151.9(4) . . ? C71 O39 W11 126.3(8) . . ? W10 O40 W12 149.9(4) . . ? C78 O42 W12 125.3(9) . . ? C4 N1 C3 107.3(9) . . ? C4 N1 C2 108.9(10) . . ? C3 N1 C2 109.1(10) . . ? C4 N1 W1 117.2(7) . . ? C3 N1 W1 111.0(7) . . ? C2 N1 W1 103.0(6) . . ? C7 N2 C5 112.2(12) . . ? C7 N2 C6 110.5(11) . . ? C5 N2 C6 110.2(11) . . ? C10 N3 C11 109.3(13) . . ? C10 N3 C9 113.2(14) . . ? C11 N3 C9 106.6(10) . . ? C10 N3 W2 108.8(8) . . ? C11 N3 W2 116.3(7) . . ? C9 N3 W2 102.7(8) . . ? C12 N4 C13 111.2(17) . . ? C12 N4 C14 109.8(16) . . ? C13 N4 C14 104.0(19) . . ? C17 N5 C18 109.3(12) . . ? C17 N5 C16 111.6(16) . . ? C18 N5 C16 105.1(12) . . ? C17 N5 W3 114.4(8) . . ? C18 N5 W3 111.6(8) . . ? C16 N5 W3 104.3(8) . . ? C20 N6 C19 109.9(18) . . ? C20 N6 C21 107.3(18) . . ? C19 N6 C21 105.0(17) . . ? C23A N7 C24 94(2) . . ? C23A N7 C25 121.5(18) . . ? C24 N7 C25 109.8(16) . . ? C24 N7 C23 121.4(18) . . ? C25 N7 C23 99.2(15) . . ? C23A N7 W4 104.2(14) . . ? C24 N7 W4 109.0(9) . . ? C25 N7 W4 116.2(7) . . ? C23 N7 W4 101.4(11) . . ? C32 N9 C31 107.7(14) . . ? C32 N9 C30 111.5(16) . . ? C31 N9 C30 107.6(12) . . ? C32 N9 W5 113.8(8) . . ? C31 N9 W5 114.2(10) . . ? C30 N9 W5 101.8(10) . . ? C33 N10 C35 114(2) . . ? C33 N10 C34 114(2) . . ? C35 N10 C34 101(2) . . ? C37 N11 C38 100(2) . . ? C37 N11 C39 118(2) . . ? C38 N11 C39 105.2(17) . . ? C38 N11 C37A 121(2) . . ? C39 N11 C37A 99.2(18) . . ? C37 N11 W6 105.1(13) . . ? C38 N11 W6 112.3(11) . . ? C39 N11 W6 115.9(9) . . ? C37A N11 W6 103.0(12) . . ? C45 N13 C46 108.9(14) . . ? C45 N13 C44 112.8(18) . . ? C46 N13 C44 106.5(15) . . ? C45 N13 W7 111.3(8) . . ? C46 N13 W7 113.7(8) . . ? C44 N13 W7 103.4(8) . . ? C49 N14 C48 108.6(18) . . ? C49 N14 C47 109.8(19) . . ? C48 N14 C47 113.5(16) . . ? C52 N15 C53 108.9(10) . . ? C52 N15 C51 107.8(10) . . ? C53 N15 C51 112.2(11) . . ? C52 N15 W8 114.9(7) . . ? C53 N15 W8 108.8(7) . . ? C51 N15 W8 104.2(7) . . ? C54 N16 C55 114.6(14) . . ? C54 N16 C56 112.7(14) . . ? C55 N16 C56 107.8(15) . . ? C54 N16 H16 107.1 . . ? C55 N16 H16 107.1 . . ? C56 N16 H16 107.1 . . ? C59 N17 C60 106.3(10) . . ? C59 N17 C58 109.2(9) . . ? C60 N17 C58 109.8(9) . . ? C59 N17 W9 112.1(7) . . ? C60 N17 W9 116.2(6) . . ? C58 N17 W9 103.1(7) . . ? C63 N18 C61 108.8(12) . . ? C63 N18 C62 110.7(15) . . ? C61 N18 C62 110.8(10) . . ? C67 N19 C66 105.3(14) . . ? C67 N19 C65A 98(2) . . ? C66 N19 C65A 122(2) . . ? C67 N19 C65 129(3) . . ? C66 N19 C65 92(3) . . ? C67 N19 W10 115.6(8) . . ? C66 N19 W10 110.9(9) . . ? C65A N19 W10 105.1(12) . . ? C65 N19 W10 101.4(18) . . ? C69 N20 C68 113(2) . . ? C69 N20 C70 103(3) . . ? C68 N20 C70 103(2) . . ? C73 N21 C72 109.2(11) . . ? C73 N21 C74 105.5(13) . . ? C72 N21 C74 107.6(14) . . ? C73 N21 W11 112.0(8) . . ? C72 N21 W11 105.9(8) . . ? C74 N21 W11 116.5(8) . . ? C76 N22 C75 109.6(16) . . ? C76 N22 C77 107.4(19) . . ? C75 N22 C77 109.2(16) . . ? C80 N23 C79 107.8(17) . . ? C80 N23 C81 102.4(19) . . ? C79 N23 C81 115(2) . . ? C80 N23 W12 112.6(10) . . ? C79 N23 W12 104.4(9) . . ? C81 N23 W12 115.2(9) . . ? C82A N24 C84 134(4) . . ? C82 N24 C84 115(3) . . ? C82A N24 C84A 145(4) . . ? C82 N24 C84A 107(3) . . ? C82A N24 C83A 98(4) . . ? C82 N24 C83A 117(3) . . ? C84 N24 C83A 57(3) . . ? C84A N24 C83A 98(3) . . ? C82A N24 C83 80(3) . . ? C82 N24 C83 116(3) . . ? C84 N24 C83 100(4) . . ? C84A N24 C83 132(3) . . ? C83A N24 C83 45(3) . . ? O4 C1 C2 107.1(10) . . ? O4 C1 C5 110.6(10) . . ? C2 C1 C5 115.0(12) . . ? O4 C1 H1 108.0 . . ? C2 C1 H1 108.0 . . ? C5 C1 H1 108.0 . . ? N1 C2 C1 112.8(11) . . ? N1 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? N1 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C1 115.3(11) . . ? N2 C5 H5A 108.4 . . ? C1 C5 H5A 108.4 . . ? N2 C5 H5B 108.4 . . ? C1 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O8 C8 C9 108.0(12) . . ? O8 C8 C12 109.4(13) . . ? C9 C8 C12 119.6(15) . . ? O8 C8 H8 106.4 . . ? C9 C8 H8 106.4 . . ? C12 C8 H8 106.4 . . ? C8 C9 N3 112.4(12) . . ? C8 C9 H9A 109.1 . . ? N3 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? N3 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C8 113.6(15) . . ? N4 C12 H12A 108.9 . . ? C8 C12 H12A 108.9 . . ? N4 C12 H12B 108.9 . . ? C8 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O12 C15 C16 110.6(14) . . ? O12 C15 C19 110.4(12) . . ? C16 C15 C19 126.5(15) . . ? O12 C15 H15 101.8 . . ? C16 C15 H15 101.8 . . ? C19 C15 H15 101.8 . . ? C15 C16 N5 114.7(13) . . ? C15 C16 H16A 108.6 . . ? N5 C16 H16A 108.6 . . ? C15 C16 H16B 108.6 . . ? N5 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C15 113.9(16) . . ? N6 C19 H19A 108.8 . . ? C15 C19 H19A 108.8 . . ? N6 C19 H19B 108.8 . . ? C15 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? N6 C20 H20A 109.5 . . ? N6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N6 C21 H21A 109.5 . . ? N6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N7 C24 H24A 109.5 . . ? N7 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N7 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 H25A 109.5 . . ? N7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 N8 C26 108(3) . . ? C27 N8 C28 112(3) . . ? C26 N8 C28 112(3) . . ? O15 C22 C23 104.7(19) . . ? O15 C22 C26 115(2) . . ? C23 C22 C26 114(2) . . ? O15 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? C26 C22 H22 107.7 . . ? C22 C23 N7 112(2) . . ? C22 C23 H23A 109.3 . . ? N7 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? N7 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? N8 C26 C22 113(2) . . ? N8 C26 H26A 109.1 . . ? C22 C26 H26A 109.1 . . ? N8 C26 H26B 109.1 . . ? C22 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? N8 C28 H28A 109.5 . . ? N8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C28A N8A C27A 113(3) . . ? C28A N8A C26A 113(3) . . ? C27A N8A C26A 116(3) . . ? C23A C22A C26A 111(4) . . ? C23A C22A O15 105(3) . . ? C26A C22A O15 103(3) . . ? C23A C22A H22A 112.2 . . ? C26A C22A H22A 112.2 . . ? O15 C22A H22A 112.2 . . ? N7 C23A C22A 110(3) . . ? N7 C23A H23C 109.7 . . ? C22A C23A H23C 109.7 . . ? N7 C23A H23D 109.7 . . ? C22A C23A H23D 109.7 . . ? H23C C23A H23D 108.2 . . ? C22A C26A N8A 117(4) . . ? C22A C26A H26C 108.0 . . ? N8A C26A H26C 108.0 . . ? C22A C26A H26D 108.0 . . ? N8A C26A H26D 108.0 . . ? H26C C26A H26D 107.3 . . ? N8A C27A H27D 109.5 . . ? N8A C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? N8A C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? N8A C28A H28D 109.5 . . ? N8A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? N8A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? O18 C29 C30 109.1(12) . . ? O18 C29 C33 107.1(14) . . ? C30 C29 C33 115.5(17) . . ? O18 C29 H29 108.3 . . ? C30 C29 H29 108.3 . . ? C33 C29 H29 108.3 . . ? C29 C30 N9 112.6(13) . . ? C29 C30 H30A 109.1 . . ? N9 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? N9 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? N9 C31 H31A 109.5 . . ? N9 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N9 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N9 C32 H32A 109.5 . . ? N9 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N9 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N10 C33 C29 115.7(18) . . ? N10 C33 H33A 108.4 . . ? C29 C33 H33A 108.4 . . ? N10 C33 H33B 108.4 . . ? C29 C33 H33B 108.4 . . ? H33A C33 H33B 107.4 . . ? N10 C34 H34A 109.5 . . ? N10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N10 C35 H35A 109.5 . . ? N10 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N10 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C40 C36 O21 116(2) . . ? C40 C36 C37 133(3) . . ? O21 C36 C37 109(2) . . ? C40 C36 H36 94.4 . . ? O21 C36 H36 94.4 . . ? C37 C36 H36 94.4 . . ? N11 C37 C36 122(2) . . ? N11 C37 H37A 106.9 . . ? C36 C37 H37A 106.9 . . ? N11 C37 H37B 106.9 . . ? C36 C37 H37B 106.9 . . ? H37A C37 H37B 106.7 . . ? C36 C40 N12 121(3) . . ? C36 C40 H40A 107.0 . . ? N12 C40 H40A 107.0 . . ? C36 C40 H40B 107.0 . . ? N12 C40 H40B 107.0 . . ? H40A C40 H40B 106.8 . . ? C42 N12 C41 98(4) . . ? C42 N12 C40 125(5) . . ? C41 N12 C40 109(4) . . ? N12 C41 H41A 109.5 . . ? N12 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N12 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N12 C42 H42A 109.5 . . ? N12 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N12 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C37A C36A C40A 139(3) . . ? C37A C36A O21 107(2) . . ? C40A C36A O21 111(2) . . ? C37A C36A H36A 96.0 . . ? C40A C36A H36A 96.0 . . ? O21 C36A H36A 96.0 . . ? C36A C37A N11 126(2) . . ? C36A C37A H37C 105.9 . . ? N11 C37A H37C 105.9 . . ? C36A C37A H37D 105.9 . . ? N11 C37A H37D 105.9 . . ? H37C C37A H37D 106.2 . . ? C36A C40A N12A 114(3) . . ? C36A C40A H40C 108.8 . . ? N12A C40A H40C 108.8 . . ? C36A C40A H40D 108.8 . . ? N12A C40A H40D 108.8 . . ? H40C C40A H40D 107.7 . . ? C41A N12A C40A 110(7) . . ? C41A N12A C42A 103(5) . . ? C40A N12A C42A 105(5) . . ? N12A C41A H41D 109.5 . . ? N12A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? N12A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? N12A C42A H42D 109.5 . . ? N12A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? N12A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? N11 C38 H38A 109.5 . . ? N11 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N11 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N11 C39 H39A 109.5 . . ? N11 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N11 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C44 C43 C47 130.6(16) . . ? C44 C43 O25 113.7(14) . . ? C47 C43 O25 115.1(14) . . ? C44 C43 H43 92.4 . . ? C47 C43 H43 92.4 . . ? O25 C43 H43 92.4 . . ? C43 C44 N13 120.1(15) . . ? C43 C44 H44A 107.3 . . ? N13 C44 H44A 107.3 . . ? C43 C44 H44B 107.3 . . ? N13 C44 H44B 107.3 . . ? H44A C44 H44B 106.9 . . ? N13 C45 H45A 109.5 . . ? N13 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N13 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N13 C46 H46A 109.5 . . ? N13 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N13 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C47 N14 117.1(17) . . ? C43 C47 H47A 108.0 . . ? N14 C47 H47A 108.0 . . ? C43 C47 H47B 108.0 . . ? N14 C47 H47B 108.0 . . ? H47A C47 H47B 107.3 . . ? N14 C48 H48A 109.5 . . ? N14 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N14 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N14 C49 H49A 109.5 . . ? N14 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N14 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O29 C50 C51 113.0(12) . . ? O29 C50 C54 110.2(11) . . ? C51 C50 C54 120.2(15) . . ? O29 C50 H50 103.8 . . ? C51 C50 H50 103.8 . . ? C54 C50 H50 103.8 . . ? C50 C51 N15 112.8(12) . . ? C50 C51 H51A 109.0 . . ? N15 C51 H51A 109.0 . . ? C50 C51 H51B 109.0 . . ? N15 C51 H51B 109.0 . . ? H51A C51 H51B 107.8 . . ? N15 C52 H52A 109.5 . . ? N15 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N15 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N15 C53 H53A 109.5 . . ? N15 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N15 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N16 C54 C50 117.7(12) . . ? N16 C54 H54A 107.9 . . ? C50 C54 H54A 107.9 . . ? N16 C54 H54B 107.9 . . ? C50 C54 H54B 107.9 . . ? H54A C54 H54B 107.2 . . ? N16 C55 H55A 109.5 . . ? N16 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N16 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N16 C56 H56A 109.5 . . ? N16 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N16 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O33 C57 C58 107.8(9) . . ? O33 C57 C61 110.6(11) . . ? C58 C57 C61 114.0(10) . . ? O33 C57 H57 108.1 . . ? C58 C57 H57 108.1 . . ? C61 C57 H57 108.1 . . ? C57 C58 N17 109.9(9) . . ? C57 C58 H58A 109.7 . . ? N17 C58 H58A 109.7 . . ? C57 C58 H58B 109.7 . . ? N17 C58 H58B 109.7 . . ? H58A C58 H58B 108.2 . . ? N17 C59 H59A 109.5 . . ? N17 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N17 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N17 C60 H60A 109.5 . . ? N17 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N17 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N18 C61 C57 114.9(10) . . ? N18 C61 H61A 108.6 . . ? C57 C61 H61A 108.6 . . ? N18 C61 H61B 108.6 . . ? C57 C61 H61B 108.6 . . ? H61A C61 H61B 107.5 . . ? N18 C62 H62A 109.5 . . ? N18 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N18 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N18 C63 H63A 109.5 . . ? N18 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N18 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 O36 109(2) . . ? C65 C64 C68 136.0(18) . . ? O36 C64 C68 113.1(14) . . ? O36 C64 C65A 109.5(14) . . ? C68 C64 C65A 129.8(19) . . ? C65 C64 H64 94.1 . . ? O36 C64 H64 94.1 . . ? C68 C64 H64 94.1 . . ? C65A C64 H64 57.2 . . ? C65 C64 H64A 62.5 . . ? O36 C64 H64A 99.1 . . ? C68 C64 H64A 99.1 . . ? C65A C64 H64A 99.1 . . ? H64 C64 H64A 155.8 . . ? C64 C65 N19 114(4) . . ? C64 C65 H65A 108.8 . . ? N19 C65 H65A 108.8 . . ? C64 C65 H65B 108.8 . . ? N19 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? N19 C65A C64 112(2) . . ? N19 C65A H65C 109.3 . . ? C64 C65A H65C 109.3 . . ? N19 C65A H65D 109.3 . . ? C64 C65A H65D 109.3 . . ? H65C C65A H65D 107.9 . . ? N19 C66 H66A 109.5 . . ? N19 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N19 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N19 C67 H67A 109.5 . . ? N19 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N19 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 N20 116.0(16) . . ? C64 C68 H68A 108.3 . . ? N20 C68 H68A 108.3 . . ? C64 C68 H68B 108.3 . . ? N20 C68 H68B 108.3 . . ? H68A C68 H68B 107.4 . . ? N20 C69 H69A 109.5 . . ? N20 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N20 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N20 C70 H70A 109.5 . . ? N20 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N20 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 O39 114.3(13) . . ? C72 C71 C75 126.7(15) . . ? O39 C71 C75 113.3(13) . . ? C72 C71 H71 97.9 . . ? O39 C71 H71 97.9 . . ? C75 C71 H71 97.9 . . ? C71 C72 N21 115.6(12) . . ? C71 C72 H72A 108.4 . . ? N21 C72 H72A 108.4 . . ? C71 C72 H72B 108.4 . . ? N21 C72 H72B 108.4 . . ? H72A C72 H72B 107.4 . . ? N21 C73 H73A 109.5 . . ? N21 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N21 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N21 C74 H74A 109.5 . . ? N21 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N21 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C71 C75 N22 117.0(14) . . ? C71 C75 H75A 108.0 . . ? N22 C75 H75A 108.0 . . ? C71 C75 H75B 108.0 . . ? N22 C75 H75B 108.0 . . ? H75A C75 H75B 107.3 . . ? N22 C76 H76A 109.5 . . ? N22 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N22 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N22 C77 H77A 109.5 . . ? N22 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N22 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C79 C78 C82A 125(3) . . ? C79 C78 O42 113.4(13) . . ? C82A C78 O42 120(3) . . ? C79 C78 C82 135(2) . . ? O42 C78 C82 105.0(16) . . ? C79 C78 H78 98.6 . . ? C82A C78 H78 64.9 . . ? O42 C78 H78 98.6 . . ? C82 C78 H78 98.6 . . ? C79 C78 H78A 93.3 . . ? C82A C78 H78A 93.3 . . ? O42 C78 H78A 93.3 . . ? C82 C78 H78A 60.5 . . ? H78 C78 H78A 158.2 . . ? C78 C79 N23 120.7(14) . . ? C78 C79 H79A 107.2 . . ? N23 C79 H79A 107.2 . . ? C78 C79 H79B 107.2 . . ? N23 C79 H79B 107.2 . . ? H79A C79 H79B 106.8 . . ? N23 C80 H80A 109.5 . . ? N23 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N23 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N23 C81 H81A 109.5 . . ? N23 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N23 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N24 C82 C78 111(2) . . ? N24 C82 H82A 109.4 . . ? C78 C82 H82A 109.4 . . ? N24 C82 H82B 109.4 . . ? C78 C82 H82B 109.4 . . ? H82A C82 H82B 108.0 . . ? N24 C83 H83A 109.5 . . ? N24 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N24 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N24 C84 H84A 109.5 . . ? N24 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N24 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C78 C82A N24 123(4) . . ? C78 C82A H82C 106.5 . . ? N24 C82A H82C 106.5 . . ? C78 C82A H82D 106.5 . . ? N24 C82A H82D 106.5 . . ? H82C C82A H82D 106.5 . . ? N24 C83A H83D 109.5 . . ? N24 C83A H83E 109.5 . . ? H83D C83A H83E 109.5 . . ? N24 C83A H83F 109.5 . . ? H83D C83A H83F 109.5 . . ? H83E C83A H83F 109.5 . . ? N24 C84A H84D 109.5 . . ? N24 C84A H84E 109.5 . . ? H84D C84A H84E 109.5 . . ? N24 C84A H84F 109.5 . . ? H84D C84A H84F 109.5 . . ? H84E C84A H84F 109.5 . . ? C91 O50 H50A 109.5 . . ? O50 C91 C92 120(2) . . ? O50 C91 C93 109.9(18) . . ? C92 C91 C93 102(2) . . ? O50 C91 H91 108.4 . . ? C92 C91 H91 108.4 . . ? C93 C91 H91 108.4 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C102 C101 C103 117(5) . 2_667 ? C102 C101 H101 121.4 . . ? C103 C101 H101 121.4 2_667 . ? C101 C102 C103 124(5) . . ? C101 C102 H102 118.0 . . ? C103 C102 H102 118.0 . . ? C101 C103 C102 119(4) 2_667 . ? C101 C103 H103 120.5 2_667 . ? C102 C103 H103 120.5 . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.884 _refine_diff_density_max 3.219 _refine_diff_density_min -2.357 _refine_diff_density_rms 0.230 data_shelxl7 _database_code_depnum_ccdc_archive 'CCDC 876659' #TrackingRef 'Compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H96 N12 O14 W4' _chemical_formula_sum 'C40 H96 N12 O14 W4' _chemical_formula_weight 1704.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 24.9274(2) _cell_length_b 24.9274(2) _cell_length_c 9.68370(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6017.21(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55569 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312 _exptl_absorpt_coefficient_mu 7.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2496 _exptl_absorpt_correction_T_max 0.6999 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '323 1.7 degree images with \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 71613 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.40 _diffrn_reflns_theta_max 30.03 _reflns_number_total 4370 _reflns_number_gt 3988 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0321P)^2^+14.8729P] 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 0.00064(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4370 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.048107(4) 0.195231(4) 0.482470(11) 0.01927(6) Uani 1 1 d . . . O1 O 0.11679(8) 0.16689(8) 0.5311(2) 0.0227(4) Uani 1 1 d . . . O2 O 0.03261(9) 0.14981(9) 0.3549(2) 0.0279(4) Uani 1 1 d . . . O3 O 0.0000 0.2500 0.4220(3) 0.0217(5) Uani 1 2 d S . . O4 O 0.01102(8) 0.17320(8) 0.6276(2) 0.0217(4) Uani 1 1 d . . . N1 N 0.10919(10) 0.24394(10) 0.3475(3) 0.0236(5) Uani 1 1 d . . . N2 N 0.22456(11) 0.14312(11) 0.6807(3) 0.0310(6) Uani 1 1 d . . . N3 N 0.24086(11) 0.14790(11) 0.3260(3) 0.0306(5) Uani 1 1 d . . . C1 C 0.16885(11) 0.18169(12) 0.4846(3) 0.0223(5) Uani 1 1 d . . . C2 C 0.16343(11) 0.23627(12) 0.4111(3) 0.0250(5) Uani 1 1 d . . . H2A H 0.1700 0.2654 0.4785 0.030 Uiso 1 1 calc R . . H2B H 0.1911 0.2389 0.3381 0.030 Uiso 1 1 calc R . . C3 C 0.10740(14) 0.22392(15) 0.2032(3) 0.0333(7) Uani 1 1 d . . . H3A H 0.0721 0.2316 0.1632 0.050 Uiso 1 1 calc R . . H3B H 0.1137 0.1851 0.2025 0.050 Uiso 1 1 calc R . . H3C H 0.1352 0.2418 0.1486 0.050 Uiso 1 1 calc R . . C4 C 0.09847(13) 0.30264(12) 0.3407(3) 0.0299(6) Uani 1 1 d . . . H4A H 0.1272 0.3203 0.2885 0.045 Uiso 1 1 calc R . . H4B H 0.0972 0.3174 0.4344 0.045 Uiso 1 1 calc R . . H4C H 0.0640 0.3089 0.2946 0.045 Uiso 1 1 calc R . . C5 C 0.20668(12) 0.19118(12) 0.6075(3) 0.0278(6) Uani 1 1 d . . . H5A H 0.2388 0.2106 0.5737 0.033 Uiso 1 1 calc R . . H5B H 0.1883 0.2149 0.6744 0.033 Uiso 1 1 calc R . . C6 C 0.18299(15) 0.12071(16) 0.7686(4) 0.0393(8) Uani 1 1 d . . . H6A H 0.1720 0.1475 0.8369 0.059 Uiso 1 1 calc R . . H6B H 0.1969 0.0889 0.8161 0.059 Uiso 1 1 calc R . . H6C H 0.1520 0.1105 0.7119 0.059 Uiso 1 1 calc R . . C7 C 0.27164(16) 0.15597(18) 0.7647(4) 0.0446(9) Uani 1 1 d . . . H7A H 0.2618 0.1823 0.8354 0.067 Uiso 1 1 calc R . . H7B H 0.2998 0.1709 0.7056 0.067 Uiso 1 1 calc R . . H7C H 0.2849 0.1233 0.8094 0.067 Uiso 1 1 calc R . . C8 C 0.18858(12) 0.13613(12) 0.3902(3) 0.0265(6) Uani 1 1 d . . . H8A H 0.1916 0.1027 0.4450 0.032 Uiso 1 1 calc R . . H8B H 0.1617 0.1299 0.3166 0.032 Uiso 1 1 calc R . . C9 C 0.23916(15) 0.14598(17) 0.1763(4) 0.0419(8) Uani 1 1 d . . . H9A H 0.2748 0.1540 0.1392 0.063 Uiso 1 1 calc R . . H9B H 0.2134 0.1725 0.1423 0.063 Uiso 1 1 calc R . . H9C H 0.2281 0.1101 0.1464 0.063 Uiso 1 1 calc R . . C10 C 0.28192(17) 0.1104(2) 0.3751(5) 0.0634(14) Uani 1 1 d . . . H10A H 0.2737 0.0743 0.3414 0.095 Uiso 1 1 calc R . . H10B H 0.2824 0.1104 0.4763 0.095 Uiso 1 1 calc R . . H10C H 0.3171 0.1216 0.3403 0.095 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 0.01821(7) 0.02046(7) 0.01912(8) -0.00119(3) -0.00009(3) 0.00123(3) O1 0.0191(9) 0.0243(10) 0.0247(10) 0.0021(7) 0.0016(7) 0.0022(7) O2 0.0284(10) 0.0280(10) 0.0272(10) -0.0050(8) -0.0034(8) 0.0033(8) O3 0.0193(12) 0.0240(13) 0.0219(13) 0.000 0.000 0.0026(10) O4 0.0206(9) 0.0211(9) 0.0233(9) -0.0008(7) -0.0003(7) -0.0008(7) N1 0.0223(11) 0.0256(12) 0.0231(11) 0.0017(9) -0.0002(9) 0.0003(9) N2 0.0273(13) 0.0309(13) 0.0348(14) 0.0031(11) -0.0088(11) 0.0029(10) N3 0.0218(12) 0.0352(14) 0.0348(14) 0.0012(11) 0.0050(10) 0.0023(10) C1 0.0170(12) 0.0230(13) 0.0270(13) -0.0011(10) -0.0006(10) 0.0003(10) C2 0.0221(13) 0.0253(13) 0.0275(14) 0.0032(11) -0.0017(10) -0.0002(10) C3 0.0330(16) 0.0451(19) 0.0218(14) -0.0004(13) -0.0007(12) 0.0010(14) C4 0.0309(15) 0.0257(14) 0.0332(16) 0.0088(12) 0.0028(12) 0.0006(11) C5 0.0252(13) 0.0263(14) 0.0319(15) -0.0003(11) -0.0081(11) -0.0012(11) C6 0.0384(18) 0.0419(19) 0.0375(18) 0.0113(15) -0.0083(14) -0.0026(15) C7 0.0325(18) 0.048(2) 0.053(2) 0.0069(17) -0.0194(16) -0.0022(16) C8 0.0223(13) 0.0260(14) 0.0314(15) -0.0025(11) 0.0030(11) 0.0008(10) C9 0.0348(17) 0.053(2) 0.0376(18) -0.0030(16) 0.0114(14) -0.0059(15) C10 0.0324(19) 0.090(4) 0.068(3) 0.035(3) 0.0206(19) 0.025(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 O2 1.719(2) . ? W1 O4 1.770(2) . ? W1 O3 1.9091(9) . ? W1 O1 1.911(2) . ? W1 O4 2.2443(19) 16_556 ? W1 N1 2.345(2) . ? O1 C1 1.422(3) . ? O3 W1 1.9091(9) 3 ? O4 W1 2.2443(19) 14_556 ? N1 C3 1.485(4) . ? N1 C4 1.489(4) . ? N1 C2 1.498(4) . ? N2 C6 1.453(5) . ? N2 C5 1.462(4) . ? N2 C7 1.464(4) . ? N3 C9 1.451(5) . ? N3 C10 1.465(5) . ? N3 C8 1.473(4) . ? C1 C5 1.537(4) . ? C1 C8 1.539(4) . ? C1 C2 1.541(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W1 O4 104.41(10) . . ? O2 W1 O3 96.29(10) . . ? O4 W1 O3 97.90(9) . . ? O2 W1 O1 97.76(9) . . ? O4 W1 O1 99.05(9) . . ? O3 W1 O1 154.51(6) . . ? O2 W1 O4 170.53(9) . 16_556 ? O4 W1 O4 85.06(8) . 16_556 ? O3 W1 O4 82.11(7) . 16_556 ? O1 W1 O4 80.54(8) . 16_556 ? O2 W1 N1 94.96(10) . . ? O4 W1 N1 160.45(9) . . ? O3 W1 N1 82.34(7) . . ? O1 W1 N1 75.36(9) . . ? O4 W1 N1 75.58(8) 16_556 . ? C1 O1 W1 130.03(17) . . ? W1 O3 W1 144.29(16) 3 . ? W1 O4 W1 139.66(11) . 14_556 ? C3 N1 C4 106.4(2) . . ? C3 N1 C2 111.8(2) . . ? C4 N1 C2 107.8(2) . . ? C3 N1 W1 109.32(19) . . ? C4 N1 W1 114.66(18) . . ? C2 N1 W1 106.93(17) . . ? C6 N2 C5 112.4(3) . . ? C6 N2 C7 109.3(3) . . ? C5 N2 C7 109.6(3) . . ? C9 N3 C10 108.9(3) . . ? C9 N3 C8 112.9(3) . . ? C10 N3 C8 110.8(3) . . ? O1 C1 C5 110.7(2) . . ? O1 C1 C8 106.8(2) . . ? C5 C1 C8 112.2(2) . . ? O1 C1 C2 107.2(2) . . ? C5 C1 C2 106.0(2) . . ? C8 C1 C2 113.9(2) . . ? N1 C2 C1 112.4(2) . . ? N1 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C1 115.9(2) . . ? N2 C5 H5A 108.3 . . ? C1 C5 H5A 108.3 . . ? N2 C5 H5B 108.3 . . ? C1 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C1 112.7(2) . . ? N3 C8 H8A 109.0 . . ? C1 C8 H8A 109.0 . . ? N3 C8 H8B 109.0 . . ? C1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.717 _refine_diff_density_min -1.326 _refine_diff_density_rms 0.128 data_k06kcm9 _database_code_depnum_ccdc_archive 'CCDC 876660' #TrackingRef 'Compound 7a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H96 N12 O14 W4, 4(H2 O)' _chemical_formula_sum 'C40 H104 N12 O18 W4' _chemical_formula_weight 1776.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 24.9240(5) _cell_length_b 24.9240(5) _cell_length_c 9.7720(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6070.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 37811 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3472 _exptl_absorpt_coefficient_mu 7.627 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.48 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method '206 1.0 degree images with \f and \w scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45789 _diffrn_reflns_av_R_equivalents 0.1427 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3466 _reflns_number_gt 2652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119 ; _computing_structure_refinement ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Institut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0208P)^2^+121.3846P] 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 3466 _refine_ls_number_parameters 182 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.055540(11) 0.297536(11) 0.26622(3) 0.01798(9) Uani 1 1 d . . . O1 O 0.0845(2) 0.36625(19) 0.2195(5) 0.0212(11) Uani 1 1 d . . . O2 O 0.0771(2) 0.2603(2) 0.1217(5) 0.0207(11) Uani 1 1 d . . . O3 O 0.0000 0.2500 0.3253(7) 0.0205(15) Uani 1 2 d S . . O4 O 0.1007(2) 0.2808(2) 0.3919(5) 0.0255(12) Uani 1 1 d . . . O5 O 0.2194(3) 0.4849(3) 0.1123(7) 0.0424(16) Uani 1 1 d D . . N1 N 0.0079(2) 0.3584(2) 0.4022(6) 0.0202(13) Uani 1 1 d . . . N2 N 0.1002(3) 0.4908(3) 0.4239(7) 0.0247(14) Uani 1 1 d . . . N3 N 0.1052(3) 0.4704(3) 0.0587(7) 0.0253(14) Uani 1 1 d . . . C1 C 0.0292(3) 0.3568(3) 0.5442(8) 0.0289(18) Uani 1 1 d . . . H1A H 0.0115 0.3846 0.5992 0.043 Uiso 1 1 calc R . . H1B H 0.0680 0.3634 0.5428 0.043 Uiso 1 1 calc R . . H1C H 0.0221 0.3215 0.5844 0.043 Uiso 1 1 calc R . . C2 C -0.0506(3) 0.3471(3) 0.4113(9) 0.0279(17) Uani 1 1 d . . . H2A H -0.0562 0.3111 0.4488 0.042 Uiso 1 1 calc R . . H2B H -0.0665 0.3493 0.3197 0.042 Uiso 1 1 calc R . . H2C H -0.0676 0.3737 0.4712 0.042 Uiso 1 1 calc R . . C3 C 0.0148(3) 0.4126(3) 0.3385(8) 0.0212(15) Uani 1 1 d . . . H3A H 0.0119 0.4405 0.4104 0.025 Uiso 1 1 calc R . . H3B H -0.0144 0.4187 0.2716 0.025 Uiso 1 1 calc R . . C4 C 0.0693(3) 0.4182(3) 0.2656(8) 0.0210(15) Uani 1 1 d . . . C5 C 0.0591(3) 0.4560(3) 0.1424(8) 0.0250(16) Uani 1 1 d . . . H5A H 0.0322 0.4388 0.0823 0.030 Uiso 1 1 calc R . . H5B H 0.0430 0.4895 0.1777 0.030 Uiso 1 1 calc R . . C6 C 0.0930(3) 0.5187(3) -0.0220(9) 0.0333(19) Uani 1 1 d . . . H6A H 0.0650 0.5104 -0.0892 0.050 Uiso 1 1 calc R . . H6B H 0.1254 0.5307 -0.0696 0.050 Uiso 1 1 calc R . . H6C H 0.0804 0.5472 0.0391 0.050 Uiso 1 1 calc R . . C7 C 0.1200(4) 0.4269(4) -0.0349(9) 0.0343(19) Uani 1 1 d . . . H7A H 0.1316 0.3956 0.0181 0.051 Uiso 1 1 calc R . . H7B H 0.1494 0.4389 -0.0941 0.051 Uiso 1 1 calc R . . H7C H 0.0890 0.4172 -0.0912 0.051 Uiso 1 1 calc R . . C8 C 0.1142(3) 0.4393(3) 0.3580(8) 0.0237(16) Uani 1 1 d . . . H8A H 0.1219 0.4123 0.4298 0.028 Uiso 1 1 calc R . . H8B H 0.1472 0.4441 0.3029 0.028 Uiso 1 1 calc R . . C9 C 0.1083(4) 0.4897(4) 0.5713(9) 0.042(2) Uani 1 1 d . . . H9A H 0.0886 0.4594 0.6106 0.063 Uiso 1 1 calc R . . H9B H 0.0951 0.5232 0.6114 0.063 Uiso 1 1 calc R . . H9C H 0.1466 0.4858 0.5911 0.063 Uiso 1 1 calc R . . C10 C 0.1312(5) 0.5355(4) 0.3659(11) 0.048(3) Uani 1 1 d . . . H10A H 0.1185 0.5694 0.4052 0.073 Uiso 1 1 calc R . . H10B H 0.1264 0.5363 0.2664 0.073 Uiso 1 1 calc R . . H10C H 0.1693 0.5307 0.3876 0.073 Uiso 1 1 calc R . . H51 H 0.230(6) 0.492(6) 0.028(6) 0.09(5) Uiso 1 1 d D . . H52 H 0.1839(9) 0.486(4) 0.112(10) 0.04(3) Uiso 1 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 0.01954(16) 0.01807(15) 0.01632(14) 0.00004(11) -0.00082(11) -0.00090(11) O1 0.025(3) 0.018(2) 0.020(3) -0.001(2) 0.001(2) 0.003(2) O2 0.022(3) 0.023(3) 0.017(2) -0.002(2) 0.000(2) 0.000(2) O3 0.025(4) 0.019(4) 0.018(4) 0.000 0.000 -0.001(3) O4 0.024(3) 0.030(3) 0.023(3) 0.004(2) -0.007(2) -0.002(2) O5 0.034(4) 0.064(5) 0.029(3) 0.011(3) -0.004(3) -0.008(3) N1 0.023(3) 0.022(3) 0.016(3) 0.002(2) -0.002(2) -0.002(3) N2 0.028(3) 0.018(3) 0.028(3) -0.006(3) 0.002(3) -0.003(3) N3 0.026(3) 0.023(3) 0.028(3) 0.004(3) 0.004(3) 0.002(3) C1 0.037(5) 0.035(4) 0.015(4) 0.001(3) -0.007(3) 0.002(4) C2 0.024(4) 0.028(4) 0.032(4) -0.005(3) 0.009(3) -0.004(3) C3 0.027(4) 0.014(3) 0.023(4) 0.002(3) 0.003(3) 0.000(3) C4 0.019(3) 0.014(3) 0.029(4) 0.003(3) -0.001(3) 0.000(3) C5 0.023(4) 0.025(4) 0.027(4) -0.001(3) -0.002(3) 0.001(3) C6 0.031(4) 0.033(4) 0.036(5) 0.019(4) -0.002(4) -0.001(4) C7 0.040(5) 0.037(5) 0.026(4) 0.005(4) 0.006(4) -0.003(4) C8 0.020(4) 0.020(4) 0.031(4) -0.001(3) 0.000(3) -0.001(3) C9 0.056(6) 0.039(5) 0.031(5) -0.005(4) -0.002(4) 0.002(5) C10 0.062(7) 0.026(5) 0.057(6) -0.014(4) 0.024(5) -0.012(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 O4 1.718(5) . ? W1 O2 1.773(5) . ? W1 O3 1.911(2) . ? W1 O1 1.914(5) . ? W1 O2 2.248(5) 16 ? W1 N1 2.339(6) . ? O1 C4 1.423(8) . ? O2 W1 2.248(5) 14 ? O3 W1 1.911(2) 3 ? N1 C1 1.486(9) . ? N1 C2 1.488(9) . ? N1 C3 1.499(9) . ? N2 C9 1.455(11) . ? N2 C10 1.469(11) . ? N2 C8 1.479(9) . ? N3 C5 1.454(10) . ? N3 C7 1.465(11) . ? N3 C6 1.471(10) . ? C3 C4 1.541(10) . ? C4 C8 1.530(10) . ? C4 C5 1.549(10) . ? 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 104.1(2) . . ? O4 W1 O3 96.2(2) . . ? O2 W1 O3 97.8(2) . . ? O4 W1 O1 98.0(2) . . ? O2 W1 O1 99.4(2) . . ? O3 W1 O1 154.15(15) . . ? O4 W1 O2 170.7(2) . 16 ? O2 W1 O2 85.1(2) . 16 ? O3 W1 O2 81.69(19) . 16 ? O1 W1 O2 80.8(2) . 16 ? O4 W1 N1 94.8(2) . . ? O2 W1 N1 160.9(2) . . ? O3 W1 N1 82.11(19) . . ? O1 W1 N1 75.3(2) . . ? O2 W1 N1 76.0(2) 16 . ? C4 O1 W1 129.7(4) . . ? W1 O2 W1 139.5(3) . 14 ? W1 O3 W1 144.8(4) . 3 ? C1 N1 C2 106.8(6) . . ? C1 N1 C3 111.8(6) . . ? C2 N1 C3 107.8(6) . . ? C1 N1 W1 109.5(5) . . ? C2 N1 W1 114.1(5) . . ? C3 N1 W1 106.9(4) . . ? C9 N2 C10 108.9(8) . . ? C9 N2 C8 112.4(7) . . ? C10 N2 C8 111.5(6) . . ? C5 N3 C7 111.6(6) . . ? C5 N3 C6 109.9(6) . . ? C7 N3 C6 108.8(7) . . ? N1 C3 C4 112.0(6) . . ? O1 C4 C8 107.7(6) . . ? O1 C4 C3 107.4(6) . . ? C8 C4 C3 113.8(6) . . ? O1 C4 C5 110.6(6) . . ? C8 C4 C5 111.7(6) . . ? C3 C4 C5 105.7(6) . . ? N3 C5 C4 117.2(6) . . ? N2 C8 C4 112.4(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.056 _refine_diff_density_min -1.499 _refine_diff_density_rms 0.198