data_x11139 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H70 Cl O2 P W' _chemical_formula_weight 941.32 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' 'P' 'P' 0.1023 0.0942 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.6931(16) _cell_length_b 8.9674(6) _cell_length_c 23.7379(17) _cell_angle_alpha 90.00 _cell_angle_beta 104.2850(10) _cell_angle_gamma 90.00 _cell_volume 4681.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 30.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 2.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6250 _exptl_absorpt_correction_T_max 0.8812 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 108649 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 30.32 _reflns_number_total 14056 _reflns_number_gt 12290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7.0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+2.3303P] 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 14056 _refine_ls_number_parameters 576 _refine_ls_number_restraints 267 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0422 _refine_ls_wR_factor_gt 0.0403 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.009 _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 0.204150(16) 0.14185(5) 0.486211(19) 0.01070(4) Uani 0.9130(18) 1 d PDU A 1 Cl1 Cl 0.24268(5) 0.39081(11) 0.49489(4) 0.01633(14) Uani 0.9130(18) 1 d PDU A 1 O2 O 0.12949(6) 0.18537(14) 0.47948(6) 0.0175(3) Uani 0.9130(18) 1 d PDU A 1 C1 C 0.23251(8) 0.0631(2) 0.56253(7) 0.0159(3) Uani 0.9130(18) 1 d PDU A 1 H1A H 0.2744(7) 0.039(2) 0.5657(9) 0.019 Uiso 0.9130(18) 1 d PD A 1 C2 C 0.21223(10) 0.0401(2) 0.61790(9) 0.0183(4) Uani 0.9130(18) 1 d PDU A 1 C3 C 0.24690(17) 0.1534(4) 0.66260(13) 0.0262(6) Uani 0.9130(18) 1 d PDU A 1 H3A H 0.2345 0.1422 0.6991 0.039 Uiso 0.9130(18) 1 calc PR A 1 H3B H 0.2376 0.2547 0.6476 0.039 Uiso 0.9130(18) 1 calc PR A 1 H3C H 0.2907 0.1354 0.6696 0.039 Uiso 0.9130(18) 1 calc PR A 1 C4 C 0.22882(11) -0.1199(2) 0.63958(9) 0.0301(5) Uani 0.9130(18) 1 d PDU A 1 H4A H 0.2155 -0.1370 0.6753 0.045 Uiso 0.9130(18) 1 calc PR A 1 H4B H 0.2730 -0.1335 0.6475 0.045 Uiso 0.9130(18) 1 calc PR A 1 H4C H 0.2085 -0.1911 0.6097 0.045 Uiso 0.9130(18) 1 calc PR A 1 C5 C 0.14362(9) 0.0639(3) 0.60906(8) 0.0275(4) Uani 0.9130(18) 1 d PDU A 1 H5A H 0.1325 0.0479 0.6460 0.041 Uiso 0.9130(18) 1 calc PR A 1 H5B H 0.1215 -0.0069 0.5800 0.041 Uiso 0.9130(18) 1 calc PR A 1 H5C H 0.1330 0.1660 0.5956 0.041 Uiso 0.9130(18) 1 calc PR A 1 W1A W 0.1900(2) 0.1446(5) 0.4789(2) 0.0158(5) Uani 0.0870(18) 1 d PDU A 2 Cl1A Cl 0.2370(6) 0.3784(14) 0.5026(6) 0.01633(14) Uani 0.0870(18) 1 d PDU A 2 O2A O 0.1179(5) 0.2030(15) 0.4477(7) 0.0175(3) Uani 0.0870(18) 1 d PDU A 2 C1A C 0.1820(8) 0.0850(19) 0.5548(6) 0.0159(3) Uani 0.0870(18) 1 d PDU A 2 H1A1 H 0.1427 0.1097 0.5592 0.019 Uiso 0.0870(18) 1 calc PR A 2 C2A C 0.2190(9) 0.011(2) 0.6096(8) 0.019(2) Uani 0.0870(18) 1 d PDU A 2 C3A C 0.2403(17) 0.136(3) 0.6536(12) 0.021(4) Uani 0.0870(18) 1 d PDU A 2 H3A1 H 0.2648 0.2075 0.6379 0.032 Uiso 0.0870(18) 1 calc PR A 2 H3A2 H 0.2650 0.0940 0.6899 0.032 Uiso 0.0870(18) 1 calc PR A 2 H3A3 H 0.2049 0.1872 0.6612 0.032 Uiso 0.0870(18) 1 calc PR A 2 C4A C 0.2742(8) -0.067(3) 0.5968(9) 0.031(3) Uani 0.0870(18) 1 d PDU A 2 H4A1 H 0.2992 0.0069 0.5828 0.047 Uiso 0.0870(18) 1 calc PR A 2 H4A2 H 0.2605 -0.1433 0.5671 0.047 Uiso 0.0870(18) 1 calc PR A 2 H4A3 H 0.2983 -0.1131 0.6325 0.047 Uiso 0.0870(18) 1 calc PR A 2 C5A C 0.1791(10) -0.100(2) 0.6324(8) 0.027(3) Uani 0.0870(18) 1 d PDU A 2 H5A1 H 0.1440 -0.0476 0.6402 0.040 Uiso 0.0870(18) 1 calc PR A 2 H5A2 H 0.2028 -0.1455 0.6685 0.040 Uiso 0.0870(18) 1 calc PR A 2 H5A3 H 0.1648 -0.1779 0.6033 0.040 Uiso 0.0870(18) 1 calc PR A 2 O1 O 0.26295(5) 0.10232(12) 0.43920(5) 0.0134(2) Uani 1 1 d D . . C11 C 0.30537(7) 0.18330(16) 0.42054(6) 0.0118(3) Uani 1 1 d . A . C12 C 0.29133(7) 0.23452(17) 0.36276(6) 0.0134(3) Uani 1 1 d . . . C21 C 0.38348(7) 0.12982(17) 0.51547(6) 0.0120(3) Uani 1 1 d . A . C22 C 0.39126(7) -0.02766(17) 0.51695(7) 0.0145(3) Uani 1 1 d . . . C27 C 0.38571(7) -0.11716(17) 0.46107(7) 0.0157(3) Uani 1 1 d . . . H27 H 0.3477 -0.0843 0.4326 0.019 Uiso 1 1 calc R . . C28 C 0.43958(7) -0.0850(2) 0.43417(7) 0.0201(3) Uani 1 1 d . . . H28A H 0.4407 0.0218 0.4256 0.030 Uiso 1 1 calc R . . H28B H 0.4347 -0.1421 0.3981 0.030 Uiso 1 1 calc R . . H28C H 0.4776 -0.1141 0.4616 0.030 Uiso 1 1 calc R . . C29 C 0.38167(8) -0.28663(18) 0.46877(8) 0.0218(3) Uani 1 1 d . . . H29A H 0.4209 -0.3243 0.4915 0.033 Uiso 1 1 calc R . . H29B H 0.3714 -0.3348 0.4305 0.033 Uiso 1 1 calc R . . H29C H 0.3501 -0.3089 0.4892 0.033 Uiso 1 1 calc R . . C23 C 0.40821(8) -0.09858(18) 0.57048(7) 0.0188(3) Uani 1 1 d D . . H23 H 0.4124 -0.2040 0.5714 0.023 Uiso 1 1 calc R . . C24 C 0.41928(8) -0.02109(19) 0.62303(7) 0.0210(3) Uani 1 1 d DU B . C30 C 0.43987(10) -0.1061(2) 0.68008(8) 0.0299(4) Uani 1 1 d DU . . H30A H 0.4301 -0.2139 0.6719 0.036 Uiso 0.695(17) 1 calc PR B 1 H30B H 0.4143 -0.1982 0.6735 0.036 Uiso 0.305(17) 1 calc PR B 2 C31 C 0.4109(4) -0.0584(12) 0.7274(3) 0.0358(16) Uani 0.695(17) 1 d PDU B 1 H31A H 0.4277 -0.1174 0.7625 0.054 Uiso 0.695(17) 1 calc PR B 1 H31B H 0.3669 -0.0741 0.7148 0.054 Uiso 0.695(17) 1 calc PR B 1 H31C H 0.4193 0.0475 0.7359 0.054 Uiso 0.695(17) 1 calc PR B 1 C32 C 0.51018(19) -0.0914(10) 0.7022(2) 0.0419(14) Uani 0.695(17) 1 d PDU B 1 H32A H 0.5294 -0.1222 0.6714 0.063 Uiso 0.695(17) 1 calc PR B 1 H32B H 0.5245 -0.1554 0.7363 0.063 Uiso 0.695(17) 1 calc PR B 1 H32C H 0.5208 0.0125 0.7128 0.063 Uiso 0.695(17) 1 calc PR B 1 C31A C 0.4225(9) -0.031(2) 0.7311(7) 0.033(3) Uani 0.305(17) 1 d PDU B 2 H31D H 0.4339 -0.0957 0.7654 0.050 Uiso 0.305(17) 1 calc PR B 2 H31E H 0.3785 -0.0139 0.7214 0.050 Uiso 0.305(17) 1 calc PR B 2 H31F H 0.4438 0.0644 0.7394 0.050 Uiso 0.305(17) 1 calc PR B 2 C32A C 0.5016(5) -0.163(2) 0.6906(5) 0.044(3) Uani 0.305(17) 1 d PDU B 2 H32D H 0.5065 -0.2165 0.6561 0.066 Uiso 0.305(17) 1 calc PR B 2 H32E H 0.5094 -0.2310 0.7239 0.066 Uiso 0.305(17) 1 calc PR B 2 H32F H 0.5303 -0.0796 0.6989 0.066 Uiso 0.305(17) 1 calc PR B 2 C25 C 0.41453(8) 0.13316(19) 0.62069(7) 0.0191(3) Uani 1 1 d D . . H25 H 0.4234 0.1879 0.6560 0.023 Uiso 1 1 calc R B . C26 C 0.39712(7) 0.21109(17) 0.56800(6) 0.0139(3) Uani 1 1 d . A . C33 C 0.39754(7) 0.38097(16) 0.56990(7) 0.0141(3) Uani 1 1 d . . . H33 H 0.3768 0.4189 0.5304 0.017 Uiso 1 1 calc R B . C34 C 0.46348(7) 0.43809(18) 0.58528(7) 0.0190(3) Uani 1 1 d . B . H34A H 0.4851 0.3977 0.6231 0.029 Uiso 1 1 calc R . . H34B H 0.4635 0.5473 0.5871 0.029 Uiso 1 1 calc R . . H34C H 0.4838 0.4057 0.5554 0.029 Uiso 1 1 calc R . . C35 C 0.36430(8) 0.4440(2) 0.61370(7) 0.0209(3) Uani 1 1 d . B . H35A H 0.3240 0.3980 0.6072 0.031 Uiso 1 1 calc R . . H35B H 0.3598 0.5522 0.6086 0.031 Uiso 1 1 calc R . . H35C H 0.3878 0.4220 0.6533 0.031 Uiso 1 1 calc R . . C13 C 0.33324(7) 0.32540(17) 0.34478(7) 0.0160(3) Uani 1 1 d . A . H13 H 0.3234 0.3643 0.3064 0.019 Uiso 1 1 calc R . . C14 C 0.38906(7) 0.35989(18) 0.38214(7) 0.0162(3) Uani 1 1 d . . . H14 H 0.4165 0.4254 0.3701 0.019 Uiso 1 1 calc R A . C15 C 0.40421(7) 0.29735(17) 0.43737(7) 0.0145(3) Uani 1 1 d . A . H15 H 0.4433 0.3164 0.4621 0.017 Uiso 1 1 calc R . . C16 C 0.36361(7) 0.20722(16) 0.45759(6) 0.0122(3) Uani 1 1 d . . . C41 C 0.23638(7) 0.17855(17) 0.31883(6) 0.0141(3) Uani 1 1 d . A . C42 C 0.24300(7) 0.04916(18) 0.28698(6) 0.0150(3) Uani 1 1 d . . . C47 C 0.30379(7) -0.03164(18) 0.29594(7) 0.0168(3) Uani 1 1 d . A . H47 H 0.3319 0.0095 0.3318 0.020 Uiso 1 1 calc R . . C48 C 0.29905(8) -0.20017(19) 0.30386(7) 0.0218(3) Uani 1 1 d . . . H48A H 0.2796 -0.2201 0.3356 0.033 Uiso 1 1 calc R A . H48B H 0.3399 -0.2441 0.3132 0.033 Uiso 1 1 calc R . . H48C H 0.2747 -0.2443 0.2678 0.033 Uiso 1 1 calc R . . C49 C 0.33155(8) -0.0001(2) 0.24446(8) 0.0270(4) Uani 1 1 d . . . H49A H 0.3035 -0.0340 0.2084 0.040 Uiso 1 1 calc R A . H49B H 0.3703 -0.0534 0.2500 0.040 Uiso 1 1 calc R . . H49C H 0.3386 0.1073 0.2420 0.040 Uiso 1 1 calc R . . C43 C 0.19328(7) -0.00115(19) 0.24414(7) 0.0177(3) Uani 1 1 d . A . H43 H 0.1977 -0.0883 0.2228 0.021 Uiso 1 1 calc R . . C44 C 0.13727(7) 0.07189(19) 0.23146(7) 0.0179(3) Uani 1 1 d . . . C50 C 0.08493(8) 0.0074(2) 0.18474(7) 0.0245(4) Uani 1 1 d . A . H50 H 0.1023 -0.0267 0.1521 0.029 Uiso 1 1 calc R . . C51 C 0.03497(9) 0.1190(2) 0.15940(8) 0.0307(4) Uani 1 1 d . . . H51A H 0.0134 0.1457 0.1890 0.046 Uiso 1 1 calc R A . H51B H 0.0063 0.0744 0.1259 0.046 Uiso 1 1 calc R . . H51C H 0.0530 0.2087 0.1470 0.046 Uiso 1 1 calc R . . C52 C 0.05857(10) -0.1299(2) 0.20758(10) 0.0397(5) Uani 1 1 d . . . H52A H 0.0912 -0.2017 0.2227 0.060 Uiso 1 1 calc R A . H52B H 0.0279 -0.1758 0.1759 0.060 Uiso 1 1 calc R . . H52C H 0.0397 -0.1002 0.2388 0.060 Uiso 1 1 calc R . . C45 C 0.13197(7) 0.19953(19) 0.26301(7) 0.0173(3) Uani 1 1 d . A . H45 H 0.0942 0.2510 0.2549 0.021 Uiso 1 1 calc R . . C46 C 0.18067(7) 0.25472(18) 0.30644(6) 0.0151(3) Uani 1 1 d . . . C53 C 0.17377(7) 0.40215(18) 0.33590(7) 0.0166(3) Uani 1 1 d . A . H53 H 0.2082 0.4110 0.3714 0.020 Uiso 1 1 calc R . . C54 C 0.11437(8) 0.4158(2) 0.35475(8) 0.0252(4) Uani 1 1 d . . . H54A H 0.0803 0.4246 0.3203 0.038 Uiso 1 1 calc R A . H54B H 0.1159 0.5045 0.3792 0.038 Uiso 1 1 calc R . . H54C H 0.1087 0.3269 0.3769 0.038 Uiso 1 1 calc R . . C55 C 0.17915(10) 0.5304(2) 0.29470(9) 0.0308(4) Uani 1 1 d . . . H55A H 0.1466 0.5222 0.2590 0.046 Uiso 1 1 calc R A . H55B H 0.2187 0.5250 0.2850 0.046 Uiso 1 1 calc R . . H55C H 0.1757 0.6258 0.3137 0.046 Uiso 1 1 calc R . . P1 P 0.166134(19) -0.10795(4) 0.442714(17) 0.01440(8) Uani 1 1 d D . . C61 C 0.22639(8) -0.24011(19) 0.44499(8) 0.0222(3) Uani 1 1 d . A . H61A H 0.2474 -0.2603 0.4855 0.033 Uiso 1 1 calc R . . H61B H 0.2553 -0.1989 0.4245 0.033 Uiso 1 1 calc R . . H61C H 0.2093 -0.3331 0.4261 0.033 Uiso 1 1 calc R . . C62 C 0.12747(8) -0.0891(2) 0.36651(7) 0.0230(3) Uani 1 1 d . A . H62A H 0.1563 -0.0536 0.3448 0.035 Uiso 1 1 calc R . . H62B H 0.0941 -0.0175 0.3624 0.035 Uiso 1 1 calc R . . H62C H 0.1112 -0.1862 0.3512 0.035 Uiso 1 1 calc R . . C63 C 0.11103(7) -0.19955(18) 0.47462(7) 0.0152(3) Uani 1 1 d . A . C64 C 0.12453(8) -0.33153(19) 0.50590(7) 0.0205(3) Uani 1 1 d . . . H64 H 0.1632 -0.3773 0.5102 0.025 Uiso 1 1 calc R A . C65 C 0.08116(9) -0.3967(2) 0.53095(8) 0.0273(4) Uani 1 1 d . A . H65 H 0.0902 -0.4877 0.5518 0.033 Uiso 1 1 calc R . . C66 C 0.02534(9) -0.3296(2) 0.52551(8) 0.0284(4) Uani 1 1 d . . . H66 H -0.0034 -0.3727 0.5438 0.034 Uiso 1 1 calc R A . C67 C 0.01111(8) -0.2002(2) 0.49362(8) 0.0252(4) Uani 1 1 d . A . H67 H -0.0278 -0.1558 0.4891 0.030 Uiso 1 1 calc R . . C68 C 0.05369(7) -0.1349(2) 0.46820(7) 0.0206(3) Uani 1 1 d . . . H68 H 0.0438 -0.0458 0.4463 0.025 Uiso 1 1 calc R A . 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 0.01015(10) 0.01101(4) 0.01173(9) 0.00039(5) 0.00423(7) 0.00006(7) Cl1 0.0164(3) 0.0114(3) 0.0215(4) -0.0013(2) 0.0054(2) -0.00072(18) O2 0.0140(6) 0.0174(6) 0.0216(7) 0.0012(5) 0.0053(5) 0.0011(5) C1 0.0164(8) 0.0160(8) 0.0160(7) 0.0003(6) 0.0054(6) -0.0009(6) C2 0.0199(9) 0.0219(10) 0.0135(8) 0.0015(7) 0.0049(7) -0.0019(8) C3 0.0293(14) 0.0320(13) 0.0174(12) -0.0059(10) 0.0060(11) -0.0064(11) C4 0.0447(13) 0.0246(10) 0.0205(9) 0.0063(8) 0.0072(9) -0.0035(9) C5 0.0217(9) 0.0451(13) 0.0179(9) 0.0003(8) 0.0089(7) -0.0027(9) W1A 0.0215(14) 0.0156(6) 0.0123(10) 0.0004(6) 0.0078(10) -0.0007(11) Cl1A 0.0164(3) 0.0114(3) 0.0215(4) -0.0013(2) 0.0054(2) -0.00072(18) O2A 0.0140(6) 0.0174(6) 0.0216(7) 0.0012(5) 0.0053(5) 0.0011(5) C1A 0.0164(8) 0.0160(8) 0.0160(7) 0.0003(6) 0.0054(6) -0.0009(6) C2A 0.018(4) 0.024(5) 0.015(4) 0.000(3) 0.003(4) -0.003(4) C3A 0.023(9) 0.029(8) 0.015(6) 0.002(6) 0.009(6) -0.007(6) C4A 0.031(6) 0.043(8) 0.020(7) 0.004(6) 0.006(6) 0.014(6) C5A 0.036(7) 0.031(7) 0.013(6) 0.003(5) 0.005(6) -0.012(6) O1 0.0113(5) 0.0114(5) 0.0179(5) 0.0001(4) 0.0045(4) -0.0011(4) C11 0.0109(7) 0.0094(6) 0.0157(7) -0.0014(5) 0.0044(5) 0.0004(5) C12 0.0109(7) 0.0134(7) 0.0154(7) -0.0012(5) 0.0020(5) 0.0015(5) C21 0.0110(6) 0.0140(7) 0.0108(6) 0.0010(5) 0.0025(5) -0.0003(5) C22 0.0114(7) 0.0141(7) 0.0184(7) 0.0006(6) 0.0045(6) 0.0002(6) C27 0.0147(7) 0.0124(7) 0.0191(7) -0.0006(6) 0.0025(6) 0.0026(6) C28 0.0178(8) 0.0212(8) 0.0223(8) -0.0042(7) 0.0068(6) 0.0014(7) C29 0.0221(9) 0.0132(8) 0.0279(9) -0.0009(6) 0.0021(7) 0.0015(6) C23 0.0219(8) 0.0143(7) 0.0203(8) 0.0046(6) 0.0055(6) 0.0028(6) C24 0.0259(9) 0.0204(8) 0.0166(7) 0.0054(6) 0.0050(6) 0.0018(7) C30 0.0450(11) 0.0244(9) 0.0183(8) 0.0069(7) 0.0042(8) 0.0031(8) C31 0.027(2) 0.059(4) 0.0204(18) 0.0177(19) 0.0055(17) -0.003(2) C32 0.0338(17) 0.064(4) 0.028(2) 0.021(2) 0.0077(14) 0.023(2) C31A 0.038(8) 0.043(7) 0.019(3) 0.009(4) 0.009(5) 0.011(6) C32A 0.049(5) 0.055(7) 0.025(4) 0.009(4) 0.004(3) 0.025(5) C25 0.0228(8) 0.0205(8) 0.0139(7) -0.0004(6) 0.0044(6) 0.0004(7) C26 0.0123(7) 0.0152(7) 0.0145(7) -0.0001(6) 0.0039(5) 0.0012(6) C33 0.0151(7) 0.0130(7) 0.0137(7) -0.0005(5) 0.0028(6) 0.0004(5) C34 0.0181(8) 0.0170(8) 0.0210(8) -0.0016(6) 0.0032(6) -0.0019(6) C35 0.0218(8) 0.0221(8) 0.0196(8) -0.0034(6) 0.0069(7) 0.0017(7) C13 0.0162(7) 0.0175(8) 0.0141(7) 0.0017(6) 0.0036(6) -0.0009(6) C14 0.0149(7) 0.0174(7) 0.0168(7) 0.0007(6) 0.0051(6) -0.0041(6) C15 0.0111(7) 0.0160(7) 0.0160(7) -0.0028(6) 0.0026(6) -0.0019(6) C16 0.0121(7) 0.0109(7) 0.0135(7) -0.0013(5) 0.0034(5) 0.0017(5) C41 0.0128(7) 0.0159(7) 0.0128(7) 0.0012(5) 0.0017(5) -0.0019(6) C42 0.0145(7) 0.0171(7) 0.0135(7) 0.0010(6) 0.0039(6) -0.0012(6) C47 0.0149(7) 0.0179(8) 0.0176(7) -0.0003(6) 0.0042(6) 0.0004(6) C48 0.0256(9) 0.0180(8) 0.0223(8) -0.0015(7) 0.0069(7) 0.0010(7) C49 0.0237(9) 0.0304(10) 0.0308(9) 0.0060(8) 0.0141(8) 0.0049(8) C43 0.0192(8) 0.0194(8) 0.0148(7) -0.0028(6) 0.0049(6) -0.0035(6) C44 0.0163(7) 0.0226(8) 0.0138(7) 0.0008(6) 0.0018(6) -0.0045(6) C50 0.0183(8) 0.0321(10) 0.0197(8) -0.0059(7) -0.0018(7) -0.0042(7) C51 0.0255(10) 0.0321(11) 0.0267(9) 0.0066(8) -0.0086(7) -0.0083(8) C52 0.0271(10) 0.0256(10) 0.0536(13) 0.0016(9) -0.0144(9) -0.0070(8) C45 0.0126(7) 0.0223(8) 0.0157(7) 0.0023(6) 0.0011(6) 0.0004(6) C46 0.0137(7) 0.0177(7) 0.0134(7) 0.0016(6) 0.0025(6) -0.0015(6) C53 0.0155(7) 0.0178(7) 0.0158(7) -0.0009(6) 0.0024(6) 0.0008(6) C54 0.0194(8) 0.0297(9) 0.0283(9) -0.0032(8) 0.0093(7) 0.0013(7) C55 0.0476(12) 0.0172(8) 0.0340(10) -0.0022(7) 0.0222(9) -0.0019(8) P1 0.01592(19) 0.01282(18) 0.01638(18) 0.00011(14) 0.00764(15) -0.00080(14) C61 0.0209(8) 0.0175(8) 0.0325(9) -0.0021(7) 0.0147(7) -0.0002(6) C62 0.0298(9) 0.0229(8) 0.0171(7) 0.0000(7) 0.0072(7) -0.0044(7) C63 0.0152(7) 0.0156(7) 0.0158(7) -0.0020(6) 0.0060(6) -0.0033(6) C64 0.0218(8) 0.0203(8) 0.0212(8) 0.0020(6) 0.0085(7) 0.0006(6) C65 0.0364(11) 0.0230(9) 0.0260(9) 0.0044(7) 0.0146(8) -0.0073(8) C66 0.0308(10) 0.0317(10) 0.0285(9) -0.0086(8) 0.0184(8) -0.0163(8) C67 0.0169(8) 0.0295(9) 0.0317(9) -0.0123(8) 0.0110(7) -0.0057(7) C68 0.0162(8) 0.0223(8) 0.0235(8) -0.0034(7) 0.0055(6) -0.0018(7) _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 1.7072(13) . ? W1 C1 1.9024(17) . ? W1 O1 1.9714(11) . ? W1 Cl1 2.3879(9) . ? W1 P1 2.5276(6) . ? C1 C2 1.510(3) . ? C1 H1A 0.960(15) . ? C2 C5 1.534(3) . ? C2 C3 1.538(3) . ? C2 C4 1.540(3) . ? 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 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? W1A O2A 1.705(12) . ? W1A C1A 1.931(13) . ? W1A O1 2.131(5) . ? W1A Cl1A 2.356(12) . ? W1A P1 2.436(5) . ? C1A C2A 1.516(17) . ? C1A H1A1 0.9500 . ? C2A C4A 1.527(14) . ? C2A C3A 1.529(15) . ? C2A C5A 1.532(17) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A H1A 1.20(3) . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? O1 C11 1.3641(17) . ? C11 C12 1.406(2) . ? C11 C16 1.411(2) . ? C12 C13 1.397(2) . ? C12 C41 1.501(2) . ? C21 C26 1.411(2) . ? C21 C22 1.423(2) . ? C21 C16 1.506(2) . ? C22 C23 1.388(2) . ? C22 C27 1.529(2) . ? C27 C29 1.536(2) . ? C27 C28 1.540(2) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C23 C24 1.396(2) . ? C23 H23 0.9500 . ? C24 C25 1.387(2) . ? C24 C30 1.523(2) . ? C30 C32A 1.452(9) . ? C30 C31 1.497(6) . ? C30 C31A 1.520(11) . ? C30 C32 1.557(5) . ? C30 H30A 1.0000 . ? C30 H30B 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C25 C26 1.402(2) . ? C25 H25 0.9500 . ? C26 C33 1.524(2) . ? C33 C35 1.535(2) . ? C33 C34 1.538(2) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C13 C14 1.390(2) . ? C13 H13 0.9500 . ? C14 C15 1.389(2) . ? C14 H14 0.9500 . ? C15 C16 1.397(2) . ? C15 H15 0.9500 . ? C41 C46 1.403(2) . ? C41 C42 1.413(2) . ? C42 C43 1.395(2) . ? C42 C47 1.526(2) . ? C47 C48 1.530(2) . ? C47 C49 1.533(2) . ? C47 H47 1.0000 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C43 C44 1.395(2) . ? C43 H43 0.9500 . ? C44 C45 1.389(2) . ? C44 C50 1.525(2) . ? C50 C51 1.521(3) . ? C50 C52 1.525(3) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C45 C46 1.402(2) . ? C45 H45 0.9500 . ? C46 C53 1.522(2) . ? C53 C54 1.527(2) . ? C53 C55 1.534(2) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? P1 C61 1.8002(17) . ? P1 C63 1.8108(15) . ? P1 C62 1.8130(17) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.391(2) . ? C63 C68 1.398(2) . ? C64 C65 1.398(2) . ? C64 H64 0.9500 . ? C65 C66 1.379(3) . ? C65 H65 0.9500 . ? C66 C67 1.380(3) . ? C66 H66 0.9500 . ? C67 C68 1.388(2) . ? C67 H67 0.9500 . ? C68 H68 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 O2 W1 C1 105.59(7) . . ? O2 W1 O1 141.51(6) . . ? C1 W1 O1 110.80(6) . . ? O2 W1 Cl1 97.36(5) . . ? C1 W1 Cl1 103.54(6) . . ? O1 W1 Cl1 86.12(4) . . ? O2 W1 P1 86.19(5) . . ? C1 W1 P1 93.52(6) . . ? O1 W1 P1 79.62(3) . . ? Cl1 W1 P1 160.84(3) . . ? C2 C1 W1 140.84(14) . . ? C2 C1 H1A 114.2(12) . . ? W1 C1 H1A 104.7(12) . . ? C1 C2 C5 112.28(17) . . ? C1 C2 C3 107.2(2) . . ? C5 C2 C3 109.4(2) . . ? C1 C2 C4 108.44(17) . . ? C5 C2 C4 109.37(18) . . ? C3 C2 C4 110.1(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O2A W1A C1A 100.9(8) . . ? O2A W1A O1 129.0(5) . . ? C1A W1A O1 128.7(5) . . ? O2A W1A Cl1A 99.2(6) . . ? C1A W1A Cl1A 99.5(6) . . ? O1 W1A Cl1A 84.8(3) . . ? O2A W1A P1 91.5(5) . . ? C1A W1A P1 90.4(6) . . ? O1 W1A P1 78.92(16) . . ? Cl1A W1A P1 163.7(4) . . ? C2A C1A W1A 139.7(12) . . ? C2A C1A H1A1 110.2 . . ? W1A C1A H1A1 110.2 . . ? C1A C2A C4A 109.7(14) . . ? C1A C2A C3A 106.2(16) . . ? C4A C2A C3A 109.4(19) . . ? C1A C2A C5A 109.7(15) . . ? C4A C2A C5A 111.1(15) . . ? C3A C2A C5A 110.5(17) . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2A C4A H1A 83.8(15) . . ? C2A C4A H4A1 109.5 . . ? H1A C4A H4A1 33.9 . . ? C2A C4A H4A2 109.5 . . ? H1A C4A H4A2 99.1 . . ? H4A1 C4A H4A2 109.5 . . ? C2A C4A H4A3 109.5 . . ? H1A C4A H4A3 141.2 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C2A C5A H5A1 109.5 . . ? C2A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C2A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C11 O1 W1 135.93(9) . . ? C11 O1 W1A 137.40(16) . . ? W1 O1 W1A 7.94(13) . . ? O1 C11 C12 118.83(13) . . ? O1 C11 C16 120.40(13) . . ? C12 C11 C16 120.66(13) . . ? C13 C12 C11 118.75(14) . . ? C13 C12 C41 119.62(13) . . ? C11 C12 C41 121.20(13) . . ? C26 C21 C22 119.47(13) . . ? C26 C21 C16 121.29(13) . . ? C22 C21 C16 119.19(13) . . ? C23 C22 C21 118.84(14) . . ? C23 C22 C27 119.92(14) . . ? C21 C22 C27 121.09(13) . . ? C22 C27 C29 114.24(13) . . ? C22 C27 C28 110.96(13) . . ? C29 C27 C28 108.15(13) . . ? C22 C27 H27 107.8 . . ? C29 C27 H27 107.8 . . ? C28 C27 H27 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C22 C23 C24 122.57(15) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 117.74(15) . . ? C25 C24 C30 122.56(16) . . ? C23 C24 C30 119.57(15) . . ? C32A C30 C31 123.7(6) . . ? C32A C30 C31A 116.6(9) . . ? C31 C30 C31A 13.4(10) . . ? C32A C30 C24 113.5(5) . . ? C31 C30 C24 115.4(4) . . ? C31A C30 C24 113.8(9) . . ? C32A C30 C32 26.8(6) . . ? C31 C30 C32 109.0(4) . . ? C31A C30 C32 98.1(8) . . ? C24 C30 C32 108.7(2) . . ? C32A C30 H30A 81.5 . . ? C31 C30 H30A 107.8 . . ? C31A C30 H30A 119.6 . . ? C24 C30 H30A 107.8 . . ? C32 C30 H30A 107.8 . . ? C32A C30 H30B 103.6 . . ? C31 C30 H30B 90.5 . . ? C31A C30 H30B 103.6 . . ? C24 C30 H30B 103.6 . . ? C32 C30 H30B 129.0 . . ? H30A C30 H30B 22.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C31A H31D 109.5 . . ? C30 C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C30 C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C30 C32A H32D 109.5 . . ? C30 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C30 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C24 C25 C26 122.33(15) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C25 C26 C21 118.88(14) . . ? C25 C26 C33 118.27(14) . . ? C21 C26 C33 122.73(13) . . ? C26 C33 C35 112.79(13) . . ? C26 C33 C34 109.80(13) . . ? C35 C33 C34 109.18(13) . . ? C26 C33 H33 108.3 . . ? C35 C33 H33 108.3 . . ? C34 C33 H33 108.3 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C14 C13 C12 121.11(14) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 119.13(14) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 121.83(14) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C11 118.00(13) . . ? C15 C16 C21 120.39(13) . . ? C11 C16 C21 121.47(13) . . ? C46 C41 C42 119.80(14) . . ? C46 C41 C12 122.28(14) . . ? C42 C41 C12 117.81(13) . . ? C43 C42 C41 118.82(14) . . ? C43 C42 C47 119.28(14) . . ? C41 C42 C47 121.82(14) . . ? C42 C47 C48 113.43(13) . . ? C42 C47 C49 109.66(13) . . ? C48 C47 C49 109.60(14) . . ? C42 C47 H47 108.0 . . ? C48 C47 H47 108.0 . . ? C49 C47 H47 108.0 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C42 C43 C44 122.39(15) . . ? C42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C45 C44 C43 117.77(14) . . ? C45 C44 C50 123.31(15) . . ? C43 C44 C50 118.91(15) . . ? C51 C50 C44 114.13(15) . . ? C51 C50 C52 110.61(16) . . ? C44 C50 C52 110.55(15) . . ? C51 C50 H50 107.1 . . ? C44 C50 H50 107.1 . . ? C52 C50 H50 107.1 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C44 C45 C46 121.99(15) . . ? C44 C45 H45 119.0 . . ? C46 C45 H45 119.0 . . ? C45 C46 C41 119.22(15) . . ? C45 C46 C53 119.52(14) . . ? C41 C46 C53 121.08(14) . . ? C46 C53 C54 113.75(14) . . ? C46 C53 C55 108.96(13) . . ? C54 C53 C55 109.99(14) . . ? C46 C53 H53 108.0 . . ? C54 C53 H53 108.0 . . ? C55 C53 H53 108.0 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C61 P1 C63 106.66(8) . . ? C61 P1 C62 105.56(9) . . ? C63 P1 C62 104.20(8) . . ? C61 P1 W1A 120.02(13) . . ? C63 P1 W1A 113.01(12) . . ? C62 P1 W1A 106.03(13) . . ? C61 P1 W1 113.02(6) . . ? C63 P1 W1 115.63(5) . . ? C62 P1 W1 110.95(6) . . ? W1A P1 W1 7.22(11) . . ? P1 C61 H61A 109.5 . . ? P1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? P1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? P1 C62 H62A 109.5 . . ? P1 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? P1 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C68 119.17(15) . . ? C64 C63 P1 121.70(12) . . ? C68 C63 P1 119.12(12) . . ? C63 C64 C65 119.85(16) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C66 C65 C64 120.30(17) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? C65 C66 C67 120.24(16) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C66 C67 C68 119.95(17) . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C67 C68 C63 120.45(17) . . ? C67 C68 H68 119.8 . . ? C63 C68 H68 119.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.656 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.071 #===END data_x11080 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H67 N O2 W' _chemical_formula_weight 861.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.7275(18) _cell_length_b 15.986(2) _cell_length_c 19.325(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.046(2) _cell_angle_gamma 90.00 _cell_volume 4274.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9177 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 30.58 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4938 _exptl_absorpt_correction_T_max 0.8752 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 89374 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 30.32 _reflns_number_total 12819 _reflns_number_gt 10812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7.0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0045P)^2^+13.4383P] 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 12819 _refine_ls_number_parameters 524 _refine_ls_number_restraints 739 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.000 _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 0.187491(9) 0.328682(7) 0.357774(6) 0.01566(4) Uani 0.9787(3) 1 d PD A 1 W1A W 0.1267(4) 0.3119(3) 0.3935(3) 0.01566(4) Uani 0.0213(3) 1 d PD A 2 O2 O 0.21556(19) 0.37502(14) 0.28879(13) 0.0278(5) Uani 1 1 d . . . C1 C 0.0589(2) 0.36387(19) 0.33836(19) 0.0248(7) Uani 1 1 d D . . H1 H 0.033(3) 0.329(2) 0.3675(19) 0.030 Uiso 1 1 d D . . C2 C -0.0109(3) 0.4254(2) 0.2864(2) 0.0333(8) Uani 1 1 d . A . C3 C -0.0181(3) 0.4102(3) 0.2071(2) 0.0401(10) Uani 1 1 d . . . H3A H 0.0452 0.4198 0.2021 0.060 Uiso 1 1 calc R A . H3B H -0.0656 0.4486 0.1745 0.060 Uiso 1 1 calc R . . H3C H -0.0384 0.3524 0.1933 0.060 Uiso 1 1 calc R . . C4 C -0.1118(3) 0.4148(3) 0.2933(3) 0.0498(12) Uani 1 1 d . . . H4A H -0.1361 0.3584 0.2775 0.075 Uiso 1 1 calc R A . H4B H -0.1564 0.4562 0.2621 0.075 Uiso 1 1 calc R . . H4C H -0.1069 0.4231 0.3447 0.075 Uiso 1 1 calc R . . C5 C 0.0258(4) 0.5151(3) 0.3071(3) 0.0689(18) Uani 1 1 d . . . H5A H 0.0278 0.5274 0.3573 0.103 Uiso 1 1 calc R A . H5B H -0.0178 0.5546 0.2726 0.103 Uiso 1 1 calc R . . H5C H 0.0909 0.5206 0.3046 0.103 Uiso 1 1 calc R . . N1 N 0.2594(2) 0.38904(16) 0.45126(14) 0.0199(5) Uani 1 1 d . . . C6 C 0.1326(3) 0.4267(2) 0.5083(2) 0.0368(9) Uani 1 1 d . . . H6A H 0.1311 0.4561 0.5524 0.055 Uiso 1 1 calc R A . H6B H 0.1140 0.3682 0.5104 0.055 Uiso 1 1 calc R . . H6C H 0.0873 0.4534 0.4644 0.055 Uiso 1 1 calc R . . C7 C 0.2315(3) 0.4305(2) 0.50515(19) 0.0254(7) Uani 1 1 d . A . C8 C 0.3136(3) 0.4669(2) 0.55353(19) 0.0316(8) Uani 1 1 d . . . H8 H 0.3163 0.4987 0.5957 0.038 Uiso 1 1 calc R A . C9 C 0.3924(3) 0.4496(2) 0.5310(2) 0.0305(8) Uani 1 1 d . A . H9 H 0.4571 0.4677 0.5547 0.037 Uiso 1 1 calc R . . C11 C 0.4129(3) 0.3714(2) 0.4210(2) 0.0318(8) Uani 1 1 d . . . H11A H 0.3948 0.4049 0.3759 0.048 Uiso 1 1 calc R A . H11B H 0.3964 0.3126 0.4084 0.048 Uiso 1 1 calc R . . H11C H 0.4826 0.3764 0.4473 0.048 Uiso 1 1 calc R . . C10 C 0.3595(2) 0.40219(19) 0.46904(18) 0.0231(6) Uani 1 1 d . A . O1 O 0.19530(16) 0.21266(12) 0.36997(11) 0.0172(4) Uani 1 1 d D . . C21 C 0.1929(2) 0.12769(16) 0.36173(15) 0.0145(5) Uani 1 1 d . A . C22 C 0.1245(2) 0.08198(17) 0.38221(15) 0.0157(5) Uani 1 1 d DU . . C31 C 0.0547(6) 0.1302(4) 0.4067(5) 0.0166(6) Uani 0.637(5) 1 d PDU A 1 C32 C -0.0392(6) 0.1454(6) 0.3572(4) 0.0166(10) Uani 0.637(5) 1 d PDU A 1 C37 C -0.0728(9) 0.1106(9) 0.2789(5) 0.0184(10) Uani 0.637(5) 1 d PDU A 1 H37 H -0.0308 0.0617 0.2782 0.022 Uiso 0.637(5) 1 calc PR A 1 C38 C -0.0604(12) 0.1761(15) 0.2249(6) 0.0286(19) Uani 0.637(5) 1 d PDU A 1 H38A H -0.0822 0.1526 0.1750 0.043 Uiso 0.637(5) 1 calc PR A 1 H38B H 0.0079 0.1918 0.2392 0.043 Uiso 0.637(5) 1 calc PR A 1 H38C H -0.0990 0.2257 0.2259 0.043 Uiso 0.637(5) 1 calc PR A 1 C39 C -0.1774(8) 0.0799(6) 0.2544(8) 0.0269(19) Uani 0.637(5) 1 d PDU A 1 H39A H -0.1960 0.0576 0.2043 0.040 Uiso 0.637(5) 1 calc PR A 1 H39B H -0.2201 0.1266 0.2555 0.040 Uiso 0.637(5) 1 calc PR A 1 H39C H -0.1832 0.0358 0.2879 0.040 Uiso 0.637(5) 1 calc PR A 1 C33 C -0.1015(6) 0.1953(5) 0.3797(3) 0.0179(12) Uani 0.637(5) 1 d PDU A 1 H33 H -0.1642 0.2068 0.3457 0.022 Uiso 0.637(5) 1 calc PR A 1 C34 C -0.0750(4) 0.2290(4) 0.4502(3) 0.0217(9) Uani 0.637(5) 1 d PDU A 1 C40 C -0.1475(4) 0.2852(4) 0.4685(3) 0.0285(9) Uani 0.637(5) 1 d PDU A 1 H40 H -0.1816 0.3212 0.4250 0.034 Uiso 0.637(5) 1 calc PR A 1 C41 C -0.1011(10) 0.3406(6) 0.5360(5) 0.041(2) Uani 0.637(5) 1 d PDU A 1 H41A H -0.1509 0.3751 0.5450 0.062 Uiso 0.637(5) 1 calc PR A 1 H41B H -0.0525 0.3768 0.5272 0.062 Uiso 0.637(5) 1 calc PR A 1 H41C H -0.0700 0.3053 0.5791 0.062 Uiso 0.637(5) 1 calc PR A 1 C42 C -0.2229(4) 0.2268(4) 0.4858(4) 0.0336(11) Uani 0.637(5) 1 d PDU A 1 H42A H -0.2709 0.2612 0.4974 0.050 Uiso 0.637(5) 1 calc PR A 1 H42B H -0.1895 0.1911 0.5281 0.050 Uiso 0.637(5) 1 calc PR A 1 H42C H -0.2554 0.1918 0.4428 0.050 Uiso 0.637(5) 1 calc PR A 1 C35 C 0.0164(5) 0.2102(4) 0.4998(3) 0.0219(10) Uani 0.637(5) 1 d PDU A 1 H35 H 0.0350 0.2313 0.5486 0.026 Uiso 0.637(5) 1 calc PR A 1 C36 C 0.0812(7) 0.1610(6) 0.4792(4) 0.0203(10) Uani 0.637(5) 1 d PDU A 1 C43 C 0.1787(7) 0.1383(7) 0.5361(7) 0.0240(11) Uani 0.637(5) 1 d PDU A 1 H43 H 0.2182 0.1114 0.5093 0.029 Uiso 0.637(5) 1 calc PR A 1 C44 C 0.2352(11) 0.2141(7) 0.5771(11) 0.029(2) Uani 0.637(5) 1 d PDU A 1 H44A H 0.2975 0.1956 0.6121 0.043 Uiso 0.637(5) 1 calc PR A 1 H44B H 0.1981 0.2422 0.6038 0.043 Uiso 0.637(5) 1 calc PR A 1 H44C H 0.2463 0.2530 0.5417 0.043 Uiso 0.637(5) 1 calc PR A 1 C45 C 0.1643(10) 0.0733(8) 0.5897(8) 0.039(2) Uani 0.637(5) 1 d PDU A 1 H45A H 0.2272 0.0582 0.6258 0.059 Uiso 0.637(5) 1 calc PR A 1 H45B H 0.1335 0.0233 0.5623 0.059 Uiso 0.637(5) 1 calc PR A 1 H45C H 0.1231 0.0968 0.6152 0.059 Uiso 0.637(5) 1 calc PR A 1 C31A C 0.0542(10) 0.1246(6) 0.4113(8) 0.0166(6) Uani 0.363(5) 1 d PDU A 2 C32A C -0.0424(11) 0.1411(11) 0.3665(8) 0.0166(10) Uani 0.363(5) 1 d PDU A 2 C37A C -0.0790(16) 0.1129(17) 0.2864(9) 0.0184(10) Uani 0.363(5) 1 d PDU A 2 H37A H -0.0479 0.0576 0.2848 0.022 Uiso 0.363(5) 1 calc PR A 2 C38A C -0.047(2) 0.172(3) 0.2371(13) 0.0286(19) Uani 0.363(5) 1 d PDU A 2 H38D H -0.0713 0.1521 0.1862 0.043 Uiso 0.363(5) 1 calc PR A 2 H38E H 0.0239 0.1748 0.2542 0.043 Uiso 0.363(5) 1 calc PR A 2 H38F H -0.0727 0.2285 0.2393 0.043 Uiso 0.363(5) 1 calc PR A 2 C39A C -0.1880(15) 0.0992(13) 0.2529(16) 0.0269(19) Uani 0.363(5) 1 d PDU A 2 H39D H -0.2047 0.0812 0.2016 0.040 Uiso 0.363(5) 1 calc PR A 2 H39E H -0.2217 0.1515 0.2548 0.040 Uiso 0.363(5) 1 calc PR A 2 H39F H -0.2076 0.0560 0.2809 0.040 Uiso 0.363(5) 1 calc PR A 2 C33A C -0.1034(11) 0.1841(9) 0.3961(6) 0.0179(12) Uani 0.363(5) 1 d PDU A 2 H33A H -0.1679 0.1963 0.3659 0.022 Uiso 0.363(5) 1 calc PR A 2 C34A C -0.0695(8) 0.2094(7) 0.4704(6) 0.0217(9) Uani 0.363(5) 1 d PDU A 2 C40A C -0.1355(6) 0.2579(6) 0.5016(6) 0.0285(9) Uani 0.363(5) 1 d PDU A 2 H40A H -0.1327 0.2313 0.5491 0.034 Uiso 0.363(5) 1 calc PR A 2 C41A C -0.1053(18) 0.3498(9) 0.5165(11) 0.041(2) Uani 0.363(5) 1 d PDU A 2 H41D H -0.1493 0.3784 0.5369 0.062 Uiso 0.363(5) 1 calc PR A 2 H41E H -0.1080 0.3770 0.4704 0.062 Uiso 0.363(5) 1 calc PR A 2 H41F H -0.0392 0.3529 0.5519 0.062 Uiso 0.363(5) 1 calc PR A 2 C42A C -0.2409(6) 0.2627(7) 0.4515(6) 0.0336(11) Uani 0.363(5) 1 d PDU A 2 H42D H -0.2778 0.2950 0.4759 0.050 Uiso 0.363(5) 1 calc PR A 2 H42E H -0.2677 0.2061 0.4413 0.050 Uiso 0.363(5) 1 calc PR A 2 H42F H -0.2451 0.2901 0.4051 0.050 Uiso 0.363(5) 1 calc PR A 2 C35A C 0.0241(8) 0.1894(7) 0.5147(6) 0.0219(10) Uani 0.363(5) 1 d PDU A 2 H35A H 0.0457 0.2038 0.5655 0.026 Uiso 0.363(5) 1 calc PR A 2 C36A C 0.0869(11) 0.1486(12) 0.4859(8) 0.0203(10) Uani 0.363(5) 1 d PDU A 2 C43A C 0.1879(12) 0.1252(13) 0.5372(12) 0.0240(11) Uani 0.363(5) 1 d PDU A 2 H43A H 0.2240 0.1015 0.5063 0.029 Uiso 0.363(5) 1 calc PR A 2 C44A C 0.245(2) 0.1996(15) 0.580(2) 0.029(2) Uani 0.363(5) 1 d PDU A 2 H44D H 0.3088 0.1804 0.6125 0.043 Uiso 0.363(5) 1 calc PR A 2 H44E H 0.2103 0.2254 0.6091 0.043 Uiso 0.363(5) 1 calc PR A 2 H44F H 0.2542 0.2408 0.5450 0.043 Uiso 0.363(5) 1 calc PR A 2 C45A C 0.1823(19) 0.0572(16) 0.5917(15) 0.039(2) Uani 0.363(5) 1 d PDU A 2 H45D H 0.2477 0.0432 0.6244 0.059 Uiso 0.363(5) 1 calc PR A 2 H45E H 0.1514 0.0071 0.5644 0.059 Uiso 0.363(5) 1 calc PR A 2 H45F H 0.1443 0.0778 0.6210 0.059 Uiso 0.363(5) 1 calc PR A 2 C23 C 0.1234(2) -0.00473(18) 0.37628(18) 0.0212(6) Uani 1 1 d . A . H23 H 0.0777 -0.0370 0.3895 0.025 Uiso 1 1 calc R . . C24 C 0.1904(2) -0.04331(18) 0.35071(18) 0.0212(6) Uani 1 1 d . . . H24 H 0.1906 -0.1026 0.3474 0.025 Uiso 1 1 calc R A . C25 C 0.2574(2) 0.00222(18) 0.32975(17) 0.0190(6) Uani 1 1 d . A . H25 H 0.3017 -0.0260 0.3118 0.023 Uiso 1 1 calc R . . C26 C 0.2594(2) 0.08900(17) 0.33514(15) 0.0149(5) Uani 1 1 d . . . C51 C 0.3278(2) 0.13998(17) 0.31087(15) 0.0149(5) Uani 1 1 d . A . C52 C 0.2961(2) 0.17740(18) 0.24089(15) 0.0161(5) Uani 1 1 d . . . C57 C 0.1935(2) 0.16143(19) 0.18763(16) 0.0193(6) Uani 1 1 d . A . H57 H 0.1525 0.1465 0.2178 0.023 Uiso 1 1 calc R . . C58 C 0.1470(3) 0.2367(2) 0.14027(18) 0.0292(7) Uani 1 1 d . . . H58A H 0.1799 0.2478 0.1049 0.044 Uiso 1 1 calc R A . H58B H 0.1526 0.2858 0.1719 0.044 Uiso 1 1 calc R . . H58C H 0.0786 0.2249 0.1136 0.044 Uiso 1 1 calc R . . C59 C 0.1931(3) 0.0866(2) 0.1385(2) 0.0346(9) Uani 1 1 d . . . H59A H 0.2366 0.0977 0.1109 0.052 Uiso 1 1 calc R A . H59B H 0.1274 0.0773 0.1040 0.052 Uiso 1 1 calc R . . H59C H 0.2152 0.0367 0.1691 0.052 Uiso 1 1 calc R . . C53 C 0.3602(2) 0.22499(18) 0.21887(16) 0.0181(6) Uani 1 1 d . A . H53 H 0.3384 0.2497 0.1713 0.022 Uiso 1 1 calc R . . C54 C 0.4549(2) 0.23750(18) 0.26407(16) 0.0178(6) Uani 1 1 d . . . C60 C 0.5226(2) 0.29205(19) 0.23970(18) 0.0214(6) Uani 1 1 d . A . H60 H 0.4863 0.3116 0.1885 0.026 Uiso 1 1 calc R . . C61 C 0.5543(3) 0.3698(2) 0.2884(2) 0.0326(8) Uani 1 1 d . . . H61A H 0.4971 0.4001 0.2896 0.049 Uiso 1 1 calc R A . H61B H 0.5927 0.4062 0.2682 0.049 Uiso 1 1 calc R . . H61C H 0.5934 0.3527 0.3385 0.049 Uiso 1 1 calc R . . C62 C 0.6104(3) 0.2432(2) 0.2373(2) 0.0291(7) Uani 1 1 d . . . H62A H 0.6454 0.2202 0.2863 0.044 Uiso 1 1 calc R A . H62B H 0.6532 0.2806 0.2224 0.044 Uiso 1 1 calc R . . H62C H 0.5891 0.1973 0.2017 0.044 Uiso 1 1 calc R . . C55 C 0.4868(2) 0.19855(18) 0.33293(17) 0.0187(6) Uani 1 1 d . A . H55 H 0.5519 0.2062 0.3643 0.022 Uiso 1 1 calc R . . C56 C 0.4258(2) 0.14896(18) 0.35672(15) 0.0172(6) Uani 1 1 d . . . C63 C 0.4629(2) 0.1049(2) 0.43151(16) 0.0218(6) Uani 1 1 d . A . H63 H 0.4320 0.0484 0.4248 0.026 Uiso 1 1 calc R . . C64 C 0.4327(3) 0.1507(2) 0.48973(18) 0.0308(8) Uani 1 1 d . . . H64A H 0.4641 0.2056 0.4995 0.046 Uiso 1 1 calc R A . H64B H 0.4522 0.1178 0.5353 0.046 Uiso 1 1 calc R . . H64C H 0.3623 0.1580 0.4717 0.046 Uiso 1 1 calc R . . C65 C 0.5722(3) 0.0911(2) 0.46019(19) 0.0300(8) Uani 1 1 d . . . H65A H 0.5917 0.0649 0.4217 0.045 Uiso 1 1 calc R A . H65B H 0.5898 0.0546 0.5035 0.045 Uiso 1 1 calc R . . H65C H 0.6051 0.1451 0.4738 0.045 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 0.01939(6) 0.00911(5) 0.01713(5) -0.00039(4) 0.00451(4) -0.00138(5) W1A 0.01939(6) 0.00911(5) 0.01713(5) -0.00039(4) 0.00451(4) -0.00138(5) O2 0.0401(15) 0.0186(11) 0.0239(11) 0.0020(9) 0.0099(11) -0.0040(10) C1 0.0239(16) 0.0134(13) 0.0302(16) 0.0008(12) 0.0003(13) -0.0015(12) C2 0.0257(18) 0.0187(15) 0.044(2) 0.0020(14) -0.0027(16) 0.0047(13) C3 0.032(2) 0.036(2) 0.043(2) 0.0180(17) -0.0001(17) -0.0019(16) C4 0.037(2) 0.062(3) 0.046(2) 0.007(2) 0.009(2) 0.029(2) C5 0.081(4) 0.0153(17) 0.077(4) 0.003(2) -0.016(3) 0.009(2) N1 0.0239(14) 0.0152(11) 0.0200(12) -0.0014(9) 0.0067(10) -0.0015(10) C6 0.044(2) 0.0326(19) 0.044(2) -0.0119(16) 0.0288(19) -0.0057(17) C7 0.0326(18) 0.0197(14) 0.0271(16) -0.0063(12) 0.0143(14) -0.0059(13) C8 0.043(2) 0.0276(17) 0.0233(16) -0.0073(13) 0.0104(15) -0.0121(16) C9 0.0291(19) 0.0250(16) 0.0302(17) 0.0007(13) 0.0009(15) -0.0082(14) C11 0.0231(17) 0.0222(16) 0.052(2) -0.0029(15) 0.0153(16) -0.0013(13) C10 0.0226(16) 0.0161(13) 0.0263(15) 0.0021(11) 0.0030(13) -0.0002(12) O1 0.0221(11) 0.0105(9) 0.0192(10) -0.0018(7) 0.0073(9) -0.0009(8) C21 0.0161(13) 0.0103(11) 0.0135(11) -0.0003(9) 0.0003(10) 0.0002(10) C22 0.0178(13) 0.0136(12) 0.0142(12) -0.0002(9) 0.0038(10) -0.0001(10) C31 0.0197(13) 0.0142(14) 0.0179(14) 0.0009(11) 0.0090(10) -0.0011(11) C32 0.0190(13) 0.0128(15) 0.021(2) -0.0007(16) 0.0099(13) -0.0041(11) C37 0.0171(19) 0.0167(15) 0.021(2) -0.0024(16) 0.0061(15) 0.0014(14) C38 0.031(5) 0.032(3) 0.019(4) 0.000(4) 0.003(4) -0.013(4) C39 0.021(3) 0.025(5) 0.0311(19) -0.004(4) 0.004(2) -0.004(3) C33 0.0148(13) 0.019(2) 0.023(2) -0.001(2) 0.0099(19) -0.0032(15) C34 0.0223(14) 0.022(2) 0.027(2) -0.0041(17) 0.0169(17) -0.0016(15) C40 0.0252(17) 0.034(2) 0.034(2) -0.0081(17) 0.0191(19) 0.0009(16) C41 0.041(3) 0.044(3) 0.045(5) -0.018(3) 0.023(4) -0.007(2) C42 0.026(2) 0.040(3) 0.042(3) -0.012(2) 0.022(2) -0.004(2) C35 0.0273(16) 0.020(3) 0.021(2) -0.0020(18) 0.0125(16) -0.0012(17) C36 0.0229(14) 0.020(3) 0.0192(16) -0.0005(17) 0.0081(12) -0.0009(14) C43 0.0269(19) 0.025(3) 0.0188(13) -0.002(2) 0.0062(15) 0.0026(17) C44 0.026(4) 0.032(4) 0.023(2) -0.003(4) 0.001(2) 0.002(3) C45 0.041(5) 0.036(5) 0.033(2) 0.012(3) 0.002(3) 0.001(3) C31A 0.0197(13) 0.0142(14) 0.0179(14) 0.0009(11) 0.0090(10) -0.0011(11) C32A 0.0190(13) 0.0128(15) 0.021(2) -0.0007(16) 0.0099(13) -0.0041(11) C37A 0.0171(19) 0.0167(15) 0.021(2) -0.0024(16) 0.0061(15) 0.0014(14) C38A 0.031(5) 0.032(3) 0.019(4) 0.000(4) 0.003(4) -0.013(4) C39A 0.021(3) 0.025(5) 0.0311(19) -0.004(4) 0.004(2) -0.004(3) C33A 0.0148(13) 0.019(2) 0.023(2) -0.001(2) 0.0099(19) -0.0032(15) C34A 0.0223(14) 0.022(2) 0.027(2) -0.0041(17) 0.0169(17) -0.0016(15) C40A 0.0252(17) 0.034(2) 0.034(2) -0.0081(17) 0.0191(19) 0.0009(16) C41A 0.041(3) 0.044(3) 0.045(5) -0.018(3) 0.023(4) -0.007(2) C42A 0.026(2) 0.040(3) 0.042(3) -0.012(2) 0.022(2) -0.004(2) C35A 0.0273(16) 0.020(3) 0.021(2) -0.0020(18) 0.0125(16) -0.0012(17) C36A 0.0229(14) 0.020(3) 0.0192(16) -0.0005(17) 0.0081(12) -0.0009(14) C43A 0.0269(19) 0.025(3) 0.0188(13) -0.002(2) 0.0062(15) 0.0026(17) C44A 0.026(4) 0.032(4) 0.023(2) -0.003(4) 0.001(2) 0.002(3) C45A 0.041(5) 0.036(5) 0.033(2) 0.012(3) 0.002(3) 0.001(3) C23 0.0235(16) 0.0141(13) 0.0287(15) 0.0024(11) 0.0123(13) -0.0051(11) C24 0.0176(14) 0.0117(12) 0.0342(17) -0.0010(11) 0.0088(13) -0.0039(11) C25 0.0213(15) 0.0145(13) 0.0238(14) -0.0032(10) 0.0110(12) 0.0007(11) C26 0.0166(14) 0.0124(12) 0.0152(12) -0.0008(9) 0.0047(11) -0.0027(10) C51 0.0157(13) 0.0130(11) 0.0164(12) -0.0020(10) 0.0059(10) -0.0011(10) C52 0.0182(13) 0.0140(12) 0.0158(12) -0.0007(10) 0.0054(10) 0.0036(11) C57 0.0167(13) 0.0216(14) 0.0188(13) 0.0022(11) 0.0048(11) 0.0028(11) C58 0.0308(18) 0.0263(16) 0.0234(15) 0.0032(13) 0.0003(14) 0.0069(14) C59 0.0270(19) 0.0269(17) 0.039(2) -0.0102(15) -0.0031(16) -0.0022(14) C53 0.0240(15) 0.0135(12) 0.0176(13) 0.0026(10) 0.0081(12) 0.0015(11) C54 0.0218(15) 0.0132(12) 0.0209(13) 0.0007(10) 0.0106(12) -0.0016(11) C60 0.0231(16) 0.0191(14) 0.0250(15) 0.0027(11) 0.0123(13) -0.0025(12) C61 0.041(2) 0.0226(16) 0.039(2) -0.0015(14) 0.0199(17) -0.0119(15) C62 0.0265(18) 0.0325(18) 0.0355(18) 0.0052(14) 0.0201(15) 0.0006(14) C55 0.0179(14) 0.0165(12) 0.0211(13) 0.0010(10) 0.0058(11) -0.0025(11) C56 0.0195(14) 0.0155(13) 0.0156(12) 0.0003(10) 0.0046(11) -0.0019(10) C63 0.0204(15) 0.0223(14) 0.0186(13) 0.0039(11) 0.0013(12) -0.0088(12) C64 0.0315(19) 0.042(2) 0.0171(14) 0.0000(13) 0.0061(13) -0.0073(15) C65 0.0249(18) 0.0325(18) 0.0260(16) 0.0108(14) 0.0003(14) -0.0037(14) _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 1.695(2) . ? W1 O1 1.868(2) . ? W1 C1 1.886(4) . ? W1 N1 2.001(3) . ? W1A C1 1.447(6) . ? W1A O1 2.015(6) . ? W1A N1 2.257(6) . ? W1A H1 1.32(4) . ? C1 C2 1.525(5) . ? C1 H1 0.959(18) . ? C2 C3 1.520(6) . ? C2 C5 1.536(5) . ? C2 C4 1.546(6) . ? 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 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N1 C7 1.409(4) . ? N1 C10 1.410(4) . ? C6 C7 1.480(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.378(5) . ? C8 C9 1.401(6) . ? C8 H8 0.9500 . ? C9 C10 1.358(5) . ? C9 H9 0.9500 . ? C11 C10 1.491(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O1 C21 1.367(3) . ? C21 C26 1.396(4) . ? C21 C22 1.408(4) . ? C22 C23 1.391(4) . ? C22 C31 1.486(7) . ? C22 C31A 1.500(11) . ? C31 C36 1.407(7) . ? C31 C32 1.407(7) . ? C32 C33 1.393(7) . ? C32 C37 1.527(7) . ? C37 C39 1.530(8) . ? C37 C38 1.533(9) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C33 C34 1.391(7) . ? C33 H33 0.9500 . ? C34 C35 1.391(7) . ? C34 C40 1.527(7) . ? C40 C41 1.530(8) . ? C40 C42 1.572(7) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C35 C36 1.397(7) . ? C35 H35 0.9500 . ? C36 C43 1.523(7) . ? C43 C44 1.529(8) . ? C43 C45 1.531(8) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C31A C36A 1.407(11) . ? C31A C32A 1.413(11) . ? C32A C33A 1.400(12) . ? C32A C37A 1.522(11) . ? C37A C39A 1.527(12) . ? C37A C38A 1.532(12) . ? C37A H37A 1.0000 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C33A C34A 1.408(11) . ? C33A H33A 0.9500 . ? C34A C35A 1.388(11) . ? C34A C40A 1.520(10) . ? C40A C42A 1.524(11) . ? C40A C41A 1.534(12) . ? C40A H40A 1.0000 . ? C41A H41D 0.9800 . ? C41A H41E 0.9800 . ? C41A H41F 0.9800 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C35A C36A 1.395(12) . ? C35A H35A 0.9500 . ? C36A C43A 1.524(11) . ? C43A C44A 1.527(12) . ? C43A C45A 1.536(12) . ? C43A H43A 1.0000 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? C23 C24 1.391(4) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C26 1.391(4) . ? C25 H25 0.9500 . ? C26 C51 1.491(4) . ? C51 C52 1.404(4) . ? C51 C56 1.418(4) . ? C52 C53 1.388(4) . ? C52 C57 1.531(4) . ? C57 C58 1.525(4) . ? C57 C59 1.526(5) . ? C57 H57 1.0000 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C53 C54 1.382(4) . ? C53 H53 0.9500 . ? C54 C55 1.397(4) . ? C54 C60 1.517(4) . ? C60 C62 1.525(5) . ? C60 C61 1.532(5) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C55 C56 1.390(4) . ? C55 H55 0.9500 . ? C56 C63 1.530(4) . ? C63 C65 1.527(5) . ? C63 C64 1.531(5) . ? C63 H63 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 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 O1 120.79(10) . . ? O2 W1 C1 102.26(14) . . ? O1 W1 C1 109.59(12) . . ? O2 W1 N1 107.63(11) . . ? O1 W1 N1 111.97(10) . . ? C1 W1 N1 102.73(13) . . ? C1 W1A O1 124.0(4) . . ? C1 W1A N1 108.2(3) . . ? O1 W1A N1 97.2(2) . . ? C1 W1A H1 40.2(9) . . ? O1 W1A H1 127.7(17) . . ? N1 W1A H1 133.7(16) . . ? W1A C1 C2 174.1(4) . . ? W1A C1 W1 44.8(3) . . ? C2 C1 W1 136.7(3) . . ? W1A C1 H1 63(2) . . ? C2 C1 H1 117(2) . . ? W1 C1 H1 106(2) . . ? C3 C2 C1 111.0(3) . . ? C3 C2 C5 107.9(4) . . ? C1 C2 C5 109.5(3) . . ? C3 C2 C4 109.5(3) . . ? C1 C2 C4 108.9(3) . . ? C5 C2 C4 110.1(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N1 C10 107.2(3) . . ? C7 N1 W1 134.1(2) . . ? C10 N1 W1 118.5(2) . . ? C7 N1 W1A 101.5(2) . . ? C10 N1 W1A 149.1(3) . . ? W1 N1 W1A 35.84(15) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N1 106.8(3) . . ? C8 C7 C6 129.5(3) . . ? N1 C7 C6 123.5(3) . . ? C7 C8 C9 109.5(3) . . ? C7 C8 H8 125.2 . . ? C9 C8 H8 125.2 . . ? C10 C9 C8 107.5(3) . . ? C10 C9 H9 126.3 . . ? C8 C9 H9 126.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C10 N1 109.0(3) . . ? C9 C10 C11 128.9(3) . . ? N1 C10 C11 122.0(3) . . ? C21 O1 W1 166.91(19) . . ? C21 O1 W1A 144.5(3) . . ? W1 O1 W1A 39.90(16) . . ? O1 C21 C26 119.4(3) . . ? O1 C21 C22 118.4(3) . . ? C26 C21 C22 122.3(2) . . ? C23 C22 C21 118.9(3) . . ? C23 C22 C31 123.6(3) . . ? C21 C22 C31 117.4(3) . . ? C23 C22 C31A 119.6(4) . . ? C21 C22 C31A 121.5(4) . . ? C31 C22 C31A 4.9(5) . . ? C36 C31 C32 119.3(6) . . ? C36 C31 C22 120.8(6) . . ? C32 C31 C22 119.9(6) . . ? C33 C32 C31 119.1(6) . . ? C33 C32 C37 119.5(6) . . ? C31 C32 C37 121.3(7) . . ? C32 C37 C39 111.9(8) . . ? C32 C37 C38 110.6(8) . . ? C39 C37 C38 110.6(8) . . ? C32 C37 H37 107.8 . . ? C39 C37 H37 107.8 . . ? C38 C37 H37 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C34 C33 C32 122.2(6) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C33 C34 C35 118.1(5) . . ? C33 C34 C40 118.1(5) . . ? C35 C34 C40 123.7(5) . . ? C34 C40 C41 113.2(7) . . ? C34 C40 C42 107.5(5) . . ? C41 C40 C42 107.7(6) . . ? C34 C40 H40 109.4 . . ? C41 C40 H40 109.4 . . ? C42 C40 H40 109.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C34 C35 C36 121.3(6) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C35 C36 C31 119.8(6) . . ? C35 C36 C43 119.7(6) . . ? C31 C36 C43 120.5(7) . . ? C36 C43 C44 113.4(7) . . ? C36 C43 C45 109.6(7) . . ? C44 C43 C45 111.4(8) . . ? C36 C43 H43 107.4 . . ? C44 C43 H43 107.4 . . ? C45 C43 H43 107.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C36A C31A C32A 119.7(10) . . ? C36A C31A C22 118.0(10) . . ? C32A C31A C22 122.3(11) . . ? C33A C32A C31A 119.6(10) . . ? C33A C32A C37A 120.5(11) . . ? C31A C32A C37A 119.9(11) . . ? C32A C37A C39A 115.3(14) . . ? C32A C37A C38A 111.8(13) . . ? C39A C37A C38A 109.3(15) . . ? C32A C37A H37A 106.7 . . ? C39A C37A H37A 106.7 . . ? C38A C37A H37A 106.7 . . ? C37A C38A H38D 109.5 . . ? C37A C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37A C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37A C39A H39D 109.5 . . ? C37A C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37A C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C32A C33A C34A 120.4(11) . . ? C32A C33A H33A 119.8 . . ? C34A C33A H33A 119.8 . . ? C35A C34A C33A 119.5(9) . . ? C35A C34A C40A 120.5(9) . . ? C33A C34A C40A 120.0(9) . . ? C34A C40A C42A 115.1(8) . . ? C34A C40A C41A 112.3(11) . . ? C42A C40A C41A 103.8(11) . . ? C34A C40A H40A 108.5 . . ? C42A C40A H40A 108.5 . . ? C41A C40A H40A 108.5 . . ? C40A C41A H41D 109.5 . . ? C40A C41A H41E 109.5 . . ? H41D C41A H41E 109.5 . . ? C40A C41A H41F 109.5 . . ? H41D C41A H41F 109.5 . . ? H41E C41A H41F 109.5 . . ? C40A C42A H42D 109.5 . . ? C40A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C40A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C34A C35A C36A 121.0(10) . . ? C34A C35A H35A 119.5 . . ? C36A C35A H35A 119.5 . . ? C35A C36A C31A 119.7(10) . . ? C35A C36A C43A 119.2(11) . . ? C31A C36A C43A 120.9(12) . . ? C36A C43A C44A 113.4(13) . . ? C36A C43A C45A 110.5(12) . . ? C44A C43A C45A 109.4(14) . . ? C36A C43A H43A 107.8 . . ? C44A C43A H43A 107.8 . . ? C45A C43A H43A 107.8 . . ? C43A C44A H44D 109.5 . . ? C43A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C43A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C43A C45A H45D 109.5 . . ? C43A C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? C43A C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? C24 C23 C22 118.8(3) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 122.1(3) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 118.1(3) . . ? C25 C26 C51 121.4(3) . . ? C21 C26 C51 120.5(2) . . ? C52 C51 C56 119.3(3) . . ? C52 C51 C26 119.9(3) . . ? C56 C51 C26 120.8(2) . . ? C53 C52 C51 119.5(3) . . ? C53 C52 C57 120.3(3) . . ? C51 C52 C57 120.1(3) . . ? C58 C57 C59 109.9(3) . . ? C58 C57 C52 114.1(3) . . ? C59 C57 C52 109.9(3) . . ? C58 C57 H57 107.5 . . ? C59 C57 H57 107.5 . . ? C52 C57 H57 107.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C54 C53 C52 122.0(3) . . ? C54 C53 H53 119.0 . . ? C52 C53 H53 119.0 . . ? C53 C54 C55 118.4(3) . . ? C53 C54 C60 121.0(3) . . ? C55 C54 C60 120.6(3) . . ? C54 C60 C62 111.7(3) . . ? C54 C60 C61 111.7(3) . . ? C62 C60 C61 110.6(3) . . ? C54 C60 H60 107.5 . . ? C62 C60 H60 107.5 . . ? C61 C60 H60 107.5 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C56 C55 C54 121.6(3) . . ? C56 C55 H55 119.2 . . ? C54 C55 H55 119.2 . . ? C55 C56 C51 119.1(3) . . ? C55 C56 C63 120.9(3) . . ? C51 C56 C63 120.1(3) . . ? C65 C63 C56 113.6(3) . . ? C65 C63 C64 109.7(3) . . ? C56 C63 C64 112.0(3) . . ? C65 C63 H63 107.1 . . ? C56 C63 H63 107.1 . . ? C64 C63 H63 107.1 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.917 _refine_diff_density_min -1.870 _refine_diff_density_rms 0.121 #===END data_x11146 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.50 H72 N O2 P W' _chemical_formula_weight 939.91 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' 'P' 'P' 0.1023 0.0942 '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 13.4162(7) _cell_length_b 13.5775(7) _cell_length_c 14.7782(8) _cell_angle_alpha 71.8330(10) _cell_angle_beta 65.5150(10) _cell_angle_gamma 83.6550(10) _cell_volume 2327.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9231 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 30.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 2.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8415 _exptl_absorpt_correction_T_max 0.9507 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 105170 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 30.32 _reflns_number_total 13947 _reflns_number_gt 12112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7.0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+2.3910P] 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 13947 _refine_ls_number_parameters 541 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.034 _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 0.356233(8) 0.330004(8) 0.245351(7) 0.01224(3) Uani 1 1 d . . . O2 O 0.39571(14) 0.40449(13) 0.11810(13) 0.0168(3) Uani 1 1 d . . . C1 C 0.47009(19) 0.35963(19) 0.27841(19) 0.0154(4) Uani 1 1 d D . . H1 H 0.455(2) 0.321(2) 0.3490(14) 0.018 Uiso 1 1 d D . . C2 C 0.57560(19) 0.4230(2) 0.22989(19) 0.0172(5) Uani 1 1 d . . . C3 C 0.5497(2) 0.5186(2) 0.2699(2) 0.0266(6) Uani 1 1 d . . . H3A H 0.4969 0.5614 0.2454 0.040 Uiso 1 1 calc R . . H3B H 0.6172 0.5592 0.2436 0.040 Uiso 1 1 calc R . . H3C H 0.5185 0.4962 0.3461 0.040 Uiso 1 1 calc R . . C4 C 0.6226(2) 0.4570(2) 0.1116(2) 0.0265(6) Uani 1 1 d . . . H4A H 0.6412 0.3957 0.0866 0.040 Uiso 1 1 calc R . . H4B H 0.6886 0.5000 0.0843 0.040 Uiso 1 1 calc R . . H4C H 0.5681 0.4971 0.0878 0.040 Uiso 1 1 calc R . . C5 C 0.6607(2) 0.3589(2) 0.2672(2) 0.0267(6) Uani 1 1 d . . . H5A H 0.6299 0.3358 0.3435 0.040 Uiso 1 1 calc R . . H5B H 0.7266 0.4016 0.2410 0.040 Uiso 1 1 calc R . . H5C H 0.6796 0.2983 0.2411 0.040 Uiso 1 1 calc R . . N1 N 0.38922(16) 0.18966(15) 0.21154(15) 0.0153(4) Uani 1 1 d . . . C6 C 0.5404(2) 0.1145(2) 0.2707(2) 0.0239(5) Uani 1 1 d . . . H6A H 0.5945 0.1697 0.2215 0.036 Uiso 1 1 calc R . . H6B H 0.5775 0.0482 0.2810 0.036 Uiso 1 1 calc R . . H6C H 0.5030 0.1297 0.3375 0.036 Uiso 1 1 calc R . . C7 C 0.4584(2) 0.10842(19) 0.22847(19) 0.0179(5) Uani 1 1 d . . . C8 C 0.4427(2) 0.0321(2) 0.1934(2) 0.0229(5) Uani 1 1 d . . . H8 H 0.4792 -0.0322 0.1961 0.027 Uiso 1 1 calc R . . C9 C 0.3622(2) 0.0657(2) 0.1522(2) 0.0224(5) Uani 1 1 d . . . H9 H 0.3351 0.0282 0.1223 0.027 Uiso 1 1 calc R . . C10 C 0.3309(2) 0.16196(19) 0.16332(18) 0.0179(5) Uani 1 1 d . . . C11 C 0.2542(2) 0.2343(2) 0.1264(2) 0.0219(5) Uani 1 1 d . . . H11A H 0.2958 0.2934 0.0687 0.033 Uiso 1 1 calc R . . H11B H 0.2012 0.2591 0.1836 0.033 Uiso 1 1 calc R . . H11C H 0.2152 0.1978 0.1026 0.033 Uiso 1 1 calc R . . O1 O 0.24552(13) 0.25612(13) 0.38164(12) 0.0146(3) Uani 1 1 d . . . C21 C 0.16100(19) 0.24007(17) 0.47533(17) 0.0136(4) Uani 1 1 d . . . C22 C 0.05451(19) 0.22004(18) 0.48783(18) 0.0151(4) Uani 1 1 d . . . C31 C 0.02892(19) 0.20039(19) 0.40534(18) 0.0160(5) Uani 1 1 d . . . C32 C 0.0700(2) 0.11139(19) 0.37284(19) 0.0176(5) Uani 1 1 d . . . C37 C 0.1480(2) 0.04059(19) 0.4115(2) 0.0202(5) Uani 1 1 d . . . H37A H 0.1509 -0.0255 0.3967 0.030 Uiso 1 1 calc R . . H37B H 0.1224 0.0281 0.4867 0.030 Uiso 1 1 calc R . . H37C H 0.2212 0.0731 0.3761 0.030 Uiso 1 1 calc R . . C33 C 0.0350(2) 0.0863(2) 0.3061(2) 0.0221(5) Uani 1 1 d . . . H33 H 0.0624 0.0258 0.2851 0.026 Uiso 1 1 calc R . . C34 C -0.0380(2) 0.1460(2) 0.2693(2) 0.0239(6) Uani 1 1 d . . . C38 C -0.0748(3) 0.1169(3) 0.1969(2) 0.0349(7) Uani 1 1 d . . . H38A H -0.0329 0.1580 0.1251 0.052 Uiso 1 1 calc R . . H38B H -0.1530 0.1308 0.2157 0.052 Uiso 1 1 calc R . . H38C H -0.0625 0.0430 0.2032 0.052 Uiso 1 1 calc R . . C35 C -0.0772(2) 0.2342(2) 0.3010(2) 0.0236(5) Uani 1 1 d . . . H35 H -0.1267 0.2767 0.2757 0.028 Uiso 1 1 calc R . . C36 C -0.04600(19) 0.2621(2) 0.3689(2) 0.0191(5) Uani 1 1 d . . . C39 C -0.0974(2) 0.3565(2) 0.4024(2) 0.0228(5) Uani 1 1 d . . . H39A H -0.1146 0.4060 0.3468 0.034 Uiso 1 1 calc R . . H39B H -0.0460 0.3890 0.4167 0.034 Uiso 1 1 calc R . . H39C H -0.1648 0.3357 0.4655 0.034 Uiso 1 1 calc R . . C23 C -0.0311(2) 0.21184(19) 0.58496(19) 0.0185(5) Uani 1 1 d . . . H23 H -0.1037 0.2007 0.5939 0.022 Uiso 1 1 calc R . . C24 C -0.0135(2) 0.2194(2) 0.66847(19) 0.0211(5) Uani 1 1 d . . . H24 H -0.0735 0.2161 0.7329 0.025 Uiso 1 1 calc R . . C25 C 0.0929(2) 0.2317(2) 0.65681(19) 0.0202(5) Uani 1 1 d . . . H25 H 0.1056 0.2341 0.7147 0.024 Uiso 1 1 calc R . . C26 C 0.1818(2) 0.24073(19) 0.56129(18) 0.0163(5) Uani 1 1 d . . . C41 C 0.2957(2) 0.24022(19) 0.55571(18) 0.0168(5) Uani 1 1 d . . . C42 C 0.3556(2) 0.1486(2) 0.55051(19) 0.0190(5) Uani 1 1 d . . . C47 C 0.3081(2) 0.0540(2) 0.5491(2) 0.0248(6) Uani 1 1 d . . . H47A H 0.3189 0.0603 0.4778 0.037 Uiso 1 1 calc R . . H47B H 0.2296 0.0479 0.5936 0.037 Uiso 1 1 calc R . . H47C H 0.3449 -0.0079 0.5751 0.037 Uiso 1 1 calc R . . C43 C 0.4599(2) 0.1439(2) 0.5495(2) 0.0222(5) Uani 1 1 d . . . H43 H 0.4999 0.0819 0.5455 0.027 Uiso 1 1 calc R . . C44 C 0.5078(2) 0.2268(2) 0.55411(19) 0.0224(5) Uani 1 1 d . . . C48 C 0.6217(2) 0.2180(3) 0.5530(2) 0.0306(6) Uani 1 1 d . . . H48A H 0.6757 0.2211 0.4828 0.046 Uiso 1 1 calc R . . H48B H 0.6273 0.1519 0.6020 0.046 Uiso 1 1 calc R . . H48C H 0.6357 0.2754 0.5735 0.046 Uiso 1 1 calc R . . C45 C 0.4476(2) 0.3160(2) 0.5612(2) 0.0227(5) Uani 1 1 d . . . H45 H 0.4789 0.3732 0.5650 0.027 Uiso 1 1 calc R . . C46 C 0.3419(2) 0.3240(2) 0.56288(19) 0.0206(5) Uani 1 1 d . . . C49 C 0.2825(3) 0.4234(2) 0.5716(3) 0.0337(7) Uani 1 1 d . . . H49A H 0.2912 0.4453 0.6252 0.051 Uiso 1 1 calc R . . H49B H 0.2045 0.4126 0.5906 0.051 Uiso 1 1 calc R . . H49C H 0.3131 0.4773 0.5047 0.051 Uiso 1 1 calc R . . P1 P 0.23854(5) 0.49111(5) 0.26911(5) 0.01376(11) Uani 1 1 d . . . C51 C 0.1536(2) 0.4971(2) 0.1982(2) 0.0216(5) Uani 1 1 d . . . H51A H 0.1047 0.5561 0.2042 0.032 Uiso 1 1 calc R . . H51B H 0.1099 0.4328 0.2274 0.032 Uiso 1 1 calc R . . H51C H 0.2005 0.5056 0.1247 0.032 Uiso 1 1 calc R . . C52 C 0.1405(2) 0.4984(2) 0.39578(19) 0.0205(5) Uani 1 1 d . . . H52A H 0.1797 0.5081 0.4356 0.031 Uiso 1 1 calc R . . H52B H 0.0966 0.4340 0.4332 0.031 Uiso 1 1 calc R . . H52C H 0.0924 0.5571 0.3870 0.031 Uiso 1 1 calc R . . C53 C 0.30922(18) 0.61626(18) 0.20624(18) 0.0134(4) Uani 1 1 d . . . C54 C 0.3833(2) 0.63957(19) 0.10214(18) 0.0173(5) Uani 1 1 d . . . H54 H 0.3976 0.5892 0.0660 0.021 Uiso 1 1 calc R . . C55 C 0.4361(2) 0.73585(19) 0.05127(19) 0.0185(5) Uani 1 1 d . . . H55 H 0.4859 0.7514 -0.0197 0.022 Uiso 1 1 calc R . . C56 C 0.4164(2) 0.80925(19) 0.1038(2) 0.0204(5) Uani 1 1 d . . . H56 H 0.4525 0.8751 0.0690 0.024 Uiso 1 1 calc R . . C57 C 0.3438(2) 0.7863(2) 0.2070(2) 0.0217(5) Uani 1 1 d . . . H57 H 0.3303 0.8367 0.2430 0.026 Uiso 1 1 calc R . . C58 C 0.2908(2) 0.69051(19) 0.25836(19) 0.0176(5) Uani 1 1 d . . . H58 H 0.2416 0.6753 0.3295 0.021 Uiso 1 1 calc R . . C1S C 0.1531(3) 0.8014(3) 1.0421(3) 0.0456(9) Uani 1 1 d D . . H1S1 H 0.1764 0.7849 0.9763 0.068 Uiso 1 1 calc R . . H1S2 H 0.0864 0.7613 1.0934 0.068 Uiso 1 1 calc R . . H1S3 H 0.2113 0.7838 1.0679 0.068 Uiso 1 1 calc R . . C2S C 0.1307(3) 0.9144(3) 1.0248(3) 0.0448(8) Uani 1 1 d D . . H2S1 H 0.1068 0.9298 1.0920 0.054 Uiso 1 1 calc R . . H2S2 H 0.0691 0.9303 1.0025 0.054 Uiso 1 1 calc R . . C3S C 0.2254(3) 0.9846(3) 0.9462(3) 0.0409(8) Uani 1 1 d D . . H3S1 H 0.2498 0.9682 0.8796 0.049 Uiso 1 1 calc R . . H3S2 H 0.2866 0.9687 0.9692 0.049 Uiso 1 1 calc R . . C4S C 0.2053(3) 1.0996(3) 0.9259(3) 0.0519(10) Uani 1 1 d D . . H4S1 H 0.1463 1.1163 0.9001 0.062 Uiso 1 1 calc R . . H4S2 H 0.1786 1.1160 0.9927 0.062 Uiso 1 1 calc R . . C5S C 0.3033(3) 1.1684(3) 0.8491(4) 0.0629(12) Uani 1 1 d D . . H5S1 H 0.3588 1.1595 0.8779 0.094 Uiso 1 1 calc R . . H5S2 H 0.2810 1.2409 0.8353 0.094 Uiso 1 1 calc R . . H5S3 H 0.3340 1.1495 0.7841 0.094 Uiso 1 1 calc R . . C1T C 0.0957(11) 0.4071(10) 0.8747(9) 0.078(3) Uani 0.50 1 d PDU A -1 H1T1 H 0.1550 0.3624 0.8455 0.117 Uiso 0.50 1 calc PR A -1 H1T2 H 0.1173 0.4798 0.8360 0.117 Uiso 0.50 1 calc PR A -1 H1T3 H 0.0294 0.3907 0.8695 0.117 Uiso 0.50 1 calc PR A -1 C2T C 0.0740(11) 0.3897(11) 0.9849(9) 0.089(4) Uani 0.50 1 d PDU A -1 H2T1 H 0.1436 0.4000 0.9891 0.107 Uiso 0.50 1 calc PR A -1 H2T2 H 0.0503 0.3164 1.0230 0.107 Uiso 0.50 1 calc PR A -1 C3T C -0.0117(10) 0.4581(9) 1.0405(10) 0.087(3) Uani 0.50 1 d PDU A -1 H3T1 H -0.0816 0.4425 1.0396 0.104 Uiso 0.50 1 calc PR A -1 H3T2 H -0.0212 0.4335 1.1142 0.104 Uiso 0.50 1 calc PR A -1 C4T C -0.0010(10) 0.5688(10) 1.0093(10) 0.085(3) Uani 0.50 1 d PDU A -1 H4T1 H 0.0017 0.5955 0.9378 0.102 Uiso 0.50 1 calc PR A -1 H4T2 H 0.0706 0.5861 1.0057 0.102 Uiso 0.50 1 calc PR A -1 C5T C -0.0865(13) 0.6265(12) 1.0744(11) 0.092(5) Uani 0.50 1 d PDU A -1 H5T1 H -0.0694 0.7010 1.0439 0.137 Uiso 0.50 1 calc PR A -1 H5T2 H -0.0884 0.6040 1.1449 0.137 Uiso 0.50 1 calc PR A -1 H5T3 H -0.1581 0.6125 1.0773 0.137 Uiso 0.50 1 calc PR A -1 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 0.01160(4) 0.01124(4) 0.01141(4) -0.00406(3) -0.00151(3) -0.00063(3) O2 0.0171(8) 0.0165(9) 0.0163(8) -0.0065(7) -0.0050(7) -0.0002(7) C1 0.0140(11) 0.0142(11) 0.0151(11) -0.0046(9) -0.0029(9) -0.0003(9) C2 0.0133(11) 0.0201(12) 0.0163(11) -0.0041(9) -0.0047(9) -0.0012(9) C3 0.0211(13) 0.0263(15) 0.0351(15) -0.0123(12) -0.0101(12) -0.0050(11) C4 0.0187(13) 0.0365(16) 0.0188(12) -0.0024(11) -0.0038(11) -0.0098(11) C5 0.0192(13) 0.0287(15) 0.0301(14) -0.0021(12) -0.0118(12) -0.0033(11) N1 0.0169(10) 0.0121(10) 0.0128(9) -0.0056(8) -0.0007(8) -0.0003(8) C6 0.0269(14) 0.0172(13) 0.0252(13) -0.0064(11) -0.0093(11) 0.0052(10) C7 0.0193(12) 0.0109(11) 0.0167(11) -0.0030(9) -0.0013(10) 0.0003(9) C8 0.0246(13) 0.0131(12) 0.0238(13) -0.0058(10) -0.0029(11) 0.0011(10) C9 0.0251(13) 0.0174(13) 0.0211(12) -0.0091(10) -0.0022(11) -0.0045(10) C10 0.0182(12) 0.0158(12) 0.0148(11) -0.0056(9) -0.0003(9) -0.0032(9) C11 0.0213(13) 0.0202(13) 0.0234(13) -0.0070(10) -0.0069(11) -0.0031(10) O1 0.0135(8) 0.0151(8) 0.0113(7) -0.0034(6) -0.0010(6) -0.0016(6) C21 0.0134(10) 0.0093(10) 0.0130(10) -0.0027(8) -0.0009(9) 0.0003(8) C22 0.0144(11) 0.0125(11) 0.0149(11) -0.0044(9) -0.0021(9) -0.0002(9) C31 0.0126(11) 0.0156(11) 0.0146(11) -0.0042(9) 0.0001(9) -0.0039(9) C32 0.0160(11) 0.0158(12) 0.0151(11) -0.0037(9) -0.0001(9) -0.0039(9) C37 0.0226(13) 0.0156(12) 0.0186(12) -0.0050(10) -0.0041(10) -0.0021(10) C33 0.0194(12) 0.0239(14) 0.0211(12) -0.0117(11) -0.0015(10) -0.0046(10) C34 0.0188(12) 0.0318(15) 0.0197(12) -0.0095(11) -0.0033(10) -0.0064(11) C38 0.0308(16) 0.050(2) 0.0324(16) -0.0203(15) -0.0134(13) -0.0035(14) C35 0.0161(12) 0.0295(15) 0.0233(13) -0.0061(11) -0.0068(11) -0.0020(10) C36 0.0112(11) 0.0208(13) 0.0210(12) -0.0063(10) -0.0016(9) -0.0023(9) C39 0.0159(12) 0.0233(14) 0.0272(13) -0.0081(11) -0.0070(11) 0.0033(10) C23 0.0142(11) 0.0167(12) 0.0193(12) -0.0059(10) -0.0010(9) -0.0004(9) C24 0.0186(12) 0.0226(13) 0.0155(11) -0.0067(10) 0.0002(10) 0.0009(10) C25 0.0220(13) 0.0228(13) 0.0152(11) -0.0083(10) -0.0057(10) 0.0029(10) C26 0.0171(11) 0.0146(11) 0.0150(11) -0.0050(9) -0.0042(9) 0.0017(9) C41 0.0164(11) 0.0194(12) 0.0114(10) -0.0032(9) -0.0038(9) 0.0015(9) C42 0.0172(12) 0.0216(13) 0.0151(11) -0.0043(10) -0.0042(10) -0.0001(10) C47 0.0245(14) 0.0178(13) 0.0325(15) -0.0077(11) -0.0125(12) 0.0036(10) C43 0.0218(13) 0.0227(13) 0.0186(12) -0.0054(10) -0.0062(10) 0.0045(10) C44 0.0200(12) 0.0315(15) 0.0156(11) -0.0047(11) -0.0081(10) -0.0015(11) C48 0.0243(14) 0.0397(18) 0.0292(15) -0.0068(13) -0.0141(12) -0.0006(12) C45 0.0241(13) 0.0266(14) 0.0192(12) -0.0056(11) -0.0099(11) -0.0048(11) C46 0.0237(13) 0.0208(13) 0.0172(11) -0.0052(10) -0.0084(10) 0.0000(10) C49 0.0384(17) 0.0286(16) 0.0481(19) -0.0203(14) -0.0258(16) 0.0067(13) P1 0.0134(3) 0.0114(3) 0.0141(3) -0.0039(2) -0.0030(2) -0.0004(2) C51 0.0187(12) 0.0204(13) 0.0255(13) -0.0043(10) -0.0101(11) -0.0011(10) C52 0.0196(12) 0.0149(12) 0.0169(11) -0.0033(9) 0.0014(10) 0.0001(9) C53 0.0122(10) 0.0113(11) 0.0149(10) -0.0034(9) -0.0038(9) -0.0004(8) C54 0.0187(12) 0.0150(12) 0.0153(11) -0.0051(9) -0.0032(9) -0.0007(9) C55 0.0195(12) 0.0166(12) 0.0141(11) -0.0034(9) -0.0018(9) -0.0022(9) C56 0.0213(12) 0.0125(11) 0.0222(12) -0.0024(10) -0.0047(10) -0.0045(9) C57 0.0255(13) 0.0161(12) 0.0218(12) -0.0090(10) -0.0046(11) -0.0034(10) C58 0.0193(12) 0.0162(12) 0.0145(11) -0.0070(9) -0.0022(9) -0.0002(9) C1S 0.056(2) 0.044(2) 0.045(2) -0.0156(17) -0.0284(19) 0.0118(17) C2S 0.046(2) 0.044(2) 0.0393(19) -0.0132(16) -0.0128(16) 0.0045(17) C3S 0.0348(18) 0.043(2) 0.0403(19) -0.0161(16) -0.0076(15) 0.0008(15) C4S 0.046(2) 0.050(2) 0.048(2) -0.0177(19) -0.0072(18) 0.0036(18) C5S 0.049(2) 0.038(2) 0.070(3) -0.006(2) -0.001(2) 0.0021(18) C1T 0.044(6) 0.077(8) 0.104(8) -0.003(7) -0.035(6) -0.014(5) C2T 0.059(6) 0.083(7) 0.100(8) 0.017(6) -0.037(7) -0.008(5) C3T 0.073(6) 0.087(6) 0.099(8) -0.007(5) -0.042(6) -0.020(5) C4T 0.060(6) 0.091(6) 0.112(10) -0.010(6) -0.053(6) -0.012(5) C5T 0.070(8) 0.087(9) 0.098(13) -0.001(9) -0.030(10) -0.012(7) _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 1.7165(17) . ? W1 C1 1.900(2) . ? W1 O1 1.9644(16) . ? W1 N1 2.0738(19) . ? W1 P1 2.5802(6) . ? C1 C2 1.517(3) . ? C1 H1 0.955(17) . ? C2 C4 1.521(3) . ? C2 C3 1.537(4) . ? C2 C5 1.539(4) . ? 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 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N1 C7 1.391(3) . ? N1 C10 1.398(3) . ? C6 C7 1.493(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.364(3) . ? C8 C9 1.416(4) . ? C8 H8 0.9500 . ? C9 C10 1.367(3) . ? C9 H9 0.9500 . ? C10 C11 1.493(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O1 C21 1.347(3) . ? C21 C22 1.409(3) . ? C21 C26 1.412(3) . ? C22 C23 1.398(3) . ? C22 C31 1.498(3) . ? C31 C36 1.408(3) . ? C31 C32 1.411(3) . ? C32 C33 1.393(3) . ? C32 C37 1.508(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C33 C34 1.380(4) . ? C33 H33 0.9500 . ? C34 C35 1.392(4) . ? C34 C38 1.512(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C35 C36 1.394(4) . ? C35 H35 0.9500 . ? C36 C39 1.511(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C23 C24 1.383(3) . ? C23 H23 0.9500 . ? C24 C25 1.388(4) . ? C24 H24 0.9500 . ? C25 C26 1.400(3) . ? C25 H25 0.9500 . ? C26 C41 1.495(3) . ? C41 C46 1.405(4) . ? C41 C42 1.409(3) . ? C42 C43 1.389(4) . ? C42 C47 1.505(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C43 C44 1.389(4) . ? C43 H43 0.9500 . ? C44 C45 1.386(4) . ? C44 C48 1.513(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C45 C46 1.401(4) . ? C45 H45 0.9500 . ? C46 C49 1.504(4) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? P1 C52 1.814(2) . ? P1 C53 1.814(2) . ? P1 C51 1.823(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C58 1.394(3) . ? C53 C54 1.398(3) . ? C54 C55 1.388(3) . ? C54 H54 0.9500 . ? C55 C56 1.386(3) . ? C55 H55 0.9500 . ? C56 C57 1.382(4) . ? C56 H56 0.9500 . ? C57 C58 1.384(3) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C1S C2S 1.493(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.493(5) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.510(5) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.504(5) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C1T C2T 1.473(11) . ? C1T H1T1 0.9800 . ? C1T H1T2 0.9800 . ? C1T H1T3 0.9800 . ? C2T C3T 1.522(11) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.432(10) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T C5T 1.487(12) . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? C5T H5T1 0.9800 . ? C5T H5T2 0.9800 . ? C5T H5T3 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 C1 101.92(9) . . ? O2 W1 O1 152.48(7) . . ? C1 W1 O1 103.16(9) . . ? O2 W1 N1 95.00(8) . . ? C1 W1 N1 107.98(9) . . ? O1 W1 N1 87.91(7) . . ? O2 W1 P1 79.55(6) . . ? C1 W1 P1 99.17(7) . . ? O1 W1 P1 85.43(5) . . ? N1 W1 P1 152.84(6) . . ? C2 C1 W1 140.99(18) . . ? C2 C1 H1 110.7(17) . . ? W1 C1 H1 108.4(17) . . ? C1 C2 C4 112.7(2) . . ? C1 C2 C3 107.2(2) . . ? C4 C2 C3 109.9(2) . . ? C1 C2 C5 109.3(2) . . ? C4 C2 C5 109.4(2) . . ? C3 C2 C5 108.3(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N1 C10 107.1(2) . . ? C7 N1 W1 134.31(16) . . ? C10 N1 W1 118.55(16) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N1 108.9(2) . . ? C8 C7 C6 128.8(2) . . ? N1 C7 C6 122.2(2) . . ? C7 C8 C9 107.8(2) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? C10 C9 C8 107.4(2) . . ? C10 C9 H9 126.3 . . ? C8 C9 H9 126.3 . . ? C9 C10 N1 108.7(2) . . ? C9 C10 C11 129.0(2) . . ? N1 C10 C11 122.1(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C21 O1 W1 159.81(15) . . ? O1 C21 C22 120.6(2) . . ? O1 C21 C26 118.7(2) . . ? C22 C21 C26 120.7(2) . . ? C23 C22 C21 117.9(2) . . ? C23 C22 C31 118.2(2) . . ? C21 C22 C31 123.8(2) . . ? C36 C31 C32 119.2(2) . . ? C36 C31 C22 121.0(2) . . ? C32 C31 C22 119.4(2) . . ? C33 C32 C31 119.2(2) . . ? C33 C32 C37 119.1(2) . . ? C31 C32 C37 121.7(2) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C33 C32 122.4(2) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 117.8(2) . . ? C33 C34 C38 121.3(3) . . ? C35 C34 C38 120.8(3) . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C35 C36 122.1(3) . . ? C34 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C35 C36 C31 119.3(2) . . ? C35 C36 C39 117.8(2) . . ? C31 C36 C39 122.9(2) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C24 C23 C22 122.2(2) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 119.1(2) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 121.2(2) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C21 118.5(2) . . ? C25 C26 C41 119.3(2) . . ? C21 C26 C41 121.9(2) . . ? C46 C41 C42 119.1(2) . . ? C46 C41 C26 122.8(2) . . ? C42 C41 C26 117.9(2) . . ? C43 C42 C41 119.5(2) . . ? C43 C42 C47 118.7(2) . . ? C41 C42 C47 121.7(2) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C43 C44 122.1(3) . . ? C42 C43 H43 119.0 . . ? C44 C43 H43 119.0 . . ? C45 C44 C43 118.0(2) . . ? C45 C44 C48 121.8(3) . . ? C43 C44 C48 120.2(3) . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C45 C46 121.8(2) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? C45 C46 C41 119.4(2) . . ? C45 C46 C49 118.0(2) . . ? C41 C46 C49 122.5(2) . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 P1 C53 104.95(11) . . ? C52 P1 C51 103.62(13) . . ? C53 P1 C51 102.69(11) . . ? C52 P1 W1 122.10(9) . . ? C53 P1 W1 116.99(8) . . ? C51 P1 W1 103.94(9) . . ? P1 C51 H51A 109.5 . . ? P1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? P1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? P1 C52 H52A 109.5 . . ? P1 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? P1 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 118.9(2) . . ? C58 C53 P1 121.91(18) . . ? C54 C53 P1 119.16(18) . . ? C55 C54 C53 120.4(2) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C56 C55 C54 120.1(2) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C57 C56 C55 119.8(2) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C56 C57 C58 120.5(2) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C57 C58 C53 120.3(2) . . ? C57 C58 H58 119.8 . . ? C53 C58 H58 119.8 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S C2S C3S 114.9(3) . . ? C1S C2S H2S1 108.5 . . ? C3S C2S H2S1 108.5 . . ? C1S C2S H2S2 108.5 . . ? C3S C2S H2S2 108.5 . . ? H2S1 C2S H2S2 107.5 . . ? C2S C3S C4S 116.4(3) . . ? C2S C3S H3S1 108.2 . . ? C4S C3S H3S1 108.2 . . ? C2S C3S H3S2 108.2 . . ? C4S C3S H3S2 108.2 . . ? H3S1 C3S H3S2 107.4 . . ? C5S C4S C3S 115.2(3) . . ? C5S C4S H4S1 108.5 . . ? C3S C4S H4S1 108.5 . . ? C5S C4S H4S2 108.5 . . ? C3S C4S H4S2 108.5 . . ? H4S1 C4S H4S2 107.5 . . ? C4S C5S H5S1 109.5 . . ? C4S C5S H5S2 109.5 . . ? H5S1 C5S H5S2 109.5 . . ? C4S C5S H5S3 109.5 . . ? H5S1 C5S H5S3 109.5 . . ? H5S2 C5S H5S3 109.5 . . ? C2T C1T H1T1 109.5 . . ? C2T C1T H1T2 109.5 . . ? H1T1 C1T H1T2 109.5 . . ? C2T C1T H1T3 109.5 . . ? H1T1 C1T H1T3 109.5 . . ? H1T2 C1T H1T3 109.5 . . ? C1T C2T C3T 116.2(10) . . ? C1T C2T H2T1 108.2 . . ? C3T C2T H2T1 108.2 . . ? C1T C2T H2T2 108.2 . . ? C3T C2T H2T2 108.2 . . ? H2T1 C2T H2T2 107.4 . . ? C4T C3T C2T 123.3(10) . . ? C4T C3T H3T1 106.5 . . ? C2T C3T H3T1 106.5 . . ? C4T C3T H3T2 106.5 . . ? C2T C3T H3T2 106.5 . . ? H3T1 C3T H3T2 106.5 . . ? C3T C4T C5T 118.2(11) . . ? C3T C4T H4T1 107.8 . . ? C5T C4T H4T1 107.8 . . ? C3T C4T H4T2 107.8 . . ? C5T C4T H4T2 107.8 . . ? H4T1 C4T H4T2 107.1 . . ? C4T C5T H5T1 109.5 . . ? C4T C5T H5T2 109.5 . . ? H5T1 C5T H5T2 109.5 . . ? C4T C5T H5T3 109.5 . . ? H5T1 C5T H5T3 109.5 . . ? H5T2 C5T H5T3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.589 _refine_diff_density_min -1.184 _refine_diff_density_rms 0.115 #===END data_x11151 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H43 B F15 N O2 W' _chemical_formula_weight 1205.54 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2954(11) _cell_length_b 21.6218(18) _cell_length_c 16.9582(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.976(2) _cell_angle_gamma 90.00 _cell_volume 4863.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9617 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 30.51 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2392 _exptl_absorpt_coefficient_mu 2.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6244 _exptl_absorpt_correction_T_max 0.9184 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 116266 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.32 _reflns_number_total 14569 _reflns_number_gt 11902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2010.7.0 (Bruker-AXS, 2010)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+5.2779P] 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 14569 _refine_ls_number_parameters 672 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.026 _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 0.503728(6) 0.112688(4) 0.254389(5) 0.01664(3) Uani 1 1 d . . . C1 C 0.48390(17) 0.12743(11) 0.36073(14) 0.0231(5) Uani 1 1 d D . . H1 H 0.4262(16) 0.1516(11) 0.3428(15) 0.028 Uiso 1 1 d D . . C2 C 0.51412(18) 0.13033(11) 0.44835(14) 0.0249(5) Uani 1 1 d . . . C3 C 0.58057(19) 0.07487(13) 0.47311(15) 0.0308(5) Uani 1 1 d . . . H3A H 0.5424 0.0365 0.4633 0.046 Uiso 1 1 calc R . . H3B H 0.6016 0.0780 0.5295 0.046 Uiso 1 1 calc R . . H3C H 0.6403 0.0745 0.4424 0.046 Uiso 1 1 calc R . . C4 C 0.4207(2) 0.13028(14) 0.49637(15) 0.0348(6) Uani 1 1 d . . . H4A H 0.3750 0.1635 0.4776 0.052 Uiso 1 1 calc R . . H4B H 0.4412 0.1368 0.5524 0.052 Uiso 1 1 calc R . . H4C H 0.3860 0.0904 0.4899 0.052 Uiso 1 1 calc R . . C5 C 0.5741(3) 0.19014(14) 0.46467(17) 0.0452(8) Uani 1 1 d . . . H5A H 0.6348 0.1896 0.4350 0.068 Uiso 1 1 calc R . . H5B H 0.5935 0.1933 0.5213 0.068 Uiso 1 1 calc R . . H5C H 0.5323 0.2258 0.4481 0.068 Uiso 1 1 calc R . . N1 N 0.39799(13) 0.05167(9) 0.22453(11) 0.0203(4) Uani 1 1 d . . . C6 C 0.31342(18) 0.02445(12) 0.35111(15) 0.0278(5) Uani 1 1 d . . . H6A H 0.2632 -0.0054 0.3672 0.042 Uiso 1 1 calc R . . H6B H 0.2909 0.0665 0.3624 0.042 Uiso 1 1 calc R . . H6C H 0.3782 0.0165 0.3805 0.042 Uiso 1 1 calc R . . C7 C 0.32550(17) 0.01802(11) 0.26464(15) 0.0244(5) Uani 1 1 d . . . C8 C 0.27401(18) -0.01934(12) 0.21134(16) 0.0299(5) Uani 1 1 d . . . H8A H 0.2213 -0.0470 0.2225 0.036 Uiso 1 1 calc R . . C9 C 0.31276(19) -0.00992(12) 0.13567(16) 0.0305(5) Uani 1 1 d . . . H9A H 0.2897 -0.0299 0.0879 0.037 Uiso 1 1 calc R . . C10 C 0.38777(17) 0.03225(11) 0.14367(14) 0.0241(5) Uani 1 1 d . . . C11 C 0.45541(18) 0.05573(12) 0.08374(14) 0.0272(5) Uani 1 1 d . . . H11A H 0.5240 0.0403 0.0962 0.041 Uiso 1 1 calc R . . H11B H 0.4558 0.1010 0.0846 0.041 Uiso 1 1 calc R . . H11C H 0.4309 0.0413 0.0311 0.041 Uiso 1 1 calc R . . O1 O 0.48706(11) 0.18590(7) 0.19734(9) 0.0196(3) Uani 1 1 d . . . C21 C 0.45668(16) 0.24743(10) 0.19145(13) 0.0198(4) Uani 1 1 d . . . C22 C 0.35511(17) 0.26237(11) 0.19757(14) 0.0233(5) Uani 1 1 d . . . C31 C 0.28006(16) 0.21569(11) 0.22158(14) 0.0223(4) Uani 1 1 d . . . C32 C 0.23533(17) 0.17309(11) 0.16767(14) 0.0239(5) Uani 1 1 d . . . C37 C 0.25789(19) 0.17428(13) 0.08135(14) 0.0305(5) Uani 1 1 d . . . H37A H 0.2372 0.1350 0.0565 0.046 Uiso 1 1 calc R . . H37B H 0.3304 0.1804 0.0772 0.046 Uiso 1 1 calc R . . H37C H 0.2206 0.2083 0.0546 0.046 Uiso 1 1 calc R . . C33 C 0.16610(17) 0.13039(11) 0.19460(14) 0.0251(5) Uani 1 1 d . . . H33A H 0.1367 0.1007 0.1587 0.030 Uiso 1 1 calc R . . C34 C 0.13937(16) 0.13034(11) 0.27235(14) 0.0251(5) Uani 1 1 d . . . C38 C 0.06393(19) 0.08469(13) 0.29960(16) 0.0333(6) Uani 1 1 d . . . H38A H -0.0039 0.0968 0.2791 0.050 Uiso 1 1 calc R . . H38B H 0.0671 0.0841 0.3575 0.050 Uiso 1 1 calc R . . H38C H 0.0795 0.0434 0.2800 0.050 Uiso 1 1 calc R . . C35 C 0.18323(17) 0.17369(11) 0.32430(14) 0.0249(5) Uani 1 1 d . . . H35A H 0.1649 0.1742 0.3775 0.030 Uiso 1 1 calc R . . C36 C 0.25378(17) 0.21680(11) 0.30063(14) 0.0235(5) Uani 1 1 d . . . C39 C 0.29910(19) 0.26359(12) 0.35848(15) 0.0300(5) Uani 1 1 d . . . H39A H 0.2712 0.3046 0.3455 0.045 Uiso 1 1 calc R . . H39B H 0.3724 0.2645 0.3555 0.045 Uiso 1 1 calc R . . H39C H 0.2832 0.2522 0.4121 0.045 Uiso 1 1 calc R . . C23 C 0.32738(19) 0.32442(12) 0.18613(16) 0.0314(6) Uani 1 1 d . . . H23A H 0.2588 0.3360 0.1887 0.038 Uiso 1 1 calc R . . C24 C 0.3978(2) 0.36893(12) 0.17120(17) 0.0347(6) Uani 1 1 d . . . H24A H 0.3775 0.4108 0.1637 0.042 Uiso 1 1 calc R . . C25 C 0.4984(2) 0.35277(11) 0.16714(15) 0.0289(5) Uani 1 1 d . . . H25A H 0.5464 0.3838 0.1572 0.035 Uiso 1 1 calc R . . C26 C 0.52983(17) 0.29146(10) 0.17747(13) 0.0219(4) Uani 1 1 d . . . C41 C 0.63876(17) 0.27460(10) 0.17523(14) 0.0216(4) Uani 1 1 d . . . C42 C 0.67589(17) 0.25569(11) 0.10436(14) 0.0241(5) Uani 1 1 d . . . C47 C 0.60580(19) 0.24929(14) 0.03103(15) 0.0337(6) Uani 1 1 d . . . H47A H 0.5475 0.2241 0.0429 0.051 Uiso 1 1 calc R . . H47B H 0.6415 0.2293 -0.0107 0.051 Uiso 1 1 calc R . . H47C H 0.5828 0.2903 0.0132 0.051 Uiso 1 1 calc R . . C43 C 0.77830(18) 0.24214(11) 0.10317(16) 0.0280(5) Uani 1 1 d . . . H43A H 0.8044 0.2304 0.0546 0.034 Uiso 1 1 calc R . . C44 C 0.84324(18) 0.24519(11) 0.17052(17) 0.0291(5) Uani 1 1 d . . . C48 C 0.95335(19) 0.22740(14) 0.1677(2) 0.0406(7) Uani 1 1 d . . . H48A H 0.9583 0.1875 0.1409 0.061 Uiso 1 1 calc R . . H48B H 0.9844 0.2242 0.2216 0.061 Uiso 1 1 calc R . . H48C H 0.9885 0.2591 0.1387 0.061 Uiso 1 1 calc R . . C45 C 0.80420(19) 0.26336(11) 0.24061(16) 0.0293(5) Uani 1 1 d . . . H45A H 0.8476 0.2648 0.2875 0.035 Uiso 1 1 calc R . . C46 C 0.70320(19) 0.27955(11) 0.24420(14) 0.0258(5) Uani 1 1 d . . . C49 C 0.6649(2) 0.30305(14) 0.32053(16) 0.0394(7) Uani 1 1 d . . . H49A H 0.6566 0.3480 0.3176 0.059 Uiso 1 1 calc R . . H49B H 0.7134 0.2926 0.3647 0.059 Uiso 1 1 calc R . . H49C H 0.5998 0.2837 0.3288 0.059 Uiso 1 1 calc R . . O2 O 0.62013(11) 0.07505(7) 0.24762(9) 0.0206(3) Uani 1 1 d . . . B1 B 0.69887(18) 0.02139(11) 0.24149(15) 0.0179(5) Uani 1 1 d . . . C51 C 0.62932(16) -0.03965(10) 0.21952(13) 0.0198(4) Uani 1 1 d . . . C52 C 0.63056(17) -0.07477(11) 0.15082(13) 0.0224(4) Uani 1 1 d . . . F1 F 0.69716(11) -0.06285(7) 0.09565(8) 0.0286(3) Uani 1 1 d . . . C53 C 0.56569(19) -0.12406(11) 0.13335(14) 0.0270(5) Uani 1 1 d . . . F2 F 0.57293(13) -0.15689(7) 0.06667(9) 0.0381(4) Uani 1 1 d . . . C54 C 0.49525(18) -0.13990(11) 0.18546(15) 0.0279(5) Uani 1 1 d . . . F3 F 0.43244(12) -0.18761(7) 0.16928(10) 0.0393(4) Uani 1 1 d . . . C55 C 0.49102(16) -0.10716(10) 0.25481(14) 0.0244(5) Uani 1 1 d . . . F4 F 0.42457(10) -0.12343(7) 0.30769(9) 0.0309(3) Uani 1 1 d . . . C56 C 0.55694(16) -0.05860(10) 0.26975(13) 0.0202(4) Uani 1 1 d . . . F5 F 0.54951(10) -0.02849(6) 0.33919(8) 0.0242(3) Uani 1 1 d . . . C61 C 0.75984(15) 0.02011(10) 0.32900(13) 0.0180(4) Uani 1 1 d . . . C62 C 0.77606(16) -0.03148(10) 0.37710(13) 0.0202(4) Uani 1 1 d . . . F6 F 0.74172(10) -0.08768(6) 0.35348(8) 0.0252(3) Uani 1 1 d . . . C63 C 0.83008(17) -0.02974(11) 0.44980(13) 0.0234(5) Uani 1 1 d . . . F7 F 0.84415(11) -0.08133(7) 0.49344(8) 0.0322(3) Uani 1 1 d . . . C64 C 0.87158(17) 0.02524(12) 0.47691(14) 0.0254(5) Uani 1 1 d . . . F8 F 0.92558(11) 0.02693(8) 0.54722(8) 0.0355(4) Uani 1 1 d . . . C65 C 0.85922(17) 0.07778(11) 0.43176(15) 0.0260(5) Uani 1 1 d . . . F9 F 0.90032(12) 0.13143(7) 0.45710(10) 0.0389(4) Uani 1 1 d . . . C66 C 0.80408(16) 0.07424(10) 0.35919(14) 0.0216(4) Uani 1 1 d . . . F10 F 0.79482(11) 0.12729(6) 0.31700(9) 0.0291(3) Uani 1 1 d . . . C71 C 0.77808(16) 0.03798(10) 0.17561(13) 0.0209(4) Uani 1 1 d . . . C72 C 0.87259(18) 0.00857(11) 0.17784(14) 0.0239(5) Uani 1 1 d . . . F11 F 0.89610(11) -0.03428(7) 0.23445(9) 0.0313(3) Uani 1 1 d . . . C73 C 0.94550(18) 0.01943(12) 0.12545(16) 0.0295(5) Uani 1 1 d . . . F12 F 1.03539(11) -0.00938(8) 0.13391(10) 0.0406(4) Uani 1 1 d . . . C74 C 0.9254(2) 0.06026(12) 0.06413(15) 0.0308(5) Uani 1 1 d . . . F13 F 0.99559(13) 0.07227(8) 0.01328(10) 0.0443(4) Uani 1 1 d . . . C75 C 0.8325(2) 0.08835(11) 0.05588(15) 0.0294(5) Uani 1 1 d . . . F14 F 0.81050(14) 0.12581(7) -0.00633(9) 0.0417(4) Uani 1 1 d . . . C76 C 0.76263(18) 0.07762(11) 0.11136(15) 0.0264(5) Uani 1 1 d . . . F15 F 0.67282(11) 0.10731(7) 0.09873(9) 0.0358(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01431(4) 0.01603(4) 0.01941(4) 0.00380(3) -0.00004(3) 0.00058(3) C1 0.0196(10) 0.0241(11) 0.0255(11) 0.0033(9) 0.0016(9) -0.0009(8) C2 0.0267(12) 0.0269(11) 0.0208(11) 0.0019(9) 0.0005(9) 0.0001(9) C3 0.0271(12) 0.0424(15) 0.0230(12) 0.0051(10) 0.0013(10) 0.0062(11) C4 0.0383(15) 0.0430(15) 0.0238(12) 0.0024(11) 0.0066(11) 0.0109(12) C5 0.066(2) 0.0375(16) 0.0311(15) 0.0009(12) -0.0061(14) -0.0182(15) N1 0.0152(8) 0.0209(9) 0.0241(9) 0.0042(7) -0.0026(7) -0.0012(7) C6 0.0198(11) 0.0330(13) 0.0309(13) 0.0102(10) 0.0033(9) -0.0005(9) C7 0.0170(10) 0.0247(11) 0.0312(12) 0.0077(9) 0.0000(9) -0.0007(8) C8 0.0220(11) 0.0271(12) 0.0398(14) 0.0069(10) -0.0030(10) -0.0063(9) C9 0.0276(12) 0.0294(13) 0.0333(13) -0.0013(10) -0.0078(10) -0.0037(10) C10 0.0220(11) 0.0241(11) 0.0254(11) 0.0033(9) -0.0041(9) 0.0009(9) C11 0.0292(12) 0.0295(12) 0.0224(11) 0.0024(9) -0.0025(9) -0.0011(10) O1 0.0182(7) 0.0159(7) 0.0248(8) 0.0055(6) 0.0017(6) 0.0014(6) C21 0.0209(10) 0.0180(10) 0.0207(10) 0.0040(8) 0.0035(8) 0.0033(8) C22 0.0219(11) 0.0235(11) 0.0251(11) 0.0069(9) 0.0057(9) 0.0039(9) C31 0.0160(10) 0.0238(11) 0.0274(12) 0.0078(9) 0.0037(8) 0.0050(8) C32 0.0176(10) 0.0295(12) 0.0247(11) 0.0077(9) 0.0019(8) 0.0070(9) C37 0.0296(13) 0.0376(14) 0.0246(12) 0.0036(10) 0.0035(10) 0.0040(11) C33 0.0167(10) 0.0302(12) 0.0280(12) 0.0025(9) -0.0023(9) 0.0019(9) C34 0.0144(10) 0.0314(12) 0.0294(12) 0.0087(9) 0.0017(9) 0.0006(8) C38 0.0213(12) 0.0442(15) 0.0344(14) 0.0073(12) 0.0013(10) -0.0075(11) C35 0.0183(10) 0.0315(12) 0.0254(11) 0.0070(9) 0.0040(9) 0.0029(9) C36 0.0182(10) 0.0256(11) 0.0270(12) 0.0034(9) 0.0047(9) 0.0041(8) C39 0.0273(12) 0.0325(13) 0.0306(13) 0.0004(10) 0.0051(10) -0.0004(10) C23 0.0267(12) 0.0262(12) 0.0427(15) 0.0086(11) 0.0122(11) 0.0096(10) C24 0.0396(15) 0.0187(11) 0.0475(16) 0.0084(11) 0.0153(12) 0.0074(10) C25 0.0340(13) 0.0166(11) 0.0373(14) 0.0044(9) 0.0112(11) 0.0007(9) C26 0.0233(11) 0.0194(10) 0.0236(11) 0.0027(8) 0.0049(9) 0.0008(8) C41 0.0214(10) 0.0169(10) 0.0269(11) 0.0050(8) 0.0043(9) -0.0032(8) C42 0.0212(11) 0.0229(11) 0.0282(12) -0.0007(9) 0.0022(9) -0.0028(9) C47 0.0240(12) 0.0489(16) 0.0286(13) -0.0051(12) 0.0035(10) -0.0013(11) C43 0.0230(11) 0.0259(12) 0.0355(14) -0.0022(10) 0.0051(10) -0.0021(9) C44 0.0206(11) 0.0196(11) 0.0467(15) 0.0041(10) -0.0003(10) -0.0010(9) C48 0.0228(13) 0.0353(15) 0.063(2) 0.0024(14) -0.0012(13) 0.0018(11) C45 0.0297(12) 0.0231(11) 0.0338(13) 0.0065(10) -0.0075(10) -0.0059(9) C46 0.0304(12) 0.0217(11) 0.0254(12) 0.0047(9) 0.0017(10) -0.0045(9) C49 0.0450(16) 0.0445(17) 0.0284(14) 0.0003(12) 0.0015(12) -0.0072(13) O2 0.0165(7) 0.0173(7) 0.0275(8) 0.0040(6) -0.0015(6) -0.0004(6) B1 0.0154(10) 0.0159(11) 0.0222(12) 0.0015(9) -0.0011(9) 0.0005(8) C51 0.0171(10) 0.0189(10) 0.0229(11) 0.0031(8) -0.0030(8) -0.0001(8) C52 0.0213(10) 0.0234(11) 0.0220(11) 0.0044(9) -0.0017(8) -0.0024(8) F1 0.0320(8) 0.0308(7) 0.0232(7) -0.0015(6) 0.0038(6) -0.0087(6) C53 0.0323(12) 0.0247(12) 0.0229(11) -0.0011(9) -0.0060(9) -0.0036(9) F2 0.0534(10) 0.0340(8) 0.0264(8) -0.0064(6) -0.0021(7) -0.0158(7) C54 0.0262(12) 0.0229(11) 0.0330(13) 0.0051(10) -0.0089(10) -0.0087(9) F3 0.0404(9) 0.0334(8) 0.0426(9) 0.0023(7) -0.0072(7) -0.0216(7) C55 0.0189(10) 0.0224(10) 0.0315(12) 0.0077(9) -0.0011(9) -0.0034(9) F4 0.0236(7) 0.0304(8) 0.0388(8) 0.0082(6) 0.0042(6) -0.0078(6) C56 0.0183(10) 0.0203(10) 0.0215(10) 0.0025(8) -0.0026(8) 0.0011(8) F5 0.0219(6) 0.0244(7) 0.0266(7) 0.0010(5) 0.0039(5) -0.0012(5) C61 0.0128(9) 0.0202(10) 0.0212(10) -0.0001(8) 0.0021(8) 0.0014(7) C62 0.0155(9) 0.0212(10) 0.0237(11) -0.0015(8) 0.0003(8) 0.0037(8) F6 0.0284(7) 0.0176(6) 0.0286(7) 0.0020(5) -0.0052(6) 0.0025(5) C63 0.0211(11) 0.0280(12) 0.0213(11) 0.0029(9) 0.0014(9) 0.0072(9) F7 0.0370(8) 0.0335(8) 0.0252(7) 0.0075(6) -0.0036(6) 0.0087(6) C64 0.0186(10) 0.0371(13) 0.0200(11) -0.0042(9) -0.0015(8) 0.0041(9) F8 0.0319(8) 0.0496(10) 0.0235(7) -0.0068(7) -0.0090(6) 0.0043(7) C65 0.0210(11) 0.0281(12) 0.0287(12) -0.0067(10) 0.0000(9) -0.0029(9) F9 0.0374(9) 0.0348(8) 0.0428(9) -0.0107(7) -0.0089(7) -0.0109(7) C66 0.0150(9) 0.0220(11) 0.0277(11) 0.0018(9) 0.0009(8) -0.0005(8) F10 0.0280(7) 0.0217(7) 0.0368(8) 0.0033(6) -0.0040(6) -0.0057(5) C71 0.0192(10) 0.0202(10) 0.0227(11) 0.0004(8) -0.0017(8) -0.0051(8) C72 0.0225(11) 0.0274(12) 0.0218(11) -0.0013(9) 0.0007(9) -0.0019(9) F11 0.0277(7) 0.0348(8) 0.0317(8) 0.0048(6) 0.0038(6) 0.0103(6) C73 0.0213(11) 0.0356(13) 0.0319(13) -0.0074(11) 0.0050(10) -0.0013(10) F12 0.0256(8) 0.0537(10) 0.0433(9) -0.0090(8) 0.0083(7) 0.0060(7) C74 0.0343(13) 0.0337(13) 0.0257(12) -0.0070(10) 0.0112(10) -0.0104(11) F13 0.0462(10) 0.0510(10) 0.0385(9) -0.0065(8) 0.0234(8) -0.0155(8) C75 0.0397(14) 0.0239(12) 0.0247(12) 0.0015(9) 0.0025(10) -0.0080(10) F14 0.0611(11) 0.0352(9) 0.0295(8) 0.0093(7) 0.0070(8) -0.0068(8) C76 0.0264(12) 0.0241(11) 0.0283(12) 0.0040(9) -0.0015(9) -0.0027(9) F15 0.0301(8) 0.0366(8) 0.0401(9) 0.0170(7) -0.0022(6) 0.0032(6) _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 1.7594(15) . ? W1 O1 1.8603(14) . ? W1 C1 1.868(2) . ? W1 N1 1.9685(18) . ? W1 H1 2.06(2) . ? C1 C2 1.513(3) . ? C1 H1 0.960(16) . ? C2 C3 1.531(3) . ? C2 C4 1.532(4) . ? C2 C5 1.534(4) . ? 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 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? N1 C7 1.418(3) . ? N1 C10 1.431(3) . ? C6 C7 1.493(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.361(3) . ? C8 C9 1.430(4) . ? C8 H8A 0.9500 . ? C9 C10 1.351(3) . ? C9 H9A 0.9500 . ? C10 C11 1.492(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O1 C21 1.392(2) . ? C21 C26 1.393(3) . ? C21 C22 1.399(3) . ? C22 C23 1.401(3) . ? C22 C31 1.495(3) . ? C31 C32 1.401(3) . ? C31 C36 1.409(3) . ? C32 C33 1.402(3) . ? C32 C37 1.515(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C33 C34 1.389(3) . ? C33 H33A 0.9500 . ? C34 C35 1.387(3) . ? C34 C38 1.503(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C35 C36 1.401(3) . ? C35 H35A 0.9500 . ? C36 C39 1.506(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C23 C24 1.379(4) . ? C23 H23A 0.9500 . ? C24 C25 1.388(4) . ? C24 H24A 0.9500 . ? C25 C26 1.397(3) . ? C25 H25A 0.9500 . ? C26 C41 1.496(3) . ? C41 C42 1.392(3) . ? C41 C46 1.405(3) . ? C42 C43 1.394(3) . ? C42 C47 1.508(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C43 C44 1.385(4) . ? C43 H43A 0.9500 . ? C44 C45 1.386(4) . ? C44 C48 1.518(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C45 C46 1.393(3) . ? C45 H45A 0.9500 . ? C46 C49 1.512(4) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? O2 B1 1.571(3) . ? B1 C71 1.628(3) . ? B1 C51 1.639(3) . ? B1 C61 1.641(3) . ? C51 C56 1.391(3) . ? C51 C52 1.392(3) . ? C52 F1 1.357(3) . ? C52 C53 1.390(3) . ? C53 F2 1.344(3) . ? C53 C54 1.375(4) . ? C54 F3 1.344(3) . ? C54 C55 1.377(3) . ? C55 F4 1.348(3) . ? C55 C56 1.380(3) . ? C56 F5 1.355(3) . ? C61 C62 1.390(3) . ? C61 C66 1.392(3) . ? C62 F6 1.349(2) . ? C62 C63 1.384(3) . ? C63 F7 1.345(3) . ? C63 C64 1.376(3) . ? C64 F8 1.349(2) . ? C64 C65 1.373(3) . ? C65 F9 1.340(3) . ? C65 C66 1.390(3) . ? C66 F10 1.353(3) . ? C71 C76 1.390(3) . ? C71 C72 1.406(3) . ? C72 F11 1.355(3) . ? C72 C73 1.380(3) . ? C73 F12 1.347(3) . ? C73 C74 1.376(4) . ? C74 F13 1.339(3) . ? C74 C75 1.375(4) . ? C75 F14 1.346(3) . ? C75 C76 1.387(4) . ? C76 F15 1.359(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 W1 O1 115.68(7) . . ? O2 W1 C1 109.00(9) . . ? O1 W1 C1 109.70(9) . . ? O2 W1 N1 106.80(7) . . ? O1 W1 N1 112.29(7) . . ? C1 W1 N1 102.51(9) . . ? O2 W1 H1 136.4(5) . . ? O1 W1 H1 89.1(6) . . ? C1 W1 H1 27.8(5) . . ? N1 W1 H1 94.4(7) . . ? C2 C1 W1 155.41(18) . . ? C2 C1 H1 116.1(16) . . ? W1 C1 H1 87.2(16) . . ? C1 C2 C3 110.2(2) . . ? C1 C2 C4 110.6(2) . . ? C3 C2 C4 109.1(2) . . ? C1 C2 C5 108.1(2) . . ? C3 C2 C5 109.1(2) . . ? C4 C2 C5 109.6(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 N1 C10 106.64(18) . . ? C7 N1 W1 135.84(16) . . ? C10 N1 W1 117.49(15) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N1 108.3(2) . . ? C8 C7 C6 128.6(2) . . ? N1 C7 C6 123.1(2) . . ? C7 C8 C9 108.4(2) . . ? C7 C8 H8A 125.8 . . ? C9 C8 H8A 125.8 . . ? C10 C9 C8 108.4(2) . . ? C10 C9 H9A 125.8 . . ? C8 C9 H9A 125.8 . . ? C9 C10 N1 108.3(2) . . ? C9 C10 C11 129.6(2) . . ? N1 C10 C11 122.1(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C21 O1 W1 150.93(14) . . ? O1 C21 C26 117.58(19) . . ? O1 C21 C22 119.47(19) . . ? C26 C21 C22 122.9(2) . . ? C21 C22 C23 117.2(2) . . ? C21 C22 C31 122.0(2) . . ? C23 C22 C31 120.6(2) . . ? C32 C31 C36 120.7(2) . . ? C32 C31 C22 121.8(2) . . ? C36 C31 C22 117.5(2) . . ? C31 C32 C33 118.6(2) . . ? C31 C32 C37 121.1(2) . . ? C33 C32 C37 120.3(2) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C33 C32 121.8(2) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? C35 C34 C33 118.6(2) . . ? C35 C34 C38 120.6(2) . . ? C33 C34 C38 120.8(2) . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C35 C36 121.9(2) . . ? C34 C35 H35A 119.1 . . ? C36 C35 H35A 119.1 . . ? C35 C36 C31 118.5(2) . . ? C35 C36 C39 120.4(2) . . ? C31 C36 C39 121.1(2) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C24 C23 C22 121.2(2) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C26 120.9(2) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C21 C26 C25 117.6(2) . . ? C21 C26 C41 121.75(19) . . ? C25 C26 C41 120.6(2) . . ? C42 C41 C46 120.6(2) . . ? C42 C41 C26 119.7(2) . . ? C46 C41 C26 119.7(2) . . ? C41 C42 C43 118.7(2) . . ? C41 C42 C47 120.2(2) . . ? C43 C42 C47 121.1(2) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C43 C42 122.1(2) . . ? C44 C43 H43A 118.9 . . ? C42 C43 H43A 118.9 . . ? C43 C44 C45 118.1(2) . . ? C43 C44 C48 120.6(3) . . ? C45 C44 C48 121.2(2) . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 C45 C46 121.9(2) . . ? C44 C45 H45A 119.1 . . ? C46 C45 H45A 119.1 . . ? C45 C46 C41 118.6(2) . . ? C45 C46 C49 120.3(2) . . ? C41 C46 C49 121.1(2) . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? B1 O2 W1 159.91(13) . . ? O2 B1 C71 110.40(17) . . ? O2 B1 C51 103.99(16) . . ? C71 B1 C51 113.77(19) . . ? O2 B1 C61 104.01(17) . . ? C71 B1 C61 108.77(17) . . ? C51 B1 C61 115.30(18) . . ? C56 C51 C52 113.6(2) . . ? C56 C51 B1 120.1(2) . . ? C52 C51 B1 126.2(2) . . ? F1 C52 C53 115.1(2) . . ? F1 C52 C51 121.31(19) . . ? C53 C52 C51 123.6(2) . . ? F2 C53 C54 120.1(2) . . ? F2 C53 C52 120.3(2) . . ? C54 C53 C52 119.6(2) . . ? F3 C54 C53 120.1(2) . . ? F3 C54 C55 120.5(2) . . ? C53 C54 C55 119.4(2) . . ? F4 C55 C54 120.1(2) . . ? F4 C55 C56 120.9(2) . . ? C54 C55 C56 119.0(2) . . ? F5 C56 C55 116.2(2) . . ? F5 C56 C51 119.07(19) . . ? C55 C56 C51 124.7(2) . . ? C62 C61 C66 114.5(2) . . ? C62 C61 B1 126.23(19) . . ? C66 C61 B1 119.22(19) . . ? F6 C62 C63 115.7(2) . . ? F6 C62 C61 120.87(19) . . ? C63 C62 C61 123.4(2) . . ? F7 C63 C64 119.7(2) . . ? F7 C63 C62 120.8(2) . . ? C64 C63 C62 119.5(2) . . ? F8 C64 C65 120.4(2) . . ? F8 C64 C63 119.7(2) . . ? C65 C64 C63 119.9(2) . . ? F9 C65 C64 120.4(2) . . ? F9 C65 C66 120.6(2) . . ? C64 C65 C66 118.9(2) . . ? F10 C66 C65 116.4(2) . . ? F10 C66 C61 119.86(19) . . ? C65 C66 C61 123.7(2) . . ? C76 C71 C72 112.5(2) . . ? C76 C71 B1 127.3(2) . . ? C72 C71 B1 120.09(19) . . ? F11 C72 C73 115.8(2) . . ? F11 C72 C71 119.3(2) . . ? C73 C72 C71 124.9(2) . . ? F12 C73 C74 120.1(2) . . ? F12 C73 C72 120.7(2) . . ? C74 C73 C72 119.2(2) . . ? F13 C74 C75 120.7(2) . . ? F13 C74 C73 120.3(2) . . ? C75 C74 C73 119.1(2) . . ? F14 C75 C74 119.4(2) . . ? F14 C75 C76 120.8(2) . . ? C74 C75 C76 119.8(2) . . ? F15 C76 C75 115.9(2) . . ? F15 C76 C71 119.7(2) . . ? C75 C76 C71 124.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.800 _refine_diff_density_min -1.005 _refine_diff_density_rms 0.086