data_pl323 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H35 N O W' _chemical_formula_sum 'C24 H35 N O W' _chemical_formula_weight 537.38 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 'P21/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 12.7252(6) _cell_length_b 11.7231(5) _cell_length_c 15.2438(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.146(2) _cell_angle_gamma 90.00 _cell_volume 2223.15(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.9 _exptl_crystal_description rod _exptl_crystal_colour 'yellow orange' _exptl_crystal_size_max 1.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 5.209 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.594 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27675 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.87 _reflns_number_total 5262 _reflns_number_gt 4639 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR-92' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _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^)+(0.0373P)^2^+1.4463P] 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 5262 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.249465(8) 0.209581(9) 0.941712(8) 0.01516(5) Uani 1 1 d . . . N1 N -0.2319(2) 0.28811(18) 0.84652(19) 0.0174(5) Uani 1 1 d . . . C12 C -0.3326(3) 0.5319(3) 0.8875(3) 0.0358(9) Uani 1 1 d . . . H12A H -0.3123 0.6107 0.8772 0.054 Uiso 1 1 calc R . . H12B H -0.4102 0.5281 0.8846 0.054 Uiso 1 1 calc R . . H12C H -0.3141 0.4823 0.8413 0.054 Uiso 1 1 calc R . . C3 C -0.0803(2) 0.1323(3) 0.9558(2) 0.0199(6) Uani 1 1 d . . . C16 C -0.3049(2) 0.0114(3) 0.9227(2) 0.0234(7) Uani 1 1 d . . . O1 O -0.2278(2) 0.3278(2) 0.77313(17) 0.0358(6) Uani 1 1 d . . . C1 C -0.1276(3) 0.2282(3) 1.0841(2) 0.0225(7) Uani 1 1 d . . . C18 C -0.4272(2) 0.1580(3) 0.8846(2) 0.0230(7) Uani 1 1 d . . . C2 C -0.0698(3) 0.2256(3) 1.0181(2) 0.0216(7) Uani 1 1 d . . . C4 C -0.0238(2) 0.1338(3) 0.8792(2) 0.0203(6) Uani 1 1 d . . . C19 C -0.4121(2) 0.1382(3) 0.9791(2) 0.0215(6) Uani 1 1 d . . . C15 C -0.3360(2) 0.0486(3) 1.0022(2) 0.0211(6) Uani 1 1 d . . . C13 C -0.3033(3) 0.5727(3) 1.0509(3) 0.0391(9) Uani 1 1 d . . . H13A H -0.2911 0.6521 1.0355 0.059 Uiso 1 1 calc R . . H13B H -0.2592 0.5550 1.1102 0.059 Uiso 1 1 calc R . . H13C H -0.3794 0.5619 1.0520 0.059 Uiso 1 1 calc R . . C17 C -0.3592(3) 0.0793(3) 0.8501(2) 0.0236(7) Uani 1 1 d . . . C10 C -0.3079(2) 0.3693(3) 1.0001(2) 0.0208(6) Uani 1 1 d . . . H10A H -0.3874 0.3681 0.9825 0.025 Uiso 1 1 calc R . . H10B H -0.2895 0.3601 1.0662 0.025 Uiso 1 1 calc R . . C11 C -0.2722(3) 0.4925(3) 0.9801(2) 0.0232(7) Uani 1 1 d . . . C5 C -0.0102(2) 0.0331(3) 0.8335(2) 0.0260(7) Uani 1 1 d . . . H5 H -0.0390 -0.0362 0.8507 0.031 Uiso 1 1 calc R . . C14 C -0.1509(3) 0.5053(3) 0.9861(3) 0.0275(7) Uani 1 1 d . . . H14A H -0.1295 0.4593 0.9391 0.041 Uiso 1 1 calc R . . H14B H -0.1119 0.4792 1.0451 0.041 Uiso 1 1 calc R . . H14C H -0.1339 0.5856 0.9780 0.041 Uiso 1 1 calc R . . C24 C -0.4730(3) 0.1900(3) 1.0442(3) 0.0359(9) Uani 1 1 d . . . H24A H -0.5246 0.1342 1.0581 0.054 Uiso 1 1 calc R . . H24B H -0.5117 0.2579 1.0173 0.054 Uiso 1 1 calc R . . H24C H -0.4224 0.2113 1.0995 0.054 Uiso 1 1 calc R . . C6 C 0.0443(3) 0.0321(3) 0.7636(2) 0.0320(8) Uani 1 1 d . . . H6 H 0.0520 -0.0376 0.7337 0.038 Uiso 1 1 calc R . . C23 C -0.5063(3) 0.2390(4) 0.8279(3) 0.0372(9) Uani 1 1 d . . . H23A H -0.5686 0.1959 0.7957 0.056 Uiso 1 1 calc R . . H23B H -0.4714 0.2776 0.7846 0.056 Uiso 1 1 calc R . . H23C H -0.5300 0.2958 0.8667 0.056 Uiso 1 1 calc R . . C20 C -0.3050(3) -0.0075(3) 1.0929(3) 0.0387(9) Uani 1 1 d . . . H20A H -0.3007 0.0503 1.1400 0.058 Uiso 1 1 calc R . . H20B H -0.2349 -0.0447 1.0986 0.058 Uiso 1 1 calc R . . H20C H -0.3592 -0.0646 1.0991 0.058 Uiso 1 1 calc R . . C22 C -0.3543(3) 0.0655(4) 0.7531(2) 0.0402(9) Uani 1 1 d . . . H22A H -0.2803 0.0481 0.7485 0.060 Uiso 1 1 calc R . . H22B H -0.3776 0.1364 0.7208 0.060 Uiso 1 1 calc R . . H22C H -0.4017 0.0029 0.7269 0.060 Uiso 1 1 calc R . . C8 C 0.0750(3) 0.2323(3) 0.7815(3) 0.0310(8) Uani 1 1 d . . . H8 H 0.1046 0.3011 0.7644 0.037 Uiso 1 1 calc R . . C9 C 0.0198(3) 0.2338(3) 0.8508(3) 0.0274(7) Uani 1 1 d . . . H9 H 0.0112 0.3040 0.8796 0.033 Uiso 1 1 calc R . . C7 C 0.0876(3) 0.1315(3) 0.7366(2) 0.0330(8) Uani 1 1 d . . . H7 H 0.1249 0.1308 0.6888 0.040 Uiso 1 1 calc R . . C21 C -0.2399(3) -0.0932(3) 0.9135(3) 0.0404(9) Uani 1 1 d . . . H21A H -0.2869 -0.1603 0.9055 0.061 Uiso 1 1 calc R . . H21B H -0.1835 -0.1026 0.9677 0.061 Uiso 1 1 calc R . . H21C H -0.2069 -0.0848 0.8613 0.061 Uiso 1 1 calc R . . H1A H -0.154(2) 0.163(3) 1.110(2) 0.012(8) Uiso 1 1 d . . . H3 H -0.083(2) 0.054(3) 0.980(2) 0.014(8) Uiso 1 1 d . . . H2 H -0.034(3) 0.295(3) 1.001(3) 0.017(9) Uiso 1 1 d . . . H1B H -0.125(3) 0.292(3) 1.123(3) 0.034(12) Uiso 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 0.01527(7) 0.01546(8) 0.01530(8) -0.00009(4) 0.00445(5) -0.00110(4) N1 0.0185(12) 0.0146(12) 0.0183(15) 0.0020(10) 0.0019(11) 0.0000(9) C12 0.0370(19) 0.0288(19) 0.039(2) 0.0069(16) 0.0034(17) 0.0032(15) C3 0.0167(13) 0.0187(14) 0.0235(17) 0.0006(13) 0.0026(12) 0.0009(11) C16 0.0219(15) 0.0158(14) 0.0326(19) -0.0042(13) 0.0059(13) -0.0063(11) O1 0.0415(14) 0.0443(14) 0.0239(14) 0.0111(12) 0.0124(11) 0.0055(12) C1 0.0222(15) 0.0278(17) 0.0173(17) -0.0016(14) 0.0035(13) -0.0016(13) C18 0.0156(13) 0.0241(16) 0.0275(18) 0.0001(13) 0.0007(12) -0.0059(12) C2 0.0150(14) 0.0242(16) 0.0237(18) 0.0007(13) -0.0005(13) -0.0004(12) C4 0.0165(13) 0.0231(15) 0.0212(16) 0.0012(13) 0.0038(12) 0.0040(12) C19 0.0197(14) 0.0247(16) 0.0225(17) -0.0024(13) 0.0100(12) -0.0090(12) C15 0.0237(14) 0.0224(15) 0.0174(16) -0.0003(13) 0.0047(12) -0.0098(12) C13 0.052(2) 0.0207(17) 0.051(3) -0.0032(16) 0.026(2) -0.0012(16) C17 0.0245(15) 0.0280(16) 0.0185(16) -0.0054(13) 0.0053(13) -0.0105(13) C10 0.0228(14) 0.0203(14) 0.0227(17) -0.0013(13) 0.0124(12) -0.0036(12) C11 0.0259(15) 0.0192(15) 0.0263(18) 0.0001(13) 0.0092(14) 0.0000(12) C5 0.0233(15) 0.0243(16) 0.0301(19) -0.0013(14) 0.0050(14) 0.0017(12) C14 0.0255(16) 0.0220(16) 0.036(2) -0.0002(14) 0.0090(15) -0.0042(13) C24 0.036(2) 0.0327(19) 0.046(3) -0.0113(17) 0.0241(19) -0.0131(15) C6 0.0348(18) 0.037(2) 0.0255(19) -0.0064(15) 0.0087(15) 0.0064(15) C23 0.0255(18) 0.039(2) 0.042(2) 0.0096(19) -0.0047(16) -0.0021(16) C20 0.043(2) 0.037(2) 0.031(2) 0.0107(16) -0.0036(17) -0.0177(17) C22 0.049(2) 0.051(2) 0.023(2) -0.0145(17) 0.0130(17) -0.0146(19) C8 0.0331(19) 0.0358(19) 0.028(2) 0.0086(16) 0.0140(16) 0.0031(15) C9 0.0292(17) 0.0214(15) 0.033(2) -0.0001(14) 0.0091(15) 0.0009(13) C7 0.0295(17) 0.046(2) 0.0251(19) 0.0021(16) 0.0101(14) 0.0091(16) C21 0.0348(19) 0.0226(17) 0.067(3) -0.0087(18) 0.0190(19) -0.0039(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 N1 1.772(3) . ? W1 C10 2.265(3) . ? W1 C3 2.304(3) . ? W1 C18 2.326(3) . ? W1 C17 2.327(3) . ? W1 C2 2.345(3) . ? W1 C1 2.397(3) . ? W1 C19 2.410(3) . ? W1 C16 2.428(3) . ? W1 C15 2.460(3) . ? N1 O1 1.223(4) . ? C12 C11 1.530(5) . ? C3 C2 1.437(5) . ? C3 C4 1.494(4) . ? C16 C17 1.420(5) . ? C16 C15 1.420(5) . ? C16 C21 1.502(5) . ? C1 C2 1.365(5) . ? C18 C19 1.432(5) . ? C18 C17 1.439(5) . ? C18 C23 1.516(5) . ? C4 C5 1.400(4) . ? C4 C9 1.404(5) . ? C19 C15 1.422(5) . ? C19 C24 1.509(5) . ? C15 C20 1.507(5) . ? C13 C11 1.545(5) . ? C17 C22 1.501(5) . ? C10 C11 1.564(4) . ? C11 C14 1.534(4) . ? C5 C6 1.389(5) . ? C6 C7 1.388(5) . ? C8 C9 1.386(5) . ? C8 C7 1.391(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W1 C10 90.06(11) . . ? N1 W1 C3 90.25(12) . . ? C10 W1 C3 131.78(11) . . ? N1 W1 C18 96.26(12) . . ? C10 W1 C18 89.31(11) . . ? C3 W1 C18 138.48(12) . . ? N1 W1 C17 90.72(11) . . ? C10 W1 C17 125.00(12) . . ? C3 W1 C17 103.21(11) . . ? C18 W1 C17 36.04(12) . . ? N1 W1 C2 95.00(12) . . ? C10 W1 C2 96.02(11) . . ? C3 W1 C2 35.99(11) . . ? C18 W1 C2 167.54(11) . . ? C17 W1 C2 138.59(12) . . ? N1 W1 C1 121.66(12) . . ? C10 W1 C1 76.83(12) . . ? C3 W1 C1 62.45(12) . . ? C18 W1 C1 139.06(12) . . ? C17 W1 C1 142.71(12) . . ? C2 W1 C1 33.44(12) . . ? N1 W1 C19 129.56(11) . . ? C10 W1 C19 79.89(10) . . ? C3 W1 C19 132.35(11) . . ? C18 W1 C19 35.13(11) . . ? C17 W1 C19 58.50(11) . . ? C2 W1 C19 134.97(12) . . ? C1 W1 C19 103.99(11) . . ? N1 W1 C16 118.88(11) . . ? C10 W1 C16 136.62(11) . . ? C3 W1 C16 82.93(11) . . ? C18 W1 C16 58.09(11) . . ? C17 W1 C16 34.66(12) . . ? C2 W1 C16 111.38(11) . . ? C1 W1 C16 108.16(12) . . ? C19 W1 C16 56.87(11) . . ? N1 W1 C15 148.12(11) . . ? C10 W1 C15 106.07(11) . . ? C3 W1 C15 98.42(11) . . ? C18 W1 C15 57.60(11) . . ? C17 W1 C15 57.46(11) . . ? C2 W1 C15 110.00(11) . . ? C1 W1 C15 89.19(11) . . ? C19 W1 C15 33.94(11) . . ? C16 W1 C15 33.78(11) . . ? O1 N1 W1 169.7(2) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 W1 73.56(17) . . ? C4 C3 W1 121.1(2) . . ? C17 C16 C15 108.4(3) . . ? C17 C16 C21 124.9(3) . . ? C15 C16 C21 126.0(3) . . ? C17 C16 W1 68.77(17) . . ? C15 C16 W1 74.34(17) . . ? C21 C16 W1 129.8(2) . . ? C2 C1 W1 71.17(19) . . ? C19 C18 C17 107.5(3) . . ? C19 C18 C23 127.5(3) . . ? C17 C18 C23 124.8(3) . . ? C19 C18 W1 75.64(17) . . ? C17 C18 W1 72.02(17) . . ? C23 C18 W1 121.8(2) . . ? C1 C2 C3 120.9(3) . . ? C1 C2 W1 75.39(19) . . ? C3 C2 W1 70.45(17) . . ? C5 C4 C9 116.9(3) . . ? C5 C4 C3 120.6(3) . . ? C9 C4 C3 122.5(3) . . ? C15 C19 C18 108.0(3) . . ? C15 C19 C24 123.5(3) . . ? C18 C19 C24 128.1(3) . . ? C15 C19 W1 74.96(17) . . ? C18 C19 W1 69.22(16) . . ? C24 C19 W1 127.0(2) . . ? C16 C15 C19 108.3(3) . . ? C16 C15 C20 125.6(3) . . ? C19 C15 C20 125.6(3) . . ? C16 C15 W1 71.88(17) . . ? C19 C15 W1 71.10(17) . . ? C20 C15 W1 128.9(2) . . ? C16 C17 C18 107.8(3) . . ? C16 C17 C22 126.4(3) . . ? C18 C17 C22 125.6(3) . . ? C16 C17 W1 76.57(18) . . ? C18 C17 W1 71.94(17) . . ? C22 C17 W1 121.2(2) . . ? C11 C10 W1 123.6(2) . . ? C12 C11 C14 109.3(3) . . ? C12 C11 C13 107.9(3) . . ? C14 C11 C13 107.5(3) . . ? C12 C11 C10 110.4(3) . . ? C14 C11 C10 114.2(3) . . ? C13 C11 C10 107.3(3) . . ? C6 C5 C4 121.5(3) . . ? C7 C6 C5 120.9(3) . . ? C9 C8 C7 121.0(3) . . ? C8 C9 C4 121.4(3) . . ? C6 C7 C8 118.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 W1 N1 O1 -134.6(13) . . . . ? C3 W1 N1 O1 93.7(13) . . . . ? C18 W1 N1 O1 -45.3(13) . . . . ? C17 W1 N1 O1 -9.6(13) . . . . ? C2 W1 N1 O1 129.4(13) . . . . ? C1 W1 N1 O1 150.9(13) . . . . ? C19 W1 N1 O1 -57.7(14) . . . . ? C16 W1 N1 O1 11.6(14) . . . . ? C15 W1 N1 O1 -12.9(14) . . . . ? N1 W1 C3 C2 98.2(2) . . . . ? C10 W1 C3 C2 7.9(3) . . . . ? C18 W1 C3 C2 -162.1(2) . . . . ? C17 W1 C3 C2 -171.03(19) . . . . ? C1 W1 C3 C2 -27.97(19) . . . . ? C19 W1 C3 C2 -111.8(2) . . . . ? C16 W1 C3 C2 -142.7(2) . . . . ? C15 W1 C3 C2 -112.6(2) . . . . ? N1 W1 C3 C4 -18.5(2) . . . . ? C10 W1 C3 C4 -108.8(3) . . . . ? C18 W1 C3 C4 81.3(3) . . . . ? C17 W1 C3 C4 72.3(3) . . . . ? C2 W1 C3 C4 -116.6(3) . . . . ? C1 W1 C3 C4 -144.6(3) . . . . ? C19 W1 C3 C4 131.5(2) . . . . ? C16 W1 C3 C4 100.6(3) . . . . ? C15 W1 C3 C4 130.8(2) . . . . ? N1 W1 C16 C17 -39.4(2) . . . . ? C10 W1 C16 C17 86.4(2) . . . . ? C3 W1 C16 C17 -125.8(2) . . . . ? C18 W1 C16 C17 39.25(19) . . . . ? C2 W1 C16 C17 -148.22(19) . . . . ? C1 W1 C16 C17 176.33(19) . . . . ? C19 W1 C16 C17 81.2(2) . . . . ? C15 W1 C16 C17 117.5(3) . . . . ? N1 W1 C16 C15 -156.85(18) . . . . ? C10 W1 C16 C15 -31.0(3) . . . . ? C3 W1 C16 C15 116.8(2) . . . . ? C18 W1 C16 C15 -78.2(2) . . . . ? C17 W1 C16 C15 -117.5(3) . . . . ? C2 W1 C16 C15 94.3(2) . . . . ? C1 W1 C16 C15 58.9(2) . . . . ? C19 W1 C16 C15 -36.28(18) . . . . ? N1 W1 C16 C21 79.0(4) . . . . ? C10 W1 C16 C21 -155.2(3) . . . . ? C3 W1 C16 C21 -7.4(4) . . . . ? C18 W1 C16 C21 157.6(4) . . . . ? C17 W1 C16 C21 118.4(4) . . . . ? C2 W1 C16 C21 -29.9(4) . . . . ? C1 W1 C16 C21 -65.3(4) . . . . ? C19 W1 C16 C21 -160.5(4) . . . . ? C15 W1 C16 C21 -124.2(4) . . . . ? N1 W1 C1 C2 -41.6(2) . . . . ? C10 W1 C1 C2 -123.3(2) . . . . ? C3 W1 C1 C2 30.00(19) . . . . ? C18 W1 C1 C2 163.42(19) . . . . ? C17 W1 C1 C2 105.0(2) . . . . ? C19 W1 C1 C2 160.8(2) . . . . ? C16 W1 C1 C2 101.5(2) . . . . ? C15 W1 C1 C2 129.9(2) . . . . ? N1 W1 C18 C19 -163.24(19) . . . . ? C10 W1 C18 C19 -73.26(19) . . . . ? C3 W1 C18 C19 99.3(2) . . . . ? C17 W1 C18 C19 114.2(3) . . . . ? C2 W1 C18 C19 42.3(6) . . . . ? C1 W1 C18 C19 -4.5(3) . . . . ? C16 W1 C18 C19 76.5(2) . . . . ? C15 W1 C18 C19 36.34(18) . . . . ? N1 W1 C18 C17 82.6(2) . . . . ? C10 W1 C18 C17 172.6(2) . . . . ? C3 W1 C18 C17 -14.9(3) . . . . ? C2 W1 C18 C17 -71.9(6) . . . . ? C1 W1 C18 C17 -118.6(2) . . . . ? C19 W1 C18 C17 -114.2(3) . . . . ? C16 W1 C18 C17 -37.71(19) . . . . ? C15 W1 C18 C17 -77.8(2) . . . . ? N1 W1 C18 C23 -37.8(3) . . . . ? C10 W1 C18 C23 52.2(3) . . . . ? C3 W1 C18 C23 -135.3(3) . . . . ? C17 W1 C18 C23 -120.3(4) . . . . ? C2 W1 C18 C23 167.8(5) . . . . ? C1 W1 C18 C23 121.0(3) . . . . ? C19 W1 C18 C23 125.5(4) . . . . ? C16 W1 C18 C23 -158.0(3) . . . . ? C15 W1 C18 C23 161.8(3) . . . . ? W1 C1 C2 C3 -56.0(3) . . . . ? C4 C3 C2 C1 175.1(3) . . . . ? W1 C3 C2 C1 58.3(3) . . . . ? C4 C3 C2 W1 116.8(3) . . . . ? N1 W1 C2 C1 145.5(2) . . . . ? C10 W1 C2 C1 54.9(2) . . . . ? C3 W1 C2 C1 -131.0(3) . . . . ? C18 W1 C2 C1 -60.0(6) . . . . ? C17 W1 C2 C1 -117.8(2) . . . . ? C19 W1 C2 C1 -26.8(3) . . . . ? C16 W1 C2 C1 -90.8(2) . . . . ? C15 W1 C2 C1 -54.7(2) . . . . ? N1 W1 C2 C3 -83.5(2) . . . . ? C10 W1 C2 C3 -174.10(19) . . . . ? C18 W1 C2 C3 71.0(6) . . . . ? C17 W1 C2 C3 13.3(3) . . . . ? C1 W1 C2 C3 131.0(3) . . . . ? C19 W1 C2 C3 104.2(2) . . . . ? C16 W1 C2 C3 40.2(2) . . . . ? C15 W1 C2 C3 76.4(2) . . . . ? C2 C3 C4 C5 162.9(3) . . . . ? W1 C3 C4 C5 -108.5(3) . . . . ? C2 C3 C4 C9 -15.7(4) . . . . ? W1 C3 C4 C9 72.9(4) . . . . ? C17 C18 C19 C15 0.0(3) . . . . ? C23 C18 C19 C15 175.2(3) . . . . ? W1 C18 C19 C15 -65.5(2) . . . . ? C17 C18 C19 C24 -173.2(3) . . . . ? C23 C18 C19 C24 2.0(5) . . . . ? W1 C18 C19 C24 121.4(3) . . . . ? C17 C18 C19 W1 65.5(2) . . . . ? C23 C18 C19 W1 -119.3(3) . . . . ? N1 W1 C19 C15 138.17(18) . . . . ? C10 W1 C19 C15 -140.2(2) . . . . ? C3 W1 C19 C15 -1.4(3) . . . . ? C18 W1 C19 C15 116.3(3) . . . . ? C17 W1 C19 C15 77.3(2) . . . . ? C2 W1 C19 C15 -51.8(2) . . . . ? C1 W1 C19 C15 -66.7(2) . . . . ? C16 W1 C19 C15 36.11(18) . . . . ? N1 W1 C19 C18 21.8(2) . . . . ? C10 W1 C19 C18 103.4(2) . . . . ? C3 W1 C19 C18 -117.7(2) . . . . ? C17 W1 C19 C18 -39.01(19) . . . . ? C2 W1 C19 C18 -168.15(18) . . . . ? C1 W1 C19 C18 176.99(19) . . . . ? C16 W1 C19 C18 -80.2(2) . . . . ? C15 W1 C19 C18 -116.3(3) . . . . ? N1 W1 C19 C24 -101.0(3) . . . . ? C10 W1 C19 C24 -19.4(3) . . . . ? C3 W1 C19 C24 119.5(3) . . . . ? C18 W1 C19 C24 -122.8(4) . . . . ? C17 W1 C19 C24 -161.8(4) . . . . ? C2 W1 C19 C24 69.1(4) . . . . ? C1 W1 C19 C24 54.2(3) . . . . ? C16 W1 C19 C24 157.0(4) . . . . ? C15 W1 C19 C24 120.9(4) . . . . ? C17 C16 C15 C19 1.5(3) . . . . ? C21 C16 C15 C19 -169.6(3) . . . . ? W1 C16 C15 C19 62.2(2) . . . . ? C17 C16 C15 C20 174.0(3) . . . . ? C21 C16 C15 C20 2.9(5) . . . . ? W1 C16 C15 C20 -125.3(3) . . . . ? C17 C16 C15 W1 -60.7(2) . . . . ? C21 C16 C15 W1 128.2(3) . . . . ? C18 C19 C15 C16 -0.9(3) . . . . ? C24 C19 C15 C16 172.6(3) . . . . ? W1 C19 C15 C16 -62.7(2) . . . . ? C18 C19 C15 C20 -173.5(3) . . . . ? C24 C19 C15 C20 0.1(5) . . . . ? W1 C19 C15 C20 124.8(3) . . . . ? C18 C19 C15 W1 61.7(2) . . . . ? C24 C19 C15 W1 -124.7(3) . . . . ? N1 W1 C15 C16 40.7(3) . . . . ? C10 W1 C15 C16 158.39(19) . . . . ? C3 W1 C15 C16 -63.6(2) . . . . ? C18 W1 C15 C16 79.8(2) . . . . ? C17 W1 C15 C16 36.77(18) . . . . ? C2 W1 C15 C16 -98.8(2) . . . . ? C1 W1 C15 C16 -125.6(2) . . . . ? C19 W1 C15 C16 117.4(3) . . . . ? N1 W1 C15 C19 -76.8(3) . . . . ? C10 W1 C15 C19 41.0(2) . . . . ? C3 W1 C15 C19 178.98(19) . . . . ? C18 W1 C15 C19 -37.65(18) . . . . ? C17 W1 C15 C19 -80.7(2) . . . . ? C2 W1 C15 C19 143.72(19) . . . . ? C1 W1 C15 C19 117.00(19) . . . . ? C16 W1 C15 C19 -117.4(3) . . . . ? N1 W1 C15 C20 162.3(3) . . . . ? C10 W1 C15 C20 -80.0(3) . . . . ? C3 W1 C15 C20 58.0(3) . . . . ? C18 W1 C15 C20 -158.6(4) . . . . ? C17 W1 C15 C20 158.4(4) . . . . ? C2 W1 C15 C20 22.7(4) . . . . ? C1 W1 C15 C20 -4.0(3) . . . . ? C19 W1 C15 C20 -121.0(4) . . . . ? C16 W1 C15 C20 121.6(4) . . . . ? C15 C16 C17 C18 -1.5(3) . . . . ? C21 C16 C17 C18 169.8(3) . . . . ? W1 C16 C17 C18 -65.7(2) . . . . ? C15 C16 C17 C22 -176.7(3) . . . . ? C21 C16 C17 C22 -5.5(5) . . . . ? W1 C16 C17 C22 119.0(3) . . . . ? C15 C16 C17 W1 64.2(2) . . . . ? C21 C16 C17 W1 -124.5(3) . . . . ? C19 C18 C17 C16 0.9(3) . . . . ? C23 C18 C17 C16 -174.4(3) . . . . ? W1 C18 C17 C16 68.8(2) . . . . ? C19 C18 C17 C22 176.2(3) . . . . ? C23 C18 C17 C22 0.9(5) . . . . ? W1 C18 C17 C22 -115.9(3) . . . . ? C19 C18 C17 W1 -67.9(2) . . . . ? C23 C18 C17 W1 116.7(3) . . . . ? N1 W1 C17 C16 146.2(2) . . . . ? C10 W1 C17 C16 -123.19(19) . . . . ? C3 W1 C17 C16 55.8(2) . . . . ? C18 W1 C17 C16 -114.1(3) . . . . ? C2 W1 C17 C16 47.9(3) . . . . ? C1 W1 C17 C16 -5.8(3) . . . . ? C19 W1 C17 C16 -76.1(2) . . . . ? C15 W1 C17 C16 -35.82(18) . . . . ? N1 W1 C17 C18 -99.7(2) . . . . ? C10 W1 C17 C18 -9.1(2) . . . . ? C3 W1 C17 C18 169.90(19) . . . . ? C2 W1 C17 C18 161.9(2) . . . . ? C1 W1 C17 C18 108.3(2) . . . . ? C19 W1 C17 C18 38.01(19) . . . . ? C16 W1 C17 C18 114.1(3) . . . . ? C15 W1 C17 C18 78.3(2) . . . . ? N1 W1 C17 C22 21.6(3) . . . . ? C10 W1 C17 C22 112.2(3) . . . . ? C3 W1 C17 C22 -68.8(3) . . . . ? C18 W1 C17 C22 121.3(4) . . . . ? C2 W1 C17 C22 -76.8(3) . . . . ? C1 W1 C17 C22 -130.4(3) . . . . ? C19 W1 C17 C22 159.3(3) . . . . ? C16 W1 C17 C22 -124.6(4) . . . . ? C15 W1 C17 C22 -160.5(3) . . . . ? N1 W1 C10 C11 -28.4(3) . . . . ? C3 W1 C10 C11 62.0(3) . . . . ? C18 W1 C10 C11 -124.7(3) . . . . ? C17 W1 C10 C11 -119.3(2) . . . . ? C2 W1 C10 C11 66.6(3) . . . . ? C1 W1 C10 C11 94.2(3) . . . . ? C19 W1 C10 C11 -158.7(3) . . . . ? C16 W1 C10 C11 -163.2(2) . . . . ? C15 W1 C10 C11 179.5(2) . . . . ? W1 C10 C11 C12 77.9(3) . . . . ? W1 C10 C11 C14 -45.6(4) . . . . ? W1 C10 C11 C13 -164.7(2) . . . . ? C9 C4 C5 C6 0.3(5) . . . . ? C3 C4 C5 C6 -178.4(3) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C7 C8 C9 C4 1.1(6) . . . . ? C5 C4 C9 C8 -0.9(5) . . . . ? C3 C4 C9 C8 177.8(3) . . . . ? C5 C6 C7 C8 0.0(5) . . . . ? C9 C8 C7 C6 -0.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.504 _refine_diff_density_min -1.371 _refine_diff_density_rms 0.149