# This journal is © The Owner Societies 1999 # CCDC Number: 1326/5 data_koss28 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H61 F O4' _chemical_formula_weight 744.99 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 12.8581(2) _cell_length_b 12.8581(2) _cell_length_c 13.2833(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2196.14(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 13945 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.70 _reflns_number_total 2666 _reflns_number_gt 2024 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0995P)^2^+0.0740P] 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 SHELXL _refine_ls_extinction_coef 0.011(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2666 _refine_ls_number_parameters 288 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C8 C 0.51683(8) 0.33713(8) 0.54056(9) 0.0465(3) Uani 1 d . . . C2A C 0.4727(5) 0.0386(5) 0.6669(5) 0.061(2) Uani 0.67 d P A 1 C4A C 0.5495(7) 0.1981(6) 0.6688(5) 0.055(2) Uani 0.67 d P A 1 C6A C 0.4374(5) 0.1560(4) 0.5462(5) 0.0512(17) Uani 0.67 d P B 1 O7A O 0.3802(3) 0.1840(3) 0.4525(2) 0.0427(8) Uani 0.67 d P B 1 C3A C 0.5426(4) 0.1045(5) 0.7146(4) 0.0620(18) Uani 0.67 d PD A 1 C9A C 0.6084(5) 0.0722(5) 0.8092(5) 0.0666(14) Uani 0.67 d P A 1 C10A C 0.5947(3) 0.1552(3) 0.8903(2) 0.1050(9) Uani 0.67 d PD A 1 H10A H 0.5241 0.1545 0.9139 0.157 Uiso 0.67 calc PR A 1 H10B H 0.6105 0.2223 0.8627 0.157 Uiso 0.67 calc PR A 1 H10C H 0.6408 0.1408 0.9454 0.157 Uiso 0.67 calc PR A 1 C11A C 0.7247(2) 0.0729(3) 0.7755(3) 0.1050(10) Uani 0.67 d PD A 1 H11A H 0.7445 0.1423 0.7570 0.158 Uiso 0.67 calc PR A 1 H11B H 0.7334 0.0275 0.7188 0.158 Uiso 0.67 calc PR A 1 H11C H 0.7676 0.0494 0.8301 0.158 Uiso 0.67 calc PR A 1 C12A C 0.5810(4) -0.0338(3) 0.8473(4) 0.1271(19) Uani 0.67 d PD A 1 H12A H 0.6259 -0.0515 0.9025 0.191 Uiso 0.67 calc PR A 1 H12B H 0.5896 -0.0837 0.7942 0.191 Uiso 0.67 calc PR A 1 H12C H 0.5100 -0.0342 0.8697 0.191 Uiso 0.67 calc PR A 1 C1 C 0.41592(7) 0.05968(7) 0.58375(8) 0.0421(3) Uani 1 d . C 2 C5 C 0.50207(7) 0.22822(7) 0.58351(7) 0.0424(3) Uani 1 d . C 2 C2B C 0.4723(6) 0.0263(8) 0.6714(5) 0.0291(15) Uani 0.33 d P C 2 C4B C 0.5657(12) 0.1982(10) 0.6690(6) 0.0326(14) Uani 0.33 d P C 2 C6B C 0.4273(6) 0.1598(4) 0.5346(7) 0.0208(11) Uani 0.33 d P C 2 O7B O 0.3865(10) 0.1872(12) 0.4563(9) 0.084(4) Uani 0.33 d P C 2 C3B C 0.5458(7) 0.0953(7) 0.7111(6) 0.0364(19) Uani 0.33 d PD C 2 C9B C 0.6095(15) 0.0566(13) 0.7942(12) 0.087(4) Uani 0.33 d P C 2 C10B C 0.6792(6) 0.1408(6) 0.8424(4) 0.1050(9) Uani 0.33 d PD C 2 H10D H 0.7359 0.1565 0.7980 0.157 Uiso 0.33 calc PR C 2 H10E H 0.7061 0.1156 0.9053 0.157 Uiso 0.33 calc PR C 2 H10F H 0.6390 0.2025 0.8540 0.157 Uiso 0.33 calc PR C 2 C11B C 0.6764(5) -0.0367(6) 0.7682(5) 0.113(2) Uani 0.33 d PD C 2 H11D H 0.6329 -0.0963 0.7576 0.170 Uiso 0.33 calc PR C 2 H11E H 0.7237 -0.0504 0.8226 0.170 Uiso 0.33 calc PR C 2 H11F H 0.7152 -0.0224 0.7080 0.170 Uiso 0.33 calc PR C 2 C12B C 0.5335(6) 0.0170(8) 0.8829(5) 0.114(3) Uani 0.33 d PD C 2 H12D H 0.5003 0.0758 0.9138 0.170 Uiso 0.33 calc PR C 2 H12E H 0.5735 -0.0198 0.9325 0.170 Uiso 0.33 calc PR C 2 H12F H 0.4817 -0.0285 0.8553 0.170 Uiso 0.33 calc PR C 2 H1 H 0.5111(12) 0.3357(11) 0.4665(11) 0.056(4) Uiso 1 d . . . H3 H 0.5843(12) 0.3597(11) 0.5570(10) 0.052(3) Uiso 1 d . . . H2A H 0.464(3) -0.014(3) 0.695(3) 0.063(16) Uiso 0.67 d P . . H2B H 0.465(3) -0.045(4) 0.701(3) 0.030(12) Uiso 0.33 d P . . H2A H 0.6030(16) 0.2484(15) 0.7026(15) 0.037(5) Uiso 0.67 d P . . H2B H 0.620(7) 0.233(6) 0.665(6) 0.10(2) Uiso 0.33 d P . . H7A H 0.151(2) 0.174(3) 0.4421(18) 0.057(6) Uiso 0.67 d P . . H7B H 0.257(5) 0.125(3) 0.438(3) 0.037(9) Uiso 0.33 d P . . F1 F 0.287(2) 0.3002(16) 0.0746(9) 0.68(4) Uani 0.25 d PDU . . C1G C 0.2661(14) 0.2757(9) -0.0249(6) 0.102(7) Uani 0.25 d PDU . . C2G C 0.1691(9) 0.2554(8) -0.0542(9) 0.114(6) Uani 0.25 d PDU . . C3G C 0.1483(8) 0.2315(9) -0.1507(7) 0.106(5) Uani 0.25 d PDU . . C4G C 0.2269(10) 0.2283(10) -0.2176(6) 0.086(6) Uani 0.25 d PDU . . C5G C 0.3243(8) 0.2485(12) -0.1887(8) 0.137(8) Uani 0.25 d PDU . . C6G C 0.3447(11) 0.2723(11) -0.0925(9) 0.149(10) Uani 0.25 d PDU . . H2G H 0.1175 0.2587 -0.0064 0.083 Uiso 0.25 d P . . H3G H 0.0784 0.2183 -0.1685 0.089 Uiso 0.25 d P . . H4G H 0.2124 0.2113 -0.2839 0.050 Uiso 0.25 d P . . H5G H 0.3769 0.2440 -0.2349 0.063 Uiso 0.25 d P . . H6G H 0.4138 0.2845 -0.0713 0.091 Uiso 0.25 d P . . 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 C8 0.0372(5) 0.0414(5) 0.0609(6) 0.0032(4) 0.0102(4) -0.0016(4) C2A 0.058(3) 0.039(2) 0.086(3) 0.0100(13) 0.0127(18) -0.0014(12) C4A 0.041(3) 0.0450(18) 0.079(3) -0.0075(15) -0.0024(13) -0.0072(16) C6A 0.045(2) 0.063(2) 0.0449(19) 0.0006(11) 0.0024(13) 0.0126(12) O7A 0.0465(16) 0.0444(16) 0.0373(10) 0.0012(9) -0.0018(10) 0.0031(13) C3A 0.057(3) 0.058(3) 0.070(3) -0.0059(17) -0.0164(18) 0.0002(16) C9A 0.078(2) 0.0550(15) 0.066(3) 0.016(2) -0.031(2) -0.0124(14) C10A 0.138(2) 0.1092(18) 0.0674(14) 0.0015(13) -0.0329(14) -0.0168(19) C11A 0.0765(15) 0.108(2) 0.130(2) -0.0017(18) -0.0502(16) 0.0155(15) C12A 0.167(4) 0.081(2) 0.134(3) 0.048(2) -0.086(3) -0.036(2) C1 0.0369(4) 0.0373(4) 0.0521(6) -0.0047(4) 0.0052(4) 0.0014(3) C5 0.0356(4) 0.0382(4) 0.0534(5) -0.0007(4) 0.0079(4) 0.0006(3) C2B 0.029(2) 0.027(3) 0.031(2) 0.0030(17) -0.0100(16) -0.0052(17) C4B 0.021(3) 0.040(3) 0.037(3) 0.0077(18) -0.0017(13) -0.0024(16) C6B 0.0172(15) 0.0157(16) 0.030(2) -0.0041(13) 0.0002(15) -0.0024(12) O7B 0.068(5) 0.076(6) 0.108(7) -0.007(5) 0.001(4) -0.017(4) C3B 0.042(3) 0.025(2) 0.043(3) 0.0101(18) 0.007(2) -0.0047(19) C9B 0.090(6) 0.100(8) 0.072(5) -0.025(4) -0.009(4) -0.009(4) C10B 0.138(2) 0.1092(18) 0.0674(14) 0.0015(13) -0.0329(14) -0.0168(19) C11B 0.096(4) 0.143(6) 0.101(4) 0.026(4) -0.029(3) 0.045(4) C12B 0.107(5) 0.164(8) 0.070(3) 0.050(5) 0.003(3) 0.003(5) F1 0.230(7) 0.290(8) 0.110(3) -0.120(4) 0.080(4) 0.010(6) C1G 0.116(15) 0.109(16) 0.081(3) -0.038(8) -0.027(11) 0.031(9) C2G 0.063(8) 0.166(13) 0.115(8) -0.026(9) 0.010(6) 0.017(8) C3G 0.060(6) 0.148(12) 0.112(11) -0.027(11) -0.010(7) 0.003(7) C4G 0.114(16) 0.072(9) 0.071(3) -0.022(7) -0.015(9) 0.005(4) C5G 0.060(9) 0.246(19) 0.106(10) -0.077(12) 0.017(6) -0.015(10) C6G 0.068(6) 0.178(15) 0.20(2) -0.133(17) 0.001(11) -0.017(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C8 C5 1.5239(13) . ? C8 C1 1.5243(13) 3 ? C2A C3A 1.389(8) . ? C4A C3A 1.351(9) . ? C6A O7A 1.489(8) . ? C3A C9A 1.570(7) . ? C9A C12A 1.496(6) . ? C9A C10A 1.526(9) . ? C9A C11A 1.560(8) . ? C1 C2B 1.437(7) . ? C1 C6B 1.451(7) . ? C1 C8 1.5243(13) 4 ? C5 C4B 1.451(10) . ? C5 C6B 1.457(7) . ? C2B C3B 1.400(11) . ? C4B C3B 1.458(13) . ? C6B O7B 1.217(17) . ? C3B C9B 1.462(18) . ? C9B C11B 1.515(19) . ? C9B C10B 1.545(18) . ? C9B C12B 1.61(2) . ? F1 F1 1.13(3) 3 ? F1 F1 1.13(3) 4 ? F1 C1G 1.384(12) . ? F1 C1G 1.579(16) 4 ? F1 F1 1.60(5) 2 ? F1 C1G 1.607(18) 3 ? F1 C1G 1.78(2) 2 ? F1 C2G 1.802(15) 4 ? C1G C1G 0.551(17) 3 ? C1G C1G 0.551(17) 4 ? C1G C1G 0.78(2) 2 ? C1G C2G 0.822(14) 4 ? C1G C2G 1.00(3) 2 ? C1G C2G 1.333(14) . ? C1G C6G 1.353(18) . ? C1G C6G 1.356(18) 3 ? C1G C2G 1.452(16) 3 ? C1G F1 1.579(16) 3 ? C1G F1 1.607(18) 4 ? C2G C6G 0.65(2) 2 ? C2G C1G 0.822(14) 3 ? C2G C1G 1.00(3) 2 ? C2G C3G 1.345(12) . ? C2G C1G 1.452(16) 4 ? C2G C6G 1.464(15) 3 ? C2G C2G 1.475(17) 4 ? C2G C2G 1.475(17) 3 ? C2G C5G 1.789(18) 2 ? C2G F1 1.802(15) 3 ? C2G C6G 1.918(17) 4 ? C3G C5G 0.666(13) 2 ? C3G C6G 0.780(15) 2 ? C3G C4G 1.346(11) . ? C3G C4G 1.460(16) 4 ? C3G C5G 1.559(17) 4 ? C3G C4G 1.819(14) 3 ? C3G C5G 1.855(19) 3 ? C3G C3G 1.879(14) 4 ? C3G C3G 1.879(14) 3 ? C3G C4G 1.906(17) 2 ? C3G C6G 1.939(17) 3 ? C4G C4G 0.577(13) 4 ? C4G C4G 0.577(13) 3 ? C4G C5G 0.82(2) 2 ? C4G C4G 0.816(18) 2 ? C4G C5G 0.826(15) 4 ? C4G C5G 1.33(2) 3 ? C4G C5G 1.336(12) . ? C4G C3G 1.460(16) 3 ? C4G C3G 1.819(14) 4 ? C4G C6G 1.900(15) 2 ? C4G C3G 1.906(17) 2 ? C5G C3G 0.666(13) 2 ? C5G C4G 0.82(2) 2 ? C5G C4G 0.826(15) 3 ? C5G C4G 1.33(2) 4 ? C5G C6G 1.340(12) . ? C5G C5G 1.352(15) 4 ? C5G C5G 1.352(15) 3 ? C5G C3G 1.559(17) 3 ? C5G C2G 1.789(18) 2 ? C5G C3G 1.855(19) 4 ? C5G C6G 1.875(13) 4 ? C6G C2G 0.65(2) 2 ? C6G C3G 0.780(15) 2 ? C6G C1G 1.356(18) 4 ? C6G C2G 1.464(15) 4 ? C6G C6G 1.77(2) 4 ? C6G C6G 1.77(2) 3 ? C6G C1G 1.79(2) 3 ? C6G C1G 1.79(2) 2 ? C6G C5G 1.875(13) 3 ? C6G C4G 1.900(15) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C8 C1 112.93(8) . 3 ? C4A C3A C2A 112.4(6) . . ? C4A C3A C9A 124.0(6) . . ? C2A C3A C9A 123.5(5) . . ? C12A C9A C10A 111.7(5) . . ? C12A C9A C11A 109.1(5) . . ? C10A C9A C11A 108.0(5) . . ? C12A C9A C3A 112.6(5) . . ? C10A C9A C3A 108.5(4) . . ? C11A C9A C3A 106.6(4) . . ? C2B C1 C6B 125.4(6) . . ? C2B C1 C8 116.5(4) . 4 ? C6B C1 C8 118.0(4) . 4 ? C4B C5 C6B 124.1(7) . . ? C4B C5 C8 117.9(5) . . ? C6B C5 C8 118.0(4) . . ? C3B C2B C1 117.1(8) . . ? C5 C4B C3B 116.3(10) . . ? O7B C6B C1 126.7(9) . . ? O7B C6B C5 119.4(8) . . ? C1 C6B C5 113.6(7) . . ? C2B C3B C9B 116.5(9) . . ? C2B C3B C4B 123.3(9) . . ? C9B C3B C4B 120.1(11) . . ? C3B C9B C11B 114.6(12) . . ? C3B C9B C10B 113.5(11) . . ? C11B C9B C10B 108.6(12) . . ? C3B C9B C12B 108.7(13) . . ? C11B C9B C12B 105.1(10) . . ? C10B C9B C12B 105.6(11) . . ? F1 F1 F1 90.000(3) 3 4 ? F1 F1 C1G 77.0(10) 3 . ? F1 F1 C1G 78.7(4) 4 . ? F1 F1 C1G 80.1(3) 3 4 ? F1 F1 C1G 58.7(7) 4 4 ? C1G F1 C1G 20.1(5) . 4 ? F1 F1 F1 45.000(2) 3 2 ? F1 F1 F1 45.000(4) 4 2 ? C1G F1 F1 72.7(9) . 2 ? C1G F1 F1 60.7(6) 4 2 ? F1 F1 C1G 57.6(8) 3 3 ? F1 F1 C1G 78.9(8) 4 3 ? C1G F1 C1G 19.5(7) . 3 ? C1G F1 C1G 28.3(8) 4 3 ? F1 F1 C1G 59.0(11) 2 3 ? F1 F1 C1G 62.5(5) 3 2 ? F1 F1 C1G 61.1(7) 4 2 ? C1G F1 C1G 24.8(7) . 2 ? C1G F1 C1G 17.7(5) 4 2 ? F1 F1 C1G 48.0(8) 2 2 ? C1G F1 C1G 17.8(4) 3 2 ? F1 F1 C2G 79.2(12) 3 4 ? F1 F1 C2G 104.5(7) 4 4 ? C1G F1 C2G 25.9(5) . 4 ? C1G F1 C2G 45.9(6) 4 4 ? F1 F1 C2G 92.6(11) 2 4 ? C1G F1 C2G 33.6(10) 3 4 ? C1G F1 C2G 47.9(7) 2 4 ? C1G C1G C1G 90.000(9) 3 4 ? C1G C1G C1G 45.000(4) 3 2 ? C1G C1G C1G 45.000(7) 4 2 ? C1G C1G C2G 92(4) 3 4 ? C1G C1G C2G 151.6(12) 4 4 ? C1G C1G C2G 130(3) 2 4 ? C1G C1G C2G 136(2) 3 2 ? C1G C1G C2G 55(3) 4 2 ? C1G C1G C2G 96(3) 2 2 ? C2G C1G C2G 107.4(16) 4 2 ? C1G C1G C2G 17.0(7) 3 . ? C1G C1G C2G 91(2) 4 . ? C1G C1G C2G 48(2) 2 . ? C2G C1G C2G 82.8(14) 4 . ? C2G C1G C2G 125.9(13) 2 . ? C1G C1G C6G 136.1(7) 3 . ? C1G C1G C6G 79(2) 4 . ? C1G C1G C6G 111.7(18) 2 . ? C2G C1G C6G 80.7(14) 4 . ? C2G C1G C6G 26.9(9) 2 . ? C2G C1G C6G 119.9(7) . . ? C1G C1G C6G 78(2) 3 3 ? C1G C1G C6G 136.0(7) 4 3 ? C1G C1G C6G 111(2) 2 3 ? C2G C1G C6G 19.8(12) 4 3 ? C2G C1G C6G 107.8(11) 2 3 ? C2G C1G C6G 66.0(6) . 3 ? C6G C1G C6G 81.6(7) . 3 ? C1G C1G F1 103.7(14) 3 . ? C1G C1G F1 100.3(7) 4 . ? C1G C1G F1 107.2(8) 2 . ? C2G C1G F1 106.7(10) 4 . ? C2G C1G F1 107.6(14) 2 . ? C2G C1G F1 120.2(15) . . ? C6G C1G F1 119.9(14) . . ? C6G C1G F1 123.6(8) 3 . ? C1G C1G C2G 67(2) 3 3 ? C1G C1G C2G 28.6(18) 4 3 ? C1G C1G C2G 25.7(17) 2 3 ? C2G C1G C2G 131.1(14) 4 3 ? C2G C1G C2G 71.2(9) 2 3 ? C2G C1G C2G 63.8(7) . 3 ? C6G C1G C2G 86.2(7) . 3 ? C6G C1G C2G 111.8(8) 3 3 ? F1 C1G C2G 120.5(7) . 3 ? C1G C1G F1 59.6(10) 3 3 ? C1G C1G F1 102.0(13) 4 3 ? C1G C1G F1 77.8(14) 2 3 ? C2G C1G F1 103(2) 4 3 ? C2G C1G F1 144.1(11) 2 3 ? C2G C1G F1 75.9(10) . 3 ? C6G C1G F1 164.1(10) . 3 ? C6G C1G F1 107.4(13) 3 3 ? F1 C1G F1 44.3(13) . 3 ? C2G C1G F1 101.9(11) 3 3 ? C1G C1G F1 98.9(6) 3 4 ? C1G C1G F1 56.8(12) 4 4 ? C1G C1G F1 73.9(10) 2 4 ? C2G C1G F1 150.1(15) 4 4 ? C2G C1G F1 83.9(17) 2 4 ? C2G C1G F1 113.5(12) . 4 ? C6G C1G F1 109.0(15) . 4 ? C6G C1G F1 166.2(15) 3 4 ? F1 C1G F1 43.7(11) . 4 ? C2G C1G F1 78.5(9) 3 4 ? F1 C1G F1 60.3(16) 3 4 ? C6G C2G C1G 135(3) 2 3 ? C6G C2G C1G 108(2) 2 2 ? C1G C2G C1G 33.3(18) 3 2 ? C6G C2G C1G 126(2) 2 . ? C1G C2G C1G 11.3(6) 3 . ? C1G C2G C1G 35.6(12) 2 . ? C6G C2G C3G 21.4(13) 2 . ? C1G C2G C3G 131.4(13) 3 . ? C1G C2G C3G 116.4(11) 2 . ? C1G C2G C3G 120.6(9) . . ? C6G C2G C1G 111.4(19) 2 4 ? C1G C2G C1G 24.3(19) 3 4 ? C1G C2G C1G 15.3(7) 2 4 ? C1G C2G C1G 22.3(7) . 4 ? C3G C2G C1G 113.6(8) . 4 ? C6G C2G C6G 107.5(17) 2 3 ? C1G C2G C6G 65.7(16) 3 3 ? C1G C2G C6G 91.1(16) 2 3 ? C1G C2G C6G 57.7(7) . 3 ? C3G C2G C6G 87.2(8) . 3 ? C1G C2G C6G 75.9(12) 4 3 ? C6G C2G C2G 124.7(15) 2 4 ? C1G C2G C2G 40.5(14) 3 4 ? C1G C2G C2G 68.7(8) 2 4 ? C1G C2G C2G 33.6(5) . 4 ? C3G C2G C2G 107.4(5) . 4 ? C1G C2G C2G 54.2(8) 4 4 ? C6G C2G C2G 25.4(9) 3 4 ? C6G C2G C2G 76(2) 2 3 ? C1G C2G C2G 63.7(13) 3 3 ? C1G C2G C2G 32.1(7) 2 3 ? C1G C2G C2G 62.0(7) . 3 ? C3G C2G C2G 87.6(6) . 3 ? C1G C2G C2G 40.1(8) 4 3 ? C6G C2G C2G 104.5(8) 3 3 ? C2G C2G C2G 90.000(2) 4 3 ? C6G C2G C5G 37.9(12) 2 2 ? C1G C2G C5G 115.9(13) 3 2 ? C1G C2G C5G 109.7(12) 2 2 ? C1G C2G C5G 104.7(8) . 2 ? C3G C2G C5G 18.4(6) . 2 ? C1G C2G C5G 102.6(8) 4 2 ? C6G C2G C5G 69.6(6) 3 2 ? C2G C2G C5G 89.0(5) 4 2 ? C2G C2G C5G 87.0(6) 3 2 ? C6G C2G F1 159(2) 2 3 ? C1G C2G F1 47.4(8) 3 3 ? C1G C2G F1 62.5(11) 2 3 ? C1G C2G F1 58.2(7) . 3 ? C3G C2G F1 178.8(10) . 3 ? C1G C2G F1 65.2(9) 4 3 ? C6G C2G F1 92.4(9) 3 3 ? C2G C2G F1 71.8(7) 4 3 ? C2G C2G F1 91.4(9) 3 3 ? C5G C2G F1 160.8(10) 2 3 ? C6G C2G C6G 67.1(16) 2 4 ? C1G C2G C6G 68.9(16) 3 4 ? C1G C2G C6G 42.3(9) 2 4 ? C1G C2G C6G 63.9(6) . 4 ? C3G C2G C6G 74.4(6) . 4 ? C1G C2G C6G 44.7(6) 4 4 ? C6G C2G C6G 94.5(10) 3 4 ? C2G C2G C6G 85.5(7) 4 4 ? C2G C2G C6G 16.0(4) 3 4 ? C5G C2G C6G 71.6(8) 2 4 ? F1 C2G C6G 104.5(11) 3 4 ? C5G C3G C6G 136(2) 2 2 ? C5G C3G C2G 121.9(17) 2 . ? C6G C3G C2G 17.6(13) 2 . ? C5G C3G C4G 28(2) 2 . ? C6G C3G C4G 124.5(15) 2 . ? C2G C3G C4G 119.1(8) . . ? C5G C3G C4G 13.3(12) 2 4 ? C6G C3G C4G 123.0(16) 2 4 ? C2G C3G C4G 110.9(8) . 4 ? C4G C3G C4G 23.3(6) . 4 ? C5G C3G C5G 60(2) 2 4 ? C6G C3G C5G 101.3(16) 2 4 ? C2G C3G C5G 104.5(8) . 4 ? C4G C3G C5G 32.0(4) . 4 ? C4G C3G C5G 52.4(6) 4 4 ? C5G C3G C4G 35.2(16) 2 3 ? C6G C3G C4G 112.4(15) 2 3 ? C2G C3G C4G 107.4(8) . 3 ? C4G C3G C4G 12.1(3) . 3 ? C4G C3G C4G 26.0(6) 4 3 ? C5G C3G C4G 26.7(8) 4 3 ? C5G C3G C5G 33.7(12) 2 3 ? C6G C3G C5G 103.2(15) 2 3 ? C2G C3G C5G 88.3(8) . 3 ? C4G C3G C5G 45.8(5) . 3 ? C4G C3G C5G 25.2(6) 4 3 ? C5G C3G C5G 67.5(7) 4 3 ? C4G C3G C5G 42.6(5) 3 3 ? C5G C3G C3G 51.9(16) 2 4 ? C6G C3G C3G 89.2(12) 2 4 ? C2G C3G C3G 72.5(5) . 4 ? C4G C3G C3G 66.3(4) . 4 ? C4G C3G C3G 45.4(5) 4 4 ? C5G C3G C3G 84.7(7) 4 4 ? C4G C3G C3G 62.0(4) 3 4 ? C5G C3G C3G 20.5(3) 3 4 ? C5G C3G C3G 77.6(17) 2 3 ? C6G C3G C3G 82.5(14) 2 3 ? C2G C3G C3G 88.1(5) . 3 ? C4G C3G C3G 50.6(6) . 3 ? C4G C3G C3G 68.3(3) 4 3 ? C5G C3G C3G 19.6(5) 4 3 ? C4G C3G C3G 42.6(3) 3 3 ? C5G C3G C3G 77.2(4) 3 3 ? C3G C3G C3G 90.000(1) 4 3 ? C5G C3G C4G 25.6(13) 2 2 ? C6G C3G C4G 112.5(15) 2 2 ? C2G C3G C4G 102.4(7) . 2 ? C4G C3G C4G 21.4(6) . 2 ? C4G C3G C4G 12.6(3) 4 2 ? C5G C3G C4G 43.8(9) 4 2 ? C4G C3G C4G 17.6(3) 3 2 ? C5G C3G C4G 25.3(5) 3 2 ? C3G C3G C4G 45.4(4) 4 2 ? C3G C3G C4G 57.5(4) 3 2 ? C5G C3G C6G 74.6(15) 2 3 ? C6G C3G C6G 65.9(14) 2 3 ? C2G C3G C6G 49.0(5) . 3 ? C4G C3G C6G 83.8(5) . 3 ? C4G C3G C6G 66.2(6) 4 3 ? C5G C3G C6G 92.3(8) 4 3 ? C4G C3G C6G 76.1(7) 3 3 ? C5G C3G C6G 41.3(4) 3 3 ? C3G C3G C6G 23.5(4) 4 3 ? C3G C3G C6G 89.7(5) 3 3 ? C4G C3G C6G 62.5(6) 2 3 ? C4G C4G C4G 90.000(4) 4 3 ? C4G C4G C5G 70(3) 4 2 ? C4G C4G C5G 144.6(17) 3 2 ? C4G C4G C4G 45.000(3) 4 2 ? C4G C4G C4G 45.000(5) 3 2 ? C5G C4G C4G 110(3) 2 2 ? C4G C4G C5G 144(2) 4 4 ? C4G C4G C5G 69(3) 3 4 ? C5G C4G C5G 110.6(13) 2 4 ? C4G C4G C5G 108(3) 2 4 ? C4G C4G C5G 20.9(12) 4 3 ? C4G C4G C5G 78(2) 3 3 ? C5G C4G C5G 73.6(11) 2 3 ? C4G C4G C5G 36(2) 2 3 ? C5G C4G C5G 123.1(14) 4 3 ? C4G C4G C5G 77(2) 4 . ? C4G C4G C5G 21.3(14) 3 . ? C5G C4G C5G 123.3(13) 2 . ? C4G C4G C5G 35(2) 2 . ? C5G C4G C5G 73.2(13) 4 . ? C5G C4G C5G 60.9(5) 3 . ? C4G C4G C3G 90(2) 4 . ? C4G C4G C3G 138.7(6) 3 . ? C5G C4G C3G 22.4(13) 2 . ? C4G C4G C3G 121.7(15) 2 . ? C5G C4G C3G 88.4(11) 4 . ? C5G C4G C3G 87.7(6) 3 . ? C5G C4G C3G 120.6(7) . . ? C4G C4G C3G 133.8(11) 4 3 ? C4G C4G C3G 67.2(18) 3 3 ? C5G C4G C3G 105.5(15) 2 3 ? C4G C4G C3G 102.4(18) 2 3 ? C5G C4G C3G 10.7(10) 4 3 ? C5G C4G C3G 113.0(6) 3 3 ? C5G C4G C3G 67.6(5) . 3 ? C3G C4G C3G 84.0(7) . 3 ? C4G C4G C3G 29.2(4) 4 4 ? C4G C4G C3G 89.7(14) 3 4 ? C5G C4G C3G 58.6(15) 2 4 ? C4G C4G C3G 51.6(14) 2 4 ? C5G C4G C3G 118.5(10) 4 4 ? C5G C4G C3G 16.8(6) 3 4 ? C5G C4G C3G 70.1(7) . 4 ? C3G C4G C3G 71.1(6) . 4 ? C3G C4G C3G 107.8(8) 3 4 ? C4G C4G C6G 91.1(16) 4 2 ? C4G C4G C6G 119.0(6) 3 2 ? C5G C4G C6G 37.0(9) 2 2 ? C4G C4G C6G 110.8(11) 2 2 ? C5G C4G C6G 75.7(9) 4 2 ? C5G C4G C6G 82.3(6) 3 2 ? C5G C4G C6G 101.8(8) . 2 ? C3G C4G C6G 19.8(7) . 2 ? C3G C4G C6G 69.1(7) 3 2 ? C3G C4G C6G 65.9(7) 4 2 ? C4G C4G C3G 72.7(14) 4 2 ? C4G C4G C3G 33.6(9) 3 2 ? C5G C4G C3G 111.1(11) 2 2 ? C4G C4G C3G 36.9(11) 2 2 ? C5G C4G C3G 73.9(17) 4 2 ? C5G C4G C3G 54.1(7) 3 2 ? C5G C4G C3G 12.4(6) . 2 ? C3G C4G C3G 108.4(8) . 2 ? C3G C4G C3G 66.4(5) 3 2 ? C3G C4G C3G 60.6(3) 4 2 ? C6G C4G C3G 90.1(6) 2 2 ? C3G C5G C4G 130(3) 2 2 ? C3G C5G C4G 156(2) 2 3 ? C4G C5G C4G 41.1(12) 2 3 ? C3G C5G C4G 128(2) 2 4 ? C4G C5G C4G 14.5(6) 2 4 ? C4G C5G C4G 35.5(15) 3 4 ? C3G C5G C4G 141.9(19) 2 . ? C4G C5G C4G 35.1(13) 2 . ? C4G C5G C4G 14.7(8) 3 . ? C4G C5G C4G 25.0(5) 4 . ? C3G C5G C6G 24.1(14) 2 . ? C4G C5G C6G 121.4(17) 2 . ? C4G C5G C6G 132.9(12) 3 . ? C4G C5G C6G 113.7(10) 4 . ? C4G C5G C6G 120.1(9) . . ? C3G C5G C5G 130.4(16) 2 4 ? C4G C5G C5G 70.9(7) 2 4 ? C4G C5G C5G 34.5(11) 3 4 ? C4G C5G C5G 59.7(9) 4 4 ? C4G C5G C5G 35.8(7) . 4 ? C6G C5G C5G 107.4(6) . 4 ? C3G C5G C5G 95(2) 2 3 ? C4G C5G C5G 34.9(11) 2 3 ? C4G C5G C5G 71.1(9) 3 3 ? C4G C5G C5G 35.5(8) 4 3 ? C4G C5G C5G 59.4(8) . 3 ? C6G C5G C5G 88.3(7) . 3 ? C5G C5G C5G 90.000(2) 4 3 ? C3G C5G C3G 108.5(19) 2 3 ? C4G C5G C3G 94.7(13) 2 3 ? C4G C5G C3G 59.7(13) 3 3 ? C4G C5G C3G 82.1(8) 4 3 ? C4G C5G C3G 60.0(4) . 3 ? C6G C5G C3G 88.3(8) . 3 ? C5G C5G C3G 25.2(6) 4 3 ? C5G C5G C3G 106.1(7) 3 3 ? C3G C5G C2G 39.7(13) 2 2 ? C4G C5G C2G 121.1(16) 2 2 ? C4G C5G C2G 119.6(13) 3 2 ? C4G C5G C2G 109.8(10) 4 2 ? C4G C5G C2G 109.0(9) . 2 ? C6G C5G C2G 17.2(7) . 2 ? C5G C5G C2G 90.8(5) 4 2 ? C5G C5G C2G 93.0(6) 3 2 ? C3G C5G C2G 71.1(7) 3 2 ? C3G C5G C3G 81.8(17) 2 4 ? C4G C5G C3G 49.4(16) 2 4 ? C4G C5G C3G 80.8(14) 3 4 ? C4G C5G C3G 46.5(6) 4 4 ? C4G C5G C3G 67.3(5) . 4 ? C6G C5G C3G 72.7(6) . 4 ? C5G C5G C3G 91.8(9) 4 4 ? C5G C5G C3G 15.9(5) 3 4 ? C3G C5G C3G 101.9(9) 3 4 ? C2G C5G C3G 77.2(8) 2 4 ? C3G C5G C6G 85.4(16) 2 4 ? C4G C5G C6G 105.4(10) 2 4 ? C4G C5G C6G 79.0(12) 3 4 ? C4G C5G C6G 91.0(8) 4 4 ? C4G C5G C6G 74.7(6) . 4 ? C6G C5G C6G 64.3(8) . 4 ? C5G C5G C6G 45.6(4) 4 4 ? C5G C5G C6G 102.3(4) 3 4 ? C3G C5G C6G 24.1(6) 3 4 ? C2G C5G C6G 47.0(5) 2 4 ? C3G C5G C6G 92.4(7) 4 4 ? C2G C6G C3G 141(2) 2 2 ? C2G C6G C5G 124.8(18) 2 . ? C3G C6G C5G 20.4(11) 2 . ? C2G C6G C1G 45(2) 2 . ? C3G C6G C1G 138.3(15) 2 . ? C5G C6G C1G 119.6(9) . . ? C2G C6G C1G 25.6(19) 2 4 ? C3G C6G C1G 135.2(15) 2 4 ? C5G C6G C1G 114.9(9) . 4 ? C1G C6G C1G 23.5(7) . 4 ? C2G C6G C2G 78(2) 2 4 ? C3G C6G C2G 117.8(17) 2 4 ? C5G C6G C2G 107.2(8) . 4 ? C1G C6G C2G 33.6(6) . 4 ? C1G C6G C2G 56.3(8) 4 4 ? C2G C6G C6G 52.1(14) 2 4 ? C3G C6G C6G 90.4(13) 2 4 ? C5G C6G C6G 72.7(5) . 4 ? C1G C6G C6G 68.5(4) . 4 ? C1G C6G C6G 49.1(7) 4 4 ? C2G C6G C6G 91.5(8) 4 4 ? C2G C6G C6G 93.3(18) 2 3 ? C3G C6G C6G 97.5(14) 2 3 ? C5G C6G C6G 87.4(6) . 3 ? C1G C6G C6G 49.3(5) . 3 ? C1G C6G C6G 68.6(5) 4 3 ? C2G C6G C6G 20.4(6) 4 3 ? C6G C6G C6G 90.000(1) 4 3 ? C2G C6G C1G 49.0(17) 2 3 ? C3G C6G C1G 126.4(15) 2 3 ? C5G C6G C1G 107.4(8) . 3 ? C1G C6G C1G 12.3(3) . 3 ? C1G C6G C1G 23.9(9) 4 3 ? C2G C6G C1G 34.1(11) 4 3 ? C6G C6G C1G 60.5(5) 4 3 ? C6G C6G C1G 44.6(5) 3 3 ? C2G C6G C1G 36.7(16) 2 2 ? C3G C6G C1G 124.5(15) 2 2 ? C5G C6G C1G 104.1(8) . 2 ? C1G C6G C1G 23.8(6) . 2 ? C1G C6G C1G 12.3(4) 4 2 ? C2G C6G C1G 51.7(11) 4 2 ? C6G C6G C1G 44.7(3) 4 2 ? C6G C6G C1G 60.4(5) 3 2 ? C1G C6G C1G 17.7(4) 3 2 ? C2G C6G C5G 124(2) 2 3 ? C3G C6G C5G 54.6(13) 2 3 ? C5G C6G C5G 46.1(6) . 3 ? C1G C6G C5G 87.9(7) . 3 ? C1G C6G C5G 99.4(7) 4 3 ? C2G C6G C5G 63.4(6) 4 3 ? C6G C6G C5G 88.1(4) 4 3 ? C6G C6G C5G 43.0(4) 3 3 ? C1G C6G C5G 78.8(6) 3 3 ? C1G C6G C5G 87.5(7) 2 3 ? C2G C6G C4G 124(2) 2 2 ? C3G C6G C4G 35.7(9) 2 2 ? C5G C6G C4G 21.6(9) . 2 ? C1G C6G C4G 102.6(9) . 2 ? C1G C6G C4G 105.1(9) 4 2 ? C2G C6G C4G 85.7(10) 4 2 ? C6G C6G C4G 75.0(4) 4 2 ? C6G C6G C4G 65.8(6) 3 2 ? C1G C6G C4G 91.1(8) 3 2 ? C1G C6G C4G 93.0(8) 2 2 ? C5G C6G C4G 25.3(5) 3 2 ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 0.257 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.035