# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1182 data_xr120 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H35 F15 N3 O3.50 Sm' _chemical_formula_weight 952.98 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 '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' _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 10.745(1) _cell_length_b 10.773(1) _cell_length_c 18.216(2) _cell_angle_alpha 98.42(1) _cell_angle_beta 95.81(1) _cell_angle_gamma 114.02(1) _cell_volume 1874.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203 _cell_measurement_reflns_used 27 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 1.679 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.76 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/PC' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7673 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6535 _reflns_number_observed 5796 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS 2.10b (Siemens, 1994)' _computing_cell_refinement 'XSCANS 2.10b (Siemens, 1994)' _computing_data_reduction 'XSCANS 2.10b (Siemens, 1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL PC 4.2/360 (Siemens, 1990)' _computing_publication_material 'SHELXTL PC 4.2/360 (Siemens, 1990)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent THF is comprised of atoms O(4), C(31), C(32), C(33), and C(34), and was refined at half occupancy based on elemental analysis. The atoms in the solvent THF were refined with isotropic temperature factors. Hydrogen atoms were not fixed on the solvent THF. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+3.1239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6535 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_obs 0.0404 _refine_ls_wR_factor_all 0.1218 _refine_ls_wR_factor_obs 0.1165 _refine_ls_goodness_of_fit_all 1.109 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 1.109 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sm1 Sm 0.16393(3) 0.05638(3) 0.226477(13) 0.03232(11) Uani 1 d . . F2 F -0.0661(4) 0.3671(4) 0.3318(2) 0.0616(10) Uani 1 d . . F3 F -0.1293(5) 0.5329(5) 0.2521(3) 0.0745(12) Uani 1 d . . F4 F -0.0948(5) 0.5277(4) 0.1068(2) 0.0737(12) Uani 1 d . . F5 F 0.0087(4) 0.3548(4) 0.0411(2) 0.0594(9) Uani 1 d . . F6 F 0.0704(4) 0.1854(4) 0.1196(2) 0.0490(8) Uani 1 d . . F8 F 0.3272(5) -0.0191(4) -0.0275(2) 0.0645(10) Uani 1 d . . F9 F 0.4060(5) -0.2225(5) -0.0683(3) 0.0818(14) Uani 1 d . . F10 F 0.3816(5) -0.4143(4) 0.0188(3) 0.0788(13) Uani 1 d . . F11 F 0.2695(4) -0.4004(4) 0.1452(3) 0.0692(11) Uani 1 d . . F12 F 0.1819(4) -0.2023(3) 0.1837(2) 0.0492(8) Uani 1 d . . F14 F -0.0137(5) -0.2712(5) 0.4121(3) 0.0809(13) Uani 1 d . . F15 F 0.0490(6) -0.1796(8) 0.5635(3) 0.115(2) Uani 1 d . . F16 F 0.2093(6) 0.0920(8) 0.6263(2) 0.125(3) Uani 1 d . . F17 F 0.3172(6) 0.2722(7) 0.5338(3) 0.098(2) Uani 1 d . . F18 F 0.2577(4) 0.1820(4) 0.3825(2) 0.0586(9) Uani 1 d . . O1 O -0.0658(4) -0.1145(4) 0.1608(2) 0.0446(9) Uani 1 d . . O2 O 0.3400(4) 0.2949(4) 0.2252(2) 0.0483(10) Uani 1 d . . O3 O 0.3935(4) 0.0608(4) 0.2722(2) 0.0490(10) Uani 1 d . . O4 O 0.6240(17) 0.2678(17) 0.4579(9) 0.114(5) Uiso 0.50 d P . N1 N 0.0435(6) 0.1879(6) 0.2654(3) 0.0449(12) Uani 1 d . . N2 N 0.2167(5) 0.0015(5) 0.1061(3) 0.0402(11) Uani 1 d . . N3 N 0.0931(5) -0.0849(6) 0.3152(3) 0.0438(11) Uani 1 d . . HN1 H 0.0380(91) 0.1998(90) 0.3037(48) 0.080 Uiso 1 d . . HN2 H 0.1983(90) 0.0377(89) 0.0764(49) 0.080 Uiso 1 d . . HN3 H 0.0432(87) -0.1768(89) 0.2941(47) 0.080 Uiso 1 d . . C1 C 0.0060(5) 0.2706(6) 0.2285(3) 0.0370(11) Uani 1 d . . C2 C -0.0477(6) 0.3624(6) 0.2587(3) 0.0428(13) Uani 1 d . . C3 C -0.0815(6) 0.4458(6) 0.2187(4) 0.0493(14) Uani 1 d . . C4 C -0.0648(7) 0.4432(6) 0.1452(4) 0.0489(14) Uani 1 d . . C5 C -0.0124(6) 0.3565(6) 0.1128(3) 0.0439(13) Uani 1 d . . C6 C 0.0195(6) 0.2734(6) 0.1527(3) 0.0385(12) Uani 1 d . . C7 C 0.2545(5) -0.1006(5) 0.0812(3) 0.0345(11) Uani 1 d . . C8 C 0.3115(6) -0.1140(6) 0.0163(3) 0.0446(13) Uani 1 d . . C9 C 0.3531(6) -0.2178(7) -0.0048(4) 0.053(2) Uani 1 d . . C10 C 0.3388(7) -0.3151(6) 0.0380(4) 0.054(2) Uani 1 d . . C11 C 0.2833(6) -0.3075(6) 0.1014(4) 0.0470(14) Uani 1 d . . C12 C 0.2409(6) -0.2045(5) 0.1214(3) 0.0378(12) Uani 1 d . . C13 C 0.1210(6) -0.0468(7) 0.3914(3) 0.0465(14) Uani 1 d . . C14 C 0.0701(8) -0.1370(9) 0.4411(4) 0.062(2) Uani 1 d . . C15 C 0.1027(10) -0.0886(13) 0.5194(5) 0.081(3) Uani 1 d . . C16 C 0.1858(10) 0.0470(14) 0.5507(4) 0.088(3) Uani 1 d . . C17 C 0.2369(8) 0.1383(10) 0.5047(4) 0.071(2) Uani 1 d . . C18 C 0.2059(7) 0.0906(8) 0.4278(3) 0.051(2) Uani 1 d . . C19 C -0.1125(7) -0.1687(7) 0.0803(3) 0.052(2) Uani 1 d . . H19A H -0.0715(7) -0.2299(7) 0.0622(3) 0.062 Uiso 1 calc R . H19B H -0.0876(7) -0.0936(7) 0.0530(3) 0.062 Uiso 1 calc R . C20 C -0.2685(7) -0.2478(7) 0.0699(4) 0.057(2) Uani 1 d . . H20A H -0.3132(7) -0.2378(7) 0.0236(4) 0.068 Uiso 1 calc R . H20B H -0.2953(7) -0.3458(7) 0.0686(4) 0.068 Uiso 1 calc R . C21 C -0.3055(7) -0.1824(7) 0.1373(4) 0.054(2) Uani 1 d . . H21A H -0.3926(7) -0.2455(7) 0.1485(4) 0.065 Uiso 1 calc R . H21B H -0.3114(7) -0.0974(7) 0.1301(4) 0.065 Uiso 1 calc R . C22 C -0.1861(6) -0.1536(7) 0.1982(3) 0.0475(14) Uani 1 d . . H22A H -0.1746(6) -0.0786(7) 0.2389(3) 0.057 Uiso 1 calc R . H22B H -0.2004(6) -0.2357(7) 0.2186(3) 0.057 Uiso 1 calc R . C23 C 0.3958(8) 0.3483(7) 0.1616(4) 0.058(2) Uani 1 d . . H23A H 0.3329(8) 0.3754(7) 0.1333(4) 0.069 Uiso 1 calc R . H23B H 0.4105(8) 0.2786(7) 0.1282(4) 0.069 Uiso 1 calc R . C24 C 0.5295(9) 0.4708(8) 0.1938(5) 0.083(3) Uani 1 d . . H24A H 0.5506(9) 0.5387(8) 0.1619(5) 0.100 Uiso 1 calc R . H24B H 0.6049(9) 0.4436(8) 0.2005(5) 0.100 Uiso 1 calc R . C25 C 0.5042(11) 0.5265(8) 0.2678(5) 0.096(3) Uani 1 d . . H25A H 0.5880(11) 0.5645(8) 0.3054(5) 0.115 Uiso 1 calc R . H25B H 0.4743(11) 0.5992(8) 0.2633(5) 0.115 Uiso 1 calc R . C26 C 0.3946(10) 0.4081(8) 0.2891(5) 0.085(3) Uani 1 d . . H26A H 0.4326(10) 0.3819(8) 0.3317(5) 0.103 Uiso 1 calc R . H26B H 0.3219(10) 0.4331(8) 0.3033(5) 0.103 Uiso 1 calc R . C27 C 0.4170(7) -0.0211(8) 0.3233(4) 0.062(2) Uani 1 d . . H27A H 0.3355(7) -0.1080(8) 0.3178(4) 0.075 Uiso 1 calc R . H27B H 0.4389(7) 0.0291(8) 0.3752(4) 0.075 Uiso 1 calc R . C28 C 0.5356(10) -0.0469(12) 0.3024(7) 0.100(3) Uani 1 d . . H28A H 0.5909(10) -0.0518(12) 0.3465(7) 0.120 Uiso 1 calc R . H28B H 0.5036(10) -0.1330(12) 0.2656(7) 0.120 Uiso 1 calc R . C29 C 0.6132(10) 0.0687(11) 0.2715(8) 0.104(4) Uani 1 d . . H29A H 0.6526(10) 0.0395(11) 0.2304(8) 0.125 Uiso 1 calc R . H29B H 0.6883(10) 0.1385(11) 0.3097(8) 0.125 Uiso 1 calc R . C30 C 0.5196(7) 0.1263(8) 0.2437(5) 0.067(2) Uani 1 d . . H30A H 0.5603(7) 0.2261(8) 0.2618(5) 0.081 Uiso 1 calc R . H30B H 0.5012(7) 0.1066(8) 0.1890(5) 0.081 Uiso 1 calc R . C31 C 0.7121(23) 0.4062(23) 0.4613(12) 0.097(6) Uiso 0.50 d P . C32 C 0.7618(21) 0.4534(21) 0.5414(11) 0.088(5) Uiso 0.50 d P . C33 C 0.7076(17) 0.3384(17) 0.5801(9) 0.070(4) Uiso 0.50 d P . C34 C 0.6271(15) 0.2190(15) 0.5216(8) 0.058(3) Uiso 0.50 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 Sm1 0.0385(2) 0.0340(2) 0.0279(2) 0.00853(10) 0.01061(10) 0.01714(12) F2 0.078(3) 0.075(3) 0.048(2) 0.010(2) 0.027(2) 0.046(2) F3 0.092(3) 0.071(3) 0.081(3) 0.005(2) 0.015(2) 0.060(3) F4 0.100(3) 0.061(2) 0.073(3) 0.023(2) 0.002(2) 0.048(2) F5 0.076(3) 0.063(2) 0.038(2) 0.014(2) 0.008(2) 0.028(2) F6 0.065(2) 0.053(2) 0.039(2) 0.0064(15) 0.017(2) 0.035(2) F8 0.090(3) 0.068(2) 0.043(2) 0.024(2) 0.035(2) 0.032(2) F9 0.085(3) 0.092(3) 0.066(3) -0.008(2) 0.041(2) 0.038(3) F10 0.071(3) 0.056(2) 0.107(4) -0.019(2) 0.008(2) 0.039(2) F11 0.073(3) 0.040(2) 0.096(3) 0.022(2) 0.007(2) 0.024(2) F12 0.062(2) 0.046(2) 0.043(2) 0.0176(15) 0.021(2) 0.021(2) F14 0.086(3) 0.091(3) 0.091(3) 0.061(3) 0.044(3) 0.042(3) F15 0.145(5) 0.223(7) 0.081(3) 0.111(4) 0.080(3) 0.140(5) F16 0.133(5) 0.283(9) 0.028(2) 0.024(3) 0.016(2) 0.157(6) F17 0.088(3) 0.139(5) 0.056(3) -0.028(3) -0.011(2) 0.060(3) F18 0.060(2) 0.064(2) 0.046(2) 0.007(2) 0.007(2) 0.023(2) O1 0.043(2) 0.054(2) 0.031(2) 0.005(2) 0.010(2) 0.016(2) O2 0.060(3) 0.035(2) 0.046(2) 0.007(2) 0.021(2) 0.015(2) O3 0.043(2) 0.057(3) 0.053(2) 0.021(2) 0.013(2) 0.023(2) N1 0.063(3) 0.050(3) 0.033(2) 0.013(2) 0.018(2) 0.032(3) N2 0.053(3) 0.039(3) 0.036(2) 0.014(2) 0.018(2) 0.023(2) N3 0.047(3) 0.055(3) 0.032(2) 0.015(2) 0.011(2) 0.021(2) C1 0.034(3) 0.038(3) 0.038(3) 0.007(2) 0.009(2) 0.014(2) C2 0.045(3) 0.044(3) 0.039(3) 0.003(2) 0.007(2) 0.022(3) C3 0.048(3) 0.041(3) 0.060(4) -0.001(3) 0.006(3) 0.025(3) C4 0.052(4) 0.044(3) 0.051(3) 0.011(3) 0.002(3) 0.022(3) C5 0.045(3) 0.041(3) 0.037(3) 0.006(2) 0.004(2) 0.011(3) C6 0.039(3) 0.036(3) 0.041(3) 0.006(2) 0.011(2) 0.016(2) C7 0.037(3) 0.031(3) 0.032(3) 0.003(2) 0.009(2) 0.012(2) C8 0.046(3) 0.046(3) 0.039(3) 0.007(2) 0.013(2) 0.017(3) C9 0.042(3) 0.054(4) 0.049(3) -0.014(3) 0.015(3) 0.014(3) C10 0.043(3) 0.039(3) 0.071(4) -0.011(3) 0.004(3) 0.018(3) C11 0.043(3) 0.026(3) 0.061(4) 0.003(2) -0.002(3) 0.008(2) C12 0.036(3) 0.033(3) 0.038(3) 0.004(2) 0.007(2) 0.010(2) C13 0.043(3) 0.076(4) 0.041(3) 0.029(3) 0.021(3) 0.037(3) C14 0.066(4) 0.106(6) 0.054(4) 0.047(4) 0.031(3) 0.062(5) C15 0.093(6) 0.165(10) 0.050(4) 0.064(6) 0.041(4) 0.100(7) C16 0.096(6) 0.194(11) 0.025(3) 0.026(5) 0.017(4) 0.112(8) C17 0.063(4) 0.125(7) 0.037(4) -0.004(4) 0.000(3) 0.062(5) C18 0.050(3) 0.081(5) 0.034(3) 0.012(3) 0.010(3) 0.040(4) C19 0.055(4) 0.055(4) 0.032(3) -0.004(3) 0.006(3) 0.016(3) C20 0.063(4) 0.047(4) 0.043(3) 0.001(3) 0.002(3) 0.012(3) C21 0.047(3) 0.058(4) 0.051(4) 0.014(3) 0.007(3) 0.016(3) C22 0.043(3) 0.054(4) 0.039(3) 0.012(3) 0.011(2) 0.013(3) C23 0.074(5) 0.041(3) 0.060(4) 0.018(3) 0.033(3) 0.020(3) C24 0.083(6) 0.062(5) 0.090(6) 0.028(4) 0.034(5) 0.009(4) C25 0.105(7) 0.048(4) 0.090(6) 0.002(4) 0.010(5) -0.005(5) C26 0.098(6) 0.055(4) 0.068(5) -0.012(4) 0.024(5) 0.003(4) C27 0.055(4) 0.079(5) 0.065(4) 0.025(4) 0.007(3) 0.038(4) C28 0.077(6) 0.131(9) 0.132(9) 0.070(7) 0.034(6) 0.068(6) C29 0.066(5) 0.095(7) 0.178(11) 0.038(7) 0.052(6) 0.050(5) C30 0.041(4) 0.069(5) 0.093(6) 0.028(4) 0.021(4) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 N3 2.352(5) . ? Sm1 N1 2.360(5) . ? Sm1 N2 2.371(5) . ? Sm1 O1 2.444(4) . ? Sm1 O2 2.500(4) . ? Sm1 O3 2.502(4) . ? Sm1 F18 2.847(4) . ? Sm1 F12 2.870(3) . ? Sm1 F6 2.876(3) . ? F2 C2 1.361(7) . ? F3 C3 1.343(7) . ? F4 C4 1.343(7) . ? F5 C5 1.346(7) . ? F6 C6 1.372(6) . ? F8 C8 1.355(7) . ? F9 C9 1.342(7) . ? F10 C10 1.341(7) . ? F11 C11 1.340(7) . ? F12 C12 1.358(6) . ? F14 C14 1.341(10) . ? F15 C15 1.343(10) . ? F16 C16 1.353(8) . ? F17 C17 1.333(11) . ? F18 C18 1.358(7) . ? O1 C19 1.450(6) . ? O1 C22 1.461(7) . ? O2 C26 1.432(8) . ? O2 C23 1.445(7) . ? O3 C30 1.440(8) . ? O3 C27 1.443(8) . ? O4 C34 1.34(2) . ? O4 C31 1.39(2) . ? N1 C1 1.350(7) . ? N2 C7 1.356(7) . ? N3 C13 1.355(7) . ? C1 C6 1.406(7) . ? C1 C2 1.408(8) . ? C2 C3 1.369(9) . ? C3 C4 1.367(9) . ? C4 C5 1.368(9) . ? C5 C6 1.356(8) . ? C7 C12 1.393(7) . ? C7 C8 1.399(7) . ? C8 C9 1.384(9) . ? C9 C10 1.366(10) . ? C10 C11 1.360(9) . ? C11 C12 1.377(8) . ? C13 C18 1.398(9) . ? C13 C14 1.409(9) . ? C14 C15 1.400(11) . ? C15 C16 1.359(14) . ? C16 C17 1.365(13) . ? C17 C18 1.376(9) . ? C19 C20 1.515(9) . ? C20 C21 1.496(9) . ? C21 C22 1.504(9) . ? C23 C24 1.486(11) . ? C24 C25 1.490(12) . ? C25 C26 1.476(11) . ? C27 C28 1.484(11) . ? C28 C29 1.421(13) . ? C29 C30 1.467(12) . ? C31 C32 1.44(3) . ? C32 C33 1.46(2) . ? C33 C34 1.43(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 N3 Sm1 N1 93.1(2) . . ? N3 Sm1 N2 129.1(2) . . ? N1 Sm1 N2 129.7(2) . . ? N3 Sm1 O1 78.7(2) . . ? N1 Sm1 O1 83.5(2) . . ? N2 Sm1 O1 80.36(15) . . ? N3 Sm1 O2 137.6(2) . . ? N1 Sm1 O2 79.9(2) . . ? N2 Sm1 O2 83.10(15) . . ? O1 Sm1 O2 140.35(14) . . ? N3 Sm1 O3 82.4(2) . . ? N1 Sm1 O3 135.0(2) . . ? N2 Sm1 O3 83.1(2) . . ? O1 Sm1 O3 137.93(14) . . ? O2 Sm1 O3 74.37(14) . . ? N3 Sm1 F18 61.7(2) . . ? N1 Sm1 F18 69.68(15) . . ? N2 Sm1 F18 149.03(15) . . ? O1 Sm1 F18 129.54(11) . . ? O2 Sm1 F18 76.89(12) . . ? O3 Sm1 F18 68.95(12) . . ? N3 Sm1 F12 68.39(14) . . ? N1 Sm1 F12 152.2(2) . . ? N2 Sm1 F12 61.22(13) . . ? O1 Sm1 F12 72.92(12) . . ? O2 Sm1 F12 127.81(12) . . ? O3 Sm1 F12 65.20(12) . . ? F18 Sm1 F12 114.71(10) . . ? N3 Sm1 F6 143.50(14) . . ? N1 Sm1 F6 61.13(13) . . ? N2 Sm1 F6 68.65(13) . . ? O1 Sm1 F6 73.40(12) . . ? O2 Sm1 F6 67.03(13) . . ? O3 Sm1 F6 134.00(12) . . ? F18 Sm1 F6 122.39(10) . . ? F12 Sm1 F6 122.85(9) . . ? C6 F6 Sm1 112.2(3) . . ? C12 F12 Sm1 111.1(3) . . ? C18 F18 Sm1 112.6(3) . . ? C19 O1 C22 109.0(4) . . ? C19 O1 Sm1 128.0(3) . . ? C22 O1 Sm1 121.8(3) . . ? C26 O2 C23 107.5(5) . . ? C26 O2 Sm1 124.1(4) . . ? C23 O2 Sm1 128.2(4) . . ? C30 O3 C27 107.6(5) . . ? C30 O3 Sm1 126.4(4) . . ? C27 O3 Sm1 125.2(4) . . ? C34 O4 C31 117.2(16) . . ? C1 N1 Sm1 128.8(4) . . ? C7 N2 Sm1 127.4(3) . . ? C13 N3 Sm1 128.3(4) . . ? N1 C1 C6 121.3(5) . . ? N1 C1 C2 126.2(5) . . ? C6 C1 C2 112.5(5) . . ? F2 C2 C3 119.2(5) . . ? F2 C2 C1 117.3(5) . . ? C3 C2 C1 123.5(5) . . ? F3 C3 C4 119.5(6) . . ? F3 C3 C2 120.0(6) . . ? C4 C3 C2 120.6(5) . . ? F4 C4 C3 120.3(6) . . ? F4 C4 C5 121.0(6) . . ? C3 C4 C5 118.6(5) . . ? F5 C5 C6 119.9(5) . . ? F5 C5 C4 119.8(5) . . ? C6 C5 C4 120.3(5) . . ? C5 C6 F6 120.0(5) . . ? C5 C6 C1 124.5(5) . . ? F6 C6 C1 115.5(5) . . ? N2 C7 C12 120.7(5) . . ? N2 C7 C8 126.2(5) . . ? C12 C7 C8 113.1(5) . . ? F8 C8 C9 118.6(5) . . ? F8 C8 C7 117.8(5) . . ? C9 C8 C7 123.6(6) . . ? F9 C9 C10 120.5(6) . . ? F9 C9 C8 119.3(6) . . ? C10 C9 C8 120.2(6) . . ? F10 C10 C11 120.7(7) . . ? F10 C10 C9 120.6(6) . . ? C11 C10 C9 118.7(6) . . ? F11 C11 C10 120.1(6) . . ? F11 C11 C12 119.4(6) . . ? C10 C11 C12 120.5(6) . . ? F12 C12 C11 119.1(5) . . ? F12 C12 C7 117.0(5) . . ? C11 C12 C7 123.9(5) . . ? N3 C13 C18 121.1(5) . . ? N3 C13 C14 125.0(7) . . ? C18 C13 C14 113.9(6) . . ? F14 C14 C15 119.8(7) . . ? F14 C14 C13 118.9(6) . . ? C15 C14 C13 121.3(9) . . ? F15 C15 C16 120.2(9) . . ? F15 C15 C14 118.3(11) . . ? C16 C15 C14 121.4(8) . . ? F16 C16 C15 120.0(10) . . ? F16 C16 C17 120.7(11) . . ? C15 C16 C17 119.2(7) . . ? F17 C17 C16 120.5(7) . . ? F17 C17 C18 120.0(8) . . ? C16 C17 C18 119.4(9) . . ? F18 C18 C17 119.0(7) . . ? F18 C18 C13 116.3(5) . . ? C17 C18 C13 124.7(7) . . ? O1 C19 C20 105.5(5) . . ? C21 C20 C19 104.0(5) . . ? C20 C21 C22 102.0(6) . . ? O1 C22 C21 104.6(5) . . ? O2 C23 C24 105.9(6) . . ? C23 C24 C25 103.0(7) . . ? C26 C25 C24 106.2(6) . . ? O2 C26 C25 107.7(7) . . ? O3 C27 C28 105.6(6) . . ? C29 C28 C27 104.6(7) . . ? C28 C29 C30 108.1(7) . . ? O3 C30 C29 106.5(7) . . ? O4 C31 C32 100.6(17) . . ? C31 C32 C33 110.6(17) . . ? C34 C33 C32 105.1(14) . . ? O4 C34 C33 105.6(14) . . ? _refine_diff_density_max 1.492 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.117 #=========END=========== data_xr130 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H16 F30 N3 Nd' _chemical_formula_weight 1372.90 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 22.964(4) _cell_length_b 8.712(2) _cell_length_c 24.927(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.47(1) _cell_angle_gamma 90.00 _cell_volume 4756.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 198 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour 'light blue' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.917 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2668 _exptl_absorpt_coefficient_mu 1.252 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.79 _exptl_special_details ; ? ; _diffrn_ambient_temperature 198 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/PC' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7834 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.1113 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6217 _reflns_number_observed 3827 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS 2.10b (Siemens, 1994)' _computing_cell_refinement 'XSCANS 2.10b (Siemens, 1994)' _computing_data_reduction 'XSCANS 2.10b (Siemens, 1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL PC 4.2/360 (Siemens, 1990)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A lattice toluene is comprised of atoms C(37) thru C(43). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6213 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_obs 0.0577 _refine_ls_wR_factor_all 0.1252 _refine_ls_wR_factor_obs 0.1015 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_goodness_of_fit_obs 1.152 _refine_ls_restrained_S_all 1.069 _refine_ls_restrained_S_obs 1.152 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Nd1 Nd 0.23889(2) 0.18343(7) 0.17926(2) 0.0454(2) Uani 1 d . . N1 N 0.3119(3) 0.0062(9) 0.2355(3) 0.046(2) Uani 1 d . . N2 N 0.2603(3) 0.0918(9) 0.0967(3) 0.043(2) Uani 1 d . . N3 N 0.1333(3) 0.1907(9) 0.1309(2) 0.039(2) Uani 1 d . . C1 C 0.3661(4) -0.0174(12) 0.2213(4) 0.044(2) Uani 1 d . . C2 C 0.4170(5) 0.0733(14) 0.2401(4) 0.060(3) Uani 1 d . . C3 C 0.4682(5) 0.0637(15) 0.2230(5) 0.068(3) Uani 1 d . . C4 C 0.4706(5) -0.0436(15) 0.1848(4) 0.059(3) Uani 1 d . . C5 C 0.4224(5) -0.1423(13) 0.1649(4) 0.055(3) Uani 1 d . . C6 C 0.3716(5) -0.1297(13) 0.1837(4) 0.058(3) Uani 1 d . . F2 F 0.4163(3) 0.1850(10) 0.2776(3) 0.109(3) Uani 1 d . . F3 F 0.5147(3) 0.1581(10) 0.2429(3) 0.124(3) Uani 1 d . . F4 F 0.5193(3) -0.0544(8) 0.1661(3) 0.088(2) Uani 1 d . . F5 F 0.4235(3) -0.2480(8) 0.1260(3) 0.097(2) Uani 1 d . . F6 F 0.3255(3) -0.2278(7) 0.1621(3) 0.081(2) Uani 1 d . . C7 C 0.3001(4) -0.0902(12) 0.2759(4) 0.043(2) Uani 1 d . . C8 C 0.3399(5) -0.1889(14) 0.3135(4) 0.053(3) Uani 1 d . . C9 C 0.3221(5) -0.2770(12) 0.3515(4) 0.057(3) Uani 1 d . . C10 C 0.2641(6) -0.2699(14) 0.3544(4) 0.067(3) Uani 1 d . . C11 C 0.2231(5) -0.1715(15) 0.3196(4) 0.061(3) Uani 1 d . . C12 C 0.2423(5) -0.0875(12) 0.2812(4) 0.048(3) Uani 1 d . . F8 F 0.3979(3) -0.2045(8) 0.3126(2) 0.070(2) Uani 1 d . . F9 F 0.3619(3) -0.3745(7) 0.3848(2) 0.082(2) Uani 1 d . . F10 F 0.2464(3) -0.3556(8) 0.3917(2) 0.097(2) Uani 1 d . . F11 F 0.1658(3) -0.1590(9) 0.3208(2) 0.088(2) Uani 1 d . . F12 F 0.2004(2) 0.0094(7) 0.2448(2) 0.0559(15) Uani 1 d . . C13 C 0.2159(4) -0.0044(11) 0.0604(3) 0.041(2) Uani 1 d . . C14 C 0.1860(4) -0.1166(11) 0.0824(4) 0.042(2) Uani 1 d . . C15 C 0.1408(4) -0.2048(12) 0.0512(4) 0.047(3) Uani 1 d . . C16 C 0.1212(4) -0.1867(14) -0.0061(4) 0.052(3) Uani 1 d . . C17 C 0.1474(5) -0.0778(13) -0.0304(4) 0.050(3) Uani 1 d . . C18 C 0.1946(4) 0.0099(12) 0.0020(4) 0.048(3) Uani 1 d . . F14 F 0.2060(2) -0.1319(6) 0.1397(2) 0.0501(14) Uani 1 d . . F15 F 0.1162(2) -0.3126(7) 0.0765(2) 0.0634(15) Uani 1 d . . F16 F 0.0763(2) -0.2779(7) -0.0375(2) 0.073(2) Uani 1 d . . F17 F 0.1276(2) -0.0578(7) -0.0860(2) 0.072(2) Uani 1 d . . F18 F 0.2177(2) 0.1189(6) -0.0235(2) 0.058(2) Uani 1 d . . C19 C 0.3141(5) 0.1254(12) 0.0852(4) 0.046(3) Uani 1 d . . C20 C 0.3408(4) 0.0441(13) 0.0506(4) 0.048(3) Uani 1 d . . C21 C 0.3972(5) 0.0830(14) 0.0455(4) 0.059(3) Uani 1 d . . C22 C 0.4298(5) 0.2003(16) 0.0753(4) 0.063(3) Uani 1 d . . C23 C 0.4057(5) 0.2847(13) 0.1104(4) 0.061(3) Uani 1 d . . C24 C 0.3496(5) 0.2415(12) 0.1131(4) 0.053(3) Uani 1 d . . F20 F 0.3148(3) -0.0813(7) 0.0222(2) 0.067(2) Uani 1 d . . F21 F 0.4223(3) 0.0000(8) 0.0125(2) 0.077(2) Uani 1 d . . F22 F 0.4854(3) 0.2400(8) 0.0708(2) 0.085(2) Uani 1 d . . F23 F 0.4363(3) 0.4002(8) 0.1419(3) 0.087(2) Uani 1 d . . F24 F 0.3277(2) 0.3194(7) 0.1523(2) 0.0614(15) Uani 1 d . . C25 C 0.0819(4) 0.1713(13) 0.1508(3) 0.043(2) Uani 1 d . . C26 C 0.0675(5) 0.0255(13) 0.1668(4) 0.047(3) Uani 1 d . . C27 C 0.0183(5) 0.0058(15) 0.1878(4) 0.057(3) Uani 1 d . . C28 C -0.0173(5) 0.1307(16) 0.1921(4) 0.058(3) Uani 1 d . . C29 C -0.0049(5) 0.2696(15) 0.1751(4) 0.056(3) Uani 1 d . . C30 C 0.0444(4) 0.2893(13) 0.1560(4) 0.049(3) Uani 1 d . . F26 F 0.0991(2) -0.0976(6) 0.1617(2) 0.0536(15) Uani 1 d . . F27 F 0.0037(3) -0.1368(7) 0.2002(2) 0.071(2) Uani 1 d . . F28 F -0.0656(2) 0.1077(8) 0.2116(2) 0.075(2) Uani 1 d . . F29 F -0.0398(3) 0.3902(8) 0.1797(2) 0.075(2) Uani 1 d . . F30 F 0.0553(2) 0.4319(7) 0.1392(2) 0.061(2) Uani 1 d . . C31 C 0.1175(4) 0.2467(11) 0.0751(4) 0.041(2) Uani 1 d . . C32 C 0.0675(4) 0.2001(12) 0.0309(4) 0.046(2) Uani 1 d . . C33 C 0.0575(5) 0.2513(12) -0.0228(4) 0.049(3) Uani 1 d . . C34 C 0.0964(5) 0.3504(12) -0.0363(4) 0.057(3) Uani 1 d . . C35 C 0.1470(5) 0.4024(12) 0.0054(4) 0.049(3) Uani 1 d . . C36 C 0.1553(4) 0.3512(11) 0.0598(4) 0.043(3) Uani 1 d . . F31 F 0.0295(2) 0.0973(7) 0.0409(2) 0.061(2) Uani 1 d . . F32 F 0.0093(3) 0.1987(8) -0.0639(2) 0.079(2) Uani 1 d . . F33 F 0.0877(3) 0.3983(8) -0.0896(2) 0.083(2) Uani 1 d . . F34 F 0.1862(3) 0.5022(7) -0.0051(2) 0.071(2) Uani 1 d . . F35 F 0.2055(2) 0.4060(6) 0.1008(2) 0.0548(15) Uani 1 d . . C37 C 0.2086(6) 0.3396(15) 0.2891(5) 0.067(3) Uani 1 d . . C38 C 0.1792(6) 0.4360(16) 0.2478(6) 0.076(4) Uani 1 d . . H38 H 0.1372(6) 0.4494(16) 0.2398(6) 0.091 Uiso 1 calc R . C39 C 0.2091(10) 0.5127(17) 0.2182(5) 0.098(5) Uani 1 d . . H39 H 0.1873(10) 0.5796(17) 0.1903(5) 0.117 Uiso 1 calc R . C40 C 0.2678(12) 0.4985(24) 0.2263(9) 0.137(9) Uani 1 d . . H40 H 0.2867(12) 0.5506(24) 0.2035(9) 0.164 Uiso 1 calc R . C41 C 0.3018(7) 0.4034(25) 0.2698(9) 0.127(9) Uani 1 d . . H41 H 0.3440(7) 0.3970(25) 0.2786(9) 0.152 Uiso 1 calc R . C42 C 0.2695(8) 0.3174(17) 0.2999(4) 0.092(4) Uani 1 d . . H42 H 0.2899(8) 0.2463(17) 0.3268(4) 0.110 Uiso 1 calc R . C43 C 0.1721(8) 0.2635(16) 0.3229(6) 0.155(8) Uani 1 d . . H43A H 0.1983(8) 0.1979(16) 0.3508(6) 0.232 Uiso 1 calc R . H43B H 0.1399(8) 0.2036(16) 0.2984(6) 0.232 Uiso 1 calc R . H43C H 0.1548(8) 0.3406(16) 0.3411(6) 0.232 Uiso 1 calc R . C44 C 0.4022(8) 0.3733(25) -0.0614(5) 0.104(6) Uani 1 d . . C45 C 0.3450(7) 0.3128(20) -0.0582(5) 0.091(4) Uani 1 d . . H45 H 0.3334(7) 0.2131(20) -0.0700(5) 0.109 Uiso 1 calc R . C46 C 0.3093(7) 0.3997(19) -0.0383(5) 0.094(5) Uani 1 d . . H46 H 0.2713(7) 0.3613(19) -0.0389(5) 0.113 Uiso 1 calc R . C47 C 0.3256(7) 0.5476(19) -0.0162(5) 0.093(4) Uani 1 d . . H47 H 0.3003(7) 0.6045(19) -0.0007(5) 0.112 Uiso 1 calc R . C48 C 0.3774(8) 0.6002(20) -0.0183(6) 0.116(5) Uani 1 d . . H48 H 0.3897(8) 0.6976(20) -0.0041(6) 0.139 Uiso 1 calc R . C49 C 0.4151(7) 0.5160(22) -0.0412(6) 0.096(5) Uani 1 d . . H49 H 0.4513(7) 0.5607(22) -0.0427(6) 0.115 Uiso 1 calc R . C50 C 0.4410(7) 0.2840(21) -0.0823(5) 0.157(8) Uani 1 d . . H50A H 0.4222(7) 0.1865(21) -0.0945(5) 0.236 Uiso 1 calc R . H50B H 0.4789(7) 0.2685(21) -0.0533(5) 0.236 Uiso 1 calc R . H50C H 0.4486(7) 0.3357(21) -0.1136(5) 0.236 Uiso 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 Nd1 0.0519(3) 0.0459(3) 0.0371(3) -0.0016(4) 0.0116(2) -0.0032(4) N1 0.050(5) 0.044(5) 0.045(4) 0.004(4) 0.014(4) -0.006(4) N2 0.054(5) 0.030(5) 0.042(4) -0.005(4) 0.010(4) -0.009(4) N3 0.053(4) 0.033(4) 0.029(4) 0.004(4) 0.013(3) 0.003(5) C1 0.051(7) 0.041(7) 0.038(5) 0.010(5) 0.013(5) 0.002(6) C2 0.062(7) 0.078(9) 0.043(6) -0.011(6) 0.020(6) -0.013(7) C3 0.053(7) 0.074(9) 0.081(8) -0.005(8) 0.027(7) -0.018(7) C4 0.064(8) 0.070(9) 0.052(7) 0.019(7) 0.029(6) 0.023(8) C5 0.066(8) 0.057(9) 0.041(6) 0.002(6) 0.014(6) 0.018(7) C6 0.052(7) 0.052(8) 0.065(7) 0.001(6) 0.009(6) 0.010(6) F2 0.080(4) 0.140(7) 0.114(5) -0.073(6) 0.038(4) -0.040(5) F3 0.082(5) 0.124(7) 0.178(7) -0.048(6) 0.059(5) -0.047(5) F4 0.083(4) 0.092(5) 0.105(5) 0.013(4) 0.051(4) 0.012(4) F5 0.099(5) 0.096(6) 0.102(5) -0.033(5) 0.040(4) 0.022(4) F6 0.067(4) 0.057(5) 0.116(5) -0.031(4) 0.021(4) 0.002(4) C7 0.053(6) 0.039(7) 0.033(5) -0.004(5) 0.008(5) 0.001(6) C8 0.062(7) 0.053(7) 0.048(6) -0.014(7) 0.022(5) -0.010(7) C9 0.073(8) 0.047(8) 0.050(6) 0.006(6) 0.014(6) 0.002(7) C10 0.090(9) 0.060(9) 0.055(7) 0.008(6) 0.028(7) -0.012(8) C11 0.063(7) 0.061(8) 0.064(7) -0.003(7) 0.029(6) -0.008(8) C12 0.056(7) 0.053(7) 0.034(5) -0.008(5) 0.010(5) -0.001(6) F8 0.076(4) 0.085(5) 0.052(3) 0.025(4) 0.022(3) 0.018(4) F9 0.114(5) 0.066(5) 0.062(4) 0.023(4) 0.021(4) 0.017(4) F10 0.128(5) 0.099(6) 0.074(4) 0.029(4) 0.044(4) -0.022(5) F11 0.077(4) 0.109(6) 0.089(4) 0.013(5) 0.040(3) -0.019(5) F12 0.052(3) 0.065(4) 0.051(3) -0.003(3) 0.016(3) -0.003(3) C13 0.058(6) 0.029(6) 0.037(5) -0.002(5) 0.015(5) 0.013(5) C14 0.057(6) 0.034(6) 0.037(6) 0.006(5) 0.017(5) 0.007(6) C15 0.045(6) 0.034(7) 0.064(7) -0.009(6) 0.018(5) -0.010(6) C16 0.039(5) 0.052(7) 0.056(6) -0.031(7) 0.004(5) 0.003(7) C17 0.058(7) 0.046(7) 0.043(6) -0.013(6) 0.010(5) 0.002(6) C18 0.057(7) 0.043(7) 0.050(6) 0.002(6) 0.022(5) 0.004(6) F14 0.060(3) 0.044(4) 0.044(3) 0.002(3) 0.011(2) -0.008(3) F15 0.064(3) 0.042(3) 0.082(4) -0.008(4) 0.019(3) -0.013(4) F16 0.067(4) 0.065(5) 0.076(4) -0.025(4) 0.004(3) -0.010(4) F17 0.080(4) 0.090(5) 0.038(3) -0.015(3) 0.003(3) 0.007(4) F18 0.082(4) 0.056(4) 0.040(3) -0.004(3) 0.022(3) -0.002(3) C19 0.059(7) 0.042(7) 0.029(5) 0.004(5) 0.002(5) -0.007(6) C20 0.054(7) 0.046(7) 0.042(6) 0.009(6) 0.010(5) -0.005(6) C21 0.071(8) 0.055(8) 0.059(7) -0.003(6) 0.032(6) 0.002(7) C22 0.061(7) 0.081(10) 0.053(6) 0.026(7) 0.027(6) -0.008(8) C23 0.068(8) 0.061(9) 0.048(6) 0.004(6) 0.010(6) -0.034(7) C24 0.063(7) 0.057(7) 0.039(6) 0.004(6) 0.015(5) -0.004(6) F20 0.073(4) 0.062(4) 0.073(4) -0.013(4) 0.030(3) 0.006(4) F21 0.072(4) 0.091(5) 0.079(4) -0.003(4) 0.041(3) 0.004(4) F22 0.072(4) 0.102(6) 0.087(4) 0.012(4) 0.034(3) -0.025(4) F23 0.082(4) 0.092(5) 0.088(5) -0.009(4) 0.026(4) -0.042(4) F24 0.067(3) 0.061(4) 0.057(3) -0.013(4) 0.021(3) -0.016(4) C25 0.052(6) 0.045(7) 0.033(5) 0.001(6) 0.012(4) 0.005(6) C26 0.056(7) 0.044(8) 0.039(6) -0.003(6) 0.013(5) -0.006(6) C27 0.068(8) 0.061(9) 0.034(6) 0.007(6) 0.006(5) -0.009(7) C28 0.053(7) 0.087(10) 0.041(6) 0.015(7) 0.023(5) 0.008(7) C29 0.060(7) 0.078(10) 0.036(6) 0.014(6) 0.023(5) 0.020(7) C30 0.062(7) 0.049(8) 0.035(5) 0.000(5) 0.015(5) 0.008(6) F26 0.073(4) 0.036(4) 0.052(3) -0.001(3) 0.021(3) -0.003(3) F27 0.090(4) 0.068(5) 0.059(4) 0.004(3) 0.029(3) -0.019(4) F28 0.067(4) 0.103(5) 0.063(3) 0.010(4) 0.033(3) -0.004(4) F29 0.074(4) 0.097(5) 0.063(4) 0.014(4) 0.031(3) 0.030(4) F30 0.077(4) 0.052(4) 0.062(4) 0.011(3) 0.032(3) 0.010(3) C31 0.048(6) 0.033(6) 0.046(6) -0.007(5) 0.020(5) 0.011(5) C32 0.056(6) 0.040(7) 0.045(6) -0.001(6) 0.022(5) -0.008(6) C33 0.064(7) 0.046(7) 0.037(6) -0.006(5) 0.014(5) -0.002(6) C34 0.089(8) 0.048(8) 0.035(6) 0.008(6) 0.023(6) 0.026(7) C35 0.073(7) 0.031(6) 0.057(7) 0.013(6) 0.040(6) 0.009(6) C36 0.045(6) 0.034(7) 0.047(6) -0.007(5) 0.006(5) 0.009(5) F31 0.070(4) 0.066(4) 0.044(3) -0.009(3) 0.014(3) -0.020(4) F32 0.092(4) 0.089(5) 0.040(3) 0.001(4) -0.003(3) 0.001(4) F33 0.112(5) 0.087(5) 0.049(3) 0.022(4) 0.025(3) 0.020(4) F34 0.101(5) 0.053(4) 0.074(4) 0.017(3) 0.049(4) 0.008(4) F35 0.065(4) 0.042(4) 0.060(3) 0.005(3) 0.024(3) -0.001(3) C37 0.083(9) 0.063(9) 0.055(7) -0.019(7) 0.022(6) 0.008(8) C38 0.083(9) 0.073(10) 0.067(8) -0.042(8) 0.014(8) -0.001(9) C39 0.186(18) 0.057(10) 0.068(9) -0.017(8) 0.065(12) 0.015(12) C40 0.193(23) 0.128(19) 0.139(17) -0.092(15) 0.127(18) -0.084(18) C41 0.071(11) 0.156(22) 0.150(17) -0.130(16) 0.028(12) -0.044(12) C42 0.127(13) 0.076(10) 0.049(7) -0.025(8) -0.007(8) 0.037(12) C43 0.284(21) 0.101(13) 0.153(13) -0.059(11) 0.177(15) -0.069(13) C44 0.119(15) 0.147(18) 0.045(8) 0.011(10) 0.023(8) 0.034(14) C45 0.083(10) 0.114(13) 0.069(8) 0.007(10) 0.011(7) 0.017(11) C46 0.101(12) 0.082(12) 0.082(10) 0.024(9) 0.003(8) -0.044(11) C47 0.078(10) 0.100(14) 0.108(11) 0.026(10) 0.038(9) 0.010(10) C48 0.119(14) 0.108(14) 0.122(13) 0.021(11) 0.040(11) 0.004(13) C49 0.085(11) 0.113(15) 0.086(11) 0.040(11) 0.022(9) 0.015(12) C50 0.199(17) 0.214(21) 0.062(8) -0.005(11) 0.043(10) 0.084(16) _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 Nd1 N3 2.362(6) . ? Nd1 N2 2.392(7) . ? Nd1 N1 2.397(7) . ? Nd1 F12 2.572(5) . ? Nd1 F24 2.616(5) . ? Nd1 F35 2.696(5) . ? Nd1 F14 2.940(5) . ? Nd1 C41 2.982(13) . ? Nd1 C40 2.98(2) . ? Nd1 C42 3.103(10) . ? Nd1 C39 3.167(13) . ? Nd1 C37 3.313(10) . ? N1 C7 1.399(11) . ? N1 C1 1.409(11) . ? N2 C19 1.382(11) . ? N2 C13 1.416(11) . ? N3 C31 1.414(10) . ? N3 C25 1.422(10) . ? C1 C2 1.370(13) . ? C1 C6 1.386(13) . ? C2 F2 1.354(11) . ? C2 C3 1.368(13) . ? C3 F3 1.322(12) . ? C3 C4 1.347(14) . ? C4 F4 1.337(10) . ? C4 C5 1.372(14) . ? C5 F5 1.343(11) . ? C5 C6 1.386(13) . ? C6 F6 1.340(11) . ? C7 C12 1.374(12) . ? C7 C8 1.393(13) . ? C8 F8 1.346(10) . ? C8 C9 1.373(13) . ? C9 F9 1.339(11) . ? C9 C10 1.356(14) . ? C10 F10 1.346(11) . ? C10 C11 1.373(14) . ? C11 F11 1.332(10) . ? C11 C12 1.376(13) . ? C12 F12 1.393(10) . ? C13 C18 1.394(11) . ? C13 C14 1.398(12) . ? C14 C15 1.337(12) . ? C14 F14 1.368(9) . ? C15 F15 1.345(10) . ? C15 C16 1.371(12) . ? C16 F16 1.350(10) . ? C16 C17 1.359(13) . ? C17 F17 1.335(10) . ? C17 C18 1.373(12) . ? C18 F18 1.338(10) . ? C19 C24 1.353(12) . ? C19 C20 1.392(13) . ? C20 F20 1.341(11) . ? C20 C21 1.381(13) . ? C21 F21 1.349(11) . ? C21 C22 1.350(14) . ? C22 F22 1.359(10) . ? C22 C23 1.381(14) . ? C23 F23 1.339(11) . ? C23 C24 1.362(13) . ? C24 F24 1.401(10) . ? C25 C30 1.372(13) . ? C25 C26 1.400(13) . ? C26 F26 1.322(11) . ? C26 C27 1.391(13) . ? C27 F27 1.346(12) . ? C27 C28 1.384(14) . ? C28 C29 1.340(14) . ? C28 F28 1.353(10) . ? C29 F29 1.347(11) . ? C29 C30 1.366(13) . ? C30 F30 1.358(11) . ? C31 C36 1.389(12) . ? C31 C32 1.393(12) . ? C32 F31 1.325(10) . ? C32 C33 1.364(12) . ? C33 F32 1.344(10) . ? C33 C34 1.355(13) . ? C34 F33 1.349(10) . ? C34 C35 1.382(13) . ? C35 F34 1.333(10) . ? C35 C36 1.385(12) . ? C36 F35 1.376(9) . ? C37 C38 1.343(15) . ? C37 C42 1.36(2) . ? C37 C43 1.509(15) . ? C38 C39 1.33(2) . ? C39 C40 1.31(2) . ? C40 C41 1.40(2) . ? C41 C42 1.42(2) . ? C44 C49 1.34(2) . ? C44 C50 1.40(2) . ? C44 C45 1.44(2) . ? C45 C46 1.32(2) . ? C46 C47 1.41(2) . ? C47 C48 1.29(2) . ? C48 C49 1.38(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 N3 Nd1 N2 90.8(2) . . ? N3 Nd1 N1 138.3(3) . . ? N2 Nd1 N1 90.0(2) . . ? N3 Nd1 F12 81.0(2) . . ? N2 Nd1 F12 123.2(2) . . ? N1 Nd1 F12 64.1(2) . . ? N3 Nd1 F24 128.1(2) . . ? N2 Nd1 F24 63.4(2) . . ? N1 Nd1 F24 88.8(2) . . ? F12 Nd1 F24 150.9(2) . . ? N3 Nd1 F35 65.5(2) . . ? N2 Nd1 F35 72.7(2) . . ? N1 Nd1 F35 152.1(2) . . ? F12 Nd1 F35 143.8(2) . . ? F24 Nd1 F35 64.0(2) . . ? N3 Nd1 F14 74.5(2) . . ? N2 Nd1 F14 59.9(2) . . ? N1 Nd1 F14 70.0(2) . . ? F12 Nd1 F14 63.85(15) . . ? F24 Nd1 F14 118.6(2) . . ? F35 Nd1 F14 116.10(15) . . ? N3 Nd1 C41 124.0(4) . . ? N2 Nd1 C41 133.4(4) . . ? N1 Nd1 C41 82.9(5) . . ? F12 Nd1 C41 94.6(5) . . ? F24 Nd1 C41 70.4(4) . . ? F35 Nd1 C41 93.1(5) . . ? F14 Nd1 C41 150.7(5) . . ? N3 Nd1 C40 104.5(6) . . ? N2 Nd1 C40 124.5(4) . . ? N1 Nd1 C40 109.2(6) . . ? F12 Nd1 C40 111.8(4) . . ? F24 Nd1 C40 65.5(4) . . ? F35 Nd1 C40 66.7(5) . . ? F14 Nd1 C40 175.6(3) . . ? C41 Nd1 C40 27.2(4) . . ? N3 Nd1 C42 112.6(4) . . ? N2 Nd1 C42 156.1(4) . . ? N1 Nd1 C42 76.1(3) . . ? F12 Nd1 C42 68.1(4) . . ? F24 Nd1 C42 96.4(4) . . ? F35 Nd1 C42 111.4(3) . . ? F14 Nd1 C42 129.6(3) . . ? C41 Nd1 C42 26.9(4) . . ? C40 Nd1 C42 46.7(5) . . ? N3 Nd1 C39 81.3(4) . . ? N2 Nd1 C39 133.2(3) . . ? N1 Nd1 C39 125.6(3) . . ? F12 Nd1 C39 101.1(3) . . ? F24 Nd1 C39 85.7(4) . . ? F35 Nd1 C39 62.0(3) . . ? F14 Nd1 C39 153.1(4) . . ? C41 Nd1 C39 44.5(5) . . ? C40 Nd1 C39 24.3(4) . . ? C42 Nd1 C39 50.9(3) . . ? N3 Nd1 C37 88.4(3) . . ? N2 Nd1 C37 175.2(3) . . ? N1 Nd1 C37 93.7(3) . . ? F12 Nd1 C37 61.3(3) . . ? F24 Nd1 C37 113.6(2) . . ? F35 Nd1 C37 102.7(3) . . ? F14 Nd1 C37 124.4(2) . . ? C41 Nd1 C37 44.4(4) . . ? C40 Nd1 C37 51.3(4) . . ? C42 Nd1 C37 24.1(3) . . ? C39 Nd1 C37 42.0(3) . . ? C7 N1 C1 118.0(8) . . ? C7 N1 Nd1 123.7(6) . . ? C1 N1 Nd1 117.6(5) . . ? C19 N2 C13 120.7(7) . . ? C19 N2 Nd1 122.4(6) . . ? C13 N2 Nd1 116.9(5) . . ? C31 N3 C25 112.9(6) . . ? C31 N3 Nd1 115.6(5) . . ? C25 N3 Nd1 130.6(5) . . ? C2 C1 C6 113.4(9) . . ? C2 C1 N1 123.9(9) . . ? C6 C1 N1 122.6(9) . . ? F2 C2 C3 116.6(10) . . ? F2 C2 C1 117.7(9) . . ? C3 C2 C1 125.6(11) . . ? F3 C3 C4 119.9(10) . . ? F3 C3 C2 121.2(11) . . ? C4 C3 C2 119.0(11) . . ? F4 C4 C3 120.7(12) . . ? F4 C4 C5 119.9(11) . . ? C3 C4 C5 119.3(10) . . ? F5 C5 C4 120.2(10) . . ? F5 C5 C6 119.9(11) . . ? C4 C5 C6 119.9(10) . . ? F6 C6 C1 120.1(9) . . ? F6 C6 C5 117.2(10) . . ? C1 C6 C5 122.7(11) . . ? C12 C7 C8 113.8(9) . . ? C12 C7 N1 117.4(9) . . ? C8 C7 N1 128.7(9) . . ? F8 C8 C9 117.2(10) . . ? F8 C8 C7 120.3(9) . . ? C9 C8 C7 122.5(10) . . ? F9 C9 C10 119.6(10) . . ? F9 C9 C8 119.5(10) . . ? C10 C9 C8 120.9(10) . . ? F10 C10 C9 121.1(11) . . ? F10 C10 C11 119.4(11) . . ? C9 C10 C11 119.4(10) . . ? F11 C11 C10 122.1(10) . . ? F11 C11 C12 119.8(11) . . ? C10 C11 C12 118.1(10) . . ? C11 C12 C7 125.3(10) . . ? C11 C12 F12 118.3(9) . . ? C7 C12 F12 116.5(9) . . ? C12 F12 Nd1 118.0(5) . . ? C18 C13 C14 114.4(9) . . ? C18 C13 N2 125.0(9) . . ? C14 C13 N2 120.5(8) . . ? C15 C14 F14 120.6(9) . . ? C15 C14 C13 124.1(9) . . ? F14 C14 C13 115.3(8) . . ? C14 C15 F15 119.4(9) . . ? C14 C15 C16 119.6(10) . . ? F15 C15 C16 121.0(9) . . ? F16 C16 C17 121.0(9) . . ? F16 C16 C15 119.4(11) . . ? C17 C16 C15 119.6(9) . . ? F17 C17 C16 119.7(9) . . ? F17 C17 C18 120.1(10) . . ? C16 C17 C18 120.2(9) . . ? F18 C18 C17 118.1(9) . . ? F18 C18 C13 119.6(9) . . ? C17 C18 C13 122.1(10) . . ? C14 F14 Nd1 103.4(5) . . ? C24 C19 N2 119.4(9) . . ? C24 C19 C20 112.9(10) . . ? N2 C19 C20 127.5(9) . . ? F20 C20 C21 115.6(10) . . ? F20 C20 C19 122.1(9) . . ? C21 C20 C19 122.2(10) . . ? F21 C21 C22 118.2(10) . . ? F21 C21 C20 120.7(11) . . ? C22 C21 C20 121.0(10) . . ? C21 C22 F22 121.9(11) . . ? C21 C22 C23 119.3(10) . . ? F22 C22 C23 118.8(11) . . ? F23 C23 C24 121.1(11) . . ? F23 C23 C22 122.1(10) . . ? C24 C23 C22 116.7(10) . . ? C19 C24 C23 127.8(10) . . ? C19 C24 F24 115.7(9) . . ? C23 C24 F24 116.3(10) . . ? C24 F24 Nd1 115.5(5) . . ? C30 C25 C26 116.4(9) . . ? C30 C25 N3 123.6(10) . . ? C26 C25 N3 120.0(9) . . ? F26 C26 C27 117.8(10) . . ? F26 C26 C25 121.7(9) . . ? C27 C26 C25 120.5(10) . . ? F27 C27 C28 121.0(10) . . ? F27 C27 C26 119.1(11) . . ? C28 C27 C26 119.8(11) . . ? C29 C28 F28 121.4(11) . . ? C29 C28 C27 120.0(10) . . ? F28 C28 C27 118.5(11) . . ? C28 C29 F29 119.3(9) . . ? C28 C29 C30 120.0(11) . . ? F29 C29 C30 120.6(11) . . ? F30 C30 C29 118.1(10) . . ? F30 C30 C25 118.6(9) . . ? C29 C30 C25 123.3(11) . . ? C36 C31 C32 114.1(8) . . ? C36 C31 N3 120.0(8) . . ? C32 C31 N3 125.8(9) . . ? F31 C32 C33 118.7(9) . . ? F31 C32 C31 118.8(8) . . ? C33 C32 C31 122.5(9) . . ? F32 C33 C34 118.8(9) . . ? F32 C33 C32 119.6(9) . . ? C34 C33 C32 121.6(9) . . ? F33 C34 C33 121.8(10) . . ? F33 C34 C35 118.8(10) . . ? C33 C34 C35 119.4(9) . . ? F34 C35 C36 120.0(10) . . ? F34 C35 C34 122.1(9) . . ? C36 C35 C34 117.9(9) . . ? F35 C36 C35 117.0(9) . . ? F35 C36 C31 118.4(8) . . ? C35 C36 C31 124.6(9) . . ? C36 F35 Nd1 106.4(5) . . ? C38 C37 C42 119.5(13) . . ? C38 C37 C43 117.9(14) . . ? C42 C37 C43 122.6(15) . . ? C38 C37 Nd1 78.8(6) . . ? C42 C37 Nd1 69.2(6) . . ? C43 C37 Nd1 124.8(8) . . ? C39 C38 C37 121.0(13) . . ? C39 C38 Nd1 71.6(7) . . ? C37 C38 Nd1 77.9(7) . . ? C40 C39 C38 123.2(18) . . ? C40 C39 Nd1 69.8(10) . . ? C38 C39 Nd1 84.9(8) . . ? C39 C40 C41 119.0(20) . . ? C39 C40 Nd1 85.9(10) . . ? C41 C40 Nd1 76.5(11) . . ? C40 C41 C42 117.7(17) . . ? C40 C41 Nd1 76.3(9) . . ? C42 C41 Nd1 81.3(8) . . ? C37 C42 C41 119.4(14) . . ? C37 C42 Nd1 86.6(6) . . ? C41 C42 Nd1 71.8(7) . . ? C49 C44 C50 124.4(21) . . ? C49 C44 C45 114.8(16) . . ? C50 C44 C45 120.8(20) . . ? C46 C45 C44 119.5(17) . . ? C45 C46 C47 123.5(15) . . ? C48 C47 C46 116.7(16) . . ? C47 C48 C49 121.8(17) . . ? C44 C49 C48 123.6(17) . . ? _refine_diff_density_max 0.505 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.097 #=========END=========== data_xr181 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H27 F15 N3 Si3 Sm' _chemical_formula_weight 913.14 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'Sm' 'Sm' -0.1638 3.4418 '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 10.196(4) _cell_length_b 10.868(4) _cell_length_c 16.461(7) _cell_angle_alpha 94.96(1) _cell_angle_beta 107.33(1) _cell_angle_gamma 95.26(1) _cell_volume 1721.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 198 _cell_measurement_reflns_used 26 _cell_measurement_theta_min 11.5 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'irregular plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method ? _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 1.916 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ? ; _diffrn_ambient_temperature 198 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4/PC' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5381 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4479 _reflns_number_observed 3514 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS 2.10b (Siemens)' _computing_cell_refinement 'XSCANS 2.10b (Siemens)' _computing_data_reduction 'XSCANS 2.10b (Siemens)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL PC 4.2/360 (Siemens)' _computing_publication_material 'SHELXTL PC 4.2/360 (Siemens)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0911P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4476 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_obs 0.0564 _refine_ls_wR_factor_all 0.1528 _refine_ls_wR_factor_obs 0.1359 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sm1 Sm 0.06908(6) 0.28196(5) 0.25242(3) 0.0272(2) Uani 1 d . . Si1 Si 0.3373(3) 0.1144(3) 0.3087(2) 0.0366(7) Uani 1 d . . Si2 Si -0.0510(3) 0.5641(3) 0.2248(2) 0.0395(8) Uani 1 d . . Si3 Si -0.2005(3) 0.1082(3) 0.0938(2) 0.0328(7) Uani 1 d . . F2 F 0.1342(6) 0.4193(5) 0.3969(4) 0.0388(15) Uani 1 d . . F3 F 0.2189(8) 0.5547(7) 0.5521(4) 0.064(2) Uani 1 d . . F4 F 0.4650(9) 0.5224(8) 0.6704(4) 0.080(3) Uani 1 d . . F5 F 0.6228(8) 0.3569(7) 0.6252(4) 0.069(2) Uani 1 d . . F6 F 0.5404(7) 0.2229(7) 0.4710(4) 0.059(2) Uani 1 d . . F11 F 0.2334(6) 0.3203(5) 0.1615(4) 0.041(2) Uani 1 d . . F12 F 0.4408(7) 0.3868(6) 0.0994(5) 0.059(2) Uani 1 d . . F13 F 0.5141(8) 0.6326(7) 0.0868(5) 0.067(2) Uani 1 d . . F14 F 0.3734(7) 0.8074(6) 0.1410(4) 0.054(2) Uani 1 d . . F15 F 0.1662(7) 0.7422(5) 0.2020(5) 0.052(2) Uani 1 d . . F20 F -0.0249(7) 0.2140(5) 0.3717(4) 0.046(2) Uani 1 d . . F21 F -0.0912(8) 0.1012(6) 0.4960(4) 0.060(2) Uani 1 d . . F22 F -0.2601(8) -0.1197(7) 0.4571(5) 0.073(2) Uani 1 d . . F23 F -0.3711(8) -0.2185(6) 0.2899(5) 0.061(2) Uani 1 d . . F24 F -0.3133(7) -0.1036(6) 0.1650(4) 0.048(2) Uani 1 d . . N1 N 0.2745(8) 0.2414(8) 0.3491(5) 0.035(2) Uani 1 d . . N2 N 0.0833(8) 0.4835(7) 0.2149(5) 0.026(2) Uani 1 d . . N3 N -0.1223(8) 0.1248(7) 0.2043(5) 0.028(2) Uani 1 d . . C1 C 0.3288(10) 0.3097(9) 0.4275(6) 0.030(2) Uani 1 d . . C2 C 0.2553(11) 0.4015(9) 0.4541(6) 0.032(2) Uani 1 d . . C3 C 0.2961(13) 0.4700(11) 0.5341(7) 0.046(3) Uani 1 d . . C4 C 0.4199(14) 0.4554(12) 0.5918(7) 0.053(3) Uani 1 d . . C5 C 0.4995(12) 0.3695(11) 0.5690(7) 0.046(3) Uani 1 d . . C6 C 0.4568(12) 0.3013(10) 0.4899(7) 0.042(3) Uani 1 d . . C7 C 0.1926(13) 0.0486(10) 0.2086(7) 0.044(3) Uani 1 d . . C8 C 0.3595(15) -0.0175(10) 0.3771(8) 0.057(3) Uani 1 d . . H8A H 0.2774(15) -0.0359(10) 0.3932(8) 0.085 Uiso 1 calc R . H8B H 0.4373(15) 0.0062(10) 0.4277(8) 0.085 Uiso 1 calc R . H8C H 0.3752(15) -0.0899(10) 0.3452(8) 0.085 Uiso 1 calc R . C9 C 0.4930(13) 0.1533(13) 0.2762(9) 0.060(4) Uani 1 d . . H9A H 0.5690(13) 0.1871(13) 0.3257(9) 0.090 Uiso 1 calc R . H9B H 0.4752(13) 0.2135(13) 0.2361(9) 0.090 Uiso 1 calc R . H9C H 0.5157(13) 0.0794(13) 0.2497(9) 0.090 Uiso 1 calc R . C10 C 0.1893(10) 0.5265(9) 0.1832(6) 0.027(2) Uani 1 d . . C11 C 0.2667(11) 0.4439(9) 0.1552(7) 0.035(3) Uani 1 d . . C12 C 0.3742(12) 0.4754(10) 0.1241(7) 0.038(3) Uani 1 d . . C13 C 0.4083(11) 0.5971(11) 0.1179(7) 0.042(3) Uani 1 d . . C14 C 0.3385(12) 0.6839(9) 0.1450(7) 0.039(3) Uani 1 d . . C15 C 0.2299(10) 0.6500(9) 0.1752(7) 0.033(3) Uani 1 d . . C16 C -0.1740(12) 0.4426(10) 0.2482(8) 0.048(3) Uani 1 d . . H16A H -0.1288(12) 0.4113(10) 0.3009(8) 0.072 Uiso 1 calc R . H16B H -0.2022(12) 0.3756(10) 0.2023(8) 0.072 Uiso 1 calc R . H16C H -0.2539(12) 0.4790(10) 0.2534(8) 0.072 Uiso 1 calc R . C17 C 0.0002(15) 0.6903(11) 0.3190(9) 0.064(4) Uani 1 d . . H17A H 0.0483(15) 0.6566(11) 0.3701(9) 0.095 Uiso 1 calc R . H17B H -0.0813(15) 0.7215(11) 0.3260(9) 0.095 Uiso 1 calc R . H17C H 0.0597(15) 0.7568(11) 0.3087(9) 0.095 Uiso 1 calc R . C18 C -0.1446(13) 0.6202(13) 0.1234(9) 0.062(4) Uani 1 d . . H18A H -0.0847(13) 0.6827(13) 0.1094(9) 0.093 Uiso 1 calc R . H18B H -0.2246(13) 0.6553(13) 0.1296(9) 0.093 Uiso 1 calc R . H18C H -0.1731(13) 0.5519(13) 0.0783(9) 0.093 Uiso 1 calc R . C19 C -0.1639(10) 0.0606(9) 0.2624(6) 0.028(2) Uani 1 d . . C20 C -0.1141(11) 0.1042(10) 0.3497(7) 0.035(3) Uani 1 d . . C21 C -0.1451(12) 0.0491(11) 0.4147(7) 0.040(3) Uani 1 d . . C22 C -0.2318(12) -0.0607(11) 0.3939(7) 0.043(3) Uani 1 d . . C23 C -0.2854(11) -0.1082(10) 0.3101(8) 0.041(3) Uani 1 d . . C24 C -0.2558(11) -0.0514(9) 0.2462(7) 0.034(3) Uani 1 d . . C25 C -0.3852(12) 0.1404(11) 0.0654(8) 0.049(3) Uani 1 d . . H25A H -0.3906(12) 0.2173(11) 0.0969(8) 0.074 Uiso 1 calc R . H25B H -0.4399(12) 0.0739(11) 0.0797(8) 0.074 Uiso 1 calc R . H25C H -0.4198(12) 0.1463(11) 0.0050(8) 0.074 Uiso 1 calc R . C26 C -0.0979(12) 0.2322(10) 0.0563(6) 0.040(3) Uani 1 d . . H26A H -0.0030(12) 0.2165(10) 0.0704(6) 0.060 Uiso 1 calc R . H26B H -0.1028(12) 0.3123(10) 0.0840(6) 0.060 Uiso 1 calc R . H26C H -0.1356(12) 0.2308(10) -0.0047(6) 0.060 Uiso 1 calc R . C27 C -0.1820(14) -0.0420(10) 0.0344(7) 0.051(3) Uani 1 d . . H27A H -0.0863(14) -0.0553(10) 0.0506(7) 0.076 Uiso 1 calc R . H27B H -0.2152(14) -0.0377(10) -0.0261(7) 0.076 Uiso 1 calc R . H27C H -0.2351(14) -0.1097(10) 0.0487(7) 0.076 Uiso 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 Sm1 0.0271(3) 0.0255(3) 0.0305(3) 0.0008(2) 0.0123(2) 0.0012(2) Si1 0.040(2) 0.033(2) 0.042(2) 0.0071(13) 0.0164(15) 0.0135(14) Si2 0.036(2) 0.029(2) 0.060(2) 0.0002(14) 0.026(2) 0.0077(14) Si3 0.033(2) 0.035(2) 0.030(2) -0.0038(12) 0.0112(13) 0.0011(13) F2 0.039(4) 0.040(3) 0.036(3) -0.005(3) 0.013(3) 0.001(3) F3 0.077(5) 0.060(5) 0.053(4) -0.023(3) 0.030(4) 0.002(4) F4 0.084(6) 0.104(6) 0.032(4) -0.022(4) 0.006(4) -0.023(5) F5 0.062(5) 0.078(5) 0.046(4) 0.012(4) -0.012(4) -0.009(4) F6 0.040(4) 0.068(5) 0.061(4) 0.006(4) 0.001(3) 0.014(4) F11 0.051(4) 0.029(3) 0.058(4) 0.008(3) 0.036(3) 0.012(3) F12 0.059(5) 0.057(4) 0.085(5) 0.017(4) 0.053(4) 0.023(4) F13 0.056(5) 0.068(5) 0.095(6) 0.017(4) 0.050(4) -0.001(4) F14 0.057(4) 0.038(4) 0.074(5) 0.015(3) 0.029(4) -0.002(3) F15 0.062(4) 0.024(3) 0.084(5) 0.001(3) 0.048(4) 0.005(3) F20 0.058(4) 0.040(4) 0.034(3) -0.002(3) 0.016(3) -0.020(3) F21 0.076(5) 0.073(5) 0.032(4) 0.004(3) 0.025(4) -0.012(4) F22 0.085(6) 0.076(5) 0.066(5) 0.030(4) 0.037(5) -0.016(4) F23 0.060(5) 0.049(4) 0.069(5) 0.011(3) 0.019(4) -0.021(4) F24 0.058(4) 0.042(4) 0.042(4) -0.007(3) 0.019(3) -0.011(3) N1 0.027(5) 0.042(5) 0.039(5) -0.005(4) 0.012(4) 0.011(4) N2 0.025(5) 0.024(4) 0.036(5) 0.003(4) 0.018(4) 0.009(4) N3 0.028(5) 0.028(4) 0.031(5) 0.004(4) 0.013(4) 0.005(4) C1 0.030(6) 0.033(6) 0.025(6) 0.008(5) 0.009(5) -0.012(5) C2 0.035(6) 0.039(6) 0.020(5) 0.000(5) 0.007(5) -0.001(5) C3 0.055(8) 0.046(7) 0.043(7) 0.001(6) 0.028(7) -0.003(6) C4 0.056(9) 0.056(8) 0.038(7) 0.003(6) 0.009(7) -0.018(7) C5 0.038(7) 0.051(7) 0.036(7) 0.012(6) -0.003(6) -0.011(6) C6 0.042(7) 0.037(6) 0.044(7) 0.004(5) 0.010(6) -0.010(6) C7 0.060(8) 0.040(7) 0.037(6) 0.002(5) 0.020(6) 0.008(6) C8 0.081(10) 0.030(6) 0.061(8) 0.014(6) 0.020(7) 0.010(6) C9 0.047(8) 0.077(9) 0.070(9) 0.015(7) 0.033(7) 0.027(7) C10 0.018(5) 0.033(6) 0.030(5) 0.000(4) 0.008(5) 0.005(4) C11 0.036(6) 0.026(6) 0.041(6) 0.006(5) 0.009(5) 0.003(5) C12 0.043(7) 0.041(7) 0.043(7) 0.015(5) 0.025(6) 0.019(6) C13 0.035(7) 0.053(8) 0.045(7) 0.015(6) 0.023(6) -0.009(6) C14 0.045(7) 0.028(6) 0.051(7) 0.009(5) 0.021(6) 0.004(5) C15 0.027(6) 0.034(6) 0.042(6) -0.002(5) 0.014(5) 0.007(5) C16 0.036(7) 0.045(7) 0.075(9) -0.007(6) 0.040(7) 0.001(5) C17 0.084(10) 0.041(7) 0.079(10) -0.012(7) 0.046(9) 0.022(7) C18 0.043(8) 0.066(9) 0.086(10) 0.016(7) 0.026(7) 0.022(7) C19 0.026(6) 0.029(6) 0.036(6) -0.001(5) 0.018(5) 0.016(5) C20 0.034(6) 0.038(6) 0.036(6) 0.006(5) 0.016(5) 0.000(5) C21 0.042(7) 0.052(7) 0.028(6) 0.006(5) 0.017(5) 0.002(6) C22 0.038(7) 0.052(7) 0.043(7) 0.015(6) 0.020(6) -0.001(6) C23 0.032(6) 0.030(6) 0.066(8) 0.010(6) 0.021(6) 0.000(5) C24 0.031(6) 0.025(6) 0.049(7) 0.003(5) 0.017(5) 0.001(5) C25 0.040(7) 0.053(8) 0.056(8) 0.004(6) 0.016(6) 0.010(6) C26 0.049(7) 0.048(7) 0.024(6) 0.000(5) 0.015(5) -0.003(6) C27 0.063(8) 0.040(7) 0.050(7) -0.014(6) 0.026(7) 0.008(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 Sm1 N1 2.328(8) . ? Sm1 N2 2.331(8) . ? Sm1 N3 2.363(8) . ? Sm1 F20 2.561(6) . ? Sm1 F2 2.567(5) . ? Sm1 F11 2.587(6) . ? Sm1 C7 3.058(11) . ? Sm1 Si1 3.368(3) . ? Sm1 Si2 3.421(3) . ? Sm1 Si3 3.444(3) . ? Si1 N1 1.736(8) . ? Si1 C9 1.846(12) . ? Si1 C7 1.886(12) . ? Si1 C8 1.887(11) . ? Si2 N2 1.731(8) . ? Si2 C18 1.845(13) . ? Si2 C16 1.880(11) . ? Si2 C17 1.891(12) . ? Si3 N3 1.741(8) . ? Si3 C25 1.874(12) . ? Si3 C27 1.883(10) . ? Si3 C26 1.887(11) . ? F2 C2 1.353(12) . ? F3 C3 1.334(14) . ? F4 C4 1.355(13) . ? F5 C5 1.348(13) . ? F6 C6 1.339(14) . ? F11 C11 1.374(11) . ? F12 C12 1.330(12) . ? F13 C13 1.365(12) . ? F14 C14 1.369(11) . ? F15 C15 1.354(11) . ? F20 C20 1.383(11) . ? F21 C21 1.336(12) . ? F22 C22 1.355(12) . ? F23 C23 1.370(12) . ? F24 C24 1.339(12) . ? N1 C1 1.362(12) . ? N2 C10 1.394(12) . ? N3 C19 1.373(12) . ? C1 C6 1.417(15) . ? C1 C2 1.417(15) . ? C2 C3 1.381(15) . ? C3 C4 1.37(2) . ? C4 C5 1.39(2) . ? C5 C6 1.37(2) . ? C10 C11 1.384(14) . ? C10 C15 1.397(14) . ? C11 C12 1.371(15) . ? C12 C13 1.357(15) . ? C13 C14 1.35(2) . ? C14 C15 1.376(15) . ? C19 C20 1.397(14) . ? C19 C24 1.421(14) . ? C20 C21 1.372(14) . ? C21 C22 1.37(2) . ? C22 C23 1.36(2) . ? C23 C24 1.359(15) . ? 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 Sm1 N2 112.4(3) . . ? N1 Sm1 N3 119.7(3) . . ? N2 Sm1 N3 127.9(3) . . ? N1 Sm1 F20 80.8(3) . . ? N2 Sm1 F20 125.2(2) . . ? N3 Sm1 F20 66.2(2) . . ? N1 Sm1 F2 66.9(2) . . ? N2 Sm1 F2 76.5(2) . . ? N3 Sm1 F2 123.7(2) . . ? F20 Sm1 F2 59.9(2) . . ? N1 Sm1 F11 80.9(3) . . ? N2 Sm1 F11 66.4(2) . . ? N3 Sm1 F11 120.7(2) . . ? F20 Sm1 F11 161.2(2) . . ? F2 Sm1 F11 115.5(2) . . ? N1 Sm1 C7 62.2(3) . . ? N2 Sm1 C7 133.2(3) . . ? N3 Sm1 C7 75.7(3) . . ? F20 Sm1 C7 100.6(3) . . ? F2 Sm1 C7 127.9(3) . . ? F11 Sm1 C7 67.0(2) . . ? N1 Sm1 Si1 28.7(2) . . ? N2 Sm1 Si1 125.0(2) . . ? N3 Sm1 Si1 102.0(2) . . ? F20 Sm1 Si1 92.6(2) . . ? F2 Sm1 Si1 95.49(15) . . ? F11 Sm1 Si1 69.19(14) . . ? C7 Sm1 Si1 33.7(2) . . ? N1 Sm1 Si2 127.5(2) . . ? N2 Sm1 Si2 27.5(2) . . ? N3 Sm1 Si2 108.3(2) . . ? F20 Sm1 Si2 101.6(2) . . ? F2 Sm1 Si2 69.67(15) . . ? F11 Sm1 Si2 92.74(13) . . ? C7 Sm1 Si2 157.0(2) . . ? Si1 Sm1 Si2 149.55(8) . . ? N1 Sm1 Si3 135.7(2) . . ? N2 Sm1 Si3 107.0(2) . . ? N3 Sm1 Si3 27.7(2) . . ? F20 Sm1 Si3 92.83(14) . . ? F2 Sm1 Si3 144.26(14) . . ? F11 Sm1 Si3 97.49(15) . . ? C7 Sm1 Si3 76.3(2) . . ? Si1 Sm1 Si3 109.42(8) . . ? Si2 Sm1 Si3 96.74(8) . . ? N1 Si1 C9 114.8(5) . . ? N1 Si1 C7 103.8(5) . . ? C9 Si1 C7 107.2(6) . . ? N1 Si1 C8 114.7(5) . . ? C9 Si1 C8 111.1(6) . . ? C7 Si1 C8 104.2(5) . . ? N1 Si1 Sm1 40.1(3) . . ? C9 Si1 Sm1 120.1(4) . . ? C7 Si1 Sm1 64.1(4) . . ? C8 Si1 Sm1 128.8(5) . . ? N2 Si2 C18 112.1(5) . . ? N2 Si2 C16 103.6(4) . . ? C18 Si2 C16 107.1(6) . . ? N2 Si2 C17 114.2(5) . . ? C18 Si2 C17 112.6(6) . . ? C16 Si2 C17 106.3(6) . . ? N2 Si2 Sm1 38.5(3) . . ? C18 Si2 Sm1 127.7(4) . . ? C16 Si2 Sm1 65.5(4) . . ? C17 Si2 Sm1 119.1(4) . . ? N3 Si3 C25 111.6(5) . . ? N3 Si3 C27 115.3(5) . . ? C25 Si3 C27 111.9(6) . . ? N3 Si3 C26 103.8(4) . . ? C25 Si3 C26 108.8(5) . . ? C27 Si3 C26 104.7(5) . . ? N3 Si3 Sm1 39.1(3) . . ? C25 Si3 Sm1 124.5(4) . . ? C27 Si3 Sm1 123.3(4) . . ? C26 Si3 Sm1 64.7(3) . . ? C2 F2 Sm1 115.1(5) . . ? C11 F11 Sm1 114.0(5) . . ? C20 F20 Sm1 114.8(5) . . ? C1 N1 Si1 127.5(7) . . ? C1 N1 Sm1 121.3(7) . . ? Si1 N1 Sm1 111.1(4) . . ? C10 N2 Si2 126.0(6) . . ? C10 N2 Sm1 120.0(6) . . ? Si2 N2 Sm1 114.0(4) . . ? C19 N3 Si3 126.8(7) . . ? C19 N3 Sm1 119.9(6) . . ? Si3 N3 Sm1 113.2(4) . . ? N1 C1 C6 127.3(10) . . ? N1 C1 C2 120.1(9) . . ? C6 C1 C2 112.6(9) . . ? F2 C2 C3 118.6(10) . . ? F2 C2 C1 116.5(8) . . ? C3 C2 C1 124.9(10) . . ? F3 C3 C4 120.9(11) . . ? F3 C3 C2 119.7(11) . . ? C4 C3 C2 119.2(12) . . ? F4 C4 C3 121.2(13) . . ? F4 C4 C5 119.9(12) . . ? C3 C4 C5 118.9(11) . . ? F5 C5 C6 119.9(12) . . ? F5 C5 C4 118.9(11) . . ? C6 C5 C4 121.2(11) . . ? F6 C6 C5 118.1(10) . . ? F6 C6 C1 118.8(9) . . ? C5 C6 C1 123.1(12) . . ? Si1 C7 Sm1 82.2(4) . . ? C11 C10 N2 120.5(9) . . ? C11 C10 C15 112.8(9) . . ? N2 C10 C15 126.7(9) . . ? C12 C11 F11 118.1(9) . . ? C12 C11 C10 125.6(9) . . ? F11 C11 C10 116.3(9) . . ? F12 C12 C13 121.7(10) . . ? F12 C12 C11 119.7(9) . . ? C13 C12 C11 118.6(10) . . ? C14 C13 C12 119.3(10) . . ? C14 C13 F13 120.0(10) . . ? C12 C13 F13 120.6(11) . . ? C13 C14 F14 120.2(10) . . ? C13 C14 C15 121.0(10) . . ? F14 C14 C15 118.8(10) . . ? F15 C15 C14 117.6(9) . . ? F15 C15 C10 119.8(9) . . ? C14 C15 C10 122.6(9) . . ? N3 C19 C20 120.2(9) . . ? N3 C19 C24 128.0(9) . . ? C20 C19 C24 111.8(9) . . ? C21 C20 F20 117.6(9) . . ? C21 C20 C19 126.5(10) . . ? F20 C20 C19 115.9(8) . . ? F21 C21 C22 121.3(9) . . ? F21 C21 C20 120.6(10) . . ? C22 C21 C20 118.1(10) . . ? F22 C22 C23 121.9(10) . . ? F22 C22 C21 119.4(10) . . ? C23 C22 C21 118.7(10) . . ? C24 C23 C22 122.6(10) . . ? C24 C23 F23 119.1(10) . . ? C22 C23 F23 118.3(10) . . ? F24 C24 C23 119.1(9) . . ? F24 C24 C19 118.6(9) . . ? C23 C24 C19 122.3(10) . . ? _refine_diff_density_max 1.378 _refine_diff_density_min -2.026 _refine_diff_density_rms 0.159 #=========END===========