data_global _publ_contact_author_email PHILIP.GALE@SOTON.AC.UK _publ_contact_author_name 'Dr Philip Gale' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year 2003 _journal_volume ? _journal_page_first 568 loop_ _publ_author_name S.J.Coles J.G.Frey P.A.Gale M.B.Hursthouse M.E.Light ; K.Navakhun ; G.L.Thomas data_1SiF6 _database_code_CSD 197049 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H50 F3 N5 O6 Si0.50' _chemical_formula_weight 719.85 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' F F 0.0171 0.0103 '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' _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 11.4442(6) _cell_length_b 12.3142(8) _cell_length_c 13.2507(7) _cell_angle_alpha 86.370(5) _cell_angle_beta 85.797(4) _cell_angle_gamma 78.520(2) _cell_volume 1822.82(18) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 37549 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.1 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9863 _exptl_absorpt_correction_T_max 0.9954 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 26306 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.1183 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.24 _reflns_number_total 7951 _reflns_number_gt 4165 _reflns_threshold_expression >2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.4508P] 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 0.0007(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7951 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1604 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2010 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 C1 C 0.2070(3) -0.2577(3) 0.3434(2) 0.0330(8) Uani 1 1 d . . . C2 C 0.3007(3) -0.2305(3) 0.3890(2) 0.0361(8) Uani 1 1 d . . . H2 H 0.3038 -0.2347 0.4607 0.043 Uiso 1 1 calc R . . C3 C 0.3907(3) -0.1964(3) 0.3262(2) 0.0337(8) Uani 1 1 d . . . H3 H 0.4568 -0.1771 0.3551 0.040 Uiso 1 1 calc R . . C4 C 0.3848(3) -0.1904(3) 0.2216(2) 0.0311(7) Uani 1 1 d . . . H4 H 0.4455 -0.1647 0.1794 0.037 Uiso 1 1 calc R . . C5 C 0.2899(3) -0.2220(3) 0.1784(2) 0.0299(7) Uani 1 1 d . . . C6 C 0.1992(3) -0.2564(3) 0.2399(2) 0.0310(7) Uani 1 1 d . . . H6 H 0.1341 -0.2783 0.2117 0.037 Uiso 1 1 calc R . . C7 C 0.2245(3) -0.2626(3) 0.0136(2) 0.0294(7) Uani 1 1 d . . . C8 C 0.2304(3) -0.2350(2) -0.0988(2) 0.0278(7) Uani 1 1 d . . . C9 C 0.1339(3) -0.2493(3) -0.1503(2) 0.0330(8) Uani 1 1 d . . . H9 H 0.0676 -0.2719 -0.1136 0.040 Uiso 1 1 calc R . . C10 C 0.1327(3) -0.2312(3) -0.2546(2) 0.0366(8) Uani 1 1 d . . . H10 H 0.0655 -0.2396 -0.2892 0.044 Uiso 1 1 calc R . . C11 C 0.2306(3) -0.2010(3) -0.3073(2) 0.0341(8) Uani 1 1 d . . . H11 H 0.2304 -0.1893 -0.3789 0.041 Uiso 1 1 calc R . . C12 C 0.3292(3) -0.1873(3) -0.2586(2) 0.0302(7) Uani 1 1 d . . . C13 C 0.3292(3) -0.2033(2) -0.1533(2) 0.0286(7) Uani 1 1 d . . . H13 H 0.3957 -0.1928 -0.1188 0.034 Uiso 1 1 calc R . . C14 C 0.4339(3) -0.1636(3) -0.3254(2) 0.0320(8) Uani 1 1 d . . . C15 C 0.6265(3) -0.1000(3) -0.3273(2) 0.0300(7) Uani 1 1 d . . . C16 C 0.7084(3) -0.0765(3) -0.2634(2) 0.0334(8) Uani 1 1 d . . . H16 H 0.6890 -0.0747 -0.1925 0.040 Uiso 1 1 calc R . . C17 C 0.8174(3) -0.0559(3) -0.3023(3) 0.0376(8) Uani 1 1 d . . . H17 H 0.8722 -0.0398 -0.2576 0.045 Uiso 1 1 calc R . . C18 C 0.8484(3) -0.0583(3) -0.4047(3) 0.0377(8) Uani 1 1 d . . . H18 H 0.9236 -0.0446 -0.4316 0.045 Uiso 1 1 calc R . . C19 C 0.7661(3) -0.0812(3) -0.4659(2) 0.0357(8) Uani 1 1 d . . . C20 C 0.6552(3) -0.1016(3) -0.4314(2) 0.0338(8) Uani 1 1 d . . . H20 H 0.6005 -0.1161 -0.4770 0.041 Uiso 1 1 calc R . . C21 C -0.1644(3) -0.4055(3) 0.0391(2) 0.0282(7) Uani 1 1 d . . . H21A H -0.1664 -0.4854 0.0382 0.034 Uiso 1 1 calc R . . H21B H -0.0807 -0.3995 0.0478 0.034 Uiso 1 1 calc R . . C22 C -0.1994(3) -0.3512(3) -0.0633(2) 0.0309(7) Uani 1 1 d . . . H22A H -0.1867 -0.2738 -0.0682 0.037 Uiso 1 1 calc R . . H22B H -0.2851 -0.3497 -0.0714 0.037 Uiso 1 1 calc R . . C23 C -0.1231(3) -0.4174(3) -0.1466(2) 0.0342(8) Uani 1 1 d . . . H23A H -0.0377 -0.4225 -0.1349 0.041 Uiso 1 1 calc R . . H23B H -0.1391 -0.4937 -0.1424 0.041 Uiso 1 1 calc R . . C24 C -0.1469(3) -0.3661(3) -0.2526(3) 0.0427(9) Uani 1 1 d . . . H24A H -0.2316 -0.3597 -0.2644 0.064 Uiso 1 1 calc R . . H24B H -0.0979 -0.4133 -0.3028 0.064 Uiso 1 1 calc R . . H24C H -0.1265 -0.2922 -0.2586 0.064 Uiso 1 1 calc R . . C25 C -0.2479(3) -0.2339(2) 0.1331(2) 0.0277(7) Uani 1 1 d . . . H25A H -0.2833 -0.1980 0.0705 0.033 Uiso 1 1 calc R . . H25B H -0.3024 -0.2056 0.1912 0.033 Uiso 1 1 calc R . . C26 C -0.1282(3) -0.2000(2) 0.1417(2) 0.0299(7) Uani 1 1 d . . . H26A H -0.1015 -0.2194 0.2111 0.036 Uiso 1 1 calc R . . H26B H -0.0678 -0.2414 0.0937 0.036 Uiso 1 1 calc R . . C27 C -0.1376(3) -0.0760(3) 0.1188(2) 0.0319(7) Uani 1 1 d . . . H27A H -0.1621 -0.0568 0.0487 0.038 Uiso 1 1 calc R . . H27B H -0.1995 -0.0345 0.1656 0.038 Uiso 1 1 calc R . . C28 C -0.0191(3) -0.0426(3) 0.1303(3) 0.0471(9) Uani 1 1 d . . . H28A H 0.0039 -0.0595 0.2002 0.071 Uiso 1 1 calc R . . H28B H -0.0266 0.0372 0.1141 0.071 Uiso 1 1 calc R . . H28C H 0.0422 -0.0838 0.0839 0.071 Uiso 1 1 calc R . . C29 C -0.1847(3) -0.4189(3) 0.2244(2) 0.0290(7) Uani 1 1 d . . . H29A H -0.1038 -0.4023 0.2270 0.035 Uiso 1 1 calc R . . H29B H -0.1751 -0.4997 0.2169 0.035 Uiso 1 1 calc R . . C30 C -0.2537(3) -0.3903(3) 0.3247(2) 0.0413(9) Uani 1 1 d . . . H30A H -0.2530 -0.3124 0.3383 0.050 Uiso 1 1 calc R . . H30B H -0.3378 -0.3973 0.3201 0.050 Uiso 1 1 calc R . . C31 C -0.2004(3) -0.4658(3) 0.4113(2) 0.0430(9) Uani 1 1 d . . . H31A H -0.1978 -0.5439 0.3958 0.052 Uiso 1 1 calc R . . H31B H -0.1172 -0.4565 0.4172 0.052 Uiso 1 1 calc R . . C32 C -0.2697(5) -0.4426(4) 0.5111(3) 0.0725(14) Uani 1 1 d . . . H32A H -0.2699 -0.3663 0.5283 0.109 Uiso 1 1 calc R . . H32B H -0.2324 -0.4943 0.5641 0.109 Uiso 1 1 calc R . . H32C H -0.3521 -0.4520 0.5060 0.109 Uiso 1 1 calc R . . C33 C -0.3687(3) -0.3750(3) 0.1262(2) 0.0277(7) Uani 1 1 d . . . H33A H -0.4037 -0.3310 0.0668 0.033 Uiso 1 1 calc R . . H33B H -0.4157 -0.3449 0.1875 0.033 Uiso 1 1 calc R . . C34 C -0.3820(3) -0.4950(3) 0.1190(2) 0.0310(7) Uani 1 1 d . . . H34A H -0.3320 -0.5429 0.1687 0.037 Uiso 1 1 calc R . . H34B H -0.3533 -0.5201 0.0504 0.037 Uiso 1 1 calc R . . C35 C -0.5120(3) -0.5065(3) 0.1398(3) 0.0363(8) Uani 1 1 d . . . H35A H -0.5636 -0.4442 0.1038 0.044 Uiso 1 1 calc R . . H35B H -0.5227 -0.5762 0.1117 0.044 Uiso 1 1 calc R . . C36 C -0.5527(3) -0.5074(3) 0.2514(3) 0.0465(9) Uani 1 1 d . . . H36A H -0.5023 -0.5690 0.2877 0.070 Uiso 1 1 calc R . . H36B H -0.6360 -0.5167 0.2593 0.070 Uiso 1 1 calc R . . H36C H -0.5462 -0.4371 0.2792 0.070 Uiso 1 1 calc R . . N1 N 0.1061(3) -0.2877(2) 0.4078(2) 0.0396(7) Uani 1 1 d . . . N2 N 0.2879(3) -0.2115(2) 0.0710(2) 0.0307(6) Uani 1 1 d . . . N3 N 0.5167(2) -0.1212(2) -0.2824(2) 0.0338(7) Uani 1 1 d . . . N4 N 0.7963(3) -0.0835(3) -0.5766(2) 0.0451(8) Uani 1 1 d . . . N5 N -0.2407(2) -0.3587(2) 0.13095(18) 0.0261(6) Uani 1 1 d . . . O1 O 0.0323(2) -0.3283(2) 0.36804(18) 0.0532(7) Uani 1 1 d . . . O2 O 0.1001(2) -0.2694(2) 0.49813(18) 0.0518(7) Uani 1 1 d . . . O3 O 0.1629(2) -0.32894(19) 0.04843(16) 0.0376(6) Uani 1 1 d . . . O4 O 0.4431(2) -0.1863(3) -0.41478(18) 0.0548(8) Uani 1 1 d . . . O5 O 0.8940(3) -0.0638(2) -0.6086(2) 0.0575(8) Uani 1 1 d . . . O6 O 0.7226(3) -0.1039(2) -0.63144(19) 0.0581(8) Uani 1 1 d . . . F1 F 0.52959(18) -0.13829(17) -0.01472(16) 0.0509(6) Uani 1 1 d . . . F2 F 0.35911(17) -0.00618(17) 0.03692(14) 0.0456(5) Uani 1 1 d . . . F3 F 0.46057(17) 0.02015(16) -0.12043(14) 0.0433(5) Uani 1 1 d . . . Si1 Si 0.5000 0.0000 0.0000 0.0346(3) Uani 1 2 d S . . H2N H 0.322(3) -0.164(3) 0.046(2) 0.024(9) Uiso 1 1 d . . . H3N H 0.504(3) -0.101(2) -0.229(2) 0.017(9) 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 C1 0.0327(19) 0.0333(19) 0.0307(18) -0.0007(14) 0.0006(14) -0.0017(15) C2 0.036(2) 0.041(2) 0.0296(18) -0.0037(15) -0.0046(15) -0.0010(16) C3 0.0314(19) 0.0333(19) 0.0367(19) -0.0062(14) -0.0076(15) -0.0037(15) C4 0.0299(18) 0.0286(18) 0.0332(18) -0.0014(14) -0.0028(14) -0.0015(14) C5 0.0351(19) 0.0256(17) 0.0276(17) 0.0001(13) -0.0029(14) -0.0029(14) C6 0.0326(19) 0.0326(18) 0.0284(17) 0.0012(14) -0.0057(14) -0.0070(15) C7 0.0294(18) 0.0275(17) 0.0296(17) -0.0043(14) -0.0005(14) -0.0011(15) C8 0.0315(18) 0.0213(16) 0.0293(17) -0.0022(13) 0.0006(14) -0.0029(14) C9 0.0297(19) 0.0341(19) 0.0348(19) -0.0039(14) -0.0001(14) -0.0051(15) C10 0.0298(19) 0.048(2) 0.0335(19) -0.0105(15) -0.0052(14) -0.0067(16) C11 0.039(2) 0.041(2) 0.0228(16) -0.0055(14) -0.0011(14) -0.0079(16) C12 0.0356(19) 0.0275(17) 0.0277(17) -0.0033(13) -0.0018(14) -0.0058(14) C13 0.0283(18) 0.0271(17) 0.0300(17) -0.0016(13) -0.0046(13) -0.0037(14) C14 0.0334(19) 0.0358(19) 0.0277(19) -0.0024(14) -0.0034(14) -0.0082(15) C15 0.0319(19) 0.0303(18) 0.0286(17) -0.0053(14) 0.0021(14) -0.0082(14) C16 0.036(2) 0.0294(18) 0.0334(18) -0.0053(14) 0.0015(14) -0.0029(15) C17 0.033(2) 0.036(2) 0.045(2) -0.0043(16) -0.0052(16) -0.0065(16) C18 0.033(2) 0.0302(19) 0.048(2) -0.0010(15) 0.0070(16) -0.0056(15) C19 0.043(2) 0.0327(19) 0.0331(19) -0.0034(14) 0.0063(15) -0.0135(16) C20 0.042(2) 0.0293(18) 0.0313(18) -0.0019(14) 0.0008(15) -0.0103(15) C21 0.0247(17) 0.0306(18) 0.0282(17) -0.0024(13) 0.0022(13) -0.0038(14) C22 0.0317(19) 0.0328(18) 0.0266(17) 0.0002(14) -0.0020(13) -0.0028(14) C23 0.039(2) 0.0310(18) 0.0332(18) -0.0008(14) 0.0007(14) -0.0094(15) C24 0.047(2) 0.049(2) 0.0315(19) 0.0045(16) -0.0013(15) -0.0111(18) C25 0.0266(17) 0.0266(17) 0.0294(17) -0.0039(13) -0.0039(13) -0.0021(13) C26 0.0303(18) 0.0253(17) 0.0342(18) 0.0003(13) -0.0035(14) -0.0061(14) C27 0.0330(19) 0.0304(18) 0.0326(18) 0.0013(14) -0.0050(14) -0.0066(15) C28 0.049(2) 0.036(2) 0.056(2) -0.0022(17) -0.0086(18) -0.0072(17) C29 0.0267(18) 0.0300(18) 0.0291(17) 0.0006(13) -0.0073(13) -0.0010(14) C30 0.046(2) 0.047(2) 0.0277(18) -0.0039(15) -0.0029(15) -0.0008(17) C31 0.054(2) 0.049(2) 0.0274(18) 0.0036(16) -0.0052(16) -0.0153(18) C32 0.098(4) 0.080(3) 0.032(2) -0.003(2) -0.001(2) 0.000(3) C33 0.0231(17) 0.0308(18) 0.0286(17) -0.0011(13) -0.0025(12) -0.0032(13) C34 0.0348(19) 0.0272(17) 0.0311(17) -0.0050(14) -0.0017(14) -0.0057(14) C35 0.035(2) 0.0328(19) 0.043(2) -0.0063(15) -0.0025(15) -0.0101(15) C36 0.047(2) 0.045(2) 0.049(2) -0.0032(17) 0.0106(17) -0.0174(18) N1 0.0395(18) 0.0488(19) 0.0283(17) 0.0044(13) 0.0003(13) -0.0058(15) N2 0.0343(16) 0.0321(16) 0.0281(15) 0.0045(12) -0.0007(12) -0.0148(14) N3 0.0384(18) 0.0415(17) 0.0235(16) -0.0103(13) 0.0046(13) -0.0123(13) N4 0.057(2) 0.0445(19) 0.0341(17) -0.0033(14) 0.0098(16) -0.0156(16) N5 0.0276(15) 0.0252(14) 0.0252(13) -0.0015(11) -0.0034(10) -0.0036(11) O1 0.0524(17) 0.079(2) 0.0347(14) 0.0032(13) -0.0035(12) -0.0297(15) O2 0.0513(17) 0.076(2) 0.0273(14) -0.0001(13) 0.0001(11) -0.0127(14) O3 0.0476(15) 0.0351(13) 0.0339(13) -0.0021(10) 0.0051(10) -0.0201(12) O4 0.0498(16) 0.098(2) 0.0267(14) -0.0138(13) 0.0034(11) -0.0366(15) O5 0.0534(18) 0.072(2) 0.0467(16) 0.0028(14) 0.0170(13) -0.0213(15) O6 0.072(2) 0.075(2) 0.0343(15) -0.0112(13) 0.0101(14) -0.0324(16) F1 0.0510(13) 0.0466(13) 0.0574(13) -0.0016(10) -0.0201(10) -0.0095(10) F2 0.0443(12) 0.0524(13) 0.0417(11) 0.0002(9) -0.0085(9) -0.0116(10) F3 0.0451(12) 0.0473(12) 0.0383(11) -0.0043(9) -0.0030(9) -0.0103(10) Si1 0.0370(8) 0.0354(8) 0.0326(7) 0.0009(6) -0.0074(6) -0.0091(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 C1 C2 1.376(5) . ? C1 C6 1.379(4) . ? C1 N1 1.479(4) . ? C2 C3 1.389(5) . ? C2 H2 0.9500 . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? C4 C5 1.395(4) . ? C4 H4 0.9500 . ? C5 C6 1.388(4) . ? C5 N2 1.423(4) . ? C6 H6 0.9500 . ? C7 O3 1.229(4) . ? C7 N2 1.351(4) . ? C7 C8 1.506(4) . ? C8 C9 1.386(4) . ? C8 C13 1.405(4) . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C11 1.379(5) . ? C10 H10 0.9500 . ? C11 C12 1.384(5) . ? C11 H11 0.9500 . ? C12 C13 1.396(4) . ? C12 C14 1.502(5) . ? C13 H13 0.9500 . ? C14 O4 1.227(4) . ? C14 N3 1.345(4) . ? C15 C16 1.391(5) . ? C15 C20 1.395(4) . ? C15 N3 1.415(4) . ? C16 C17 1.380(5) . ? C16 H16 0.9500 . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C18 C19 1.368(5) . ? C18 H18 0.9500 . ? C19 C20 1.382(5) . ? C19 N4 1.484(4) . ? C20 H20 0.9500 . ? C21 N5 1.519(4) . ? C21 C22 1.520(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.528(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.523(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.524(4) . ? C25 N5 1.524(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.522(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.514(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N5 1.518(4) . ? C29 C30 1.519(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.515(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.505(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N5 1.524(4) . ? C33 C34 1.525(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.526(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.517(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N1 O2 1.226(4) . ? N1 O1 1.228(4) . ? N2 H2N 0.81(3) . ? N3 H3N 0.76(3) . ? N4 O6 1.225(4) . ? N4 O5 1.229(4) . ? F1 Si1 1.690(2) . ? F2 Si1 1.665(2) . ? F3 Si1 1.6800(19) . ? Si1 F2 1.665(2) 2_655 ? Si1 F3 1.6800(19) 2_655 ? Si1 F1 1.690(2) 2_655 ? 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 C2 C1 C6 124.1(3) . . ? C2 C1 N1 118.9(3) . . ? C6 C1 N1 117.1(3) . . ? C1 C2 C3 117.3(3) . . ? C1 C2 H2 121.3 . . ? C3 C2 H2 121.3 . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 N2 122.6(3) . . ? C4 C5 N2 117.2(3) . . ? C1 C6 C5 117.7(3) . . ? C1 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? O3 C7 N2 123.5(3) . . ? O3 C7 C8 119.3(3) . . ? N2 C7 C8 117.2(3) . . ? C9 C8 C13 119.4(3) . . ? C9 C8 C7 116.2(3) . . ? C13 C8 C7 124.2(3) . . ? C8 C9 C10 120.9(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 121.6(3) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C13 119.3(3) . . ? C11 C12 C14 116.3(3) . . ? C13 C12 C14 124.2(3) . . ? C12 C13 C8 119.6(3) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? O4 C14 N3 122.6(3) . . ? O4 C14 C12 119.8(3) . . ? N3 C14 C12 117.6(3) . . ? C16 C15 C20 119.4(3) . . ? C16 C15 N3 117.5(3) . . ? C20 C15 N3 123.1(3) . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 121.3(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 117.1(3) . . ? C19 C18 H18 121.4 . . ? C17 C18 H18 121.4 . . ? C18 C19 C20 124.2(3) . . ? C18 C19 N4 118.4(3) . . ? C20 C19 N4 117.3(3) . . ? C19 C20 C15 117.6(3) . . ? C19 C20 H20 121.2 . . ? C15 C20 H20 121.2 . . ? N5 C21 C22 116.4(2) . . ? N5 C21 H21A 108.2 . . ? C22 C21 H21A 108.2 . . ? N5 C21 H21B 108.2 . . ? C22 C21 H21B 108.2 . . ? H21A C21 H21B 107.3 . . ? C21 C22 C23 108.9(3) . . ? C21 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? C21 C22 H22B 109.9 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 C23 C22 113.0(3) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N5 114.4(2) . . ? C26 C25 H25A 108.7 . . ? N5 C25 H25A 108.7 . . ? C26 C25 H25B 108.7 . . ? N5 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? C27 C26 C25 111.1(3) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 110.7(3) . . ? C28 C27 H27A 109.5 . . ? C26 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N5 C29 C30 115.6(3) . . ? N5 C29 H29A 108.4 . . ? C30 C29 H29A 108.4 . . ? N5 C29 H29B 108.4 . . ? C30 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? C31 C30 C29 111.6(3) . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C30 112.8(3) . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 C34 114.9(2) . . ? N5 C33 H33A 108.5 . . ? C34 C33 H33A 108.5 . . ? N5 C33 H33B 108.5 . . ? C34 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C33 C34 C35 111.0(3) . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? C35 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 113.8(3) . . ? C36 C35 H35A 108.8 . . ? C34 C35 H35A 108.8 . . ? C36 C35 H35B 108.8 . . ? C34 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O2 N1 O1 123.7(3) . . ? O2 N1 C1 117.9(3) . . ? O1 N1 C1 118.4(3) . . ? C7 N2 C5 126.0(3) . . ? C7 N2 H2N 121(2) . . ? C5 N2 H2N 113(2) . . ? C14 N3 C15 127.9(3) . . ? C14 N3 H3N 119(2) . . ? C15 N3 H3N 112(2) . . ? O6 N4 O5 123.5(3) . . ? O6 N4 C19 118.4(3) . . ? O5 N4 C19 118.1(3) . . ? C29 N5 C21 107.4(2) . . ? C29 N5 C33 110.9(2) . . ? C21 N5 C33 110.5(2) . . ? C29 N5 C25 111.1(2) . . ? C21 N5 C25 110.9(2) . . ? C33 N5 C25 106.0(2) . . ? F2 Si1 F2 180.00(19) . 2_655 ? F2 Si1 F3 90.88(9) . 2_655 ? F2 Si1 F3 89.12(9) 2_655 2_655 ? F2 Si1 F3 89.12(9) . . ? F2 Si1 F3 90.88(9) 2_655 . ? F3 Si1 F3 180.00(13) 2_655 . ? F2 Si1 F1 90.26(10) . 2_655 ? F2 Si1 F1 89.74(10) 2_655 2_655 ? F3 Si1 F1 89.17(10) 2_655 2_655 ? F3 Si1 F1 90.83(10) . 2_655 ? F2 Si1 F1 89.74(10) . . ? F2 Si1 F1 90.26(10) 2_655 . ? F3 Si1 F1 90.83(10) 2_655 . ? F3 Si1 F1 89.17(10) . . ? F1 Si1 F1 180.0 2_655 . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.24 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.516 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.065 #===END data_compound2F _database_code_CSD 197050 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H96 F2 N14 O20' _chemical_formula_weight 1515.63 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' F F 0.0171 0.0103 '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 18.9979(13) _cell_length_b 22.1130(11) _cell_length_c 17.9782(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.571(2) _cell_angle_gamma 90.00 _cell_volume 7549.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9800 _exptl_absorpt_correction_T_max 0.9949 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 17441 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.1192 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9304 _reflns_number_gt 4256 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] 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 9304 _refine_ls_number_parameters 981 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2200 _refine_ls_R_factor_gt 0.1121 _refine_ls_wR_factor_ref 0.3545 _refine_ls_wR_factor_gt 0.2974 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 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 F1 F 0.2799(2) 0.52308(19) 0.6471(2) 0.0588(12) Uani 1 1 d . . . F2 F 0.2539(2) 0.43829(19) 0.8227(2) 0.0687(14) Uani 1 1 d . . . N1 N 0.1423(4) 0.5311(3) 0.6642(4) 0.0578(19) Uani 1 1 d . . . H1 H 0.1885 0.5333 0.6628 0.069 Uiso 1 1 calc R . . N2 N -0.0654(6) 0.4322(5) 0.5483(6) 0.087(3) Uani 1 1 d . . . N3 N 0.1695(6) 0.3678(4) 0.4911(4) 0.072(2) Uani 1 1 d . . . N4 N 0.3499(4) 0.5219(4) 0.8633(3) 0.062(2) Uani 1 1 d . . . H4 H 0.3153 0.4983 0.8475 0.074 Uiso 1 1 calc R . . N5 N 0.4946(7) 0.3426(4) 0.8355(4) 0.082(3) Uani 1 1 d . . . N6 N 0.6011(6) 0.5265(5) 0.9355(4) 0.081(3) Uani 1 1 d . . . O1 O 0.0456(4) 0.5762(3) 0.7122(3) 0.083(2) Uani 1 1 d . . . O2 O -0.1027(4) 0.4673(4) 0.5833(4) 0.100(2) Uani 1 1 d . . . O3 O -0.0884(4) 0.3953(4) 0.5076(5) 0.104(3) Uani 1 1 d . . . O4 O 0.1466(4) 0.3316(3) 0.4482(4) 0.098(2) Uani 1 1 d . . . O5 O 0.2341(5) 0.3706(3) 0.5072(4) 0.089(2) Uani 1 1 d . . . O6 O 0.3752(3) 0.6162(3) 0.9031(3) 0.0796(19) Uani 1 1 d . . . O7 O 0.4396(5) 0.3148(3) 0.8174(4) 0.099(2) Uani 1 1 d . . . O8 O 0.5545(4) 0.3209(3) 0.8352(4) 0.092(2) Uani 1 1 d . . . O9 O 0.6546(4) 0.4979(4) 0.9499(4) 0.096(2) Uani 1 1 d . . . O10 O 0.5952(3) 0.5820(4) 0.9461(4) 0.099(2) Uani 1 1 d . . . C1 C 0.2226(5) 0.5741(4) 0.7940(5) 0.054(2) Uani 1 1 d . . . H1A H 0.2389 0.5375 0.7728 0.065 Uiso 1 1 calc R . . C2 C 0.2628(6) 0.6030(4) 0.8481(5) 0.059(2) Uani 1 1 d . . . C3 C 0.2408(6) 0.6559(5) 0.8776(5) 0.075(3) Uani 1 1 d . . . H3 H 0.2698 0.6761 0.9136 0.091 Uiso 1 1 calc R . . C4 C 0.1750(6) 0.6816(4) 0.8557(6) 0.081(3) Uani 1 1 d . . . H4A H 0.1600 0.7186 0.8768 0.097 Uiso 1 1 calc R . . C5 C 0.1323(5) 0.6517(4) 0.8024(5) 0.077(3) Uani 1 1 d . . . H5 H 0.0871 0.6668 0.7881 0.092 Uiso 1 1 calc R . . C6 C 0.1592(6) 0.5980(4) 0.7708(5) 0.065(3) Uani 1 1 d . . . C7 C 0.1107(6) 0.5683(4) 0.7129(5) 0.067(3) Uani 1 1 d . . . C8 C 0.1098(5) 0.4899(4) 0.6159(5) 0.055(2) Uani 1 1 d . . . C9 C 0.0362(5) 0.4843(4) 0.6044(5) 0.063(2) Uani 1 1 d . . . H9 H 0.0046 0.5105 0.6289 0.076 Uiso 1 1 calc R . . C10 C 0.0121(5) 0.4412(5) 0.5579(6) 0.070(3) Uani 1 1 d . . . C11 C 0.0530(7) 0.4019(4) 0.5185(5) 0.075(3) Uani 1 1 d . . . H11 H 0.0337 0.3720 0.4860 0.090 Uiso 1 1 calc R . . C12 C 0.1247(6) 0.4095(4) 0.5303(5) 0.070(3) Uani 1 1 d . . . C13 C 0.1534(5) 0.4516(4) 0.5761(5) 0.058(2) Uani 1 1 d . . . H13 H 0.2031 0.4551 0.5813 0.069 Uiso 1 1 calc R . . C14 C 0.3338(6) 0.5802(5) 0.8744(5) 0.066(3) Uani 1 1 d . . . C15 C 0.4152(5) 0.4947(4) 0.8742(4) 0.057(2) Uani 1 1 d . . . C16 C 0.4753(6) 0.5236(4) 0.9018(5) 0.067(3) Uani 1 1 d . . . H16 H 0.4726 0.5648 0.9165 0.080 Uiso 1 1 calc R . . C17 C 0.5378(6) 0.4944(4) 0.9080(4) 0.055(2) Uani 1 1 d . . . C18 C 0.5471(5) 0.4372(5) 0.8867(5) 0.070(3) Uani 1 1 d . . . H18 H 0.5920 0.4185 0.8900 0.084 Uiso 1 1 calc R . . C19 C 0.4869(6) 0.4058(4) 0.8587(5) 0.065(3) Uani 1 1 d . . . C20 C 0.4195(5) 0.4338(4) 0.8529(4) 0.066(3) Uani 1 1 d . . . H20 H 0.3792 0.4122 0.8352 0.079 Uiso 1 1 calc R . . N7 N 0.1844(4) 0.3700(3) 0.7295(4) 0.0591(19) Uani 1 1 d . . . H7 H 0.2133 0.3924 0.7568 0.071 Uiso 1 1 calc R . . N8 N -0.0623(5) 0.3204(4) 0.6698(5) 0.078(2) Uani 1 1 d . . . N9 N 0.0002(7) 0.4912(5) 0.8288(6) 0.107(3) Uani 1 1 d . . . N10 N 0.4110(3) 0.4973(3) 0.6806(3) 0.0530(18) Uani 1 1 d . . . H10 H 0.3653 0.4986 0.6713 0.064 Uiso 1 1 calc R . . N11 N 0.3877(5) 0.7073(4) 0.7480(5) 0.073(2) Uani 1 1 d . . . N12 N 0.6161(5) 0.6085(4) 0.7756(5) 0.082(2) Uani 1 1 d . . . O11 O 0.1771(3) 0.2919(3) 0.6476(3) 0.0740(18) Uani 1 1 d . . . O12 O -0.0435(4) 0.2812(4) 0.6281(5) 0.119(3) Uani 1 1 d . . . O13 O -0.1254(5) 0.3301(3) 0.6799(5) 0.124(3) Uani 1 1 d . . . O14 O -0.0649(5) 0.5083(4) 0.8179(4) 0.112(3) Uani 1 1 d . . . O15 O 0.0418(4) 0.5162(4) 0.8724(4) 0.107(3) Uani 1 1 d . . . O16 O 0.5070(3) 0.4374(3) 0.6730(3) 0.0672(17) Uani 1 1 d . . . O17 O 0.3307(5) 0.7112(3) 0.7142(5) 0.100(2) Uani 1 1 d . . . O18 O 0.4084(3) 0.7468(3) 0.7928(4) 0.0789(19) Uani 1 1 d . . . O19 O 0.6420(4) 0.6560(3) 0.7947(5) 0.109(3) Uani 1 1 d . . . O20 O 0.6487(4) 0.5601(4) 0.7773(5) 0.115(3) Uani 1 1 d . . . C21 C 0.3268(5) 0.3881(4) 0.6799(4) 0.053(2) Uani 1 1 d . . . H21 H 0.3043 0.4236 0.6972 0.063 Uiso 1 1 calc R . . C22 C 0.3982(4) 0.3891(4) 0.6626(4) 0.051(2) Uani 1 1 d . . . C23 C 0.4309(4) 0.3365(4) 0.6403(4) 0.057(2) Uani 1 1 d . . . H23 H 0.4796 0.3370 0.6297 0.068 Uiso 1 1 calc R . . C24 C 0.3934(5) 0.2835(4) 0.6335(5) 0.066(2) Uani 1 1 d . . . H24 H 0.4166 0.2474 0.6194 0.079 Uiso 1 1 calc R . . C25 C 0.3225(5) 0.2825(4) 0.6470(5) 0.063(2) Uani 1 1 d . . . H25 H 0.2964 0.2463 0.6397 0.076 Uiso 1 1 calc R . . C26 C 0.2894(5) 0.3344(4) 0.6714(4) 0.054(2) Uani 1 1 d . . . C27 C 0.2129(5) 0.3306(4) 0.6826(5) 0.057(2) Uani 1 1 d . . . C28 C 0.1108(6) 0.3784(4) 0.7385(5) 0.063(2) Uani 1 1 d . . . C29 C 0.0901(5) 0.4267(4) 0.7831(5) 0.071(3) Uani 1 1 d . . . H29 H 0.1240 0.4505 0.8098 0.085 Uiso 1 1 calc R . . C30 C 0.0188(6) 0.4389(4) 0.7870(5) 0.069(3) Uani 1 1 d . . . C31 C -0.0318(5) 0.4035(5) 0.7516(6) 0.085(3) Uani 1 1 d . . . H31 H -0.0804 0.4116 0.7578 0.103 Uiso 1 1 calc R . . C32 C -0.0112(7) 0.3573(5) 0.7082(6) 0.084(3) Uani 1 1 d . . . C33 C 0.0613(5) 0.3425(4) 0.7000(5) 0.070(3) Uani 1 1 d . . . H33 H 0.0753 0.3097 0.6697 0.085 Uiso 1 1 calc R . . C34 C 0.4443(5) 0.4427(4) 0.6716(4) 0.049(2) Uani 1 1 d . . . C35 C 0.4444(5) 0.5515(4) 0.7038(4) 0.053(2) Uani 1 1 d . . . C36 C 0.5156(5) 0.5550(4) 0.7251(4) 0.055(2) Uani 1 1 d . . . H36 H 0.5449 0.5203 0.7226 0.065 Uiso 1 1 calc R . . C37 C 0.5424(5) 0.6085(4) 0.7494(5) 0.064(2) Uani 1 1 d . . . C38 C 0.5014(6) 0.6592(4) 0.7579(5) 0.068(3) Uani 1 1 d . . . H38 H 0.5207 0.6959 0.7767 0.081 Uiso 1 1 calc R . . C39 C 0.4318(5) 0.6541(4) 0.7379(4) 0.054(2) Uani 1 1 d . . . C40 C 0.4023(5) 0.6023(4) 0.7091(4) 0.057(2) Uani 1 1 d . . . H40 H 0.3542 0.6013 0.6932 0.068 Uiso 1 1 calc R . . N13 N 0.3240(3) 0.6259(3) 0.4522(3) 0.0514(18) Uani 1 1 d . . . C41 C 0.3363(4) 0.6287(4) 0.3714(4) 0.060(2) Uani 1 1 d . . . H41A H 0.3842 0.6131 0.3626 0.072 Uiso 1 1 calc R . . H41B H 0.3356 0.6718 0.3561 0.072 Uiso 1 1 calc R . . C42 C 0.2850(5) 0.5946(4) 0.3213(5) 0.071(3) Uani 1 1 d . . . H42A H 0.2363 0.6058 0.3337 0.085 Uiso 1 1 calc R . . H42B H 0.2907 0.5506 0.3298 0.085 Uiso 1 1 calc R . . C43 C 0.2972(5) 0.6088(6) 0.2404(5) 0.101(4) Uani 1 1 d . . . H43A H 0.2921 0.6530 0.2330 0.121 Uiso 1 1 calc R . . H43B H 0.3463 0.5979 0.2291 0.121 Uiso 1 1 calc R . . C44 C 0.2515(6) 0.5791(6) 0.1889(6) 0.120(4) Uani 1 1 d . . . H44A H 0.2617 0.5356 0.1894 0.180 Uiso 1 1 calc R . . H44B H 0.2586 0.5952 0.1389 0.180 Uiso 1 1 calc R . . H44C H 0.2026 0.5857 0.2028 0.180 Uiso 1 1 calc R . . C45 C 0.3882(4) 0.6517(4) 0.4941(5) 0.062(2) Uani 1 1 d . . . H45A H 0.4303 0.6284 0.4797 0.074 Uiso 1 1 calc R . . H45B H 0.3821 0.6454 0.5480 0.074 Uiso 1 1 calc R . . C46 C 0.4023(5) 0.7187(4) 0.4806(5) 0.073(3) Uani 1 1 d . . . H46A H 0.3646 0.7430 0.5029 0.088 Uiso 1 1 calc R . . H46B H 0.4015 0.7267 0.4264 0.088 Uiso 1 1 calc R . . C47 C 0.4743(5) 0.7377(4) 0.5148(5) 0.074(3) Uani 1 1 d . . . H47A H 0.4730 0.7351 0.5697 0.088 Uiso 1 1 calc R . . H47B H 0.5113 0.7099 0.4976 0.088 Uiso 1 1 calc R . . C48 C 0.4917(5) 0.8017(4) 0.4922(5) 0.075(3) Uani 1 1 d . . . H48A H 0.4882 0.8052 0.4379 0.113 Uiso 1 1 calc R . . H48B H 0.5397 0.8116 0.5093 0.113 Uiso 1 1 calc R . . H48C H 0.4585 0.8297 0.5146 0.113 Uiso 1 1 calc R . . C49 C 0.3126(5) 0.5621(4) 0.4782(5) 0.064(2) Uani 1 1 d . . . H49A H 0.3024 0.5629 0.5319 0.077 Uiso 1 1 calc R . . H49B H 0.2707 0.5454 0.4515 0.077 Uiso 1 1 calc R . . C50 C 0.3741(5) 0.5209(4) 0.4663(5) 0.075(3) Uani 1 1 d . . . H50A H 0.3929 0.5283 0.4163 0.090 Uiso 1 1 calc R . . H50B H 0.4118 0.5302 0.5036 0.090 Uiso 1 1 calc R . . C51 C 0.3544(5) 0.4570(4) 0.4726(6) 0.082(3) Uani 1 1 d . . . H51A H 0.3173 0.4483 0.4343 0.099 Uiso 1 1 calc R . . H51B H 0.3334 0.4508 0.5218 0.099 Uiso 1 1 calc R . . C52 C 0.4111(6) 0.4126(5) 0.4644(6) 0.099(3) Uani 1 1 d . . . H52A H 0.4250 0.4111 0.4124 0.149 Uiso 1 1 calc R . . H52B H 0.3945 0.3726 0.4795 0.149 Uiso 1 1 calc R . . H52C H 0.4517 0.4243 0.4960 0.149 Uiso 1 1 calc R . . C53 C 0.2583(4) 0.6636(4) 0.4682(5) 0.058(2) Uani 1 1 d . . . H53A H 0.2639 0.7040 0.4452 0.069 Uiso 1 1 calc R . . H53B H 0.2171 0.6440 0.4433 0.069 Uiso 1 1 calc R . . C54 C 0.2420(5) 0.6725(4) 0.5481(5) 0.078(3) Uani 1 1 d . . . H54A H 0.2860 0.6810 0.5769 0.093 Uiso 1 1 calc R . . H54B H 0.2211 0.6350 0.5680 0.093 Uiso 1 1 calc R . . C55 C 0.1917(5) 0.7240(5) 0.5568(6) 0.099(3) Uani 1 1 d . . . H55A H 0.2138 0.7613 0.5380 0.119 Uiso 1 1 calc R . . H55B H 0.1491 0.7160 0.5254 0.119 Uiso 1 1 calc R . . C56 C 0.1699(6) 0.7345(7) 0.6345(6) 0.147(6) Uani 1 1 d . . . H56A H 0.1364 0.7032 0.6487 0.221 Uiso 1 1 calc R . . H56B H 0.1475 0.7743 0.6380 0.221 Uiso 1 1 calc R . . H56C H 0.2114 0.7331 0.6680 0.221 Uiso 1 1 calc R . . N14 N 0.8435(4) 0.6338(3) 0.9754(4) 0.072(2) Uani 1 1 d . . . C57 C 0.7813(4) 0.6776(4) 0.9871(5) 0.067(3) Uani 1 1 d . . . H57A H 0.7912 0.7156 0.9601 0.081 Uiso 1 1 calc R . . H57B H 0.7386 0.6595 0.9634 0.081 Uiso 1 1 calc R . . C58 C 0.7651(4) 0.6932(4) 1.0627(5) 0.068(3) Uani 1 1 d . . . H58A H 0.8056 0.7148 1.0861 0.081 Uiso 1 1 calc R . . H58B H 0.7572 0.6557 1.0914 0.081 Uiso 1 1 calc R . . C59 C 0.7003(5) 0.7327(4) 1.0653(5) 0.073(3) Uani 1 1 d . . . H59A H 0.6584 0.7078 1.0525 0.087 Uiso 1 1 calc R . . H59B H 0.7037 0.7647 1.0271 0.087 Uiso 1 1 calc R . . C60 C 0.6896(5) 0.7630(5) 1.1421(5) 0.105(4) Uani 1 1 d . . . H60A H 0.6790 0.7319 1.1790 0.157 Uiso 1 1 calc R . . H60B H 0.6503 0.7916 1.1382 0.157 Uiso 1 1 calc R . . H60C H 0.7326 0.7845 1.1576 0.157 Uiso 1 1 calc R . . C61 C 0.9056(5) 0.6518(5) 1.0263(6) 0.084(3) Uani 1 1 d . . . H61A H 0.8890 0.6541 1.0779 0.101 Uiso 1 1 calc R . . H61B H 0.9414 0.6193 1.0248 0.101 Uiso 1 1 calc R . . C62 C 0.9403(6) 0.7108(5) 1.0075(8) 0.115(4) Uani 1 1 d . . . H62A H 0.9047 0.7435 1.0056 0.138 Uiso 1 1 calc R . . H62B H 0.9614 0.7079 0.9578 0.138 Uiso 1 1 calc R . . C63 C 0.9982(6) 0.7263(6) 1.0664(9) 0.119(4) Uani 1 1 d . . . H63A H 1.0289 0.6905 1.0741 0.143 Uiso 1 1 calc R . . H63B H 1.0277 0.7594 1.0471 0.143 Uiso 1 1 calc R . . C64 C 0.9709(7) 0.7445(8) 1.1372(8) 0.161(6) Uani 1 1 d . . . H64A H 0.9526 0.7858 1.1334 0.241 Uiso 1 1 calc R . . H64B H 1.0087 0.7429 1.1753 0.241 Uiso 1 1 calc R . . H64C H 0.9329 0.7170 1.1508 0.241 Uiso 1 1 calc R . . C65 C 0.8188(5) 0.5721(4) 0.9971(5) 0.077(3) Uani 1 1 d . . . H65A H 0.8078 0.5728 1.0506 0.092 Uiso 1 1 calc R . . H65B H 0.7745 0.5633 0.9690 0.092 Uiso 1 1 calc R . . C66 C 0.8693(5) 0.5219(4) 0.9842(5) 0.082(3) Uani 1 1 d . . . H66A H 0.9123 0.5285 1.0155 0.098 Uiso 1 1 calc R . . H66B H 0.8832 0.5226 0.9315 0.098 Uiso 1 1 calc R . . C67 C 0.8394(6) 0.4611(4) 1.0015(6) 0.089(3) Uani 1 1 d . . . H67A H 0.7929 0.4574 0.9756 0.106 Uiso 1 1 calc R . . H67B H 0.8315 0.4590 1.0556 0.106 Uiso 1 1 calc R . . C68 C 0.8838(6) 0.4083(5) 0.9801(6) 0.108(4) Uani 1 1 d . . . H68A H 0.8869 0.4067 0.9258 0.161 Uiso 1 1 calc R . . H68B H 0.8624 0.3708 0.9980 0.161 Uiso 1 1 calc R . . H68C H 0.9311 0.4127 1.0025 0.161 Uiso 1 1 calc R . . C69 C 0.8646(5) 0.6374(4) 0.8966(6) 0.084(3) Uani 1 1 d . . . H69A H 0.9102 0.6162 0.8925 0.101 Uiso 1 1 calc R . . H69B H 0.8730 0.6805 0.8848 0.101 Uiso 1 1 calc R . . C70 C 0.8155(6) 0.6127(5) 0.8383(5) 0.087(3) Uani 1 1 d . . . H70A H 0.7693 0.6333 0.8405 0.104 Uiso 1 1 calc R . . H70B H 0.8081 0.5689 0.8466 0.104 Uiso 1 1 calc R . . C71 C 0.8472(7) 0.6229(5) 0.7631(7) 0.122(4) Uani 1 1 d . . . H71A H 0.8977 0.6117 0.7653 0.146 Uiso 1 1 calc R . . H71B H 0.8437 0.6663 0.7497 0.146 Uiso 1 1 calc R . . C72 C 0.8086(8) 0.5850(7) 0.7038(6) 0.151(6) Uani 1 1 d . . . H72A H 0.8179 0.5420 0.7131 0.226 Uiso 1 1 calc R . . H72B H 0.8253 0.5959 0.6545 0.226 Uiso 1 1 calc R . . H72C H 0.7579 0.5926 0.7058 0.226 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.053(3) 0.060(3) 0.063(3) 0.003(2) 0.000(2) -0.002(2) F2 0.078(3) 0.058(3) 0.071(3) 0.010(2) 0.008(2) -0.006(2) N1 0.053(5) 0.060(5) 0.060(5) -0.002(4) 0.006(4) -0.002(4) N2 0.087(10) 0.088(8) 0.085(7) 0.013(6) -0.020(6) -0.020(6) N3 0.080(7) 0.071(6) 0.066(6) -0.003(5) -0.004(6) -0.015(6) N4 0.065(6) 0.072(6) 0.050(4) -0.004(4) 0.010(4) -0.004(4) N5 0.114(10) 0.061(7) 0.071(6) -0.001(5) 0.018(6) 0.001(6) N6 0.080(9) 0.084(8) 0.081(6) -0.008(5) 0.019(5) 0.001(7) O1 0.066(5) 0.082(5) 0.100(5) -0.009(4) 0.009(4) 0.014(4) O2 0.080(6) 0.120(7) 0.099(6) -0.002(5) -0.002(4) -0.011(5) O3 0.077(6) 0.101(6) 0.132(7) -0.004(5) -0.024(5) -0.036(5) O4 0.116(6) 0.075(5) 0.102(5) -0.039(4) 0.005(4) -0.027(4) O5 0.093(6) 0.086(5) 0.089(5) -0.018(4) 0.010(4) 0.009(4) O6 0.081(5) 0.067(5) 0.091(5) -0.027(4) -0.007(4) 0.000(4) O7 0.122(7) 0.067(5) 0.106(5) -0.012(4) -0.015(5) -0.012(5) O8 0.102(6) 0.070(5) 0.105(5) -0.015(4) 0.021(5) 0.016(4) O9 0.073(6) 0.100(6) 0.115(6) -0.008(4) 0.001(4) 0.013(5) O10 0.081(5) 0.078(6) 0.137(6) -0.019(5) 0.001(4) -0.005(4) C1 0.056(7) 0.041(5) 0.067(6) 0.011(5) 0.016(5) 0.011(5) C2 0.079(8) 0.049(6) 0.050(6) -0.012(5) 0.008(5) 0.005(6) C3 0.072(8) 0.079(8) 0.075(7) -0.002(6) 0.001(6) -0.004(6) C4 0.104(9) 0.057(7) 0.082(7) -0.023(5) 0.006(7) 0.001(6) C5 0.088(8) 0.069(7) 0.074(7) 0.001(6) 0.016(6) 0.005(6) C6 0.093(8) 0.043(6) 0.060(6) 0.001(5) 0.035(6) -0.005(6) C7 0.089(9) 0.042(6) 0.071(7) 0.001(5) 0.006(7) 0.000(6) C8 0.061(7) 0.046(6) 0.060(6) 0.013(5) -0.006(5) -0.017(5) C9 0.058(8) 0.067(7) 0.065(6) 0.011(5) 0.006(5) -0.006(5) C10 0.045(8) 0.077(8) 0.087(8) 0.011(6) -0.021(6) -0.017(6) C11 0.108(10) 0.062(7) 0.055(6) -0.001(5) 0.008(6) -0.014(7) C12 0.075(9) 0.062(7) 0.072(7) 0.003(6) 0.006(6) -0.007(6) C13 0.050(6) 0.062(6) 0.061(6) -0.004(5) 0.000(5) -0.004(5) C14 0.081(9) 0.047(7) 0.070(7) -0.009(5) 0.012(6) -0.006(6) C15 0.045(7) 0.072(7) 0.053(6) 0.001(5) 0.011(5) 0.013(6) C16 0.063(8) 0.073(7) 0.064(6) -0.008(5) 0.019(6) -0.007(7) C17 0.053(8) 0.050(7) 0.063(6) -0.008(4) 0.006(5) 0.004(6) C18 0.064(7) 0.085(9) 0.063(6) 0.011(5) 0.004(5) 0.011(6) C19 0.095(9) 0.051(7) 0.050(6) 0.003(4) 0.004(5) 0.004(6) C20 0.079(8) 0.061(7) 0.057(6) 0.000(5) 0.003(5) -0.001(6) N7 0.053(6) 0.052(5) 0.072(5) 0.009(4) 0.005(4) 0.001(4) N8 0.066(7) 0.067(6) 0.100(7) -0.013(5) 0.000(6) -0.010(5) N9 0.089(9) 0.108(9) 0.126(9) 0.005(7) 0.042(7) 0.025(7) N10 0.046(4) 0.055(5) 0.059(4) -0.009(3) 0.005(3) -0.012(4) N11 0.082(7) 0.052(6) 0.086(7) 0.009(5) 0.012(6) 0.003(6) N12 0.053(7) 0.061(7) 0.133(7) -0.008(5) -0.006(5) -0.012(5) O11 0.063(4) 0.062(4) 0.097(5) -0.010(4) -0.010(3) -0.007(3) O12 0.083(6) 0.127(8) 0.148(7) -0.040(6) -0.001(5) -0.024(5) O13 0.070(6) 0.113(7) 0.189(9) 0.017(5) 0.008(6) -0.001(5) O14 0.098(6) 0.116(7) 0.125(6) -0.018(5) 0.026(5) 0.014(5) O15 0.095(7) 0.115(7) 0.110(6) -0.053(5) 0.006(5) -0.009(5) O16 0.046(4) 0.071(4) 0.085(5) -0.017(3) 0.015(3) -0.006(3) O17 0.093(6) 0.065(5) 0.142(7) -0.001(4) -0.014(5) 0.021(4) O18 0.098(5) 0.054(4) 0.085(5) -0.005(4) 0.012(4) 0.007(4) O19 0.081(6) 0.069(5) 0.177(7) -0.008(5) -0.028(5) -0.018(4) O20 0.074(5) 0.080(6) 0.189(8) -0.031(5) -0.030(5) 0.013(4) C21 0.061(7) 0.043(6) 0.054(5) -0.001(4) 0.004(5) -0.001(5) C22 0.054(7) 0.052(6) 0.049(5) -0.007(4) 0.009(4) -0.010(5) C23 0.049(6) 0.050(6) 0.072(6) -0.002(5) 0.013(5) 0.001(5) C24 0.063(7) 0.050(6) 0.084(7) -0.007(5) -0.004(5) 0.004(5) C25 0.064(7) 0.048(6) 0.078(6) -0.008(5) -0.006(5) -0.001(5) C26 0.051(7) 0.054(7) 0.057(6) 0.006(4) 0.004(4) -0.003(5) C27 0.064(8) 0.043(6) 0.064(6) 0.000(5) -0.003(5) 0.005(5) C28 0.064(8) 0.052(6) 0.075(6) 0.020(5) 0.002(6) 0.009(5) C29 0.076(8) 0.055(6) 0.084(7) -0.001(5) 0.023(6) -0.009(5) C30 0.081(9) 0.052(7) 0.074(7) -0.005(5) 0.018(6) 0.013(6) C31 0.064(8) 0.085(9) 0.108(8) 0.010(7) 0.011(6) -0.020(7) C32 0.103(11) 0.059(7) 0.089(8) -0.008(6) -0.008(7) -0.002(7) C33 0.041(7) 0.060(7) 0.111(8) 0.008(5) 0.003(6) -0.012(5) C34 0.042(6) 0.048(6) 0.059(6) -0.005(4) 0.017(5) 0.002(5) C35 0.065(8) 0.049(6) 0.047(5) 0.000(4) 0.014(5) 0.005(5) C36 0.042(7) 0.057(6) 0.065(6) -0.015(4) 0.004(5) -0.009(5) C37 0.054(8) 0.058(7) 0.079(6) 0.000(5) 0.001(5) -0.007(6) C38 0.084(9) 0.053(7) 0.067(6) -0.003(5) 0.007(6) -0.007(6) C39 0.036(6) 0.062(7) 0.063(6) -0.005(4) -0.009(5) 0.002(5) C40 0.053(6) 0.060(7) 0.056(5) -0.003(5) -0.005(4) -0.018(5) N13 0.052(5) 0.053(5) 0.049(5) 0.005(3) 0.004(4) 0.000(4) C41 0.063(6) 0.058(6) 0.058(6) 0.011(4) 0.001(5) 0.000(5) C42 0.068(7) 0.079(7) 0.065(7) 0.010(5) -0.007(5) 0.005(5) C43 0.074(8) 0.165(12) 0.063(7) -0.011(7) -0.009(6) -0.030(7) C44 0.117(10) 0.144(12) 0.099(9) -0.005(8) -0.001(8) 0.001(9) C45 0.045(6) 0.064(7) 0.077(6) -0.004(5) -0.006(5) 0.010(5) C46 0.081(8) 0.055(7) 0.082(7) 0.014(5) -0.003(6) 0.001(5) C47 0.059(7) 0.068(7) 0.095(7) -0.011(5) -0.002(5) 0.008(5) C48 0.070(7) 0.059(7) 0.097(7) -0.001(5) -0.009(5) 0.005(5) C49 0.083(7) 0.044(6) 0.066(6) 0.014(4) 0.008(5) 0.006(5) C50 0.094(8) 0.063(7) 0.068(6) 0.004(5) 0.018(5) 0.008(6) C51 0.093(8) 0.064(8) 0.090(7) 0.010(5) -0.001(6) 0.002(6) C52 0.111(9) 0.077(8) 0.110(8) 0.015(6) 0.006(7) 0.020(7) C53 0.043(6) 0.059(6) 0.070(6) 0.004(4) 0.004(5) 0.007(4) C54 0.080(7) 0.071(7) 0.082(8) 0.004(5) 0.005(6) 0.011(6) C55 0.091(8) 0.120(10) 0.087(8) 0.001(7) 0.029(6) 0.031(7) C56 0.126(11) 0.210(16) 0.105(10) -0.035(9) -0.032(8) 0.086(10) N14 0.067(6) 0.066(6) 0.084(6) 0.025(4) 0.027(5) 0.017(4) C57 0.054(6) 0.058(6) 0.091(8) 0.015(5) 0.018(5) 0.012(5) C58 0.063(7) 0.070(7) 0.071(7) 0.016(5) 0.011(5) 0.007(5) C59 0.064(7) 0.076(7) 0.079(7) 0.001(5) 0.017(5) 0.007(5) C60 0.090(8) 0.133(10) 0.091(8) -0.003(7) 0.015(6) 0.003(7) C61 0.055(7) 0.099(9) 0.097(8) 0.014(6) -0.004(6) 0.012(6) C62 0.089(9) 0.069(8) 0.188(13) 0.010(8) 0.025(9) -0.007(7) C63 0.077(9) 0.113(11) 0.165(13) -0.004(9) -0.018(9) -0.015(7) C64 0.139(13) 0.227(18) 0.115(12) 0.061(11) -0.014(10) 0.007(12) C65 0.098(8) 0.054(6) 0.080(7) 0.029(5) 0.021(6) 0.001(6) C66 0.081(8) 0.078(8) 0.086(7) 0.032(6) 0.009(5) 0.014(6) C67 0.108(9) 0.067(8) 0.091(7) 0.015(6) 0.007(6) 0.001(6) C68 0.150(11) 0.075(8) 0.097(8) 0.008(6) -0.006(7) 0.036(8) C69 0.088(8) 0.063(7) 0.103(9) 0.015(6) 0.041(7) 0.011(6) C70 0.100(9) 0.088(8) 0.072(7) 0.029(6) 0.005(7) 0.010(6) C71 0.171(12) 0.099(10) 0.098(9) 0.025(7) 0.040(9) 0.023(9) C72 0.210(16) 0.174(14) 0.067(8) 0.027(9) -0.018(9) -0.039(12) _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 N1 C7 1.353(11) . ? N1 C8 1.393(10) . ? N2 O3 1.171(10) . ? N2 O2 1.235(11) . ? N2 C10 1.492(13) . ? N3 O4 1.185(9) . ? N3 O5 1.255(9) . ? N3 C12 1.451(12) . ? N4 C14 1.342(11) . ? N4 C15 1.388(10) . ? N5 O8 1.235(10) . ? N5 O7 1.248(10) . ? N5 C19 1.467(12) . ? N6 O9 1.219(9) . ? N6 O10 1.246(10) . ? N6 C17 1.470(12) . ? O1 C7 1.249(10) . ? O6 C14 1.223(10) . ? C1 C6 1.370(11) . ? C1 C2 1.376(11) . ? C2 C3 1.357(12) . ? C2 C14 1.503(13) . ? C3 C4 1.418(12) . ? C4 C5 1.404(12) . ? C5 C6 1.418(12) . ? C6 C7 1.521(13) . ? C8 C13 1.395(11) . ? C8 C9 1.413(11) . ? C9 C10 1.340(12) . ? C10 C11 1.375(13) . ? C11 C12 1.383(12) . ? C12 C13 1.347(12) . ? C15 C16 1.388(12) . ? C15 C20 1.404(11) . ? C16 C17 1.353(11) . ? C17 C18 1.335(12) . ? C18 C19 1.419(12) . ? C19 C20 1.423(12) . ? N7 C27 1.336(10) . ? N7 C28 1.423(10) . ? N8 O12 1.206(9) . ? N8 O13 1.237(9) . ? N8 C32 1.431(12) . ? N9 O15 1.229(12) . ? N9 O14 1.303(11) . ? N9 C30 1.429(13) . ? N10 C34 1.377(10) . ? N10 C35 1.413(10) . ? N11 O17 1.230(9) . ? N11 O18 1.244(9) . ? N11 C39 1.459(11) . ? N12 O19 1.206(9) . ? N12 O20 1.237(9) . ? N12 C37 1.465(11) . ? O11 C27 1.253(9) . ? O16 C34 1.195(8) . ? C21 C26 1.392(10) . ? C21 C22 1.400(10) . ? C22 C23 1.382(10) . ? C22 C34 1.479(11) . ? C23 C24 1.375(11) . ? C24 C25 1.375(11) . ? C25 C26 1.385(11) . ? C26 C27 1.475(11) . ? C28 C29 1.398(12) . ? C28 C33 1.400(11) . ? C29 C30 1.386(12) . ? C30 C31 1.381(12) . ? C31 C32 1.351(13) . ? C32 C33 1.426(13) . ? C35 C40 1.385(11) . ? C35 C36 1.398(11) . ? C36 C37 1.355(11) . ? C37 C38 1.374(11) . ? C38 C39 1.366(11) . ? C39 C40 1.370(11) . ? N13 C41 1.480(9) . ? N13 C49 1.502(9) . ? N13 C45 1.526(9) . ? N13 C53 1.537(9) . ? C41 C42 1.510(11) . ? C42 C43 1.512(12) . ? C43 C44 1.413(13) . ? C45 C46 1.526(11) . ? C46 C47 1.543(11) . ? C47 C48 1.510(12) . ? C49 C50 1.502(11) . ? C50 C51 1.466(12) . ? C51 C52 1.469(12) . ? C53 C54 1.490(11) . ? C54 C55 1.498(12) . ? C55 C56 1.487(13) . ? N14 C69 1.485(11) . ? N14 C65 1.498(10) . ? N14 C61 1.525(11) . ? N14 C57 1.546(10) . ? C57 C58 1.443(11) . ? C58 C59 1.512(11) . ? C59 C60 1.553(12) . ? C61 C62 1.507(13) . ? C62 C63 1.544(15) . ? C63 C64 1.445(16) . ? C65 C66 1.490(11) . ? C66 C67 1.495(12) . ? C67 C68 1.498(12) . ? C69 C70 1.489(13) . ? C70 C71 1.512(13) . ? C71 C72 1.528(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 C7 N1 C8 127.1(8) . . ? O3 N2 O2 123.1(11) . . ? O3 N2 C10 121.0(11) . . ? O2 N2 C10 115.8(10) . . ? O4 N3 O5 121.5(9) . . ? O4 N3 C12 122.4(10) . . ? O5 N3 C12 116.1(9) . . ? C14 N4 C15 127.0(8) . . ? O8 N5 O7 125.0(10) . . ? O8 N5 C19 118.0(10) . . ? O7 N5 C19 117.0(10) . . ? O9 N6 O10 123.8(10) . . ? O9 N6 C17 119.4(10) . . ? O10 N6 C17 116.7(9) . . ? C6 C1 C2 120.2(9) . . ? C3 C2 C1 120.4(9) . . ? C3 C2 C14 116.7(9) . . ? C1 C2 C14 122.8(8) . . ? C2 C3 C4 121.0(9) . . ? C5 C4 C3 119.3(9) . . ? C4 C5 C6 117.3(10) . . ? C1 C6 C5 121.6(9) . . ? C1 C6 C7 123.6(9) . . ? C5 C6 C7 114.6(10) . . ? O1 C7 N1 122.4(9) . . ? O1 C7 C6 121.9(9) . . ? N1 C7 C6 115.7(9) . . ? N1 C8 C13 117.2(8) . . ? N1 C8 C9 124.7(9) . . ? C13 C8 C9 118.1(8) . . ? C10 C9 C8 118.2(9) . . ? C9 C10 C11 125.7(10) . . ? C9 C10 N2 119.1(11) . . ? C11 C10 N2 115.2(11) . . ? C10 C11 C12 114.3(9) . . ? C13 C12 C11 123.9(10) . . ? C13 C12 N3 120.2(10) . . ? C11 C12 N3 115.9(10) . . ? C12 C13 C8 119.8(9) . . ? O6 C14 N4 122.8(10) . . ? O6 C14 C2 118.4(9) . . ? N4 C14 C2 118.8(9) . . ? N4 C15 C16 125.1(9) . . ? N4 C15 C20 115.8(9) . . ? C16 C15 C20 119.1(8) . . ? C17 C16 C15 121.4(9) . . ? C18 C17 C16 123.5(9) . . ? C18 C17 N6 116.1(9) . . ? C16 C17 N6 120.3(9) . . ? C17 C18 C19 117.1(9) . . ? C18 C19 C20 121.8(9) . . ? C18 C19 N5 118.9(10) . . ? C20 C19 N5 119.3(10) . . ? C15 C20 C19 117.2(9) . . ? C27 N7 C28 125.0(8) . . ? O12 N8 O13 121.4(9) . . ? O12 N8 C32 120.1(10) . . ? O13 N8 C32 118.6(10) . . ? O15 N9 O14 123.9(10) . . ? O15 N9 C30 122.4(11) . . ? O14 N9 C30 113.8(12) . . ? C34 N10 C35 125.1(7) . . ? O17 N11 O18 121.9(9) . . ? O17 N11 C39 119.7(9) . . ? O18 N11 C39 118.4(9) . . ? O19 N12 O20 123.1(9) . . ? O19 N12 C37 118.1(9) . . ? O20 N12 C37 118.8(9) . . ? C26 C21 C22 118.9(7) . . ? C23 C22 C21 119.8(7) . . ? C23 C22 C34 115.8(8) . . ? C21 C22 C34 124.2(8) . . ? C24 C23 C22 120.4(8) . . ? C23 C24 C25 120.4(8) . . ? C24 C25 C26 119.9(8) . . ? C25 C26 C21 120.4(8) . . ? C25 C26 C27 117.1(8) . . ? C21 C26 C27 122.4(8) . . ? O11 C27 N7 122.6(9) . . ? O11 C27 C26 119.5(8) . . ? N7 C27 C26 117.9(8) . . ? C29 C28 C33 121.4(9) . . ? C29 C28 N7 117.2(9) . . ? C33 C28 N7 121.2(9) . . ? C30 C29 C28 117.9(9) . . ? C31 C30 C29 122.4(9) . . ? C31 C30 N9 121.5(11) . . ? C29 C30 N9 116.2(10) . . ? C32 C31 C30 119.1(10) . . ? C31 C32 C33 121.9(10) . . ? C31 C32 N8 120.5(11) . . ? C33 C32 N8 117.6(10) . . ? C28 C33 C32 117.2(9) . . ? O16 C34 N10 122.9(8) . . ? O16 C34 C22 120.8(8) . . ? N10 C34 C22 116.3(8) . . ? C40 C35 C36 119.5(8) . . ? C40 C35 N10 116.9(8) . . ? C36 C35 N10 123.5(8) . . ? C37 C36 C35 119.3(8) . . ? C36 C37 C38 122.6(10) . . ? C36 C37 N12 116.8(9) . . ? C38 C37 N12 120.2(9) . . ? C39 C38 C37 116.8(9) . . ? C38 C39 C40 123.5(8) . . ? C38 C39 N11 117.1(9) . . ? C40 C39 N11 119.4(9) . . ? C39 C40 C35 118.2(8) . . ? C41 N13 C49 112.0(6) . . ? C41 N13 C45 108.8(6) . . ? C49 N13 C45 108.5(6) . . ? C41 N13 C53 108.2(6) . . ? C49 N13 C53 109.0(6) . . ? C45 N13 C53 110.3(6) . . ? N13 C41 C42 116.5(7) . . ? C41 C42 C43 110.9(8) . . ? C44 C43 C42 115.2(9) . . ? N13 C45 C46 115.2(7) . . ? C45 C46 C47 111.1(7) . . ? C48 C47 C46 110.3(7) . . ? C50 C49 N13 113.9(7) . . ? C51 C50 C49 111.9(8) . . ? C50 C51 C52 116.6(9) . . ? C54 C53 N13 116.3(7) . . ? C53 C54 C55 110.5(8) . . ? C56 C55 C54 114.3(9) . . ? C69 N14 C65 113.1(7) . . ? C69 N14 C61 109.5(7) . . ? C65 N14 C61 108.9(7) . . ? C69 N14 C57 108.9(7) . . ? C65 N14 C57 106.8(6) . . ? C61 N14 C57 109.7(7) . . ? C58 C57 N14 117.4(7) . . ? C57 C58 C59 111.3(7) . . ? C58 C59 C60 113.8(8) . . ? C62 C61 N14 115.3(9) . . ? C61 C62 C63 110.3(10) . . ? C64 C63 C62 113.6(11) . . ? C66 C65 N14 115.5(7) . . ? C65 C66 C67 112.8(8) . . ? C66 C67 C68 115.3(9) . . ? N14 C69 C70 118.1(8) . . ? C69 C70 C71 108.5(10) . . ? C70 C71 C72 110.2(11) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 F1 0.88 1.78 2.646(8) 167.1 . N4 H4 F2 0.88 1.81 2.684(9) 169.1 . N7 H7 F2 0.88 1.73 2.591(8) 167.3 . N10 H10 F1 0.88 1.75 2.609(8) 163.4 . _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.574 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.096