Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ijblin@mail.ndhu.edu.tw _publ_contact_author_name 'Ivan J. B. Lin' _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name I.J.B.Lin K.-M.Lee Y.-T.Lee data_001 _database_code_CSD 196012 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H36 F6 N3 O P' _chemical_formula_weight 467.48 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' P P 0.1023 0.0942 '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' _cell_length_a 9.3592(10) _cell_length_b 10.577(4) _cell_length_c 24.232(3) _cell_angle_alpha 78.042(17) _cell_angle_beta 83.862(7) _cell_angle_gamma 76.410(14) _cell_volume 2276.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 4.70 _cell_measurement_theta_max 9.51 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9323 _exptl_absorpt_correction_T_max 0.9828 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6160 _diffrn_reflns_av_R_equivalents 0.5863 _diffrn_reflns_av_sigmaI/netI 0.3879 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5771 _reflns_number_gt 2769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 5771 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1817 _refine_ls_R_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.3117 _refine_ls_wR_factor_gt 0.2523 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.151 _refine_ls_shift/su_mean 0.034 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 P1 P 0.3593(2) 0.4173(2) 0.13550(10) 0.0757(6) Uani 1 1 d . . . P2 P 0.9097(2) -0.0587(2) 0.17123(10) 0.0850(7) Uani 1 1 d . . . N4 N 0.5567(6) -0.1366(5) 0.1036(3) 0.0652(15) Uani 1 1 d . . . O2 O 0.4884(5) -0.1555(5) -0.0010(2) 0.0773(14) Uani 1 1 d . . . F16 F 0.4610(5) 0.2796(4) 0.1260(2) 0.1101(17) Uani 1 1 d . . . C18 C 0.4986(7) -0.0351(7) 0.1295(3) 0.0635(18) Uani 1 1 d . . . H18A H 0.5251 0.0465 0.1212 0.076 Uiso 1 1 calc R . . O1 O 0.9881(4) 0.2568(5) -0.0052(2) 0.0825(15) Uani 1 1 d . . . N1 N 0.7977(6) 0.3797(6) 0.0699(3) 0.0663(15) Uani 1 1 d . . . N5 N 0.3988(6) -0.0675(6) 0.1685(3) 0.0706(16) Uani 1 1 d . . . F25 F 0.9151(7) 0.0613(6) 0.1979(3) 0.144(2) Uani 1 1 d . . . F24 F 0.8078(7) 0.0334(6) 0.1251(3) 0.142(2) Uani 1 1 d . . . F15 F 0.2580(5) 0.5540(5) 0.1434(3) 0.132(2) Uani 1 1 d . . . N6 N 0.7236(6) -0.1832(6) -0.0349(3) 0.0835(19) Uani 1 1 d . . . H6A H 0.7025 -0.1942 -0.0670 0.100 Uiso 1 1 calc R . . H6B H 0.8133 -0.1865 -0.0287 0.100 Uiso 1 1 calc R . . C22 C 0.6182(7) -0.1613(7) 0.0050(3) 0.0693(19) Uani 1 1 d . . . C19 C 0.4885(9) -0.2376(7) 0.1276(3) 0.080(2) Uani 1 1 d . . . H19A H 0.5072 -0.3208 0.1180 0.095 Uiso 1 1 calc R . . C5 C 0.8618(7) 0.2448(7) -0.0039(3) 0.0673(18) Uani 1 1 d . . . C21 C 0.6701(7) -0.1394(8) 0.0581(3) 0.072(2) Uani 1 1 d . . . H21A H 0.7544 -0.2097 0.0699 0.086 Uiso 1 1 calc R . . H21B H 0.7019 -0.0562 0.0502 0.086 Uiso 1 1 calc R . . N3 N 0.8174(6) 0.1683(7) -0.0325(3) 0.088(2) Uani 1 1 d . . . H3A H 0.8797 0.1230 -0.0536 0.106 Uiso 1 1 calc R . . H3B H 0.7262 0.1640 -0.0298 0.106 Uiso 1 1 calc R . . C1 C 0.8092(7) 0.3394(7) 0.1251(4) 0.0693(19) Uani 1 1 d . . . H1A H 0.7780 0.2661 0.1466 0.083 Uiso 1 1 calc R . . N2 N 0.8710(6) 0.4182(6) 0.1446(3) 0.0730(17) Uani 1 1 d . . . C6 C 0.8949(10) 0.4116(10) 0.2043(4) 0.109(3) Uani 1 1 d . . . H6C H 0.9910 0.4289 0.2070 0.130 Uiso 1 1 calc R . . H6D H 0.8938 0.3231 0.2253 0.130 Uiso 1 1 calc R . . C4 C 0.7396(7) 0.3147(8) 0.0320(3) 0.074(2) Uani 1 1 d . . . H4A H 0.6711 0.3803 0.0078 0.088 Uiso 1 1 calc R . . H4B H 0.6865 0.2510 0.0543 0.088 Uiso 1 1 calc R . . F26 F 0.9041(8) -0.1775(6) 0.1430(3) 0.168(3) Uani 1 1 d . . . F23 F 0.7716(8) -0.0846(10) 0.2042(4) 0.206(4) Uani 1 1 d . . . C20 C 0.3895(9) -0.1947(7) 0.1678(4) 0.080(2) Uani 1 1 d . . . H20A H 0.3265 -0.2423 0.1909 0.096 Uiso 1 1 calc R . . F22 F 1.0472(6) -0.0319(10) 0.1328(3) 0.191(4) Uani 1 1 d . . . F14 F 0.2811(10) 0.3537(6) 0.1875(4) 0.227(5) Uani 1 1 d . . . C2 C 0.8543(7) 0.4893(8) 0.0539(4) 0.078(2) Uani 1 1 d . . . H2A H 0.8598 0.5390 0.0176 0.094 Uiso 1 1 calc R . . C31 C -0.0897(14) 0.3461(11) 0.5585(5) 0.139(4) Uani 1 1 d . . . H31A H -0.1847 0.3731 0.5421 0.167 Uiso 1 1 calc R . . H31B H -0.0405 0.4190 0.5456 0.167 Uiso 1 1 calc R . . F21 F 1.0103(9) -0.1484(7) 0.2159(3) 0.186(4) Uani 1 1 d . . . C23 C 0.3084(8) 0.0235(8) 0.2031(3) 0.082(2) Uani 1 1 d . . . H23A H 0.2064 0.0376 0.1945 0.099 Uiso 1 1 calc R . . H23B H 0.3368 0.1081 0.1922 0.099 Uiso 1 1 calc R . . C8 C 0.7959(12) 0.5108(11) 0.2903(5) 0.131(4) Uani 1 1 d . . . H8A H 0.8898 0.5324 0.2929 0.157 Uiso 1 1 calc R . . H8B H 0.7993 0.4220 0.3117 0.157 Uiso 1 1 calc R . . C3 C 0.9013(8) 0.5127(8) 0.1010(4) 0.081(2) Uani 1 1 d . . . H3C H 0.9462 0.5811 0.1030 0.098 Uiso 1 1 calc R . . F13 F 0.2461(7) 0.3957(10) 0.1021(5) 0.268(6) Uani 1 1 d . . . F12 F 0.4745(7) 0.4389(8) 0.1698(4) 0.189(4) Uani 1 1 d . . . C13 C 0.4666(15) 0.7784(15) 0.4945(6) 0.165(5) Uani 1 1 d . . . H13A H 0.3706 0.7684 0.4868 0.198 Uiso 1 1 calc R . . H13B H 0.4745 0.8674 0.4762 0.198 Uiso 1 1 calc R . . F11 F 0.4457(8) 0.4887(6) 0.0850(3) 0.183(3) Uani 1 1 d . . . C7 C 0.7777(10) 0.5110(9) 0.2303(4) 0.103(3) Uani 1 1 d . . . H7A H 0.7783 0.5989 0.2086 0.123 Uiso 1 1 calc R . . H7B H 0.6822 0.4929 0.2274 0.123 Uiso 1 1 calc R . . C24 C 0.3185(12) -0.0203(9) 0.2646(4) 0.113(3) Uani 1 1 d . . . H24A H 0.4195 -0.0328 0.2743 0.136 Uiso 1 1 calc R . . H24B H 0.2888 -0.1042 0.2766 0.136 Uiso 1 1 calc R . . C25 C 0.2185(11) 0.0839(10) 0.2947(4) 0.114(3) Uani 1 1 d . . . H25A H 0.2515 0.1662 0.2823 0.136 Uiso 1 1 calc R . . H25B H 0.1198 0.0989 0.2823 0.136 Uiso 1 1 calc R . . C10 C 0.6836(14) 0.6021(14) 0.3789(6) 0.158(5) Uani 1 1 d . . . H10A H 0.6804 0.5130 0.3987 0.190 Uiso 1 1 calc R . . H10B H 0.7789 0.6171 0.3845 0.190 Uiso 1 1 calc R . . C15 C 0.368(2) 0.853(2) 0.5871(8) 0.223(8) Uani 1 1 d . . . H15A H 0.2720 0.8411 0.5810 0.268 Uiso 1 1 calc R . . H15B H 0.3722 0.9423 0.5675 0.268 Uiso 1 1 calc R . . C32 C -0.1198(15) 0.3372(12) 0.6200(5) 0.154(5) Uani 1 1 d . . . H32A H -0.1702 0.2652 0.6332 0.184 Uiso 1 1 calc R . . H32B H -0.0252 0.3103 0.6368 0.184 Uiso 1 1 calc R . . C27 C 0.1188(13) 0.1631(11) 0.3855(4) 0.125(4) Uani 1 1 d . . . H27A H 0.1600 0.2409 0.3724 0.151 Uiso 1 1 calc R . . H27B H 0.0207 0.1846 0.3717 0.151 Uiso 1 1 calc R . . C29 C 0.0145(13) 0.2522(10) 0.4727(5) 0.131(4) Uani 1 1 d . . . H29A H 0.0585 0.3282 0.4592 0.157 Uiso 1 1 calc R . . H29B H -0.0825 0.2751 0.4579 0.157 Uiso 1 1 calc R . . C26 C 0.2100(14) 0.0547(11) 0.3565(4) 0.141(4) Uani 1 1 d . . . H26A H 0.3093 0.0336 0.3691 0.170 Uiso 1 1 calc R . . H26B H 0.1700 -0.0239 0.3690 0.170 Uiso 1 1 calc R . . C33 C -0.2021(18) 0.4476(14) 0.6435(5) 0.182(6) Uani 1 1 d . . . H33A H -0.1505 0.5189 0.6305 0.218 Uiso 1 1 calc R . . H33B H -0.2956 0.4753 0.6259 0.218 Uiso 1 1 calc R . . C9 C 0.6775(13) 0.6051(12) 0.3168(5) 0.135(4) Uani 1 1 d . . . H9A H 0.5834 0.5879 0.3110 0.162 Uiso 1 1 calc R . . H9B H 0.6796 0.6941 0.2967 0.162 Uiso 1 1 calc R . . C12 C 0.5743(16) 0.6889(15) 0.4657(6) 0.169(5) Uani 1 1 d . . . H12A H 0.6701 0.7008 0.4726 0.202 Uiso 1 1 calc R . . H12B H 0.5683 0.5999 0.4848 0.202 Uiso 1 1 calc R . . C30 C -0.0072(16) 0.2386(12) 0.5332(5) 0.154(5) Uani 1 1 d . . . H30A H -0.0541 0.1643 0.5467 0.185 Uiso 1 1 calc R . . H30B H 0.0896 0.2134 0.5481 0.185 Uiso 1 1 calc R . . C28 C 0.1024(15) 0.1437(11) 0.4456(5) 0.147(4) Uani 1 1 d . . . H28A H 0.2003 0.1210 0.4595 0.176 Uiso 1 1 calc R . . H28B H 0.0592 0.0671 0.4587 0.176 Uiso 1 1 calc R . . C34 C -0.2350(17) 0.4424(14) 0.7021(5) 0.182(6) Uani 1 1 d . . . H34A H -0.2891 0.5276 0.7086 0.273 Uiso 1 1 calc R . . H34B H -0.1450 0.4183 0.7212 0.273 Uiso 1 1 calc R . . H34C H -0.2931 0.3776 0.7163 0.273 Uiso 1 1 calc R . . C11 C 0.5750(14) 0.6911(13) 0.4057(6) 0.152(5) Uani 1 1 d . . . H11A H 0.4799 0.6779 0.3987 0.182 Uiso 1 1 calc R . . H11B H 0.5806 0.7799 0.3864 0.182 Uiso 1 1 calc R . . C16 C 0.362(3) 0.859(3) 0.6435(8) 0.293(14) Uani 1 1 d . . . H16A H 0.3520 0.7712 0.6628 0.352 Uiso 1 1 calc R . . H16B H 0.4613 0.8641 0.6499 0.352 Uiso 1 1 calc R . . C14 C 0.465(2) 0.7726(17) 0.5565(6) 0.192(6) Uani 1 1 d . . . H14A H 0.4569 0.6831 0.5741 0.231 Uiso 1 1 calc R . . H14B H 0.5619 0.7805 0.5636 0.231 Uiso 1 1 calc R . . C17 C 0.284(4) 0.932(3) 0.6714(12) 0.38(2) Uani 1 1 d . . . H17D H 0.3112 0.9069 0.7098 0.575 Uiso 1 1 calc R . . H17A H 0.1833 0.9269 0.6699 0.575 Uiso 1 1 calc R . . H17B H 0.2940 1.0214 0.6567 0.575 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 P1 0.0643(11) 0.0708(12) 0.0957(16) -0.0302(11) 0.0107(11) -0.0163(10) P2 0.0770(14) 0.0886(16) 0.0957(17) -0.0315(13) -0.0152(13) -0.0139(12) N4 0.063(3) 0.058(3) 0.078(4) -0.020(3) -0.009(3) -0.013(3) O2 0.055(3) 0.100(4) 0.088(4) -0.036(3) -0.004(2) -0.024(3) F16 0.103(3) 0.068(3) 0.154(5) -0.038(3) 0.040(3) -0.017(3) C18 0.063(4) 0.059(4) 0.078(5) -0.030(4) -0.009(4) -0.016(4) O1 0.044(2) 0.107(4) 0.104(4) -0.037(3) 0.008(2) -0.021(3) N1 0.054(3) 0.062(3) 0.086(5) -0.023(3) 0.008(3) -0.017(3) N5 0.071(4) 0.071(4) 0.075(4) -0.028(3) -0.005(3) -0.015(3) F25 0.178(5) 0.119(4) 0.153(5) -0.070(4) -0.050(4) -0.013(4) F24 0.157(5) 0.105(4) 0.175(6) 0.001(4) -0.088(5) -0.038(4) F15 0.104(3) 0.087(3) 0.194(6) -0.052(4) 0.032(4) 0.001(3) N6 0.058(3) 0.112(5) 0.087(5) -0.042(4) 0.004(3) -0.014(3) C22 0.053(4) 0.068(4) 0.093(6) -0.031(4) -0.007(4) -0.012(3) C19 0.102(6) 0.058(4) 0.079(6) -0.013(4) -0.005(5) -0.017(4) C5 0.050(4) 0.075(5) 0.072(5) -0.012(4) 0.007(3) -0.010(4) C21 0.055(4) 0.081(5) 0.090(5) -0.034(4) -0.002(4) -0.019(4) N3 0.059(3) 0.125(6) 0.095(5) -0.053(4) 0.009(3) -0.023(4) C1 0.067(4) 0.066(4) 0.068(5) -0.005(4) 0.007(4) -0.013(4) N2 0.067(4) 0.067(4) 0.085(5) -0.025(4) -0.007(3) -0.006(3) C6 0.093(6) 0.118(8) 0.120(8) -0.045(6) -0.016(6) -0.010(6) C4 0.051(4) 0.087(5) 0.088(6) -0.023(4) -0.002(4) -0.020(4) F26 0.218(7) 0.108(4) 0.203(7) -0.061(4) -0.098(6) -0.022(5) F23 0.139(5) 0.328(12) 0.170(7) -0.045(8) 0.023(5) -0.106(6) C20 0.098(6) 0.067(5) 0.084(6) -0.008(4) -0.006(5) -0.039(5) F22 0.116(4) 0.333(11) 0.172(7) -0.137(7) 0.030(4) -0.082(5) F14 0.280(9) 0.100(4) 0.258(10) -0.032(5) 0.180(8) -0.042(6) C2 0.071(4) 0.079(5) 0.080(6) -0.011(4) 0.009(4) -0.016(4) C31 0.173(10) 0.127(9) 0.117(9) -0.041(7) 0.017(8) -0.027(9) F21 0.226(7) 0.136(5) 0.199(8) 0.002(5) -0.130(7) -0.026(5) C23 0.080(5) 0.086(5) 0.083(6) -0.026(4) 0.006(4) -0.018(4) C8 0.139(9) 0.150(10) 0.109(9) -0.051(7) -0.012(7) -0.018(8) C3 0.065(4) 0.072(5) 0.110(7) -0.024(5) 0.006(5) -0.019(4) F13 0.114(5) 0.336(11) 0.427(16) -0.296(12) -0.095(7) 0.035(6) F12 0.143(5) 0.209(7) 0.245(9) -0.115(7) -0.063(6) -0.011(5) C13 0.166(11) 0.190(14) 0.139(12) -0.070(10) 0.006(9) -0.012(10) F11 0.203(6) 0.104(4) 0.186(7) -0.003(4) 0.093(6) 0.008(4) C7 0.105(6) 0.102(7) 0.105(8) -0.029(5) -0.012(5) -0.020(6) C24 0.148(8) 0.092(6) 0.096(7) -0.033(5) 0.015(6) -0.018(6) C25 0.142(8) 0.124(8) 0.081(7) -0.040(6) -0.003(6) -0.025(7) C10 0.154(10) 0.196(13) 0.134(11) -0.073(10) 0.003(8) -0.028(10) C15 0.221(18) 0.27(2) 0.198(18) -0.135(17) 0.033(14) -0.039(15) C32 0.187(11) 0.153(11) 0.132(10) -0.067(9) 0.052(9) -0.051(10) C27 0.161(9) 0.134(9) 0.085(7) -0.043(6) 0.005(6) -0.023(8) C29 0.151(9) 0.119(8) 0.128(9) -0.057(7) 0.015(7) -0.019(7) C26 0.191(11) 0.121(9) 0.097(8) -0.032(7) 0.040(7) -0.019(8) C33 0.240(15) 0.192(13) 0.116(10) -0.088(10) 0.005(10) -0.007(12) C9 0.143(9) 0.140(10) 0.117(9) -0.049(7) -0.002(7) -0.005(8) C12 0.186(13) 0.200(14) 0.110(10) -0.044(10) 0.000(9) -0.014(11) C30 0.217(13) 0.149(11) 0.093(8) -0.050(7) 0.028(8) -0.026(10) C28 0.196(12) 0.135(10) 0.100(9) -0.034(7) 0.030(8) -0.025(9) C34 0.230(14) 0.194(14) 0.115(10) -0.055(9) 0.032(10) -0.031(12) C11 0.148(10) 0.164(12) 0.140(11) -0.064(9) 0.004(8) -0.002(9) C16 0.42(4) 0.39(3) 0.133(15) -0.140(19) 0.072(18) -0.16(3) C14 0.227(17) 0.236(18) 0.113(11) -0.049(11) 0.006(10) -0.041(15) C17 0.50(5) 0.54(5) 0.24(3) -0.23(3) 0.13(3) -0.28(4) _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 P1 F13 1.484(6) . ? P1 F14 1.503(7) . ? P1 F12 1.514(6) . ? P1 F11 1.553(7) . ? P1 F15 1.567(5) . ? P1 F16 1.588(5) . ? P2 F23 1.496(7) . ? P2 F21 1.527(6) . ? P2 F25 1.552(5) . ? P2 F22 1.552(7) . ? P2 F26 1.563(6) . ? P2 F24 1.565(5) . ? N4 C18 1.332(8) . ? N4 C19 1.368(9) . ? N4 C21 1.447(9) . ? O2 C22 1.225(7) . ? C18 N5 1.307(8) . ? O1 C5 1.215(7) . ? N1 C1 1.325(9) . ? N1 C2 1.354(9) . ? N1 C4 1.468(8) . ? N5 C20 1.372(8) . ? N5 C23 1.465(9) . ? N6 C22 1.319(9) . ? C22 C21 1.500(9) . ? C19 C20 1.343(11) . ? C5 N3 1.326(8) . ? C5 C4 1.506(10) . ? C1 N2 1.304(8) . ? N2 C3 1.351(9) . ? N2 C6 1.473(11) . ? C6 C7 1.514(12) . ? C2 C3 1.354(10) . ? C31 C30 1.430(14) . ? C31 C32 1.474(15) . ? C23 C24 1.474(12) . ? C8 C7 1.480(13) . ? C8 C9 1.493(14) . ? C13 C12 1.440(17) . ? C13 C14 1.489(18) . ? C24 C25 1.525(12) . ? C25 C26 1.463(13) . ? C10 C11 1.416(15) . ? C10 C9 1.505(15) . ? C15 C14 1.36(2) . ? C15 C16 1.37(2) . ? C32 C33 1.428(15) . ? C27 C28 1.425(14) . ? C27 C26 1.510(13) . ? C29 C30 1.440(15) . ? C29 C28 1.476(13) . ? C33 C34 1.412(16) . ? C12 C11 1.449(16) . ? C16 C17 1.20(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F13 P1 F14 87.7(6) . . ? F13 P1 F12 179.8(8) . . ? F14 P1 F12 92.1(6) . . ? F13 P1 F11 96.7(7) . . ? F14 P1 F11 175.2(5) . . ? F12 P1 F11 83.5(5) . . ? F13 P1 F15 89.5(4) . . ? F14 P1 F15 88.3(4) . . ? F12 P1 F15 90.6(4) . . ? F11 P1 F15 90.0(3) . . ? F13 P1 F16 89.5(4) . . ? F14 P1 F16 92.6(3) . . ? F12 P1 F16 90.5(3) . . ? F11 P1 F16 89.2(3) . . ? F15 P1 F16 178.6(4) . . ? F23 P2 F21 93.8(5) . . ? F23 P2 F25 94.9(5) . . ? F21 P2 F25 89.0(4) . . ? F23 P2 F22 175.5(4) . . ? F21 P2 F22 89.7(5) . . ? F25 P2 F22 87.9(4) . . ? F23 P2 F26 85.8(5) . . ? F21 P2 F26 92.1(4) . . ? F25 P2 F26 178.7(4) . . ? F22 P2 F26 91.4(4) . . ? F23 P2 F24 86.6(4) . . ? F21 P2 F24 179.5(5) . . ? F25 P2 F24 91.0(3) . . ? F22 P2 F24 89.8(4) . . ? F26 P2 F24 87.9(3) . . ? C18 N4 C19 107.3(6) . . ? C18 N4 C21 126.4(6) . . ? C19 N4 C21 126.2(6) . . ? N5 C18 N4 109.8(6) . . ? C1 N1 C2 107.9(6) . . ? C1 N1 C4 126.4(6) . . ? C2 N1 C4 125.7(7) . . ? C18 N5 C20 108.2(6) . . ? C18 N5 C23 123.9(6) . . ? C20 N5 C23 127.7(7) . . ? O2 C22 N6 123.3(7) . . ? O2 C22 C21 122.5(7) . . ? N6 C22 C21 114.2(5) . . ? C20 C19 N4 107.6(7) . . ? O1 C5 N3 124.3(6) . . ? O1 C5 C4 122.5(7) . . ? N3 C5 C4 113.2(5) . . ? N4 C21 C22 112.4(5) . . ? N2 C1 N1 109.6(7) . . ? C1 N2 C3 108.3(7) . . ? C1 N2 C6 126.2(8) . . ? C3 N2 C6 125.4(7) . . ? N2 C6 C7 111.5(7) . . ? N1 C4 C5 111.2(5) . . ? C19 C20 N5 107.1(7) . . ? N1 C2 C3 106.8(7) . . ? C30 C31 C32 123.6(11) . . ? N5 C23 C24 115.5(6) . . ? C7 C8 C9 114.7(9) . . ? N2 C3 C2 107.4(7) . . ? C12 C13 C14 122.1(14) . . ? C8 C7 C6 114.4(8) . . ? C23 C24 C25 109.3(7) . . ? C26 C25 C24 117.0(9) . . ? C11 C10 C9 119.3(12) . . ? C14 C15 C16 130(2) . . ? C33 C32 C31 121.6(13) . . ? C28 C27 C26 120.4(10) . . ? C30 C29 C28 121.9(11) . . ? C25 C26 C27 116.1(9) . . ? C34 C33 C32 123.3(14) . . ? C8 C9 C10 117.2(10) . . ? C11 C12 C13 122.7(13) . . ? C31 C30 C29 121.0(11) . . ? C27 C28 C29 119.2(10) . . ? C10 C11 C12 121.0(12) . . ? C17 C16 C15 132(4) . . ? C15 C14 C13 126.3(17) . . ? _diffrn_measured_fraction_theta_max 0.720 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.720 _refine_diff_density_max 0.487 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.048