Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_jul53 _database_code_CSD 192681 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Silvio Decurtins' 'Sandra Delahaye' 'Andreas Hauser' 'Eduard Rusanov' 'Julia Rusanova' 'Helen Stoeckli-Evans' _publ_contact_author_name 'Prof Silvio Decurtins' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Berne Freiestrasse 3 Berne 3012 SWITZERLAND ; _publ_contact_author_email ' silvio.decurtins@iac.unibe.ch ' _publ_requested_journal 'J. Chem. Soc., Dalton Transactions' _publ_section_title ; Ruthenium (II) Complex of Bis(2,2'-bipyridine)(6,7-dicyanodipyrido [3,2-a:2',3'-c]phenazine):Synthesis, Structure, Electrochemical and Luminescence Studies ; _publ_section_references ; 1. Stoe & Cie (2000). IPDS Software. Stoe & Cie GmbH, Darmstadt, Germany. 2. G.M. Scheldrick, (1990) "SHELXS-97 Program for Crystal Structure Determination", Acta Crystallogr., A46, 467 473. 3. G.Scheldrick, (1999) "SHELXL-97", Universität Göttingen, Göttingen, Germany. 4. A.L.Spek, (1990) "Platon/PLUTON version Jan. 1999", Acta Crystallogr., A46, C-34. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 N10 Ru, 2(F6 P), 0.5(H2 O), 0.5(C H4 O)' _chemical_formula_sum 'C40.50 H27 F12 N10 O P2 Ru' _chemical_formula_weight 1060.73 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 '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 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 9.304(2) _cell_length_b 37.034(7) _cell_length_c 12.014(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.54(3) _cell_angle_gamma 90.00 _cell_volume 4103.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4954 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 24.08 _exptl_crystal_description needle _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.88\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24611 _diffrn_reflns_av_R_equivalents 0.1476 _diffrn_reflns_av_sigmaI/netI 0.3093 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 24.08 _reflns_number_total 6401 _reflns_number_gt 2355 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'EXPOSE (Stoe IPDS Software, 2000)' _computing_cell_refinement 'CELL (Stoe IPDS Software, 2000)' _computing_data_reduction 'INTEGRATE (Stoe IPDS Software, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON99 (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The long b axis (37.034(7) Å) required that the image plate be displaced to 80 mm, giving a resolution of 0.88 Å, in order do a void overlapped reflections. The crystal did not diffract significantly beyond 35° in 2q, hence only one-third of the unique data can be considered to be observed (I > 2s (I)). Some highly disordered solvent peaks were observed but could no be modelled satisfactorally. The SQUEEZE routine in PLATON was used to modify the HKL file and the solvent equated to one half a molecule of water and one half a molecule of methanol, per molecule of complex. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0500*P+(0.0487P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6401 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.22489(8) 0.157628(19) 0.32550(6) 0.02106(19) Uani 1 1 d . . . N1 N 0.1721(8) 0.10504(18) 0.2781(6) 0.0218(17) Uani 1 1 d . . . N2 N 0.3716(8) 0.14794(17) 0.2107(6) 0.0213(17) Uani 1 1 d . . . N3 N 0.2578(9) 0.01465(19) 0.0091(6) 0.0290(18) Uani 1 1 d . . . N4 N 0.4467(9) 0.06315(19) -0.0819(6) 0.0274(18) Uani 1 1 d . . . N5 N 0.2845(12) -0.1013(2) -0.3123(8) 0.049(2) Uani 1 1 d . . . N6 N 0.5806(12) -0.0374(2) -0.4319(8) 0.053(3) Uani 1 1 d . . . N7 N 0.3461(8) 0.13823(17) 0.4682(5) 0.0208(16) Uani 1 1 d . . . N8 N 0.0789(8) 0.16152(18) 0.4388(5) 0.0203(15) Uani 1 1 d . . . N9 N 0.0955(8) 0.18289(19) 0.1958(6) 0.0225(17) Uani 1 1 d . . . N10 N 0.2686(8) 0.21130(18) 0.3612(5) 0.0219(17) Uani 1 1 d . . . C1 C 0.0800(10) 0.0833(2) 0.3198(7) 0.026(2) Uani 1 1 d . . . H1A H 0.0313 0.0921 0.3790 0.032 Uiso 1 1 calc R . . C2 C 0.0504(11) 0.0481(2) 0.2815(7) 0.028(2) Uani 1 1 d . . . H2A H -0.0145 0.0332 0.3157 0.034 Uiso 1 1 calc R . . C3 C 0.1159(11) 0.0355(2) 0.1944(8) 0.033(2) Uani 1 1 d . . . H3A H 0.0966 0.0118 0.1660 0.040 Uiso 1 1 calc R . . C4 C 0.2132(10) 0.0583(2) 0.1469(7) 0.025(2) Uani 1 1 d . . . C5 C 0.2407(10) 0.0921(2) 0.1928(7) 0.022(2) Uani 1 1 d . . . C6 C 0.3461(10) 0.1160(2) 0.1556(6) 0.0211(19) Uani 1 1 d . . . C7 C 0.4190(10) 0.1064(2) 0.0655(7) 0.026(2) Uani 1 1 d . . . C8 C 0.5236(10) 0.1302(2) 0.0334(7) 0.028(2) Uani 1 1 d . . . H8A H 0.5736 0.1248 -0.0286 0.034 Uiso 1 1 calc R . . C9 C 0.5516(10) 0.1612(3) 0.0931(7) 0.029(2) Uani 1 1 d . . . H9A H 0.6252 0.1771 0.0752 0.034 Uiso 1 1 calc R . . C10 C 0.4731(11) 0.1696(2) 0.1801(8) 0.027(2) Uani 1 1 d . . . H10A H 0.4927 0.1917 0.2193 0.033 Uiso 1 1 calc R . . C11 C 0.2867(10) 0.0471(2) 0.0503(7) 0.023(2) Uani 1 1 d . . . C12 C 0.3839(11) 0.0714(2) 0.0076(8) 0.029(2) Uani 1 1 d . . . C13 C 0.3230(10) 0.0056(2) -0.0810(7) 0.027(2) Uani 1 1 d . . . C14 C 0.4164(10) 0.0296(2) -0.1268(7) 0.026(2) Uani 1 1 d . . . C15 C 0.4837(12) 0.0189(3) -0.2211(7) 0.034(2) Uani 1 1 d . . . H15A H 0.5501 0.0345 -0.2510 0.041 Uiso 1 1 calc R . . C16 C 0.4510(11) -0.0143(2) -0.2680(8) 0.032(2) Uani 1 1 d . . . C17 C 0.3538(11) -0.0389(2) -0.2223(8) 0.030(2) Uani 1 1 d . . . C18 C 0.2916(11) -0.0286(2) -0.1303(7) 0.030(2) Uani 1 1 d . . . H18A H 0.2270 -0.0444 -0.0995 0.036 Uiso 1 1 calc R . . C19 C 0.3163(11) -0.0739(3) -0.2744(8) 0.034(2) Uani 1 1 d . . . C20 C 0.5233(12) -0.0268(3) -0.3602(8) 0.035(2) Uani 1 1 d . . . C21 C 0.4851(11) 0.1271(2) 0.4777(7) 0.031(2) Uani 1 1 d . . . H21A H 0.5345 0.1279 0.4134 0.037 Uiso 1 1 calc R . . C22 C 0.5577(12) 0.1148(2) 0.5774(8) 0.034(2) Uani 1 1 d . . . H22A H 0.6555 0.1070 0.5806 0.041 Uiso 1 1 calc R . . C23 C 0.4911(12) 0.1135(3) 0.6716(7) 0.036(2) Uani 1 1 d . . . H23A H 0.5411 0.1053 0.7410 0.043 Uiso 1 1 calc R . . C24 C 0.3488(11) 0.1246(3) 0.6629(7) 0.033(2) Uani 1 1 d . . . H24A H 0.2991 0.1237 0.7270 0.040 Uiso 1 1 calc R . . C25 C 0.2781(10) 0.1370(2) 0.5630(7) 0.023(2) Uani 1 1 d . . . C26 C 0.1282(10) 0.1500(2) 0.5454(7) 0.026(2) Uani 1 1 d . . . C27 C 0.0367(11) 0.1495(2) 0.6273(8) 0.035(2) Uani 1 1 d . . . H27A H 0.0704 0.1405 0.7001 0.042 Uiso 1 1 calc R . . C28 C -0.1032(10) 0.1620(2) 0.6033(7) 0.029(2) Uani 1 1 d . . . H28A H -0.1664 0.1614 0.6593 0.035 Uiso 1 1 calc R . . C29 C -0.1516(11) 0.1753(2) 0.4981(8) 0.034(2) Uani 1 1 d . . . H29A H -0.2462 0.1851 0.4808 0.041 Uiso 1 1 calc R . . C30 C -0.0569(10) 0.1737(2) 0.4186(7) 0.0215(19) Uani 1 1 d . . . H30A H -0.0908 0.1818 0.3449 0.026 Uiso 1 1 calc R . . C31 C 0.0157(10) 0.1665(2) 0.1080(7) 0.029(2) Uani 1 1 d . . . H31A H 0.0168 0.1409 0.1035 0.034 Uiso 1 1 calc R . . C32 C -0.0672(11) 0.1857(3) 0.0249(8) 0.036(2) Uani 1 1 d . . . H32A H -0.1225 0.1732 -0.0352 0.043 Uiso 1 1 calc R . . C33 C -0.0707(12) 0.2236(3) 0.0280(7) 0.034(2) Uani 1 1 d . . . H33A H -0.1261 0.2374 -0.0291 0.041 Uiso 1 1 calc R . . C34 C 0.0102(11) 0.2397(3) 0.1180(7) 0.034(2) Uani 1 1 d . . . H34A H 0.0089 0.2652 0.1247 0.040 Uiso 1 1 calc R . . C35 C 0.0938(10) 0.2196(2) 0.1995(7) 0.021(2) Uani 1 1 d . . . C36 C 0.1828(10) 0.2350(2) 0.2983(7) 0.023(2) Uani 1 1 d . . . C37 C 0.1825(10) 0.2713(2) 0.3247(7) 0.029(2) Uani 1 1 d . . . H37A H 0.1203 0.2873 0.2791 0.035 Uiso 1 1 calc R . . C38 C 0.2709(11) 0.2846(2) 0.4161(8) 0.030(2) Uani 1 1 d . . . H38A H 0.2702 0.3095 0.4350 0.036 Uiso 1 1 calc R . . C39 C 0.3610(11) 0.2605(2) 0.4799(8) 0.032(2) Uani 1 1 d . . . H39A H 0.4255 0.2686 0.5429 0.038 Uiso 1 1 calc R . . C40 C 0.3551(10) 0.2246(2) 0.4500(7) 0.024(2) Uani 1 1 d . . . H40A H 0.4160 0.2081 0.4950 0.028 Uiso 1 1 calc R . . P1 P 0.0839(3) -0.08527(7) 0.1308(2) 0.0404(7) Uani 1 1 d . . . F11 F 0.2264(10) -0.0612(2) 0.1544(7) 0.093(3) Uani 1 1 d . . . F12 F -0.0568(9) -0.1093(2) 0.1129(7) 0.084(2) Uani 1 1 d . . . F13 F 0.0988(10) -0.0878(2) 0.0018(6) 0.087(3) Uani 1 1 d . . . F14 F 0.1757(11) -0.1204(2) 0.1549(8) 0.099(3) Uani 1 1 d . . . F15 F 0.0779(13) -0.0837(2) 0.2622(6) 0.114(4) Uani 1 1 d . . . F16 F -0.0037(10) -0.0492(2) 0.1141(10) 0.112(3) Uani 1 1 d . . . P2 P 0.3578(3) -0.22962(7) 0.2472(2) 0.0292(6) Uani 1 1 d . . . F21 F 0.5267(6) -0.24011(15) 0.2674(4) 0.0389(14) Uani 1 1 d . . . F22 F 0.1886(6) -0.21986(15) 0.2276(4) 0.0393(14) Uani 1 1 d . . . F23 F 0.3831(7) -0.20301(19) 0.1501(5) 0.065(2) Uani 1 1 d . . . F24 F 0.3315(7) -0.25682(19) 0.3456(5) 0.0620(19) Uani 1 1 d . . . F25 F 0.3875(7) -0.19849(17) 0.3375(5) 0.0588(18) Uani 1 1 d . . . F26 F 0.3288(8) -0.26175(18) 0.1582(6) 0.070(2) Uani 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 Ru1 0.0205(4) 0.0215(3) 0.0215(3) 0.0003(4) 0.0040(3) 0.0012(4) N1 0.015(5) 0.022(4) 0.027(4) -0.001(3) -0.004(3) 0.005(3) N2 0.015(4) 0.021(4) 0.029(4) 0.003(3) 0.004(3) 0.000(3) N3 0.026(5) 0.024(4) 0.037(4) -0.002(3) 0.004(4) 0.006(3) N4 0.026(5) 0.026(4) 0.032(4) -0.008(3) 0.010(4) -0.002(3) N5 0.054(7) 0.039(5) 0.057(6) -0.020(5) 0.021(5) 0.000(5) N6 0.059(7) 0.052(6) 0.049(6) -0.009(5) 0.013(5) 0.003(5) N7 0.015(5) 0.020(4) 0.027(4) -0.005(3) 0.001(3) 0.007(3) N8 0.020(4) 0.018(4) 0.023(4) -0.003(3) 0.006(3) -0.002(3) N9 0.017(5) 0.029(4) 0.022(4) 0.000(3) 0.007(3) 0.001(3) N10 0.026(5) 0.022(4) 0.018(4) 0.000(3) 0.005(3) 0.002(3) C1 0.020(6) 0.028(5) 0.032(5) 0.005(4) 0.009(4) -0.003(4) C2 0.032(6) 0.027(5) 0.029(5) 0.002(4) 0.017(4) -0.003(4) C3 0.031(6) 0.030(5) 0.038(6) -0.005(4) 0.002(5) -0.004(4) C4 0.028(6) 0.017(4) 0.031(5) 0.004(4) -0.001(4) -0.005(4) C5 0.028(6) 0.018(4) 0.022(5) 0.000(3) 0.007(4) 0.005(4) C6 0.023(5) 0.022(4) 0.016(4) 0.006(4) -0.005(4) 0.004(4) C7 0.020(6) 0.026(5) 0.032(5) 0.006(4) 0.003(4) 0.002(4) C8 0.029(6) 0.037(5) 0.021(5) 0.000(4) 0.011(4) 0.000(4) C9 0.031(6) 0.024(5) 0.033(5) 0.000(4) 0.011(4) 0.001(4) C10 0.032(6) 0.016(4) 0.033(5) 0.003(4) 0.002(5) -0.002(4) C11 0.026(6) 0.017(4) 0.025(5) 0.000(3) 0.005(4) 0.003(4) C12 0.025(6) 0.025(5) 0.034(5) 0.002(4) -0.002(4) 0.008(4) C13 0.027(6) 0.027(5) 0.028(5) 0.003(4) 0.006(4) 0.003(4) C14 0.026(6) 0.032(5) 0.021(4) -0.002(4) 0.006(4) -0.002(4) C15 0.047(7) 0.041(6) 0.015(4) 0.000(4) 0.008(4) 0.004(5) C16 0.036(7) 0.027(5) 0.033(5) -0.007(4) 0.004(5) 0.006(4) C17 0.023(6) 0.024(5) 0.043(6) -0.003(4) 0.009(5) 0.002(4) C18 0.034(7) 0.027(5) 0.030(5) 0.005(4) 0.007(4) 0.004(4) C19 0.030(7) 0.038(6) 0.037(5) 0.001(5) 0.009(5) 0.011(5) C20 0.038(7) 0.033(5) 0.035(6) -0.006(4) 0.006(5) 0.005(5) C21 0.036(7) 0.036(5) 0.021(5) -0.007(4) 0.004(4) 0.000(5) C22 0.034(7) 0.031(5) 0.034(6) 0.008(4) -0.005(5) 0.002(4) C23 0.043(7) 0.039(6) 0.021(5) 0.006(4) -0.012(4) 0.005(5) C24 0.025(6) 0.047(6) 0.027(5) 0.004(4) 0.002(4) 0.001(5) C25 0.032(6) 0.016(4) 0.021(4) -0.003(3) 0.004(4) 0.000(4) C26 0.021(6) 0.026(5) 0.032(5) -0.002(4) 0.006(4) -0.005(4) C27 0.044(7) 0.034(6) 0.028(5) 0.001(4) 0.013(4) 0.000(5) C28 0.034(6) 0.027(5) 0.031(5) 0.000(4) 0.019(4) -0.003(5) C29 0.027(6) 0.031(5) 0.046(6) -0.005(4) 0.010(5) 0.005(4) C30 0.022(6) 0.022(4) 0.021(4) -0.005(3) 0.003(4) 0.001(4) C31 0.029(6) 0.032(5) 0.026(5) -0.002(4) 0.008(4) 0.008(4) C32 0.028(6) 0.053(6) 0.025(5) -0.014(4) -0.005(4) -0.003(5) C33 0.041(7) 0.043(6) 0.018(5) 0.002(4) 0.004(4) 0.004(5) C34 0.023(6) 0.049(6) 0.027(5) -0.002(4) -0.003(4) 0.008(5) C35 0.026(6) 0.014(4) 0.026(5) 0.002(4) 0.011(4) 0.003(4) C36 0.023(6) 0.017(4) 0.029(5) -0.005(4) 0.007(4) 0.004(4) C37 0.031(7) 0.027(5) 0.028(5) 0.009(4) -0.002(5) 0.002(4) C38 0.031(6) 0.017(5) 0.041(5) -0.008(4) 0.003(5) -0.008(4) C39 0.037(7) 0.023(5) 0.035(5) -0.005(4) 0.003(5) -0.003(4) C40 0.024(6) 0.022(5) 0.025(5) 0.008(4) 0.005(4) 0.006(4) P1 0.0438(19) 0.0327(14) 0.0436(15) 0.0040(12) 0.0017(13) -0.0040(12) F11 0.078(7) 0.080(5) 0.113(7) 0.012(5) -0.021(5) -0.030(5) F12 0.066(6) 0.085(5) 0.102(6) -0.012(4) 0.023(5) -0.034(4) F13 0.131(8) 0.087(5) 0.048(4) -0.002(4) 0.029(5) -0.048(5) F14 0.115(8) 0.054(5) 0.113(7) -0.001(4) -0.040(5) 0.014(4) F15 0.214(12) 0.076(6) 0.060(5) -0.026(4) 0.048(6) -0.058(6) F16 0.081(7) 0.047(4) 0.194(10) -0.009(5) -0.032(6) 0.024(4) P2 0.0271(16) 0.0356(14) 0.0242(12) -0.0032(10) 0.0013(10) 0.0070(11) F21 0.029(4) 0.054(3) 0.034(3) 0.003(2) 0.008(2) 0.018(3) F22 0.031(4) 0.053(4) 0.032(3) -0.002(2) -0.003(2) 0.008(3) F23 0.052(5) 0.085(5) 0.061(4) 0.045(4) 0.017(3) 0.026(4) F24 0.035(4) 0.088(5) 0.064(4) 0.042(4) 0.012(3) 0.008(3) F25 0.043(4) 0.062(4) 0.068(4) -0.030(3) -0.008(3) 0.016(3) F26 0.058(5) 0.064(4) 0.082(5) -0.034(4) -0.016(4) 0.020(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 Ru1 N7 2.054(7) . ? Ru1 N8 2.050(6) . ? Ru1 N9 2.064(7) . ? Ru1 N10 2.062(7) . ? Ru1 N1 2.070(7) . ? Ru1 N2 2.095(7) . ? N1 C1 1.321(11) . ? N1 C5 1.363(10) . ? N2 C10 1.327(11) . ? N2 C6 1.361(10) . ? N3 C11 1.313(10) . ? N3 C13 1.351(11) . ? N4 C12 1.325(11) . ? N4 C14 1.370(11) . ? N5 C19 1.137(12) . ? N6 C20 1.139(12) . ? N7 C21 1.347(12) . ? N7 C25 1.374(10) . ? N8 C30 1.334(11) . ? N8 C26 1.371(11) . ? N9 C35 1.361(10) . ? N9 C31 1.352(11) . ? N10 C40 1.342(11) . ? N10 C36 1.350(10) . ? C1 C2 1.397(12) . ? C1 H1A 0.9500 . ? C2 C3 1.361(12) . ? C2 H2A 0.9500 . ? C3 C4 1.411(13) . ? C3 H3A 0.9500 . ? C4 C5 1.378(11) . ? C4 C11 1.482(12) . ? C5 C6 1.435(12) . ? C6 C7 1.396(12) . ? C7 C8 1.405(13) . ? C7 C12 1.488(13) . ? C8 C9 1.359(13) . ? C8 H8A 0.9500 . ? C9 C10 1.386(12) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.419(13) . ? C13 C18 1.410(12) . ? C13 C14 1.405(12) . ? C14 C15 1.420(12) . ? C15 C16 1.370(13) . ? C15 H15A 0.9500 . ? C16 C20 1.446(13) . ? C16 C17 1.443(13) . ? C17 C18 1.368(13) . ? C17 C19 1.461(14) . ? C18 H18A 0.9500 . ? C21 C22 1.374(13) . ? C21 H21A 0.9500 . ? C22 C23 1.361(14) . ? C22 H22A 0.9500 . ? C23 C24 1.377(14) . ? C23 H23A 0.9500 . ? C24 C25 1.370(12) . ? C24 H24A 0.9500 . ? C25 C26 1.464(13) . ? C26 C27 1.383(12) . ? C27 C28 1.376(14) . ? C27 H27A 0.9500 . ? C28 C29 1.375(13) . ? C28 H28A 0.9500 . ? C29 C30 1.383(12) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.375(13) . ? C31 H31A 0.9500 . ? C32 C33 1.406(13) . ? C32 H32A 0.9500 . ? C33 C34 1.369(13) . ? C33 H33A 0.9500 . ? C34 C35 1.384(13) . ? C34 H34A 0.9500 . ? C35 C36 1.471(12) . ? C36 C37 1.381(12) . ? C37 C38 1.373(13) . ? C37 H37A 0.9500 . ? C38 C39 1.383(13) . ? C38 H38A 0.9500 . ? C39 C40 1.380(12) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? P1 F16 1.564(8) . ? P1 F14 1.563(8) . ? P1 F12 1.575(8) . ? P1 F13 1.577(7) . ? P1 F15 1.588(7) . ? P1 F11 1.591(8) . ? P2 F23 1.569(6) . ? P2 F25 1.582(6) . ? P2 F24 1.596(6) . ? P2 F22 1.602(6) . ? P2 F26 1.599(7) . ? P2 F21 1.606(6) . ? 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 N7 Ru1 N8 79.0(3) . . ? N7 Ru1 N9 172.1(3) . . ? N8 Ru1 N9 95.6(3) . . ? N7 Ru1 N10 95.3(3) . . ? N8 Ru1 N10 85.6(3) . . ? N9 Ru1 N10 78.4(3) . . ? N7 Ru1 N1 89.1(3) . . ? N8 Ru1 N1 95.4(3) . . ? N9 Ru1 N1 97.2(3) . . ? N10 Ru1 N1 175.6(3) . . ? N7 Ru1 N2 99.0(3) . . ? N8 Ru1 N2 174.2(3) . . ? N9 Ru1 N2 86.9(3) . . ? N10 Ru1 N2 100.0(3) . . ? N1 Ru1 N2 79.0(3) . . ? C1 N1 C5 117.5(7) . . ? C1 N1 Ru1 127.7(6) . . ? C5 N1 Ru1 114.8(6) . . ? C10 N2 C6 118.4(7) . . ? C10 N2 Ru1 128.9(6) . . ? C6 N2 Ru1 112.5(5) . . ? C11 N3 C13 116.0(8) . . ? C12 N4 C14 116.0(8) . . ? C21 N7 C25 117.4(7) . . ? C21 N7 Ru1 126.4(6) . . ? C25 N7 Ru1 116.2(6) . . ? C30 N8 C26 117.9(7) . . ? C30 N8 Ru1 126.7(5) . . ? C26 N8 Ru1 115.4(6) . . ? C35 N9 C31 117.8(7) . . ? C35 N9 Ru1 115.9(6) . . ? C31 N9 Ru1 126.3(6) . . ? C40 N10 C36 117.1(7) . . ? C40 N10 Ru1 126.8(6) . . ? C36 N10 Ru1 115.2(5) . . ? N1 C1 C2 123.6(8) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 118.9(8) . . ? C3 C2 H2A 120.5 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 118.8(8) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 118.4(8) . . ? C5 C4 C11 119.2(7) . . ? C3 C4 C11 122.3(7) . . ? N1 C5 C4 122.6(8) . . ? N1 C5 C6 115.1(7) . . ? C4 C5 C6 122.2(7) . . ? N2 C6 C7 121.8(8) . . ? N2 C6 C5 117.8(7) . . ? C7 C6 C5 120.4(7) . . ? C6 C7 C8 118.6(8) . . ? C6 C7 C12 119.0(8) . . ? C8 C7 C12 122.4(8) . . ? C9 C8 C7 118.4(8) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C8 C9 C10 120.2(9) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? N2 C10 C9 122.5(8) . . ? N2 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? N3 C11 C12 123.6(8) . . ? N3 C11 C4 117.3(7) . . ? C12 C11 C4 119.1(7) . . ? N4 C12 C11 121.1(8) . . ? N4 C12 C7 119.2(8) . . ? C11 C12 C7 119.7(8) . . ? N3 C13 C18 118.0(8) . . ? N3 C13 C14 121.5(8) . . ? C18 C13 C14 120.4(8) . . ? N4 C14 C15 118.5(8) . . ? N4 C14 C13 121.7(8) . . ? C15 C14 C13 119.8(8) . . ? C16 C15 C14 118.7(9) . . ? C16 C15 H15A 120.7 . . ? C14 C15 H15A 120.7 . . ? C15 C16 C20 120.2(9) . . ? C15 C16 C17 121.8(8) . . ? C20 C16 C17 117.8(8) . . ? C18 C17 C19 119.4(8) . . ? C18 C17 C16 118.9(8) . . ? C19 C17 C16 121.6(8) . . ? C17 C18 C13 120.3(8) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? N5 C19 C17 177.8(11) . . ? N6 C20 C16 178.6(11) . . ? N7 C21 C22 122.2(9) . . ? N7 C21 H21A 118.9 . . ? C22 C21 H21A 118.9 . . ? C23 C22 C21 120.7(10) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 117.7(9) . . ? C22 C23 H23A 121.2 . . ? C24 C23 H23A 121.2 . . ? C25 C24 C23 120.9(9) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 N7 121.1(9) . . ? C24 C25 C26 125.1(8) . . ? N7 C25 C26 113.8(7) . . ? N8 C26 C27 120.5(9) . . ? N8 C26 C25 115.6(7) . . ? C27 C26 C25 123.8(8) . . ? C28 C27 C26 120.0(9) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 119.9(8) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 117.3(9) . . ? C30 C29 H29A 121.4 . . ? C28 C29 H29A 121.4 . . ? N8 C30 C29 124.3(8) . . ? N8 C30 H30A 117.9 . . ? C29 C30 H30A 117.9 . . ? N9 C31 C32 122.2(8) . . ? N9 C31 H31A 118.9 . . ? C32 C31 H31A 118.9 . . ? C31 C32 C33 120.6(9) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C34 C33 C32 116.3(9) . . ? C34 C33 H33A 121.9 . . ? C32 C33 H33A 121.9 . . ? C33 C34 C35 121.7(9) . . ? C33 C34 H34A 119.2 . . ? C35 C34 H34A 119.2 . . ? N9 C35 C34 121.4(8) . . ? N9 C35 C36 114.0(7) . . ? C34 C35 C36 124.5(8) . . ? N10 C36 C37 121.6(8) . . ? N10 C36 C35 115.3(7) . . ? C37 C36 C35 123.1(8) . . ? C38 C37 C36 120.8(8) . . ? C38 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? C37 C38 C39 118.0(8) . . ? C37 C38 H38A 121.0 . . ? C39 C38 H38A 121.0 . . ? C38 C39 C40 118.4(9) . . ? C38 C39 H39A 120.8 . . ? C40 C39 H39A 120.8 . . ? N10 C40 C39 124.1(8) . . ? N10 C40 H40A 118.0 . . ? C39 C40 H40A 118.0 . . ? F16 P1 F14 176.4(5) . . ? F16 P1 F12 93.1(5) . . ? F14 P1 F12 88.8(5) . . ? F16 P1 F13 92.1(6) . . ? F14 P1 F13 90.9(5) . . ? F12 P1 F13 90.6(4) . . ? F16 P1 F15 90.6(6) . . ? F14 P1 F15 86.3(5) . . ? F12 P1 F15 91.1(5) . . ? F13 P1 F15 176.7(6) . . ? F16 P1 F11 87.3(5) . . ? F14 P1 F11 90.6(5) . . ? F12 P1 F11 177.6(5) . . ? F13 P1 F11 91.7(5) . . ? F15 P1 F11 86.5(5) . . ? F23 P2 F25 91.3(4) . . ? F23 P2 F24 179.7(5) . . ? F25 P2 F24 89.0(4) . . ? F23 P2 F22 89.4(3) . . ? F25 P2 F22 90.9(3) . . ? F24 P2 F22 90.5(3) . . ? F23 P2 F26 89.9(4) . . ? F25 P2 F26 178.7(4) . . ? F24 P2 F26 89.8(4) . . ? F22 P2 F26 89.6(3) . . ? F23 P2 F21 91.4(3) . . ? F25 P2 F21 89.6(3) . . ? F24 P2 F21 88.7(3) . . ? F22 P2 F21 179.0(3) . . ? F26 P2 F21 89.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Ru1 N1 C1 74.8(8) . . . . ? N8 Ru1 N1 C1 -4.1(8) . . . . ? N9 Ru1 N1 C1 -100.5(8) . . . . ? N10 Ru1 N1 C1 -108(4) . . . . ? N2 Ru1 N1 C1 174.1(8) . . . . ? N7 Ru1 N1 C5 -106.0(6) . . . . ? N8 Ru1 N1 C5 175.1(6) . . . . ? N9 Ru1 N1 C5 78.7(6) . . . . ? N10 Ru1 N1 C5 72(4) . . . . ? N2 Ru1 N1 C5 -6.7(6) . . . . ? N7 Ru1 N2 C10 -90.9(8) . . . . ? N8 Ru1 N2 C10 -160(3) . . . . ? N9 Ru1 N2 C10 83.8(8) . . . . ? N10 Ru1 N2 C10 6.1(8) . . . . ? N1 Ru1 N2 C10 -178.3(8) . . . . ? N7 Ru1 N2 C6 95.3(6) . . . . ? N8 Ru1 N2 C6 26(3) . . . . ? N9 Ru1 N2 C6 -90.0(6) . . . . ? N10 Ru1 N2 C6 -167.7(5) . . . . ? N1 Ru1 N2 C6 7.9(5) . . . . ? N8 Ru1 N7 C21 -178.8(7) . . . . ? N9 Ru1 N7 C21 -131(2) . . . . ? N10 Ru1 N7 C21 -94.3(7) . . . . ? N1 Ru1 N7 C21 85.5(7) . . . . ? N2 Ru1 N7 C21 6.7(7) . . . . ? N8 Ru1 N7 C25 0.3(5) . . . . ? N9 Ru1 N7 C25 48(2) . . . . ? N10 Ru1 N7 C25 84.7(6) . . . . ? N1 Ru1 N7 C25 -95.4(6) . . . . ? N2 Ru1 N7 C25 -174.2(5) . . . . ? N7 Ru1 N8 C30 -180.0(7) . . . . ? N9 Ru1 N8 C30 5.9(7) . . . . ? N10 Ru1 N8 C30 83.8(7) . . . . ? N1 Ru1 N8 C30 -91.9(7) . . . . ? N2 Ru1 N8 C30 -110(3) . . . . ? N7 Ru1 N8 C26 -0.5(6) . . . . ? N9 Ru1 N8 C26 -174.6(6) . . . . ? N10 Ru1 N8 C26 -96.7(6) . . . . ? N1 Ru1 N8 C26 87.6(6) . . . . ? N2 Ru1 N8 C26 70(3) . . . . ? N7 Ru1 N9 C35 34(2) . . . . ? N8 Ru1 N9 C35 80.6(6) . . . . ? N10 Ru1 N9 C35 -3.7(6) . . . . ? N1 Ru1 N9 C35 176.8(6) . . . . ? N2 Ru1 N9 C35 -104.7(6) . . . . ? N7 Ru1 N9 C31 -147.3(19) . . . . ? N8 Ru1 N9 C31 -100.6(7) . . . . ? N10 Ru1 N9 C31 175.0(7) . . . . ? N1 Ru1 N9 C31 -4.4(7) . . . . ? N2 Ru1 N9 C31 74.1(7) . . . . ? N7 Ru1 N10 C40 2.3(7) . . . . ? N8 Ru1 N10 C40 80.8(7) . . . . ? N9 Ru1 N10 C40 177.5(7) . . . . ? N1 Ru1 N10 C40 -175(4) . . . . ? N2 Ru1 N10 C40 -97.8(7) . . . . ? N7 Ru1 N10 C36 -166.3(6) . . . . ? N8 Ru1 N10 C36 -87.7(6) . . . . ? N9 Ru1 N10 C36 8.9(6) . . . . ? N1 Ru1 N10 C36 16(4) . . . . ? N2 Ru1 N10 C36 93.7(6) . . . . ? C5 N1 C1 C2 0.2(13) . . . . ? Ru1 N1 C1 C2 179.4(7) . . . . ? N1 C1 C2 C3 -2.0(15) . . . . ? C1 C2 C3 C4 0.9(14) . . . . ? C2 C3 C4 C5 1.7(14) . . . . ? C2 C3 C4 C11 -178.6(9) . . . . ? C1 N1 C5 C4 2.6(13) . . . . ? Ru1 N1 C5 C4 -176.7(7) . . . . ? C1 N1 C5 C6 -176.3(8) . . . . ? Ru1 N1 C5 C6 4.4(9) . . . . ? C3 C4 C5 N1 -3.5(14) . . . . ? C11 C4 C5 N1 176.7(8) . . . . ? C3 C4 C5 C6 175.2(8) . . . . ? C11 C4 C5 C6 -4.6(13) . . . . ? C10 N2 C6 C7 -2.8(12) . . . . ? Ru1 N2 C6 C7 171.7(7) . . . . ? C10 N2 C6 C5 177.2(8) . . . . ? Ru1 N2 C6 C5 -8.2(9) . . . . ? N1 C5 C6 N2 2.7(11) . . . . ? C4 C5 C6 N2 -176.1(8) . . . . ? N1 C5 C6 C7 -177.2(8) . . . . ? C4 C5 C6 C7 3.9(13) . . . . ? N2 C6 C7 C8 1.4(13) . . . . ? C5 C6 C7 C8 -178.6(8) . . . . ? N2 C6 C7 C12 -178.9(8) . . . . ? C5 C6 C7 C12 1.1(13) . . . . ? C6 C7 C8 C9 1.5(13) . . . . ? C12 C7 C8 C9 -178.1(9) . . . . ? C7 C8 C9 C10 -3.1(14) . . . . ? C6 N2 C10 C9 1.2(13) . . . . ? Ru1 N2 C10 C9 -172.2(7) . . . . ? C8 C9 C10 N2 1.8(14) . . . . ? C13 N3 C11 C12 -2.2(13) . . . . ? C13 N3 C11 C4 178.1(8) . . . . ? C5 C4 C11 N3 179.9(8) . . . . ? C3 C4 C11 N3 0.1(13) . . . . ? C5 C4 C11 C12 0.2(13) . . . . ? C3 C4 C11 C12 -179.6(9) . . . . ? C14 N4 C12 C11 -2.6(13) . . . . ? C14 N4 C12 C7 176.1(8) . . . . ? N3 C11 C12 N4 3.6(14) . . . . ? C4 C11 C12 N4 -176.8(8) . . . . ? N3 C11 C12 C7 -175.1(8) . . . . ? C4 C11 C12 C7 4.6(13) . . . . ? C6 C7 C12 N4 176.1(8) . . . . ? C8 C7 C12 N4 -4.3(14) . . . . ? C6 C7 C12 C11 -5.2(13) . . . . ? C8 C7 C12 C11 174.4(9) . . . . ? C11 N3 C13 C18 -178.0(8) . . . . ? C11 N3 C13 C14 0.3(13) . . . . ? C12 N4 C14 C15 -178.4(8) . . . . ? C12 N4 C14 C13 0.7(13) . . . . ? N3 C13 C14 N4 0.5(14) . . . . ? C18 C13 C14 N4 178.8(9) . . . . ? N3 C13 C14 C15 179.5(9) . . . . ? C18 C13 C14 C15 -2.2(14) . . . . ? N4 C14 C15 C16 -178.4(9) . . . . ? C13 C14 C15 C16 2.5(14) . . . . ? C14 C15 C16 C20 -176.7(9) . . . . ? C14 C15 C16 C17 -1.8(15) . . . . ? C15 C16 C17 C18 0.7(15) . . . . ? C20 C16 C17 C18 175.6(9) . . . . ? C15 C16 C17 C19 178.4(9) . . . . ? C20 C16 C17 C19 -6.7(14) . . . . ? C19 C17 C18 C13 -178.0(9) . . . . ? C16 C17 C18 C13 -0.3(14) . . . . ? N3 C13 C18 C17 179.4(9) . . . . ? C14 C13 C18 C17 1.0(14) . . . . ? C18 C17 C19 N5 -5(31) . . . . ? C16 C17 C19 N5 177(100) . . . . ? C15 C16 C20 N6 137(53) . . . . ? C17 C16 C20 N6 -38(53) . . . . ? C25 N7 C21 C22 0.4(12) . . . . ? Ru1 N7 C21 C22 179.5(7) . . . . ? N7 C21 C22 C23 -0.5(14) . . . . ? C21 C22 C23 C24 0.7(14) . . . . ? C22 C23 C24 C25 -1.0(14) . . . . ? C23 C24 C25 N7 1.0(13) . . . . ? C23 C24 C25 C26 -178.8(8) . . . . ? C21 N7 C25 C24 -0.7(12) . . . . ? Ru1 N7 C25 C24 -179.8(7) . . . . ? C21 N7 C25 C26 179.2(7) . . . . ? Ru1 N7 C25 C26 0.0(9) . . . . ? C30 N8 C26 C27 3.1(11) . . . . ? Ru1 N8 C26 C27 -176.4(6) . . . . ? C30 N8 C26 C25 -179.8(7) . . . . ? Ru1 N8 C26 C25 0.6(9) . . . . ? C24 C25 C26 N8 179.4(8) . . . . ? N7 C25 C26 N8 -0.4(10) . . . . ? C24 C25 C26 C27 -3.6(13) . . . . ? N7 C25 C26 C27 176.5(8) . . . . ? N8 C26 C27 C28 -2.6(13) . . . . ? C25 C26 C27 C28 -179.5(8) . . . . ? C26 C27 C28 C29 -0.6(14) . . . . ? C27 C28 C29 C30 3.1(14) . . . . ? C26 N8 C30 C29 -0.4(12) . . . . ? Ru1 N8 C30 C29 179.1(6) . . . . ? C28 C29 C30 N8 -2.7(13) . . . . ? C35 N9 C31 C32 -1.0(13) . . . . ? Ru1 N9 C31 C32 -179.7(7) . . . . ? N9 C31 C32 C33 0.6(15) . . . . ? C31 C32 C33 C34 -0.9(14) . . . . ? C32 C33 C34 C35 1.8(14) . . . . ? C31 N9 C35 C34 1.8(12) . . . . ? Ru1 N9 C35 C34 -179.3(7) . . . . ? C31 N9 C35 C36 179.6(7) . . . . ? Ru1 N9 C35 C36 -1.5(9) . . . . ? C33 C34 C35 N9 -2.3(14) . . . . ? C33 C34 C35 C36 -179.8(9) . . . . ? C40 N10 C36 C37 -0.8(12) . . . . ? Ru1 N10 C36 C37 168.9(7) . . . . ? C40 N10 C36 C35 177.8(8) . . . . ? Ru1 N10 C36 C35 -12.5(9) . . . . ? N9 C35 C36 N10 9.2(11) . . . . ? C34 C35 C36 N10 -173.1(8) . . . . ? N9 C35 C36 C37 -172.2(8) . . . . ? C34 C35 C36 C37 5.6(14) . . . . ? N10 C36 C37 C38 0.5(13) . . . . ? C35 C36 C37 C38 -178.0(8) . . . . ? C36 C37 C38 C39 0.6(14) . . . . ? C37 C38 C39 C40 -1.4(14) . . . . ? C36 N10 C40 C39 0.0(13) . . . . ? Ru1 N10 C40 C39 -168.4(7) . . . . ? C38 C39 C40 N10 1.1(14) . . . . ? 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C3 H3A F16 0.9502 2.4921 3.424(11) 166.92 . ? C10 H10A F21 0.9499 2.5383 3.403(9) 151.38 2_655 ? C15 H15A F11 0.9501 2.4526 3.131(14) 128.26 3_655 ? C18 H18A F13 0.9481 2.4224 3.360(12) 169.97 . ? C21 H21A N5 0.9498 2.4121 3.252(14) 147.26 3_655 ? C27 H27A F12 0.9499 2.5442 3.441(12) 157.47 3_556 ? C28 H28A F25 0.9501 2.4780 3.134(11) 126.17 3_556 ? C31 H31A F13 0.9497 2.5034 3.317(11) 143.69 3_555 ? C32 H32A F14 0.9502 2.4392 3.311(13) 152.41 3_555 ? C33 H33A F22 0.9511 2.4664 3.125(10) 126.34 3_555 ? C33 H33A F26 0.9511 2.4511 3.370(12) 162.41 3_555 ? C39 H39A F21 0.9507 2.4978 3.170(11) 127.69 3_656 ? C39 H39A F24 0.9507 2.5103 3.320(12) 143.15 3_656 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.385 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.069 #========================================================END