# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Enzo Alessio' 'Ioannis Bratsos' 'Teresa Gianferrara' 'Elisabetta Iengo' 'Barbara Milani' 'Adrian Ostric' 'Cinzia Spagnul' 'Ennio Zangrando' _publ_contact_author_name 'Enzo Alessio' _publ_contact_author_email ALESSI@UNITS.IT _publ_section_title ; Synthetic strategies towards ruthenium-porphyrin conjugates for anticancer activity ; # Attachment 'Alessio_CIF_files_txt.txt' data_4 _database_code_depnum_ccdc_archive 'CCDC 735952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H106 N16 Ru4 S12 8+, 8(C F3 O3 S 1-), 4(C H3 N O2)' _chemical_formula_sum 'C116 H118 F24 N20 O32 Ru4 S20' _chemical_formula_weight 3805.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0074 0.0035 '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 0.0136 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0227 0.0128 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0347 0.0215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.2073 0.2439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -0.5010 1.5477 '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 23.157(5) _cell_length_b 16.581(4) _cell_length_c 20.833(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.01(3) _cell_angle_gamma 90.00 _cell_volume 7939(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3844 _exptl_absorpt_coefficient_mu 1.782 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.5723 _exptl_absorpt_correction_T_max 0.7803 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.00000 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Elettra Synchrotron, Trieste (Italy)' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'CCD MarResearch' _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 49860 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.52 _reflns_number_total 4833 _reflns_number_gt 3965 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.01 (Farrugia, 1999)' _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^ > 2\s(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^)+(0.1779P)^2^+28.8284P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4833 _refine_ls_number_parameters 733 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_gt 0.0884 _refine_ls_wR_factor_ref 0.2662 _refine_ls_wR_factor_gt 0.2515 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.141 _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 Ru1 Ru 0.12473(5) 0.19880(8) 0.39214(6) 0.0822(7) Uani 1 1 d . . . Ru2 Ru 0.67795(5) 0.19261(8) 0.15279(6) 0.0850(7) Uani 1 1 d . . . S1 S 0.15476(18) 0.0694(3) 0.4324(2) 0.0943(14) Uani 1 1 d . . . S2 S 0.13557(18) 0.1502(3) 0.2869(2) 0.0968(15) Uani 1 1 d . . . S3 S 0.02742(17) 0.1505(3) 0.3784(2) 0.0943(14) Uani 1 1 d . . . S4 S 0.74223(18) 0.2966(3) 0.1271(2) 0.0913(14) Uani 1 1 d . . . S5 S 0.75813(18) 0.1341(3) 0.2170(2) 0.0968(15) Uani 1 1 d . . . S6 S 0.70367(19) 0.1203(3) 0.0626(2) 0.1024(15) Uani 1 1 d . . . C31 C 0.1693(7) 0.0086(10) 0.3586(9) 0.097(5) Uani 1 1 d . . . H31A H 0.2017 -0.0293 0.3713 0.116 Uiso 1 1 calc R . . H31B H 0.1343 -0.0237 0.3435 0.116 Uiso 1 1 calc R . . C32 C 0.1847(7) 0.0610(11) 0.3030(9) 0.105(6) Uani 1 1 d . . . H32A H 0.1827 0.0277 0.2633 0.126 Uiso 1 1 calc R . . H32B H 0.2253 0.0802 0.3131 0.126 Uiso 1 1 calc R . . C33 C 0.0636(7) 0.1003(12) 0.2561(8) 0.109(6) Uani 1 1 d . . . H33A H 0.0563 0.1058 0.2085 0.131 Uiso 1 1 calc R . . H33B H 0.0656 0.0420 0.2666 0.131 Uiso 1 1 calc R . . C34 C 0.0120(7) 0.1403(11) 0.2879(8) 0.098(5) Uani 1 1 d . . . H34A H -0.0235 0.1073 0.2772 0.118 Uiso 1 1 calc R . . H34B H 0.0041 0.1945 0.2688 0.118 Uiso 1 1 calc R . . C35 C 0.0317(8) 0.0415(11) 0.4018(9) 0.114(6) Uani 1 1 d . . . H35A H -0.0039 0.0267 0.4211 0.136 Uiso 1 1 calc R . . H35B H 0.0327 0.0084 0.3624 0.136 Uiso 1 1 calc R . . C36 C 0.0857(7) 0.0214(10) 0.4505(9) 0.104(5) Uani 1 1 d . . . H36A H 0.0912 -0.0378 0.4516 0.124 Uiso 1 1 calc R . . H36B H 0.0780 0.0386 0.4942 0.124 Uiso 1 1 calc R . . C37 C 0.7773(8) 0.2596(12) 0.0569(9) 0.118(6) Uani 1 1 d . . . H37A H 0.7866 0.3061 0.0301 0.142 Uiso 1 1 calc R . . H37B H 0.8141 0.2319 0.0727 0.142 Uiso 1 1 calc R . . C38 C 0.7351(9) 0.1981(10) 0.0131(9) 0.112(6) Uani 1 1 d . . . H38A H 0.7575 0.1713 -0.0184 0.135 Uiso 1 1 calc R . . H38B H 0.7031 0.2290 -0.0115 0.135 Uiso 1 1 calc R . . C39 C 0.7706(9) 0.0620(11) 0.0932(8) 0.111(6) Uani 1 1 d . . . H39A H 0.7701 0.0101 0.0696 0.133 Uiso 1 1 calc R . . H39B H 0.8052 0.0926 0.0832 0.133 Uiso 1 1 calc R . . C40 C 0.7770(9) 0.0442(12) 0.1678(10) 0.135(7) Uani 1 1 d . . . H40A H 0.8176 0.0278 0.1824 0.162 Uiso 1 1 calc R . . H40B H 0.7513 -0.0014 0.1759 0.162 Uiso 1 1 calc R . . C41 C 0.8212(8) 0.2021(11) 0.2134(10) 0.115(7) Uani 1 1 d . . . H41A H 0.8457 0.2011 0.2558 0.138 Uiso 1 1 calc R . . H41B H 0.8449 0.1813 0.1805 0.138 Uiso 1 1 calc R . . C42 C 0.8036(7) 0.2918(11) 0.1962(8) 0.102(6) Uani 1 1 d . . . H42A H 0.8379 0.3212 0.1839 0.123 Uiso 1 1 calc R . . H42B H 0.7913 0.3185 0.2348 0.123 Uiso 1 1 calc R . . N1 N 0.0981(5) 0.3205(7) 0.3629(6) 0.083(4) Uani 1 1 d . . . N2 N 0.1180(5) 0.2591(8) 0.4831(6) 0.084(4) Uani 1 1 d . . . C1 C 0.0816(7) 0.3484(10) 0.2991(9) 0.097(5) Uiso 1 1 d . . . H1 H 0.0811 0.3116 0.2641 0.116 Uiso 1 1 calc R . . C2 C 0.0659(7) 0.4301(10) 0.2862(9) 0.104(5) Uiso 1 1 d . . . H2 H 0.0548 0.4477 0.2431 0.124 Uiso 1 1 calc R . . C3 C 0.0668(8) 0.4836(11) 0.3369(9) 0.112(6) Uiso 1 1 d . . . H3 H 0.0567 0.5385 0.3285 0.134 Uiso 1 1 calc R . . C4 C 0.0828(7) 0.4575(10) 0.4024(9) 0.102(5) Uiso 1 1 d . . . H4 H 0.0824 0.4942 0.4374 0.122 Uiso 1 1 calc R . . C5 C 0.0987(7) 0.3791(10) 0.4135(9) 0.093(5) Uiso 1 1 d . . . C6 C 0.1134(7) 0.3441(11) 0.4797(8) 0.092(5) Uiso 1 1 d . . . C7 C 0.1241(8) 0.3916(12) 0.5371(9) 0.115(6) Uiso 1 1 d . . . H7 H 0.1225 0.4488 0.5353 0.138 Uiso 1 1 calc R . . C8 C 0.1375(8) 0.3494(12) 0.5985(10) 0.122(6) Uiso 1 1 d . . . H8 H 0.1460 0.3803 0.6369 0.146 Uiso 1 1 calc R . . C9 C 0.1383(7) 0.2696(11) 0.6027(9) 0.103(5) Uiso 1 1 d . . . H9 H 0.1443 0.2440 0.6438 0.123 Uiso 1 1 calc R . . C10 C 0.1302(7) 0.2227(10) 0.5454(8) 0.092(5) Uiso 1 1 d . . . H10 H 0.1330 0.1657 0.5486 0.110 Uiso 1 1 calc R . . N3 N 0.6008(5) 0.2395(8) 0.0974(6) 0.088(4) Uani 1 1 d . . . N4 N 0.6132(5) 0.1056(8) 0.1737(6) 0.093(4) Uani 1 1 d . . . C11 C 0.5965(7) 0.3045(9) 0.0571(8) 0.087(5) Uiso 1 1 d . . . H11 H 0.6312 0.3336 0.0531 0.105 Uiso 1 1 calc R . . C12 C 0.5446(7) 0.3324(10) 0.0207(8) 0.099(5) Uiso 1 1 d . . . H12 H 0.5440 0.3769 -0.0081 0.119 Uiso 1 1 calc R . . C13 C 0.4937(8) 0.2890(10) 0.0303(9) 0.108(6) Uiso 1 1 d . . . H13 H 0.4574 0.3055 0.0078 0.130 Uiso 1 1 calc R . . C14 C 0.4950(8) 0.2238(11) 0.0711(9) 0.106(5) Uiso 1 1 d . . . H14 H 0.4602 0.1954 0.0763 0.128 Uiso 1 1 calc R . . C15 C 0.5507(8) 0.1983(9) 0.1067(8) 0.088(5) Uiso 1 1 d . . . C16 C 0.5546(8) 0.1296(10) 0.1502(8) 0.097(5) Uiso 1 1 d . . . C17 C 0.5073(8) 0.0858(10) 0.1718(9) 0.110(6) Uiso 1 1 d . . . H17 H 0.4685 0.1022 0.1580 0.132 Uiso 1 1 calc R . . C18 C 0.5172(8) 0.0195(10) 0.2127(8) 0.108(6) Uiso 1 1 d . . . H18 H 0.4854 -0.0086 0.2268 0.130 Uiso 1 1 calc R . . C19 C 0.5754(8) -0.0059(10) 0.2333(8) 0.105(5) Uiso 1 1 d . . . H19 H 0.5829 -0.0525 0.2595 0.126 Uiso 1 1 calc R . . C20 C 0.6214(8) 0.0399(11) 0.2136(8) 0.095(5) Uiso 1 1 d . . . H20 H 0.6602 0.0244 0.2289 0.114 Uiso 1 1 calc R . . N7 N 0.4168(5) 0.4937(7) 0.5317(5) 0.076(3) Uani 1 1 d . . . N8 N 0.4805(5) 0.4016(7) 0.4344(6) 0.080(4) Uani 1 1 d . . . H8A H 0.4894 0.4416 0.4616 0.096 Uiso 1 1 calc R . . C21 C 0.3930(6) 0.5398(8) 0.5789(7) 0.072(4) Uiso 1 1 d . . . C22 C 0.3344(6) 0.5156(9) 0.5836(7) 0.082(4) Uiso 1 1 d . . . H22 H 0.3090 0.5397 0.6107 0.098 Uiso 1 1 calc R . . C23 C 0.3210(7) 0.4520(9) 0.5428(7) 0.085(4) Uiso 1 1 d . . . H23 H 0.2856 0.4224 0.5370 0.102 Uiso 1 1 calc R . . C24 C 0.3733(6) 0.4387(8) 0.5092(7) 0.073(4) Uiso 1 1 d . . . C25 C 0.3775(6) 0.3781(8) 0.4582(7) 0.073(4) Uiso 1 1 d . . . C26 C 0.4250(7) 0.3609(8) 0.4249(7) 0.075(4) Uiso 1 1 d . . . C27 C 0.4310(7) 0.3003(8) 0.3742(7) 0.076(4) Uiso 1 1 d . . . H27 H 0.4009 0.2651 0.3563 0.091 Uiso 1 1 calc R . . C28 C 0.4854(6) 0.3019(8) 0.3567(7) 0.075(4) Uiso 1 1 d . . . H28 H 0.5004 0.2675 0.3263 0.090 Uiso 1 1 calc R . . C29 C 0.5174(7) 0.3689(9) 0.3949(8) 0.079(4) Uiso 1 1 d . . . C30 C 0.5773(6) 0.3942(8) 0.3878(7) 0.075(4) Uiso 1 1 d . . . N5 N 0.2146(5) 0.2433(7) 0.4053(6) 0.082(4) Uani 1 1 d . . . C43 C 0.2367(7) 0.2939(9) 0.3607(8) 0.079(4) Uiso 1 1 d . . . H43 H 0.2154 0.3007 0.3191 0.095 Uiso 1 1 calc R . . C44 C 0.2894(6) 0.3349(8) 0.3754(7) 0.078(4) Uiso 1 1 d . . . H44 H 0.3037 0.3685 0.3440 0.094 Uiso 1 1 calc R . . C45 C 0.3216(6) 0.3258(8) 0.4382(7) 0.073(4) Uiso 1 1 d . . . C46 C 0.3022(6) 0.2706(8) 0.4818(7) 0.078(4) Uiso 1 1 d . . . H46 H 0.3247 0.2603 0.5222 0.094 Uiso 1 1 calc R . . C47 C 0.2484(6) 0.2304(9) 0.4645(7) 0.076(4) Uiso 1 1 d . . . H47 H 0.2349 0.1935 0.4943 0.091 Uiso 1 1 calc R . . N6 N 0.6547(5) 0.2621(8) 0.2366(6) 0.080(4) Uani 1 1 d . . . C48 C 0.6445(6) 0.3420(10) 0.2322(7) 0.075(4) Uiso 1 1 d . . . H48 H 0.6525 0.3695 0.1942 0.090 Uiso 1 1 calc R . . C49 C 0.6228(6) 0.3860(9) 0.2811(7) 0.078(4) Uiso 1 1 d . . . H49 H 0.6169 0.4424 0.2758 0.093 Uiso 1 1 calc R . . C50 C 0.6091(6) 0.3472(9) 0.3399(7) 0.079(4) Uiso 1 1 d . . . C51 C 0.6224(6) 0.2634(9) 0.3451(8) 0.083(4) Uiso 1 1 d . . . H51 H 0.6158 0.2345 0.3829 0.100 Uiso 1 1 calc R . . C52 C 0.6455(6) 0.2232(9) 0.2938(8) 0.079(4) Uiso 1 1 d . . . H52 H 0.6549 0.1676 0.2986 0.095 Uiso 1 1 calc R . . S7 S 0.3638(2) 0.0608(4) 0.3539(3) 0.132(2) Uani 1 1 d D . . O1 O 0.3673(7) 0.0721(9) 0.2786(7) 0.160(6) Uani 1 1 d . . . O2 O 0.3498(6) 0.1347(9) 0.3859(9) 0.164(6) Uani 1 1 d . . . O3 O 0.3337(6) -0.0132(8) 0.3723(8) 0.151(5) Uani 1 1 d . . . C55 C 0.4401(7) 0.0406(16) 0.3779(11) 0.128(7) Uani 1 1 d D . . F1 F 0.4499(6) 0.0331(8) 0.4462(6) 0.166(5) Uani 1 1 d . . . F2 F 0.4599(4) -0.0301(7) 0.3539(5) 0.125(3) Uani 1 1 d . . . F3 F 0.4759(5) 0.1026(8) 0.3657(6) 0.140(4) Uani 1 1 d . . . S8 S 0.2269(4) 0.4223(7) 0.1727(4) 0.208(4) Uani 1 1 d D . . O4 O 0.2071(10) 0.3799(12) 0.2254(8) 0.207(8) Uani 1 1 d . . . O5 O 0.2329(7) 0.3752(9) 0.1118(7) 0.154(5) Uani 1 1 d . . . O6 O 0.2763(9) 0.4793(16) 0.1865(11) 0.265(12) Uani 1 1 d . . . C56 C 0.1646(11) 0.4926(16) 0.1407(16) 0.172(9) Uani 1 1 d D . . F4 F 0.1379(6) 0.5511(8) 0.1830(8) 0.178(5) Uani 1 1 d . . . F5 F 0.1104(5) 0.4590(11) 0.1189(7) 0.201(7) Uani 1 1 d . . . F6 F 0.1727(8) 0.5534(14) 0.0942(8) 0.250(9) Uani 1 1 d . . . S9 S 0.1671(2) 0.8974(4) 0.1221(3) 0.1156(17) Uani 1 1 d D . . O7 O 0.2013(9) 0.8256(13) 0.1452(9) 0.212(8) Uani 1 1 d U . . O8 O 0.1613(5) 0.9119(8) 0.0526(6) 0.120(4) Uani 1 1 d . . . O9 O 0.1873(10) 0.9582(14) 0.1584(9) 0.220(8) Uani 1 1 d U . . C57 C 0.0951(9) 0.8791(18) 0.1403(14) 0.155(8) Uani 1 1 d D . . F7 F 0.0625(7) 0.9536(12) 0.1228(8) 0.218(7) Uani 1 1 d . . . F8 F 0.0585(7) 0.8327(11) 0.1099(8) 0.208(7) Uani 1 1 d U . . F9 F 0.0918(5) 0.8717(11) 0.2046(7) 0.188(5) Uani 1 1 d U . . S10 S 0.0354(3) 0.7793(5) 0.3698(3) 0.149(3) Uani 1 1 d D . . O10 O 0.0713(7) 0.6904(8) 0.3678(9) 0.168(6) Uani 1 1 d U . . O11 O -0.0227(5) 0.7733(8) 0.3365(5) 0.118(4) Uani 1 1 d . . . O12 O 0.0712(5) 0.8501(8) 0.3577(6) 0.122(4) Uani 1 1 d . . . C58 C 0.0333(13) 0.7800(18) 0.4548(9) 0.152(8) Uani 1 1 d D . . F10 F -0.0016(5) 0.8513(8) 0.4656(6) 0.151(4) Uani 1 1 d . . . F11 F 0.0871(4) 0.7880(8) 0.4895(6) 0.154(5) Uani 1 1 d . . . F12 F 0.0053(4) 0.7112(7) 0.4766(5) 0.135(4) Uani 1 1 d . . . O13 O 0.2978(11) 0.5993(14) 0.0330(11) 0.235(9) Uiso 1 1 d D . . O14 O 0.3809(10) 0.5681(13) 0.0955(11) 0.222(8) Uiso 1 1 d D . . N10 N 0.3357(10) 0.5500(14) 0.0560(11) 0.175(8) Uiso 1 1 d D . . C53 C 0.3310(12) 0.4626(16) 0.0385(13) 0.184(10) Uiso 1 1 d . . . H53A H 0.2953 0.4535 0.0090 0.277 Uiso 1 1 calc R . . H53B H 0.3298 0.4304 0.0778 0.277 Uiso 1 1 calc R . . H53C H 0.3647 0.4466 0.0173 0.277 Uiso 1 1 calc R . . O15 O 0.3533(9) 0.3016(12) 0.2321(11) 0.197(7) Uiso 1 1 d D . . O16 O 0.3725(10) 0.2236(14) 0.1431(12) 0.221(8) Uiso 1 1 d D . . N11 N 0.3434(14) 0.2481(17) 0.1872(13) 0.233(11) Uiso 1 1 d D . . C54 C 0.2883(11) 0.1997(14) 0.1916(12) 0.162(9) Uiso 1 1 d . . . H54A H 0.2688 0.2199 0.2276 0.243 Uiso 1 1 calc R . . H54B H 0.2983 0.1427 0.1990 0.243 Uiso 1 1 calc R . . H54C H 0.2621 0.2052 0.1511 0.243 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 Ru1 0.0652(10) 0.1014(12) 0.0759(12) -0.0023(7) -0.0086(8) -0.0071(6) Ru2 0.0696(11) 0.1070(12) 0.0756(12) -0.0115(7) -0.0027(8) -0.0045(7) S1 0.078(3) 0.099(3) 0.101(3) 0.003(2) -0.007(3) -0.008(2) S2 0.082(3) 0.119(4) 0.084(3) -0.015(3) -0.013(3) -0.007(3) S3 0.070(3) 0.114(3) 0.094(3) -0.001(3) -0.008(2) -0.013(2) S4 0.071(3) 0.114(3) 0.086(3) -0.004(2) -0.003(3) -0.004(2) S5 0.080(3) 0.108(3) 0.098(3) -0.008(3) -0.007(3) 0.001(2) S6 0.085(3) 0.127(4) 0.092(3) -0.023(3) 0.000(3) 0.000(3) C31 0.075(11) 0.101(13) 0.115(15) 0.000(12) 0.011(11) -0.005(9) C32 0.085(12) 0.121(14) 0.106(15) -0.033(12) 0.000(11) -0.023(10) C33 0.075(12) 0.160(17) 0.088(13) -0.026(11) -0.010(11) -0.029(11) C34 0.076(12) 0.120(13) 0.093(13) -0.016(10) -0.019(10) -0.019(10) C35 0.093(13) 0.119(14) 0.126(15) 0.004(12) -0.001(12) -0.013(11) C36 0.104(13) 0.103(13) 0.101(13) 0.014(10) 0.000(12) -0.013(10) C37 0.108(14) 0.132(15) 0.119(16) 0.027(13) 0.025(13) 0.008(12) C38 0.122(15) 0.129(15) 0.080(13) -0.014(11) -0.014(12) 0.005(12) C39 0.142(16) 0.124(15) 0.077(13) -0.005(11) 0.049(13) -0.006(12) C40 0.111(15) 0.132(16) 0.15(2) -0.024(14) -0.013(14) 0.010(12) C41 0.085(12) 0.126(16) 0.124(16) 0.035(12) -0.023(11) -0.023(11) C42 0.087(12) 0.128(16) 0.083(13) 0.012(10) -0.028(10) -0.037(10) N1 0.050(7) 0.105(9) 0.093(10) 0.001(8) 0.002(7) -0.006(6) N2 0.054(7) 0.132(12) 0.066(9) 0.009(8) 0.009(6) -0.020(7) N3 0.070(8) 0.114(10) 0.078(9) -0.011(8) 0.001(7) -0.001(7) N4 0.074(9) 0.116(11) 0.088(9) -0.019(8) 0.001(7) -0.020(7) N7 0.066(7) 0.094(8) 0.062(8) -0.001(7) -0.012(7) -0.017(7) N8 0.069(8) 0.097(9) 0.074(8) -0.003(7) 0.002(7) 0.002(7) N5 0.061(8) 0.097(9) 0.081(9) -0.012(7) -0.024(7) 0.003(7) N6 0.061(8) 0.109(11) 0.070(9) -0.015(7) 0.001(6) -0.007(7) S7 0.102(4) 0.118(5) 0.173(6) -0.018(4) 0.008(4) -0.002(3) O1 0.201(16) 0.169(13) 0.098(11) -0.016(9) -0.024(10) 0.027(11) O2 0.154(12) 0.119(11) 0.239(18) -0.050(11) 0.106(12) -0.017(9) O3 0.118(10) 0.120(11) 0.220(16) -0.012(10) 0.041(10) -0.033(8) C55 0.16(2) 0.125(19) 0.098(18) 0.019(14) 0.015(16) -0.037(18) F1 0.190(12) 0.175(11) 0.120(10) -0.004(8) -0.031(9) -0.022(9) F2 0.113(8) 0.115(8) 0.143(9) -0.005(7) 0.002(7) 0.007(6) F3 0.126(9) 0.146(10) 0.143(10) 0.000(7) 0.002(7) -0.023(8) S8 0.220(9) 0.269(10) 0.126(7) -0.017(7) -0.016(7) -0.051(8) O4 0.27(2) 0.27(2) 0.086(11) 0.071(12) 0.031(13) 0.032(17) O5 0.169(13) 0.181(13) 0.112(11) -0.033(10) 0.017(10) -0.012(10) O6 0.159(16) 0.37(3) 0.25(2) -0.15(2) -0.032(15) -0.066(19) C56 0.165(13) 0.175(12) 0.170(13) 0.005(10) -0.004(10) 0.004(10) F4 0.159(11) 0.162(11) 0.213(14) -0.011(10) 0.024(10) -0.021(9) F5 0.102(9) 0.32(2) 0.171(13) -0.035(12) -0.019(8) 0.006(10) F6 0.206(16) 0.35(2) 0.180(15) 0.090(16) -0.024(13) 0.047(16) S9 0.102(4) 0.147(5) 0.095(4) 0.008(4) 0.000(3) 0.007(3) O7 0.194(13) 0.277(16) 0.169(13) 0.067(12) 0.040(11) 0.102(13) O8 0.119(9) 0.154(11) 0.091(10) 0.013(7) 0.028(8) 0.027(8) O9 0.272(17) 0.216(15) 0.166(13) -0.025(12) 0.002(13) -0.077(14) C57 0.150(12) 0.170(12) 0.145(12) 0.013(10) 0.015(10) -0.007(10) F7 0.156(12) 0.29(2) 0.215(16) 0.049(14) 0.029(11) 0.036(13) F8 0.202(12) 0.244(13) 0.181(12) -0.072(10) 0.036(10) -0.106(11) F9 0.128(9) 0.306(15) 0.129(9) 0.036(10) 0.015(8) 0.013(9) S10 0.123(5) 0.200(6) 0.114(5) 0.033(4) -0.028(4) -0.057(5) O10 0.130(10) 0.128(10) 0.243(15) -0.040(10) 0.015(10) 0.033(8) O11 0.077(8) 0.189(12) 0.085(8) -0.005(8) -0.004(7) -0.018(7) O12 0.093(8) 0.138(10) 0.137(11) -0.017(8) 0.020(8) -0.025(8) C58 0.143(12) 0.168(12) 0.143(12) -0.001(9) 0.012(10) 0.000(10) F10 0.133(9) 0.154(10) 0.171(11) -0.036(8) 0.031(8) -0.018(8) F11 0.077(7) 0.249(14) 0.130(10) -0.016(8) -0.014(7) -0.016(7) F12 0.094(7) 0.175(10) 0.128(9) 0.038(7) -0.016(6) -0.002(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 2.165(12) . ? Ru1 N1 2.175(12) . ? Ru1 N5 2.194(11) . ? Ru1 S3 2.376(4) . ? Ru1 S1 2.376(4) . ? Ru1 S2 2.378(5) . ? Ru2 N3 2.152(12) . ? Ru2 N4 2.163(12) . ? Ru2 N6 2.212(12) . ? Ru2 S5 2.361(4) . ? Ru2 S6 2.365(5) . ? Ru2 S4 2.381(5) . ? S1 C36 1.865(17) . ? S1 C31 1.902(17) . ? S2 C32 1.871(18) . ? S2 C33 1.901(15) . ? S3 C35 1.871(18) . ? S3 C34 1.883(16) . ? S4 C37 1.861(19) . ? S4 C42 1.899(15) . ? S5 C41 1.854(17) . ? S5 C40 1.89(2) . ? S6 C38 1.85(2) . ? S6 C39 1.87(2) . ? C31 C32 1.53(2) . ? C33 C34 1.58(2) . ? C35 C36 1.55(2) . ? C37 C38 1.61(2) . ? C39 C40 1.57(2) . ? C41 C42 1.57(2) . ? N1 C1 1.41(2) . ? N1 C5 1.43(2) . ? N2 C6 1.41(2) . ? N2 C10 1.429(19) . ? C1 C2 1.42(2) . ? C2 C3 1.38(2) . ? C3 C4 1.44(2) . ? C4 C5 1.36(2) . ? C5 C6 1.50(2) . ? C6 C7 1.43(2) . ? C7 C8 1.46(2) . ? C8 C9 1.33(2) . ? C9 C10 1.42(2) . ? N3 C11 1.362(19) . ? N3 C15 1.38(2) . ? N4 C20 1.369(19) . ? N4 C16 1.44(2) . ? C11 C12 1.42(2) . ? C12 C13 1.42(2) . ? C13 C14 1.37(2) . ? C14 C15 1.47(2) . ? C15 C16 1.45(2) . ? C16 C17 1.43(2) . ? C17 C18 1.39(2) . ? C18 C19 1.43(2) . ? C19 C20 1.41(2) . ? N7 C24 1.397(17) . ? N7 C21 1.410(17) . ? N8 C29 1.369(18) . ? N8 C26 1.444(18) . ? C21 C30 1.426(18) 3_666 ? C21 C22 1.430(19) . ? C22 C23 1.367(19) . ? C23 C24 1.49(2) . ? C24 C25 1.475(19) . ? C25 C26 1.400(18) . ? C25 C45 1.571(19) . ? C26 C27 1.477(19) . ? C27 C28 1.353(19) . ? C28 C29 1.509(19) . ? C29 C30 1.47(2) . ? C30 C21 1.426(18) 3_666 ? C30 C50 1.52(2) . ? N5 C43 1.395(19) . ? N5 C47 1.395(18) . ? C43 C44 1.397(19) . ? C44 C45 1.433(19) . ? C45 C46 1.400(19) . ? C46 C47 1.422(19) . ? N6 C48 1.348(18) . ? N6 C52 1.394(18) . ? C48 C49 1.396(18) . ? C49 C50 1.453(19) . ? C50 C51 1.42(2) . ? C51 C52 1.418(19) . ? S7 O2 1.449(14) . ? S7 O3 1.485(14) . ? S7 O1 1.592(15) . ? S7 C55 1.809(17) . ? C55 F3 1.36(2) . ? C55 F2 1.37(2) . ? C55 F1 1.42(2) . ? S8 O4 1.426(17) . ? S8 O6 1.48(2) . ? S8 O5 1.509(15) . ? S8 C56 1.911(18) . ? C56 F5 1.40(3) . ? C56 F6 1.43(3) . ? C56 F4 1.49(3) . ? S9 O9 1.312(19) . ? S9 O8 1.458(12) . ? S9 O7 1.478(18) . ? S9 C57 1.779(17) . ? C57 F8 1.26(3) . ? C57 F9 1.36(3) . ? C57 F7 1.47(3) . ? S10 O11 1.441(12) . ? S10 O12 1.476(13) . ? S10 O10 1.694(14) . ? S10 C58 1.779(17) . ? C58 F11 1.37(3) . ? C58 F12 1.41(3) . ? C58 F10 1.46(3) . ? O13 N10 1.252(17) . ? O14 N10 1.285(17) . ? N10 C53 1.50(3) . ? O15 N11 1.290(17) . ? O16 N11 1.270(17) . ? N11 C54 1.52(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 N2 Ru1 N1 76.6(5) . . ? N2 Ru1 N5 84.5(4) . . ? N1 Ru1 N5 87.4(4) . . ? N2 Ru1 S3 95.3(3) . . ? N1 Ru1 S3 92.7(3) . . ? N5 Ru1 S3 179.8(4) . . ? N2 Ru1 S1 99.1(4) . . ? N1 Ru1 S1 175.6(4) . . ? N5 Ru1 S1 91.6(3) . . ? S3 Ru1 S1 88.32(15) . . ? N2 Ru1 S2 172.2(4) . . ? N1 Ru1 S2 96.6(4) . . ? N5 Ru1 S2 91.4(3) . . ? S3 Ru1 S2 88.83(16) . . ? S1 Ru1 S2 87.70(16) . . ? N3 Ru2 N4 78.4(5) . . ? N3 Ru2 N6 88.2(4) . . ? N4 Ru2 N6 87.0(5) . . ? N3 Ru2 S5 175.7(4) . . ? N4 Ru2 S5 97.4(4) . . ? N6 Ru2 S5 91.0(3) . . ? N3 Ru2 S6 91.7(3) . . ? N4 Ru2 S6 94.0(4) . . ? N6 Ru2 S6 179.0(4) . . ? S5 Ru2 S6 89.12(16) . . ? N3 Ru2 S4 96.8(4) . . ? N4 Ru2 S4 174.9(4) . . ? N6 Ru2 S4 91.1(3) . . ? S5 Ru2 S4 87.43(16) . . ? S6 Ru2 S4 87.91(17) . . ? C36 S1 C31 100.3(8) . . ? C36 S1 Ru1 103.6(6) . . ? C31 S1 Ru1 105.5(6) . . ? C32 S2 C33 101.9(8) . . ? C32 S2 Ru1 103.5(6) . . ? C33 S2 Ru1 105.8(6) . . ? C35 S3 C34 99.9(8) . . ? C35 S3 Ru1 106.0(6) . . ? C34 S3 Ru1 102.3(5) . . ? C37 S4 C42 103.0(9) . . ? C37 S4 Ru2 106.4(6) . . ? C42 S4 Ru2 103.3(5) . . ? C41 S5 C40 102.8(10) . . ? C41 S5 Ru2 107.2(6) . . ? C40 S5 Ru2 103.6(6) . . ? C38 S6 C39 100.6(8) . . ? C38 S6 Ru2 104.0(6) . . ? C39 S6 Ru2 105.7(5) . . ? C32 C31 S1 113.1(11) . . ? C31 C32 S2 113.1(12) . . ? C34 C33 S2 110.6(11) . . ? C33 C34 S3 113.3(11) . . ? C36 C35 S3 113.0(12) . . ? C35 C36 S1 114.8(12) . . ? C38 C37 S4 111.1(13) . . ? C37 C38 S6 112.1(12) . . ? C40 C39 S6 114.0(12) . . ? C39 C40 S5 112.9(14) . . ? C42 C41 S5 113.7(12) . . ? C41 C42 S4 111.2(11) . . ? C1 N1 C5 116.5(13) . . ? C1 N1 Ru1 127.0(11) . . ? C5 N1 Ru1 116.5(10) . . ? C6 N2 C10 118.1(12) . . ? C6 N2 Ru1 115.4(9) . . ? C10 N2 Ru1 124.9(11) . . ? N1 C1 C2 121.5(15) . . ? C3 C2 C1 119.4(17) . . ? C2 C3 C4 120.8(17) . . ? C5 C4 C3 118.8(17) . . ? C4 C5 N1 123.0(15) . . ? C4 C5 C6 123.5(16) . . ? N1 C5 C6 113.3(14) . . ? N2 C6 C7 120.2(15) . . ? N2 C6 C5 116.1(14) . . ? C7 C6 C5 123.7(16) . . ? C6 C7 C8 117.8(17) . . ? C9 C8 C7 122.5(19) . . ? C8 C9 C10 119.5(18) . . ? C9 C10 N2 121.7(15) . . ? C11 N3 C15 118.7(13) . . ? C11 N3 Ru2 127.5(10) . . ? C15 N3 Ru2 113.7(10) . . ? C20 N4 C16 118.8(13) . . ? C20 N4 Ru2 127.2(10) . . ? C16 N4 Ru2 113.2(11) . . ? N3 C11 C12 125.4(15) . . ? C13 C12 C11 115.1(16) . . ? C14 C13 C12 122.1(18) . . ? C13 C14 C15 119.4(17) . . ? N3 C15 C16 119.2(15) . . ? N3 C15 C14 119.2(14) . . ? C16 C15 C14 121.6(16) . . ? C17 C16 N4 118.5(15) . . ? C17 C16 C15 127.1(16) . . ? N4 C16 C15 114.4(15) . . ? C18 C17 C16 121.2(17) . . ? C17 C18 C19 119.8(18) . . ? C20 C19 C18 118.2(17) . . ? N4 C20 C19 123.5(16) . . ? C24 N7 C21 105.2(11) . . ? C29 N8 C26 110.0(12) . . ? N7 C21 C30 123.3(12) . 3_666 ? N7 C21 C22 110.5(12) . . ? C30 C21 C22 126.0(14) 3_666 . ? C23 C22 C21 108.6(15) . . ? C22 C23 C24 105.7(14) . . ? N7 C24 C25 125.3(13) . . ? N7 C24 C23 109.9(12) . . ? C25 C24 C23 124.7(13) . . ? C26 C25 C24 128.4(13) . . ? C26 C25 C45 115.4(12) . . ? C24 C25 C45 116.2(12) . . ? C25 C26 N8 125.3(13) . . ? C25 C26 C27 129.8(14) . . ? N8 C26 C27 104.9(13) . . ? C28 C27 C26 110.5(13) . . ? C27 C28 C29 106.7(13) . . ? N8 C29 C30 127.7(13) . . ? N8 C29 C28 107.8(12) . . ? C30 C29 C28 124.4(15) . . ? C21 C30 C29 125.0(13) 3_666 . ? C21 C30 C50 117.9(12) 3_666 . ? C29 C30 C50 117.1(13) . . ? C43 N5 C47 118.1(12) . . ? C43 N5 Ru1 122.6(9) . . ? C47 N5 Ru1 118.7(10) . . ? N5 C43 C44 121.8(14) . . ? C43 C44 C45 119.6(15) . . ? C46 C45 C44 119.2(13) . . ? C46 C45 C25 120.6(12) . . ? C44 C45 C25 120.3(13) . . ? C45 C46 C47 119.0(14) . . ? N5 C47 C46 122.1(14) . . ? C48 N6 C52 117.9(12) . . ? C48 N6 Ru2 121.0(9) . . ? C52 N6 Ru2 120.8(10) . . ? N6 C48 C49 122.7(13) . . ? C48 C49 C50 121.3(13) . . ? C51 C50 C49 115.4(13) . . ? C51 C50 C30 124.5(13) . . ? C49 C50 C30 119.8(12) . . ? C52 C51 C50 119.9(14) . . ? N6 C52 C51 122.6(14) . . ? O2 S7 O3 116.3(9) . . ? O2 S7 O1 113.2(10) . . ? O3 S7 O1 115.7(9) . . ? O2 S7 C55 107.2(11) . . ? O3 S7 C55 104.4(10) . . ? O1 S7 C55 97.4(10) . . ? F3 C55 F2 109.8(17) . . ? F3 C55 F1 103.0(17) . . ? F2 C55 F1 105.8(16) . . ? F3 C55 S7 113.9(14) . . ? F2 C55 S7 114.6(14) . . ? F1 C55 S7 108.9(14) . . ? O4 S8 O6 118.6(14) . . ? O4 S8 O5 117.6(13) . . ? O6 S8 O5 110.1(13) . . ? O4 S8 C56 105.5(14) . . ? O6 S8 C56 102.1(15) . . ? O5 S8 C56 99.6(12) . . ? F5 C56 F6 104.3(19) . . ? F5 C56 F4 91.8(18) . . ? F6 C56 F4 92.3(18) . . ? F5 C56 S8 118.7(19) . . ? F6 C56 S8 121(2) . . ? F4 C56 S8 122.7(19) . . ? O9 S9 O8 115.4(11) . . ? O9 S9 O7 107.0(14) . . ? O8 S9 O7 115.9(9) . . ? O9 S9 C57 106.6(15) . . ? O8 S9 C57 105.4(11) . . ? O7 S9 C57 105.8(13) . . ? F8 C57 F9 109.0(18) . . ? F8 C57 F7 95(2) . . ? F9 C57 F7 103(2) . . ? F8 C57 S9 126(2) . . ? F9 C57 S9 113.2(17) . . ? F7 C57 S9 105.7(16) . . ? O11 S10 O12 119.0(8) . . ? O11 S10 O10 111.1(9) . . ? O12 S10 O10 113.6(9) . . ? O11 S10 C58 110.0(11) . . ? O12 S10 C58 104.4(11) . . ? O10 S10 C58 95.9(12) . . ? F11 C58 F12 109.4(18) . . ? F11 C58 F10 108.9(19) . . ? F12 C58 F10 108.7(19) . . ? F11 C58 S10 113.1(17) . . ? F12 C58 S10 112.6(16) . . ? F10 C58 S10 103.9(15) . . ? O13 N10 O14 125(3) . . ? O13 N10 C53 121(2) . . ? O14 N10 C53 114(2) . . ? O16 N11 O15 133(3) . . ? O16 N11 C54 114(2) . . ? O15 N11 C54 113(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 N2 Ru1 S1 C36 79.6(7) . . . . ? N1 Ru1 S1 C36 87(4) . . . . ? N5 Ru1 S1 C36 164.3(7) . . . . ? S3 Ru1 S1 C36 -15.5(6) . . . . ? S2 Ru1 S1 C36 -104.4(6) . . . . ? N2 Ru1 S1 C31 -175.5(6) . . . . ? N1 Ru1 S1 C31 -168(4) . . . . ? N5 Ru1 S1 C31 -90.8(6) . . . . ? S3 Ru1 S1 C31 89.4(5) . . . . ? S2 Ru1 S1 C31 0.5(5) . . . . ? N2 Ru1 S2 C32 130(2) . . . . ? N1 Ru1 S2 C32 159.0(6) . . . . ? N5 Ru1 S2 C32 71.4(6) . . . . ? S3 Ru1 S2 C32 -108.4(6) . . . . ? S1 Ru1 S2 C32 -20.1(6) . . . . ? N2 Ru1 S2 C33 -124(2) . . . . ? N1 Ru1 S2 C33 -94.2(7) . . . . ? N5 Ru1 S2 C33 178.2(7) . . . . ? S3 Ru1 S2 C33 -1.7(7) . . . . ? S1 Ru1 S2 C33 86.7(7) . . . . ? N2 Ru1 S3 C35 -102.0(7) . . . . ? N1 Ru1 S3 C35 -178.8(7) . . . . ? N5 Ru1 S3 C35 -64(89) . . . . ? S1 Ru1 S3 C35 -3.1(7) . . . . ? S2 Ru1 S3 C35 84.6(7) . . . . ? N2 Ru1 S3 C34 153.8(7) . . . . ? N1 Ru1 S3 C34 77.0(7) . . . . ? N5 Ru1 S3 C34 -168(100) . . . . ? S1 Ru1 S3 C34 -107.3(6) . . . . ? S2 Ru1 S3 C34 -19.6(6) . . . . ? N3 Ru2 S4 C37 -94.6(7) . . . . ? N4 Ru2 S4 C37 -115(4) . . . . ? N6 Ru2 S4 C37 177.0(7) . . . . ? S5 Ru2 S4 C37 86.1(6) . . . . ? S6 Ru2 S4 C37 -3.1(6) . . . . ? N3 Ru2 S4 C42 157.3(7) . . . . ? N4 Ru2 S4 C42 137(4) . . . . ? N6 Ru2 S4 C42 69.0(7) . . . . ? S5 Ru2 S4 C42 -22.0(7) . . . . ? S6 Ru2 S4 C42 -111.2(7) . . . . ? N3 Ru2 S5 C41 -168(5) . . . . ? N4 Ru2 S5 C41 -175.8(8) . . . . ? N6 Ru2 S5 C41 -88.7(8) . . . . ? S6 Ru2 S5 C41 90.3(8) . . . . ? S4 Ru2 S5 C41 2.3(8) . . . . ? N3 Ru2 S5 C40 84(5) . . . . ? N4 Ru2 S5 C40 75.9(8) . . . . ? N6 Ru2 S5 C40 163.0(8) . . . . ? S6 Ru2 S5 C40 -18.0(8) . . . . ? S4 Ru2 S5 C40 -106.0(8) . . . . ? N3 Ru2 S6 C38 78.1(7) . . . . ? N4 Ru2 S6 C38 156.5(7) . . . . ? N6 Ru2 S6 C38 -10(19) . . . . ? S5 Ru2 S6 C38 -106.2(6) . . . . ? S4 Ru2 S6 C38 -18.7(6) . . . . ? N3 Ru2 S6 C39 -176.5(7) . . . . ? N4 Ru2 S6 C39 -98.0(7) . . . . ? N6 Ru2 S6 C39 95(19) . . . . ? S5 Ru2 S6 C39 -0.7(6) . . . . ? S4 Ru2 S6 C39 86.8(6) . . . . ? C36 S1 C31 C32 132.6(12) . . . . ? Ru1 S1 C31 C32 25.3(12) . . . . ? S1 C31 C32 S2 -45.6(14) . . . . ? C33 S2 C32 C31 -67.2(13) . . . . ? Ru1 S2 C32 C31 42.5(12) . . . . ? C32 S2 C33 C34 136.0(13) . . . . ? Ru1 S2 C33 C34 28.1(14) . . . . ? S2 C33 C34 S3 -48.6(16) . . . . ? C35 S3 C34 C33 -65.0(14) . . . . ? Ru1 S3 C34 C33 43.9(13) . . . . ? C34 S3 C35 C36 132.2(14) . . . . ? Ru1 S3 C35 C36 26.3(15) . . . . ? S3 C35 C36 S1 -43.1(18) . . . . ? C31 S1 C36 C35 -71.6(14) . . . . ? Ru1 S1 C36 C35 37.2(14) . . . . ? C42 S4 C37 C38 137.1(12) . . . . ? Ru2 S4 C37 C38 28.8(13) . . . . ? S4 C37 C38 S6 -47.7(16) . . . . ? C39 S6 C38 C37 -67.1(14) . . . . ? Ru2 S6 C38 C37 42.1(13) . . . . ? C38 S6 C39 C40 132.7(14) . . . . ? Ru2 S6 C39 C40 24.8(15) . . . . ? S6 C39 C40 S5 -42.7(18) . . . . ? C41 S5 C40 C39 -73.1(15) . . . . ? Ru2 S5 C40 C39 38.4(15) . . . . ? C40 S5 C41 C42 132.6(14) . . . . ? Ru2 S5 C41 C42 23.8(15) . . . . ? S5 C41 C42 S4 -44.4(18) . . . . ? C37 S4 C42 C41 -68.0(15) . . . . ? Ru2 S4 C42 C41 42.6(14) . . . . ? N2 Ru1 N1 C1 -172.3(12) . . . . ? N5 Ru1 N1 C1 102.8(12) . . . . ? S3 Ru1 N1 C1 -77.4(12) . . . . ? S1 Ru1 N1 C1 180(100) . . . . ? S2 Ru1 N1 C1 11.7(12) . . . . ? N2 Ru1 N1 C5 9.5(10) . . . . ? N5 Ru1 N1 C5 -75.5(10) . . . . ? S3 Ru1 N1 C5 104.3(10) . . . . ? S1 Ru1 N1 C5 2(5) . . . . ? S2 Ru1 N1 C5 -166.5(10) . . . . ? N1 Ru1 N2 C6 -13.1(9) . . . . ? N5 Ru1 N2 C6 75.6(10) . . . . ? S3 Ru1 N2 C6 -104.6(9) . . . . ? S1 Ru1 N2 C6 166.3(9) . . . . ? S2 Ru1 N2 C6 17(3) . . . . ? N1 Ru1 N2 C10 -178.9(12) . . . . ? N5 Ru1 N2 C10 -90.2(11) . . . . ? S3 Ru1 N2 C10 89.6(11) . . . . ? S1 Ru1 N2 C10 0.5(11) . . . . ? S2 Ru1 N2 C10 -149(2) . . . . ? C5 N1 C1 C2 -1(2) . . . . ? Ru1 N1 C1 C2 -179.0(11) . . . . ? N1 C1 C2 C3 0(2) . . . . ? C1 C2 C3 C4 -1(3) . . . . ? C2 C3 C4 C5 2(3) . . . . ? C3 C4 C5 N1 -2(2) . . . . ? C3 C4 C5 C6 -176.9(16) . . . . ? C1 N1 C5 C4 2(2) . . . . ? Ru1 N1 C5 C4 -179.7(12) . . . . ? C1 N1 C5 C6 176.9(13) . . . . ? Ru1 N1 C5 C6 -4.7(17) . . . . ? C10 N2 C6 C7 3(2) . . . . ? Ru1 N2 C6 C7 -163.4(13) . . . . ? C10 N2 C6 C5 -178.2(14) . . . . ? Ru1 N2 C6 C5 15.0(16) . . . . ? C4 C5 C6 N2 168.3(14) . . . . ? N1 C5 C6 N2 -7(2) . . . . ? C4 C5 C6 C7 -13(3) . . . . ? N1 C5 C6 C7 171.6(15) . . . . ? N2 C6 C7 C8 -2(2) . . . . ? C5 C6 C7 C8 179.5(16) . . . . ? C6 C7 C8 C9 -2(3) . . . . ? C7 C8 C9 C10 5(3) . . . . ? C8 C9 C10 N2 -3(2) . . . . ? C6 N2 C10 C9 -1(2) . . . . ? Ru1 N2 C10 C9 164.8(12) . . . . ? N4 Ru2 N3 C11 -176.4(14) . . . . ? N6 Ru2 N3 C11 96.3(13) . . . . ? S5 Ru2 N3 C11 176(4) . . . . ? S6 Ru2 N3 C11 -82.7(13) . . . . ? S4 Ru2 N3 C11 5.4(13) . . . . ? N4 Ru2 N3 C15 5.4(10) . . . . ? N6 Ru2 N3 C15 -81.9(11) . . . . ? S5 Ru2 N3 C15 -2(5) . . . . ? S6 Ru2 N3 C15 99.1(11) . . . . ? S4 Ru2 N3 C15 -172.8(10) . . . . ? N3 Ru2 N4 C20 -178.5(14) . . . . ? N6 Ru2 N4 C20 -89.7(13) . . . . ? S5 Ru2 N4 C20 0.9(13) . . . . ? S6 Ru2 N4 C20 90.5(13) . . . . ? S4 Ru2 N4 C20 -158(3) . . . . ? N3 Ru2 N4 C16 -9.1(10) . . . . ? N6 Ru2 N4 C16 79.7(10) . . . . ? S5 Ru2 N4 C16 170.3(10) . . . . ? S6 Ru2 N4 C16 -100.1(10) . . . . ? S4 Ru2 N4 C16 12(4) . . . . ? C15 N3 C11 C12 -3(2) . . . . ? Ru2 N3 C11 C12 178.9(11) . . . . ? N3 C11 C12 C13 2(2) . . . . ? C11 C12 C13 C14 -1(3) . . . . ? C12 C13 C14 C15 1(3) . . . . ? C11 N3 C15 C16 -179.2(14) . . . . ? Ru2 N3 C15 C16 -0.8(19) . . . . ? C11 N3 C15 C14 2(2) . . . . ? Ru2 N3 C15 C14 -179.4(11) . . . . ? C13 C14 C15 N3 -1(2) . . . . ? C13 C14 C15 C16 -179.7(17) . . . . ? C20 N4 C16 C17 3(2) . . . . ? Ru2 N4 C16 C17 -167.8(13) . . . . ? C20 N4 C16 C15 -178.2(14) . . . . ? Ru2 N4 C16 C15 11.4(17) . . . . ? N3 C15 C16 C17 171.9(16) . . . . ? C14 C15 C16 C17 -10(3) . . . . ? N3 C15 C16 N4 -7(2) . . . . ? C14 C15 C16 N4 171.3(14) . . . . ? N4 C16 C17 C18 -2(3) . . . . ? C15 C16 C17 C18 178.6(16) . . . . ? C16 C17 C18 C19 -1(3) . . . . ? C17 C18 C19 C20 3(3) . . . . ? C16 N4 C20 C19 0(2) . . . . ? Ru2 N4 C20 C19 168.8(12) . . . . ? C18 C19 C20 N4 -3(3) . . . . ? C24 N7 C21 C30 -177.1(12) . . . 3_666 ? C24 N7 C21 C22 -2.3(14) . . . . ? N7 C21 C22 C23 3.1(16) . . . . ? C30 C21 C22 C23 177.7(13) 3_666 . . . ? C21 C22 C23 C24 -2.4(16) . . . . ? C21 N7 C24 C25 178.9(13) . . . . ? C21 N7 C24 C23 0.8(14) . . . . ? C22 C23 C24 N7 1.1(16) . . . . ? C22 C23 C24 C25 -177.1(13) . . . . ? N7 C24 C25 C26 3(2) . . . . ? C23 C24 C25 C26 -179.0(14) . . . . ? N7 C24 C25 C45 -176.8(12) . . . . ? C23 C24 C25 C45 1.1(19) . . . . ? C24 C25 C26 N8 -1(2) . . . . ? C45 C25 C26 N8 179.2(12) . . . . ? C24 C25 C26 C27 179.3(14) . . . . ? C45 C25 C26 C27 -1(2) . . . . ? C29 N8 C26 C25 178.9(13) . . . . ? C29 N8 C26 C27 -1.1(15) . . . . ? C25 C26 C27 C28 -177.7(14) . . . . ? N8 C26 C27 C28 2.3(15) . . . . ? C26 C27 C28 C29 -2.5(16) . . . . ? C26 N8 C29 C30 177.8(13) . . . . ? C26 N8 C29 C28 -0.4(15) . . . . ? C27 C28 C29 N8 1.8(15) . . . . ? C27 C28 C29 C30 -176.4(14) . . . . ? N8 C29 C30 C21 -1(2) . . . 3_666 ? C28 C29 C30 C21 176.5(13) . . . 3_666 ? N8 C29 C30 C50 -179.9(13) . . . . ? C28 C29 C30 C50 -2(2) . . . . ? N2 Ru1 N5 C43 -120.8(11) . . . . ? N1 Ru1 N5 C43 -44.0(11) . . . . ? S3 Ru1 N5 C43 -159(100) . . . . ? S1 Ru1 N5 C43 140.3(11) . . . . ? S2 Ru1 N5 C43 52.5(11) . . . . ? N2 Ru1 N5 C47 49.7(10) . . . . ? N1 Ru1 N5 C47 126.5(10) . . . . ? S3 Ru1 N5 C47 12(90) . . . . ? S1 Ru1 N5 C47 -49.2(10) . . . . ? S2 Ru1 N5 C47 -137.0(10) . . . . ? C47 N5 C43 C44 -4(2) . . . . ? Ru1 N5 C43 C44 166.6(10) . . . . ? N5 C43 C44 C45 -1(2) . . . . ? C43 C44 C45 C46 5(2) . . . . ? C43 C44 C45 C25 -173.7(12) . . . . ? C26 C25 C45 C46 112.9(15) . . . . ? C24 C25 C45 C46 -67.1(17) . . . . ? C26 C25 C45 C44 -67.9(17) . . . . ? C24 C25 C45 C44 112.0(15) . . . . ? C44 C45 C46 C47 -5(2) . . . . ? C25 C45 C46 C47 173.7(12) . . . . ? C43 N5 C47 C46 4(2) . . . . ? Ru1 N5 C47 C46 -167.1(10) . . . . ? C45 C46 C47 N5 1(2) . . . . ? N3 Ru2 N6 C48 -54.0(10) . . . . ? N4 Ru2 N6 C48 -132.4(10) . . . . ? S5 Ru2 N6 C48 130.2(10) . . . . ? S6 Ru2 N6 C48 34(20) . . . . ? S4 Ru2 N6 C48 42.8(10) . . . . ? N3 Ru2 N6 C52 120.6(10) . . . . ? N4 Ru2 N6 C52 42.1(10) . . . . ? S5 Ru2 N6 C52 -55.2(10) . . . . ? S6 Ru2 N6 C52 -151(19) . . . . ? S4 Ru2 N6 C52 -142.6(10) . . . . ? C52 N6 C48 C49 -2.9(19) . . . . ? Ru2 N6 C48 C49 171.8(10) . . . . ? N6 C48 C49 C50 -1(2) . . . . ? C48 C49 C50 C51 3.3(19) . . . . ? C48 C49 C50 C30 -171.1(13) . . . . ? C21 C30 C50 C51 119.6(15) 3_666 . . . ? C29 C30 C50 C51 -61.9(19) . . . . ? C21 C30 C50 C49 -66.6(17) 3_666 . . . ? C29 C30 C50 C49 112.0(15) . . . . ? C49 C50 C51 C52 -2.1(19) . . . . ? C30 C50 C51 C52 172.0(13) . . . . ? C48 N6 C52 C51 4.1(19) . . . . ? Ru2 N6 C52 C51 -170.6(10) . . . . ? C50 C51 C52 N6 -2(2) . . . . ? O2 S7 C55 F3 -55.3(19) . . . . ? O3 S7 C55 F3 -179.2(16) . . . . ? O1 S7 C55 F3 61.8(18) . . . . ? O2 S7 C55 F2 177.2(15) . . . . ? O3 S7 C55 F2 53.2(18) . . . . ? O1 S7 C55 F2 -65.7(16) . . . . ? O2 S7 C55 F1 59.0(18) . . . . ? O3 S7 C55 F1 -64.9(18) . . . . ? O1 S7 C55 F1 176.1(15) . . . . ? O4 S8 C56 F5 -59(3) . . . . ? O6 S8 C56 F5 176(2) . . . . ? O5 S8 C56 F5 63(2) . . . . ? O4 S8 C56 F6 170(2) . . . . ? O6 S8 C56 F6 46(3) . . . . ? O5 S8 C56 F6 -68(3) . . . . ? O4 S8 C56 F4 54(3) . . . . ? O6 S8 C56 F4 -70(3) . . . . ? O5 S8 C56 F4 177(2) . . . . ? O9 S9 C57 F8 170(3) . . . . ? O8 S9 C57 F8 47(3) . . . . ? O7 S9 C57 F8 -76(3) . . . . ? O9 S9 C57 F9 -51(2) . . . . ? O8 S9 C57 F9 -174.2(18) . . . . ? O7 S9 C57 F9 63(2) . . . . ? O9 S9 C57 F7 61(2) . . . . ? O8 S9 C57 F7 -62(2) . . . . ? O7 S9 C57 F7 174.8(17) . . . . ? O11 S10 C58 F11 -178.2(17) . . . . ? O12 S10 C58 F11 -49(2) . . . . ? O10 S10 C58 F11 67(2) . . . . ? O11 S10 C58 F12 57(2) . . . . ? O12 S10 C58 F12 -174.1(16) . . . . ? O10 S10 C58 F12 -57.8(19) . . . . ? O11 S10 C58 F10 -60.2(19) . . . . ? O12 S10 C58 F10 68.5(17) . . . . ? O10 S10 C58 F10 -175.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.161 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.103 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 735953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; fac-(1,4,7-tritiacyclononane)-(dimethylsulfoxide,S)-(5-methyl-5'-carboxyl- 2,2'-bipyridine)-ruthenium(II) bis(triflate) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H28 F6 N2 O9 Ru S6 2+, 2(S O3 C F3 1-)' _chemical_formula_sum 'C22 H28 F6 N2 O9 Ru S6' _chemical_formula_weight 871.89 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 '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' _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 10.026(3) _cell_length_b 23.075(4) _cell_length_c 14.057(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.40(2) _cell_angle_gamma 90.00 _cell_volume 3231.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7978 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _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 'image plate dip1030' _diffrn_measurement_method 'laser scanner' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35958 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7081 _reflns_number_gt 4120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Xpress' _computing_cell_refinement 'Denzo (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELX97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELX97 (Sheldrick, 1998)' _computing_molecular_graphics 'Ortep3/windows (Farrugia,1997)' _computing_publication_material 'Wingx 1.70.00 (Farrugia, 1999)' _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^)+(0.0613P)^2^] 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 7081 _refine_ls_number_parameters 418 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_restrained_S_all 0.870 _refine_ls_shift/su_max 0.000 _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 Ru Ru 0.36384(3) 0.148868(13) 0.33384(3) 0.05239(11) Uani 1 1 d . . . S1 S 0.16899(10) 0.16820(5) 0.23177(9) 0.0612(3) Uani 1 1 d . . . S2 S 0.34272(10) 0.24250(5) 0.39441(9) 0.0613(3) Uani 1 1 d . . . S3 S 0.22602(10) 0.11632(5) 0.44863(9) 0.0637(3) Uani 1 1 d . . . C11 C 0.1151(4) 0.24188(19) 0.2606(4) 0.0717(12) Uani 1 1 d . . . H11A H 0.0725 0.2600 0.2028 0.086 Uiso 1 1 calc R . . H11B H 0.0489 0.2393 0.3058 0.086 Uiso 1 1 calc R . . C12 C 0.2295(4) 0.27931(19) 0.3025(4) 0.0711(12) Uani 1 1 d . . . H12A H 0.1934 0.3136 0.3303 0.085 Uiso 1 1 calc R . . H12B H 0.2805 0.2919 0.2515 0.085 Uiso 1 1 calc R . . C13 C 0.2327(5) 0.2350(2) 0.4894(4) 0.0741(13) Uani 1 1 d . . . H13A H 0.2575 0.2638 0.5385 0.089 Uiso 1 1 calc R . . H13B H 0.1409 0.2427 0.4629 0.089 Uiso 1 1 calc R . . C14 C 0.2398(5) 0.1760(2) 0.5345(4) 0.0808(14) Uani 1 1 d . . . H14A H 0.1683 0.1726 0.5752 0.097 Uiso 1 1 calc R . . H14B H 0.3244 0.1725 0.5749 0.097 Uiso 1 1 calc R . . C15 C 0.0521(4) 0.1242(2) 0.3907(4) 0.0814(15) Uani 1 1 d . . . H15A H -0.0014 0.0923 0.4106 0.098 Uiso 1 1 calc R . . H15B H 0.0146 0.1599 0.4127 0.098 Uiso 1 1 calc R . . C16 C 0.0420(4) 0.1251(2) 0.2833(4) 0.0773(14) Uani 1 1 d . . . H16A H -0.0458 0.1398 0.2591 0.093 Uiso 1 1 calc R . . H16B H 0.0477 0.0855 0.2608 0.093 Uiso 1 1 calc R . . S4 S 0.49204(10) 0.18304(5) 0.21718(8) 0.0604(3) Uani 1 1 d . . . O4 O 0.4468(3) 0.23901(14) 0.1723(3) 0.0849(10) Uani 1 1 d . . . C17 C 0.6653(4) 0.1902(3) 0.2587(4) 0.0964(19) Uani 1 1 d . . . H17A H 0.6759 0.2170 0.3113 0.145 Uiso 1 1 calc R . . H17B H 0.7126 0.2045 0.2078 0.145 Uiso 1 1 calc R . . H17C H 0.7010 0.1532 0.2794 0.145 Uiso 1 1 calc R . . C18 C 0.5017(6) 0.1331(2) 0.1200(4) 0.0896(16) Uani 1 1 d . . . H18A H 0.4127 0.1235 0.0921 0.134 Uiso 1 1 calc R . . H18B H 0.5472 0.0986 0.1436 0.134 Uiso 1 1 calc R . . H18C H 0.5502 0.1507 0.0724 0.134 Uiso 1 1 calc R . . N1 N 0.3884(3) 0.06154(14) 0.2943(3) 0.0576(8) Uani 1 1 d . . . N2 N 0.5344(3) 0.12361(14) 0.4264(3) 0.0560(8) Uani 1 1 d . . . C1 C 0.3093(4) 0.03131(19) 0.2269(3) 0.0673(12) Uani 1 1 d . . . H1 H 0.2405 0.0508 0.1902 0.081 Uiso 1 1 calc R . . C2 C 0.3266(5) -0.0267(2) 0.2106(4) 0.0756(13) Uani 1 1 d . . . H2 H 0.2690 -0.0457 0.1643 0.091 Uiso 1 1 calc R . . C3 C 0.4297(5) -0.05749(19) 0.2628(4) 0.0691(12) Uani 1 1 d . . . C4 C 0.5122(4) -0.02603(19) 0.3311(3) 0.0647(11) Uani 1 1 d . . . H4 H 0.5828 -0.0447 0.3673 0.078 Uiso 1 1 calc R . . C5 C 0.4905(4) 0.03235(17) 0.3457(3) 0.0568(10) Uani 1 1 d . . . C6 C 0.5754(4) 0.06754(17) 0.4174(3) 0.0564(10) Uani 1 1 d . . . C7 C 0.6908(4) 0.04680(19) 0.4716(3) 0.0624(11) Uani 1 1 d . . . H7 H 0.7183 0.0087 0.4642 0.075 Uiso 1 1 calc R . . C8 C 0.7640(4) 0.0829(2) 0.5364(3) 0.0643(11) Uani 1 1 d . . . C9 C 0.7224(4) 0.1398(2) 0.5461(4) 0.0694(12) Uani 1 1 d . . . H9 H 0.7701 0.1647 0.5894 0.083 Uiso 1 1 calc R . . C10 C 0.6074(4) 0.15869(19) 0.4896(4) 0.0666(12) Uani 1 1 d . . . H10 H 0.5799 0.1969 0.4954 0.080 Uiso 1 1 calc R . . C19 C 0.4547(6) -0.1210(2) 0.2420(5) 0.0981(17) Uani 1 1 d . . . H19A H 0.3878 -0.1345 0.1928 0.147 Uiso 1 1 calc R . . H19B H 0.4502 -0.1434 0.2991 0.147 Uiso 1 1 calc R . . H19C H 0.5420 -0.1252 0.2209 0.147 Uiso 1 1 calc R . . C20 C 0.8879(5) 0.0591(3) 0.5942(4) 0.0812(14) Uani 1 1 d . . . O8 O 0.9169(4) 0.00919(19) 0.5951(4) 0.1335(18) Uani 1 1 d . . . O9 O 0.9592(4) 0.09920(18) 0.6418(4) 0.1213(15) Uani 1 1 d D . . H91 H 1.032(4) 0.083(3) 0.678(5) 0.182 Uiso 1 1 d D . . S5 S 0.83842(11) 0.28447(5) 0.49124(10) 0.0712(3) Uani 1 1 d . . . O3 O 0.8900(4) 0.24562(18) 0.4270(4) 0.1220(16) Uani 1 1 d . . . O2 O 0.6975(3) 0.29351(18) 0.4716(4) 0.1159(14) Uani 1 1 d . . . O1 O 0.8833(5) 0.2759(3) 0.5889(3) 0.159(2) Uani 1 1 d . . . C21 C 0.9146(6) 0.3511(3) 0.4706(8) 0.123(3) Uani 1 1 d . . . F1 F 0.8746(7) 0.3937(2) 0.5123(8) 0.279(5) Uani 1 1 d . . . F2 F 0.8895(7) 0.3659(3) 0.3783(7) 0.253(5) Uani 1 1 d . . . F3 F 1.0462(3) 0.34998(16) 0.4823(4) 0.1426(16) Uani 1 1 d . . . S6 S 0.17371(12) 0.48908(6) 0.29680(11) 0.0805(4) Uani 1 1 d . . . O6 O 0.1921(4) 0.43853(18) 0.2385(3) 0.1088(13) Uani 1 1 d . . . O5 O 0.0390(3) 0.49596(19) 0.3214(3) 0.1105(14) Uani 1 1 d . . . O7 O 0.2354(4) 0.54050(16) 0.2650(3) 0.0992(11) Uani 1 1 d . . . C22 C 0.2744(6) 0.4716(3) 0.4094(5) 0.0884(16) Uani 1 1 d . . . F4 F 0.2610(7) 0.5058(3) 0.4744(4) 0.249(4) Uani 1 1 d . . . F5 F 0.4018(4) 0.4695(2) 0.4020(3) 0.1560(18) Uani 1 1 d . . . F6 F 0.2494(6) 0.4211(3) 0.4406(4) 0.216(3) 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 Ru 0.04866(16) 0.04871(18) 0.0584(2) -0.00264(16) -0.00041(13) -0.00058(12) S1 0.0527(5) 0.0622(6) 0.0664(8) -0.0033(5) -0.0037(5) 0.0017(4) S2 0.0586(5) 0.0517(6) 0.0719(8) -0.0063(5) 0.0004(5) -0.0013(4) S3 0.0634(6) 0.0588(6) 0.0695(8) 0.0005(5) 0.0096(5) -0.0044(4) C11 0.065(2) 0.063(3) 0.085(4) 0.004(2) -0.003(2) 0.0109(19) C12 0.074(3) 0.055(3) 0.084(4) 0.003(2) 0.007(2) 0.011(2) C13 0.081(3) 0.071(3) 0.070(3) -0.018(3) 0.008(2) -0.002(2) C14 0.098(3) 0.073(3) 0.073(4) -0.010(3) 0.012(3) -0.007(3) C15 0.062(3) 0.079(3) 0.103(5) 0.005(3) 0.011(3) -0.011(2) C16 0.056(2) 0.080(3) 0.094(4) -0.007(3) 0.000(2) -0.012(2) S4 0.0554(5) 0.0585(6) 0.0674(8) 0.0022(5) 0.0071(5) 0.0011(4) O4 0.085(2) 0.076(2) 0.097(3) 0.0262(19) 0.0268(18) 0.0186(16) C17 0.057(3) 0.137(5) 0.095(4) 0.029(4) 0.004(3) -0.022(3) C18 0.111(4) 0.081(4) 0.081(4) -0.007(3) 0.024(3) 0.000(3) N1 0.0568(17) 0.054(2) 0.062(2) -0.0040(17) 0.0035(16) 0.0003(14) N2 0.0540(16) 0.055(2) 0.058(2) 0.0016(16) -0.0005(15) -0.0038(14) C1 0.068(2) 0.062(3) 0.069(3) -0.007(2) -0.007(2) 0.001(2) C2 0.086(3) 0.059(3) 0.079(4) -0.014(2) -0.003(3) -0.008(2) C3 0.083(3) 0.056(3) 0.069(3) -0.003(2) 0.012(2) -0.001(2) C4 0.065(2) 0.059(3) 0.070(3) 0.003(2) 0.008(2) 0.0055(19) C5 0.057(2) 0.053(2) 0.061(3) 0.000(2) 0.0058(19) -0.0003(16) C6 0.060(2) 0.052(2) 0.056(3) 0.0042(19) 0.0026(19) -0.0013(17) C7 0.061(2) 0.060(3) 0.065(3) 0.007(2) -0.001(2) 0.0011(18) C8 0.060(2) 0.067(3) 0.065(3) 0.014(2) 0.000(2) -0.0002(19) C9 0.064(2) 0.069(3) 0.071(3) 0.004(2) -0.011(2) -0.010(2) C10 0.066(2) 0.056(3) 0.075(3) 0.000(2) -0.008(2) -0.0022(18) C19 0.123(4) 0.058(3) 0.112(5) -0.005(3) 0.007(4) 0.007(3) C20 0.074(3) 0.077(4) 0.086(4) 0.006(3) -0.021(3) -0.004(2) O8 0.135(3) 0.078(3) 0.168(5) -0.023(3) -0.069(3) 0.026(2) O9 0.120(3) 0.085(3) 0.142(4) 0.010(3) -0.060(3) 0.004(2) S5 0.0636(6) 0.0704(8) 0.0792(9) -0.0020(6) 0.0063(6) 0.0014(5) O3 0.087(2) 0.106(3) 0.179(5) -0.055(3) 0.042(3) -0.011(2) O2 0.066(2) 0.113(3) 0.169(4) -0.022(3) 0.017(2) 0.0035(19) O1 0.163(4) 0.220(6) 0.085(4) 0.048(4) -0.029(3) -0.067(4) C21 0.088(4) 0.070(4) 0.206(9) 0.021(5) -0.001(5) 0.015(3) F1 0.219(6) 0.100(4) 0.542(15) -0.103(6) 0.144(8) -0.006(4) F2 0.202(6) 0.210(7) 0.324(9) 0.185(7) -0.076(6) -0.049(5) F3 0.093(2) 0.105(3) 0.227(5) 0.023(3) 0.009(3) -0.0216(19) S6 0.0766(7) 0.0767(9) 0.0852(10) 0.0029(7) -0.0044(7) -0.0022(6) O6 0.101(3) 0.099(3) 0.117(3) -0.025(3) -0.031(2) 0.004(2) O5 0.066(2) 0.135(4) 0.132(4) 0.027(3) 0.014(2) 0.006(2) O7 0.105(3) 0.082(3) 0.111(3) 0.021(2) 0.012(2) -0.0065(19) C22 0.086(4) 0.092(4) 0.084(5) 0.011(3) -0.001(3) 0.000(3) F4 0.320(8) 0.317(9) 0.093(4) -0.078(5) -0.058(4) 0.189(7) F5 0.090(2) 0.241(6) 0.129(4) 0.004(3) -0.022(2) 0.013(3) F6 0.218(5) 0.209(6) 0.198(6) 0.126(5) -0.083(4) -0.077(5) _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 Ru N2 2.112(3) . ? Ru N1 2.112(3) . ? Ru S4 2.3309(12) . ? Ru S1 2.3343(13) . ? Ru S2 2.3406(11) . ? Ru S3 2.3610(12) . ? S1 C16 1.828(5) . ? S1 C11 1.843(4) . ? S2 C12 1.831(5) . ? S2 C13 1.833(5) . ? S3 C14 1.826(5) . ? S3 C15 1.849(5) . ? C11 C12 1.502(6) . ? C13 C14 1.499(7) . ? C15 C16 1.502(7) . ? S4 O4 1.486(3) . ? S4 C17 1.778(4) . ? S4 C18 1.797(5) . ? N1 C1 1.357(5) . ? N1 C5 1.364(5) . ? N2 C10 1.355(5) . ? N2 C6 1.368(5) . ? C1 C2 1.373(6) . ? C2 C3 1.393(7) . ? C3 C4 1.398(6) . ? C3 C19 1.520(6) . ? C4 C5 1.384(6) . ? C5 C6 1.486(6) . ? C6 C7 1.397(6) . ? C7 C8 1.384(6) . ? C8 C9 1.387(6) . ? C8 C20 1.511(6) . ? C9 C10 1.395(6) . ? C20 O8 1.187(6) . ? C20 O9 1.308(6) . ? S5 O1 1.411(5) . ? S5 O3 1.411(4) . ? S5 O2 1.424(3) . ? S5 C21 1.754(7) . ? C21 F1 1.235(9) . ? C21 F3 1.311(7) . ? C21 F2 1.339(11) . ? S6 O7 1.433(4) . ? S6 O5 1.440(4) . ? S6 O6 1.449(4) . ? S6 C22 1.825(6) . ? C22 F4 1.226(7) . ? C22 F6 1.281(7) . ? C22 F5 1.294(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 N2 Ru N1 77.82(13) . . ? N2 Ru S4 93.14(9) . . ? N1 Ru S4 92.74(9) . . ? N2 Ru S1 174.89(9) . . ? N1 Ru S1 97.72(10) . . ? S4 Ru S1 89.55(4) . . ? N2 Ru S2 97.50(10) . . ? N1 Ru S2 173.96(10) . . ? S4 Ru S2 91.32(4) . . ? S1 Ru S2 86.77(4) . . ? N2 Ru S3 89.22(9) . . ? N1 Ru S3 88.32(9) . . ? S4 Ru S3 177.57(4) . . ? S1 Ru S3 88.14(5) . . ? S2 Ru S3 87.79(4) . . ? C16 S1 C11 100.4(2) . . ? C16 S1 Ru 102.96(17) . . ? C11 S1 Ru 106.68(16) . . ? C12 S2 C13 100.5(2) . . ? C12 S2 Ru 104.21(15) . . ? C13 S2 Ru 105.32(16) . . ? C14 S3 C15 102.4(2) . . ? C14 S3 Ru 101.80(16) . . ? C15 S3 Ru 105.22(18) . . ? C12 C11 S1 112.8(3) . . ? C11 C12 S2 113.3(3) . . ? C14 C13 S2 112.9(3) . . ? C13 C14 S3 114.2(4) . . ? C16 C15 S3 113.5(3) . . ? C15 C16 S1 115.7(3) . . ? O4 S4 C17 107.4(2) . . ? O4 S4 C18 105.9(3) . . ? C17 S4 C18 100.1(3) . . ? O4 S4 Ru 115.23(13) . . ? C17 S4 Ru 113.33(18) . . ? C18 S4 Ru 113.48(18) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Ru 126.7(3) . . ? C5 N1 Ru 115.7(3) . . ? C10 N2 C6 118.7(3) . . ? C10 N2 Ru 125.5(3) . . ? C6 N2 Ru 115.8(3) . . ? N1 C1 C2 122.9(4) . . ? C1 C2 C3 120.6(4) . . ? C2 C3 C4 116.4(4) . . ? C2 C3 C19 121.2(5) . . ? C4 C3 C19 122.3(4) . . ? C5 C4 C3 121.1(4) . . ? N1 C5 C4 121.5(4) . . ? N1 C5 C6 115.4(3) . . ? C4 C5 C6 123.0(4) . . ? N2 C6 C7 120.8(4) . . ? N2 C6 C5 115.1(3) . . ? C7 C6 C5 124.0(4) . . ? C8 C7 C6 119.9(4) . . ? C7 C8 C9 119.4(4) . . ? C7 C8 C20 118.6(4) . . ? C9 C8 C20 122.0(4) . . ? C8 C9 C10 118.6(4) . . ? N2 C10 C9 122.6(4) . . ? O8 C20 O9 124.2(5) . . ? O8 C20 C8 123.1(5) . . ? O9 C20 C8 112.7(5) . . ? O1 S5 O3 115.7(4) . . ? O1 S5 O2 114.3(3) . . ? O3 S5 O2 113.3(3) . . ? O1 S5 C21 100.8(4) . . ? O3 S5 C21 104.7(4) . . ? O2 S5 C21 106.3(3) . . ? F1 C21 F3 109.3(8) . . ? F1 C21 F2 102.8(7) . . ? F3 C21 F2 101.8(7) . . ? F1 C21 S5 116.6(7) . . ? F3 C21 S5 114.4(4) . . ? F2 C21 S5 110.3(6) . . ? O7 S6 O5 115.7(2) . . ? O7 S6 O6 113.8(3) . . ? O5 S6 O6 114.0(3) . . ? O7 S6 C22 103.7(3) . . ? O5 S6 C22 105.0(3) . . ? O6 S6 C22 102.7(3) . . ? F4 C22 F6 106.7(7) . . ? F4 C22 F5 106.0(6) . . ? F6 C22 F5 103.1(6) . . ? F4 C22 S6 114.1(5) . . ? F6 C22 S6 112.8(5) . . ? F5 C22 S6 113.2(5) . . ? 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 N2 Ru S1 C16 40.3(11) . . . . ? N1 Ru S1 C16 69.5(2) . . . . ? S4 Ru S1 C16 162.19(18) . . . . ? S2 Ru S1 C16 -106.46(18) . . . . ? S3 Ru S1 C16 -18.57(18) . . . . ? N2 Ru S1 C11 145.6(11) . . . . ? N1 Ru S1 C11 174.72(19) . . . . ? S4 Ru S1 C11 -92.57(17) . . . . ? S2 Ru S1 C11 -1.23(17) . . . . ? S3 Ru S1 C11 86.66(17) . . . . ? N2 Ru S2 C12 164.56(18) . . . . ? N1 Ru S2 C12 -156.5(8) . . . . ? S4 Ru S2 C12 71.22(16) . . . . ? S1 Ru S2 C12 -18.26(16) . . . . ? S3 Ru S2 C12 -106.52(16) . . . . ? N2 Ru S2 C13 -90.12(19) . . . . ? N1 Ru S2 C13 -51.2(8) . . . . ? S4 Ru S2 C13 176.53(17) . . . . ? S1 Ru S2 C13 87.05(17) . . . . ? S3 Ru S2 C13 -1.20(17) . . . . ? N2 Ru S3 C14 78.7(2) . . . . ? N1 Ru S3 C14 156.5(2) . . . . ? S4 Ru S3 C14 -87.5(10) . . . . ? S1 Ru S3 C14 -105.72(19) . . . . ? S2 Ru S3 C14 -18.88(19) . . . . ? N2 Ru S3 C15 -174.8(2) . . . . ? N1 Ru S3 C15 -97.0(2) . . . . ? S4 Ru S3 C15 19.1(11) . . . . ? S1 Ru S3 C15 0.82(19) . . . . ? S2 Ru S3 C15 87.66(19) . . . . ? C16 S1 C11 C12 133.3(4) . . . . ? Ru S1 C11 C12 26.3(4) . . . . ? S1 C11 C12 S2 -44.9(5) . . . . ? C13 S2 C12 C11 -68.2(4) . . . . ? Ru S2 C12 C11 40.7(4) . . . . ? C12 S2 C13 C14 135.4(4) . . . . ? Ru S2 C13 C14 27.3(4) . . . . ? S2 C13 C14 S3 -48.0(5) . . . . ? C15 S3 C14 C13 -66.1(4) . . . . ? Ru S3 C14 C13 42.6(4) . . . . ? C14 S3 C15 C16 128.7(4) . . . . ? Ru S3 C15 C16 22.6(4) . . . . ? S3 C15 C16 S1 -42.5(5) . . . . ? C11 S1 C16 C15 -70.3(4) . . . . ? Ru S1 C16 C15 39.7(4) . . . . ? N2 Ru S4 O4 -137.5(2) . . . . ? N1 Ru S4 O4 144.6(2) . . . . ? S1 Ru S4 O4 46.86(19) . . . . ? S2 Ru S4 O4 -39.90(19) . . . . ? S3 Ru S4 O4 28.6(11) . . . . ? N2 Ru S4 C17 -13.2(3) . . . . ? N1 Ru S4 C17 -91.2(3) . . . . ? S1 Ru S4 C17 171.1(2) . . . . ? S2 Ru S4 C17 84.4(2) . . . . ? S3 Ru S4 C17 152.9(10) . . . . ? N2 Ru S4 C18 100.1(2) . . . . ? N1 Ru S4 C18 22.2(2) . . . . ? S1 Ru S4 C18 -75.5(2) . . . . ? S2 Ru S4 C18 -162.3(2) . . . . ? S3 Ru S4 C18 -93.8(10) . . . . ? N2 Ru N1 C1 178.9(4) . . . . ? S4 Ru N1 C1 -88.5(3) . . . . ? S1 Ru N1 C1 1.4(4) . . . . ? S2 Ru N1 C1 139.3(7) . . . . ? S3 Ru N1 C1 89.3(3) . . . . ? N2 Ru N1 C5 2.4(3) . . . . ? S4 Ru N1 C5 95.0(3) . . . . ? S1 Ru N1 C5 -175.0(3) . . . . ? S2 Ru N1 C5 -37.2(10) . . . . ? S3 Ru N1 C5 -87.1(3) . . . . ? N1 Ru N2 C10 177.0(4) . . . . ? S4 Ru N2 C10 84.8(3) . . . . ? S1 Ru N2 C10 -153.4(9) . . . . ? S2 Ru N2 C10 -6.9(3) . . . . ? S3 Ru N2 C10 -94.6(3) . . . . ? N1 Ru N2 C6 -0.1(3) . . . . ? S4 Ru N2 C6 -92.3(3) . . . . ? S1 Ru N2 C6 29.4(12) . . . . ? S2 Ru N2 C6 176.0(3) . . . . ? S3 Ru N2 C6 88.3(3) . . . . ? C5 N1 C1 C2 1.4(7) . . . . ? Ru N1 C1 C2 -175.0(3) . . . . ? N1 C1 C2 C3 -1.0(7) . . . . ? C1 C2 C3 C4 0.0(7) . . . . ? C1 C2 C3 C19 -176.7(5) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C19 C3 C4 C5 177.2(4) . . . . ? C1 N1 C5 C4 -0.8(6) . . . . ? Ru N1 C5 C4 175.9(3) . . . . ? C1 N1 C5 C6 179.0(3) . . . . ? Ru N1 C5 C6 -4.2(5) . . . . ? C3 C4 C5 N1 -0.1(6) . . . . ? C3 C4 C5 C6 -180.0(4) . . . . ? C10 N2 C6 C7 -0.4(6) . . . . ? Ru N2 C6 C7 176.9(3) . . . . ? C10 N2 C6 C5 -179.3(4) . . . . ? Ru N2 C6 C5 -2.0(4) . . . . ? N1 C5 C6 N2 4.1(5) . . . . ? C4 C5 C6 N2 -176.1(4) . . . . ? N1 C5 C6 C7 -174.8(4) . . . . ? C4 C5 C6 C7 5.1(6) . . . . ? N2 C6 C7 C8 0.9(6) . . . . ? C5 C6 C7 C8 179.6(4) . . . . ? C6 C7 C8 C9 -0.6(7) . . . . ? C6 C7 C8 C20 179.8(4) . . . . ? C7 C8 C9 C10 -0.2(7) . . . . ? C20 C8 C9 C10 179.5(4) . . . . ? C6 N2 C10 C9 -0.4(6) . . . . ? Ru N2 C10 C9 -177.4(3) . . . . ? C8 C9 C10 N2 0.7(7) . . . . ? C7 C8 C20 O8 -9.1(8) . . . . ? C9 C8 C20 O8 171.2(6) . . . . ? C7 C8 C20 O9 170.4(5) . . . . ? C9 C8 C20 O9 -9.3(7) . . . . ? O1 S5 C21 F1 -66.6(9) . . . . ? O3 S5 C21 F1 173.0(9) . . . . ? O2 S5 C21 F1 52.9(10) . . . . ? O1 S5 C21 F3 62.8(8) . . . . ? O3 S5 C21 F3 -57.6(8) . . . . ? O2 S5 C21 F3 -177.8(7) . . . . ? O1 S5 C21 F2 176.8(6) . . . . ? O3 S5 C21 F2 56.3(6) . . . . ? O2 S5 C21 F2 -63.8(7) . . . . ? O7 S6 C22 F4 69.6(7) . . . . ? O5 S6 C22 F4 -52.2(7) . . . . ? O6 S6 C22 F4 -171.7(6) . . . . ? O7 S6 C22 F6 -168.4(5) . . . . ? O5 S6 C22 F6 69.8(6) . . . . ? O6 S6 C22 F6 -49.7(6) . . . . ? O7 S6 C22 F5 -51.8(5) . . . . ? O5 S6 C22 F5 -173.6(5) . . . . ? O6 S6 C22 F5 66.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 0.420 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.066