# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'James Wilton-Ely' _publ_contact_author_email J.WILTON-ELY@IMPERIAL.AC.UK _publ_section_title ; The functionalisation ruthenium(II) and osmium(II) alkenyl complexes with amine- and alkoxy-terminated dithiocarbamates ; loop_ _publ_author_name 'James Wilton-Ely' 'G Hogarth' 'Saira Naeem' 'Eleanor Ogilvie' 'Andrew J.P. White' # Attachment 'DT_Wilton-Ely_amine_terminated.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 750274' #TrackingRef 'DT_Wilton-Ely_amine_terminated.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C57 H58 N O2 P4 Ru S2, F6 P' _chemical_formula_sum 'C57 H58 F6 N O2 P5 Ru S2' _chemical_formula_weight 1223.08 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.3740(3) _cell_length_b 12.01286(19) _cell_length_c 26.6409(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.1247(14) _cell_angle_gamma 90.00 _cell_volume 5538.04(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18588 _cell_measurement_theta_min 3.0061 _cell_measurement_theta_max 29.1759 _exptl_crystal_description needles _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9832 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38280 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 29.23 _reflns_number_total 12994 _reflns_number_gt 9490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0405P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12994 _refine_ls_number_parameters 705 _refine_ls_number_restraints 386 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.004 _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 0.255326(9) 0.347626(13) 0.563482(6) 0.01650(5) Uani 1 1 d . . . S1 S 0.18906(3) 0.37866(4) 0.480702(19) 0.02431(12) Uani 1 1 d . . . C2 C 0.13237(12) 0.26627(17) 0.49031(8) 0.0257(5) Uani 1 1 d . . . S3 S 0.15680(3) 0.20462(4) 0.54768(2) 0.02680(12) Uani 1 1 d . . . N4 N 0.07373(10) 0.23525(15) 0.45718(8) 0.0347(5) Uani 1 1 d . . . C5 C 0.01677(15) 0.1546(2) 0.47002(11) 0.0462(7) Uani 1 1 d . . . H5A H -0.0340 0.1920 0.4695 0.055 Uiso 1 1 calc R . . H5B H 0.0308 0.1281 0.5048 0.055 Uiso 1 1 calc R . . C6 C 0.00885(15) 0.0546(2) 0.43523(11) 0.0494(7) Uani 1 1 d . . . H6A H -0.0376 0.0110 0.4417 0.059 Uiso 1 1 calc R . . H6B H 0.0035 0.0793 0.3996 0.059 Uiso 1 1 calc R . . O7 O 0.07550(11) -0.01130(15) 0.44460(7) 0.0527(5) Uani 1 1 d . . . C8 C 0.0738(2) -0.0989(2) 0.40835(13) 0.0702(10) Uani 1 1 d . . . H8A H 0.1200 -0.1453 0.4148 0.105 Uiso 1 1 calc R . . H8B H 0.0727 -0.0670 0.3744 0.105 Uiso 1 1 calc R . . H8C H 0.0276 -0.1446 0.4109 0.105 Uiso 1 1 calc R . . C9 C 0.05596(15) 0.3004(2) 0.41044(10) 0.0437(7) Uani 1 1 d D A . H9A H 0.0642 0.3802 0.4185 0.052 Uiso 1 1 calc R . . H9B H 0.0005 0.2907 0.3993 0.052 Uiso 1 1 calc R . . C10 C 0.10234(19) 0.2715(2) 0.36662(11) 0.0583(8) Uani 1 1 d D . . H10A H 0.1008 0.3346 0.3426 0.070 Uiso 0.898(5) 1 calc PR A 1 H10B H 0.1569 0.2581 0.3792 0.070 Uiso 0.898(5) 1 calc PR A 1 H10C H 0.1368 0.3339 0.3593 0.070 Uiso 0.102(5) 1 d PR A 2 H10D H 0.1345 0.2047 0.3747 0.070 Uiso 0.102(5) 1 d PR A 2 O11 O 0.07228(19) 0.1772(2) 0.34221(9) 0.0812(11) Uani 0.898(5) 1 d PDU A 1 C12 C 0.1034(4) 0.1540(4) 0.29642(14) 0.0983(18) Uani 0.898(5) 1 d PDU A 1 H12A H 0.0791 0.0869 0.2813 0.147 Uiso 0.898(5) 1 calc PR A 1 H12B H 0.1593 0.1421 0.3027 0.147 Uiso 0.898(5) 1 calc PR A 1 H12C H 0.0936 0.2169 0.2733 0.147 Uiso 0.898(5) 1 calc PR A 1 O11' O 0.0499(13) 0.258(2) 0.3238(6) 0.105(5) Uiso 0.102(5) 1 d PDU A 2 C12' C 0.041(3) 0.157(3) 0.2992(13) 0.104(6) Uiso 0.102(5) 1 d PDU A 2 H12D H -0.0086 0.1557 0.2786 0.156 Uiso 0.102(5) 1 calc PR A 2 H12E H 0.0426 0.0965 0.3240 0.156 Uiso 0.102(5) 1 calc PR A 2 H12F H 0.0831 0.1469 0.2773 0.156 Uiso 0.102(5) 1 calc PR A 2 P13 P 0.17637(3) 0.46934(4) 0.605421(19) 0.01968(11) Uani 1 1 d . . . C14 C 0.22472(12) 0.44217(17) 0.66854(8) 0.0258(5) Uani 1 1 d . . . H14A H 0.1878 0.4220 0.6933 0.031 Uiso 1 1 calc R . . H14B H 0.2575 0.5052 0.6814 0.031 Uiso 1 1 calc R . . P15 P 0.28213(3) 0.32195(4) 0.65014(2) 0.02232(12) Uani 1 1 d . . . C16 C 0.17644(11) 0.61980(16) 0.59619(8) 0.0229(5) Uani 1 1 d . . . C17 C 0.19147(12) 0.66355(18) 0.54989(9) 0.0293(5) Uani 1 1 d . . . H17A H 0.2010 0.6151 0.5229 0.035 Uiso 1 1 calc R . . C18 C 0.19262(14) 0.7778(2) 0.54287(11) 0.0439(7) Uani 1 1 d . . . H18A H 0.2026 0.8078 0.5111 0.053 Uiso 1 1 calc R . . C19 C 0.17926(15) 0.8477(2) 0.58199(12) 0.0484(7) Uani 1 1 d . . . H19A H 0.1803 0.9260 0.5770 0.058 Uiso 1 1 calc R . . C20 C 0.16448(15) 0.8059(2) 0.62808(11) 0.0470(7) Uani 1 1 d . . . H20A H 0.1559 0.8550 0.6550 0.056 Uiso 1 1 calc R . . C21 C 0.16213(13) 0.69195(19) 0.63523(9) 0.0338(5) Uani 1 1 d . . . H21A H 0.1507 0.6628 0.6669 0.041 Uiso 1 1 calc R . . C22 C 0.07391(12) 0.43996(17) 0.60867(8) 0.0269(5) Uani 1 1 d . . . C23 C 0.02862(12) 0.42296(18) 0.56394(10) 0.0332(5) Uani 1 1 d . . . H23A H 0.0512 0.4289 0.5329 0.040 Uiso 1 1 calc R . . C24 C -0.04921(15) 0.3974(2) 0.56379(13) 0.0514(8) Uani 1 1 d . . . H24A H -0.0795 0.3856 0.5327 0.062 Uiso 1 1 calc R . . C25 C -0.08253(16) 0.3891(2) 0.60825(15) 0.0609(9) Uani 1 1 d . . . H25A H -0.1358 0.3713 0.6081 0.073 Uiso 1 1 calc R . . C26 C -0.03930(18) 0.4063(3) 0.65245(14) 0.0660(9) Uani 1 1 d . . . H26A H -0.0627 0.4002 0.6832 0.079 Uiso 1 1 calc R . . C27 C 0.03921(16) 0.4329(2) 0.65350(11) 0.0509(7) Uani 1 1 d . . . H27A H 0.0686 0.4460 0.6847 0.061 Uiso 1 1 calc R . . C28 C 0.23971(14) 0.20343(18) 0.68105(8) 0.0291(5) Uani 1 1 d . . . C29 C 0.16062(16) 0.1850(2) 0.67276(10) 0.0403(6) Uani 1 1 d . . . H29A H 0.1296 0.2327 0.6509 0.048 Uiso 1 1 calc R . . C30 C 0.12675(18) 0.0963(2) 0.69653(11) 0.0530(8) Uani 1 1 d . . . H30A H 0.0726 0.0843 0.6911 0.064 Uiso 1 1 calc R . . C31 C 0.1712(2) 0.0267(2) 0.72762(11) 0.0580(9) Uani 1 1 d . . . H31A H 0.1477 -0.0330 0.7440 0.070 Uiso 1 1 calc R . . C32 C 0.2491(2) 0.0428(2) 0.73512(11) 0.0591(8) Uani 1 1 d . . . H32A H 0.2797 -0.0071 0.7562 0.071 Uiso 1 1 calc R . . C33 C 0.28424(17) 0.1310(2) 0.71234(10) 0.0451(7) Uani 1 1 d . . . H33A H 0.3385 0.1419 0.7181 0.054 Uiso 1 1 calc R . . C34 C 0.37664(13) 0.33531(18) 0.68598(8) 0.0295(5) Uani 1 1 d . . . C35 C 0.38660(17) 0.4031(2) 0.72809(9) 0.0452(7) Uani 1 1 d . . . H35A H 0.3437 0.4415 0.7396 0.054 Uiso 1 1 calc R . . C36 C 0.4600(2) 0.4148(2) 0.75366(11) 0.0616(10) Uani 1 1 d . . . H36A H 0.4669 0.4619 0.7823 0.074 Uiso 1 1 calc R . . C37 C 0.52180(18) 0.3589(3) 0.73771(12) 0.0612(9) Uani 1 1 d U . . H37A H 0.5717 0.3688 0.7548 0.073 Uiso 1 1 calc R . . C38 C 0.51223(15) 0.2887(3) 0.69718(11) 0.0530(8) Uani 1 1 d . . . H38A H 0.5549 0.2476 0.6870 0.064 Uiso 1 1 calc R . . C39 C 0.43952(13) 0.2780(2) 0.67101(9) 0.0380(6) Uani 1 1 d . . . H39A H 0.4331 0.2306 0.6424 0.046 Uiso 1 1 calc R . . P40 P 0.36168(3) 0.45898(4) 0.552510(19) 0.01725(11) Uani 1 1 d . . . C41 C 0.42221(11) 0.34518(15) 0.53005(8) 0.0207(4) Uani 1 1 d . . . H41A H 0.4394 0.3603 0.4963 0.025 Uiso 1 1 calc R . . H41B H 0.4673 0.3278 0.5542 0.025 Uiso 1 1 calc R . . P42 P 0.34640(3) 0.23674(4) 0.52872(2) 0.01910(11) Uani 1 1 d . . . C43 C 0.42103(11) 0.52915(16) 0.60289(7) 0.0199(4) Uani 1 1 d . . . C44 C 0.38564(12) 0.60248(17) 0.63399(8) 0.0260(5) Uani 1 1 d . . . H44A H 0.3314 0.6142 0.6290 0.031 Uiso 1 1 calc R . . C45 C 0.42871(13) 0.65852(18) 0.67220(8) 0.0320(5) Uani 1 1 d . . . H45A H 0.4042 0.7094 0.6929 0.038 Uiso 1 1 calc R . . C46 C 0.50758(13) 0.64042(18) 0.68020(8) 0.0311(5) Uani 1 1 d . . . H46A H 0.5370 0.6770 0.7071 0.037 Uiso 1 1 calc R . . C47 C 0.54326(13) 0.56932(18) 0.64904(8) 0.0303(5) Uani 1 1 d . . . H47A H 0.5976 0.5583 0.6540 0.036 Uiso 1 1 calc R . . C48 C 0.50030(12) 0.51346(17) 0.61026(8) 0.0246(5) Uani 1 1 d . . . H48A H 0.5253 0.4646 0.5888 0.030 Uiso 1 1 calc R . . C49 C 0.35673(11) 0.56549(17) 0.50305(7) 0.0213(4) Uani 1 1 d . . . C50 C 0.37394(12) 0.67741(17) 0.51408(9) 0.0292(5) Uani 1 1 d . . . H50A H 0.3930 0.6985 0.5472 0.035 Uiso 1 1 calc R . . C51 C 0.36302(14) 0.7576(2) 0.47644(10) 0.0384(6) Uani 1 1 d . . . H51A H 0.3740 0.8334 0.4842 0.046 Uiso 1 1 calc R . . C52 C 0.33661(14) 0.7283(2) 0.42822(10) 0.0417(6) Uani 1 1 d . . . H52A H 0.3297 0.7836 0.4027 0.050 Uiso 1 1 calc R . . C53 C 0.32013(14) 0.6182(2) 0.41686(9) 0.0382(6) Uani 1 1 d . . . H53A H 0.3019 0.5977 0.3835 0.046 Uiso 1 1 calc R . . C54 C 0.33004(12) 0.53767(19) 0.45405(8) 0.0276(5) Uani 1 1 d . . . H54A H 0.3184 0.4622 0.4459 0.033 Uiso 1 1 calc R . . C55 C 0.39001(12) 0.11429(17) 0.56006(8) 0.0231(4) Uani 1 1 d . . . C56 C 0.46524(13) 0.08457(19) 0.55315(9) 0.0331(5) Uani 1 1 d . . . H56A H 0.4945 0.1285 0.5321 0.040 Uiso 1 1 calc R . . C57 C 0.49810(14) -0.0088(2) 0.57679(10) 0.0394(6) Uani 1 1 d . . . H57A H 0.5502 -0.0279 0.5726 0.047 Uiso 1 1 calc R . . C58 C 0.45508(14) -0.07413(19) 0.60646(9) 0.0381(6) Uani 1 1 d . . . H58A H 0.4775 -0.1386 0.6224 0.046 Uiso 1 1 calc R . . C59 C 0.37947(15) -0.04597(19) 0.61302(9) 0.0388(6) Uani 1 1 d . . . H59A H 0.3497 -0.0913 0.6332 0.047 Uiso 1 1 calc R . . C60 C 0.34723(13) 0.04901(18) 0.58997(9) 0.0310(5) Uani 1 1 d . . . H60A H 0.2955 0.0691 0.5948 0.037 Uiso 1 1 calc R . . C61 C 0.32910(12) 0.18484(16) 0.46430(8) 0.0221(4) Uani 1 1 d . . . C62 C 0.35911(13) 0.23243(17) 0.42295(8) 0.0276(5) Uani 1 1 d . . . H62A H 0.3913 0.2962 0.4273 0.033 Uiso 1 1 calc R . . C63 C 0.34272(14) 0.18808(19) 0.37530(9) 0.0362(6) Uani 1 1 d . . . H63A H 0.3636 0.2218 0.3472 0.043 Uiso 1 1 calc R . . C64 C 0.29640(15) 0.0953(2) 0.36818(9) 0.0408(6) Uani 1 1 d . . . H64A H 0.2857 0.0644 0.3355 0.049 Uiso 1 1 calc R . . C65 C 0.26559(15) 0.0477(2) 0.40920(10) 0.0421(6) Uani 1 1 d . . . H65A H 0.2331 -0.0158 0.4045 0.051 Uiso 1 1 calc R . . C66 C 0.28145(13) 0.09116(18) 0.45671(9) 0.0323(5) Uani 1 1 d . . . H66A H 0.2600 0.0575 0.4846 0.039 Uiso 1 1 calc R . . P1 P 0.24067(12) 0.69772(14) 0.78421(5) 0.0299(4) Uani 0.870(7) 1 d PDU B 1 F1 F 0.31677(12) 0.6366(3) 0.80855(9) 0.0606(7) Uani 0.870(7) 1 d PD B 1 F2 F 0.2796(2) 0.81375(15) 0.79984(8) 0.0614(11) Uani 0.870(7) 1 d PD B 1 F3 F 0.20600(19) 0.6893(3) 0.83707(9) 0.0642(8) Uani 0.870(7) 1 d PD B 1 F4 F 0.2033(2) 0.58007(16) 0.76828(9) 0.0614(7) Uani 0.870(7) 1 d PD B 1 F5 F 0.27711(13) 0.7043(4) 0.73175(7) 0.0642(8) Uani 0.870(7) 1 d PD B 1 F6 F 0.16569(18) 0.7588(3) 0.76011(10) 0.0614(8) Uani 0.870(7) 1 d PD B 1 P1' P 0.2327(7) 0.7067(10) 0.7848(5) 0.044(4) Uiso 0.130(7) 1 d PDU B 2 F1' F 0.3160(6) 0.6840(13) 0.8126(4) 0.036(4) Uiso 0.130(7) 1 d PD B 2 F2' F 0.2321(9) 0.8275(7) 0.8094(4) 0.035(4) Uiso 0.130(7) 1 d PD B 2 F3' F 0.1931(9) 0.6592(13) 0.8319(5) 0.051(6) Uiso 0.130(7) 1 d PD B 2 F4' F 0.2336(9) 0.5862(9) 0.7609(5) 0.041(4) Uiso 0.130(7) 1 d PD B 2 F5' F 0.2712(8) 0.7569(12) 0.7378(4) 0.047(5) Uiso 0.130(7) 1 d PD B 2 F6' F 0.1496(7) 0.7293(12) 0.7575(6) 0.036(5) Uiso 0.130(7) 1 d PD B 2 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 0.01522(8) 0.01511(8) 0.01909(8) -0.00046(7) 0.00115(6) 0.00006(7) S1 0.0241(3) 0.0232(3) 0.0244(3) -0.0035(2) -0.0044(2) 0.0027(2) C2 0.0183(11) 0.0224(11) 0.0364(12) -0.0128(10) 0.0023(9) 0.0038(9) S3 0.0215(3) 0.0210(3) 0.0382(3) -0.0042(2) 0.0043(2) -0.0043(2) N4 0.0218(10) 0.0309(11) 0.0503(13) -0.0191(10) -0.0033(9) -0.0005(8) C5 0.0296(14) 0.0487(16) 0.0602(17) -0.0195(14) 0.0028(12) -0.0064(12) C6 0.0381(16) 0.0488(17) 0.0597(18) -0.0113(14) -0.0037(13) -0.0071(13) O7 0.0447(12) 0.0426(11) 0.0709(13) -0.0102(10) 0.0057(10) 0.0013(9) C8 0.076(2) 0.0451(18) 0.094(3) -0.0259(18) 0.033(2) -0.0088(16) C9 0.0377(15) 0.0441(15) 0.0453(15) -0.0140(13) -0.0188(12) 0.0077(12) C10 0.076(2) 0.0526(18) 0.0445(17) -0.0081(14) -0.0074(15) 0.0039(16) O11 0.137(3) 0.0584(19) 0.0486(15) -0.0237(13) 0.0104(16) -0.0134(16) C12 0.140(5) 0.111(3) 0.044(2) -0.026(2) 0.007(2) 0.024(3) P13 0.0180(3) 0.0198(3) 0.0213(3) -0.0019(2) 0.0018(2) 0.0013(2) C14 0.0307(12) 0.0236(11) 0.0230(11) 0.0001(9) 0.0013(9) 0.0027(9) P15 0.0254(3) 0.0204(3) 0.0210(3) 0.0031(2) 0.0014(2) 0.0013(2) C16 0.0168(10) 0.0207(10) 0.0298(11) -0.0013(9) -0.0059(8) 0.0013(8) C17 0.0223(11) 0.0249(12) 0.0406(13) 0.0026(10) 0.0023(9) 0.0023(9) C18 0.0288(14) 0.0349(14) 0.0676(19) 0.0176(14) 0.0023(12) 0.0004(11) C19 0.0329(14) 0.0201(12) 0.089(2) 0.0019(15) -0.0104(14) -0.0009(11) C20 0.0453(16) 0.0297(14) 0.0618(19) -0.0207(13) -0.0184(14) 0.0079(12) C21 0.0346(13) 0.0320(13) 0.0328(13) -0.0089(10) -0.0077(10) 0.0070(10) C22 0.0228(11) 0.0190(11) 0.0402(13) -0.0007(9) 0.0104(10) 0.0027(9) C23 0.0204(12) 0.0253(12) 0.0539(15) -0.0108(11) 0.0030(10) 0.0025(9) C24 0.0237(14) 0.0311(14) 0.098(2) -0.0186(15) -0.0047(15) 0.0006(11) C25 0.0242(15) 0.0361(15) 0.125(3) 0.0074(18) 0.0199(18) 0.0004(12) C26 0.0408(18) 0.074(2) 0.089(3) 0.021(2) 0.0389(18) 0.0089(16) C27 0.0360(16) 0.069(2) 0.0503(16) 0.0060(15) 0.0198(13) 0.0070(14) C28 0.0424(15) 0.0199(11) 0.0265(12) 0.0015(9) 0.0112(10) -0.0012(10) C29 0.0474(16) 0.0329(14) 0.0429(15) 0.0031(11) 0.0163(12) -0.0030(12) C30 0.0592(19) 0.0427(16) 0.0616(19) -0.0007(15) 0.0300(15) -0.0157(14) C31 0.094(3) 0.0335(16) 0.0513(18) 0.0071(14) 0.0321(17) -0.0162(16) C32 0.090(3) 0.0345(16) 0.0542(18) 0.0217(14) 0.0150(17) 0.0008(16) C33 0.0591(18) 0.0360(15) 0.0407(15) 0.0127(12) 0.0063(13) -0.0003(13) C34 0.0335(13) 0.0274(12) 0.0258(11) 0.0122(10) -0.0071(9) -0.0040(10) C35 0.0631(19) 0.0307(14) 0.0372(14) 0.0065(11) -0.0213(13) 0.0033(12) C36 0.092(3) 0.0337(15) 0.0500(18) 0.0149(13) -0.0437(17) -0.0138(16) C37 0.0532(18) 0.0532(18) 0.070(2) 0.0412(16) -0.0320(15) -0.0183(15) C38 0.0321(15) 0.071(2) 0.0547(18) 0.0389(16) -0.0061(13) -0.0052(14) C39 0.0288(13) 0.0504(16) 0.0339(13) 0.0187(12) -0.0013(10) 0.0002(11) P40 0.0162(3) 0.0155(2) 0.0199(3) 0.0002(2) 0.00066(19) 0.0000(2) C41 0.0184(10) 0.0163(10) 0.0274(11) -0.0032(9) 0.0018(8) 0.0006(8) P42 0.0179(3) 0.0156(3) 0.0241(3) -0.0002(2) 0.0034(2) 0.0009(2) C43 0.0208(11) 0.0157(10) 0.0229(10) 0.0030(8) 0.0007(8) -0.0042(8) C44 0.0224(11) 0.0241(11) 0.0319(12) -0.0036(9) 0.0052(9) -0.0047(9) C45 0.0374(13) 0.0273(12) 0.0325(12) -0.0092(10) 0.0092(10) -0.0081(11) C46 0.0371(13) 0.0294(12) 0.0252(11) -0.0012(10) -0.0067(9) -0.0120(10) C47 0.0232(12) 0.0293(12) 0.0369(13) 0.0020(10) -0.0061(10) -0.0037(10) C48 0.0221(11) 0.0229(11) 0.0285(11) -0.0004(9) 0.0001(9) -0.0001(9) C49 0.0164(10) 0.0235(11) 0.0245(11) 0.0056(9) 0.0048(8) 0.0032(8) C50 0.0259(12) 0.0260(12) 0.0359(13) 0.0076(10) 0.0028(10) -0.0026(9) C51 0.0316(14) 0.0273(13) 0.0568(17) 0.0151(12) 0.0059(12) -0.0007(10) C52 0.0369(15) 0.0466(16) 0.0428(15) 0.0272(13) 0.0105(12) 0.0110(12) C53 0.0339(14) 0.0534(16) 0.0276(12) 0.0139(12) 0.0036(10) 0.0097(12) C54 0.0238(12) 0.0316(12) 0.0278(11) 0.0024(10) 0.0048(9) 0.0038(9) C55 0.0248(11) 0.0172(10) 0.0275(11) 0.0003(9) 0.0025(9) 0.0030(8) C56 0.0304(13) 0.0276(12) 0.0428(14) 0.0074(11) 0.0122(10) 0.0071(10) C57 0.0311(14) 0.0359(14) 0.0518(15) 0.0089(12) 0.0075(11) 0.0146(11) C58 0.0423(15) 0.0265(12) 0.0444(15) 0.0093(11) -0.0035(11) 0.0096(11) C59 0.0407(15) 0.0296(13) 0.0465(15) 0.0142(11) 0.0059(12) -0.0007(11) C60 0.0266(12) 0.0270(12) 0.0397(13) 0.0038(10) 0.0054(10) 0.0021(10) C61 0.0198(11) 0.0172(10) 0.0295(11) -0.0054(9) 0.0032(9) 0.0043(8) C62 0.0324(13) 0.0195(11) 0.0308(12) -0.0028(9) 0.0024(10) 0.0017(9) C63 0.0477(16) 0.0331(13) 0.0277(12) -0.0034(10) 0.0029(11) 0.0030(11) C64 0.0491(16) 0.0414(15) 0.0309(13) -0.0158(12) -0.0014(11) 0.0034(12) C65 0.0417(16) 0.0348(14) 0.0501(16) -0.0192(12) 0.0050(12) -0.0088(11) C66 0.0315(13) 0.0271(12) 0.0394(13) -0.0092(11) 0.0088(10) -0.0055(10) P1 0.0412(7) 0.0275(5) 0.0208(5) -0.0013(3) 0.0020(3) 0.0005(4) F1 0.0556(14) 0.0452(17) 0.0774(16) 0.0122(12) -0.0134(10) 0.0072(10) F2 0.098(3) 0.0355(11) 0.0478(12) 0.0022(9) -0.0127(13) -0.0188(11) F3 0.0787(18) 0.087(2) 0.0287(11) 0.0056(12) 0.0156(10) -0.0083(17) F4 0.0647(19) 0.0467(12) 0.0732(15) -0.0183(10) 0.0082(13) -0.0181(11) F5 0.0585(14) 0.105(2) 0.0314(10) -0.0059(12) 0.0158(9) -0.0139(14) F6 0.0559(16) 0.0688(19) 0.0579(15) 0.0077(13) -0.0034(12) 0.0196(15) _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 P40 2.3207(5) . ? Ru P42 2.3233(5) . ? Ru P15 2.3344(5) . ? Ru P13 2.3541(5) . ? Ru S1 2.4237(5) . ? Ru S3 2.4351(5) . ? S1 C2 1.704(2) . ? C2 N4 1.340(3) . ? C2 S3 1.717(2) . ? N4 C5 1.448(3) . ? N4 C9 1.480(3) . ? C5 C6 1.516(3) . ? C6 O7 1.406(3) . ? O7 C8 1.427(3) . ? C9 C10 1.517(4) . ? C10 O11 1.385(3) . ? C10 O11' 1.404(14) . ? O11 C12 1.406(4) . ? O11' C12' 1.378(16) . ? P13 C16 1.824(2) . ? P13 C22 1.824(2) . ? P13 C14 1.841(2) . ? C14 P15 1.846(2) . ? P15 C34 1.831(2) . ? P15 C28 1.832(2) . ? C16 C17 1.387(3) . ? C16 C21 1.393(3) . ? C17 C18 1.386(3) . ? C18 C19 1.374(4) . ? C19 C20 1.372(4) . ? C20 C21 1.383(3) . ? C22 C23 1.383(3) . ? C22 C27 1.388(3) . ? C23 C24 1.386(3) . ? C24 C25 1.368(4) . ? C25 C26 1.355(5) . ? C26 C27 1.399(4) . ? C28 C29 1.390(3) . ? C28 C33 1.391(3) . ? C29 C30 1.396(3) . ? C30 C31 1.366(4) . ? C31 C32 1.364(4) . ? C32 C33 1.390(4) . ? C34 C39 1.380(3) . ? C34 C35 1.384(3) . ? C35 C36 1.398(4) . ? C36 C37 1.366(5) . ? C37 C38 1.368(4) . ? C38 C39 1.393(3) . ? P40 C43 1.824(2) . ? P40 C49 1.833(2) . ? P40 C41 1.8561(19) . ? C41 P42 1.8505(19) . ? P42 C55 1.823(2) . ? P42 C61 1.826(2) . ? C43 C48 1.387(3) . ? C43 C44 1.390(3) . ? C44 C45 1.383(3) . ? C45 C46 1.385(3) . ? C46 C47 1.377(3) . ? C47 C48 1.392(3) . ? C49 C54 1.386(3) . ? C49 C50 1.403(3) . ? C50 C51 1.391(3) . ? C51 C52 1.371(4) . ? C52 C53 1.381(4) . ? C53 C54 1.385(3) . ? C55 C60 1.381(3) . ? C55 C56 1.383(3) . ? C56 C57 1.384(3) . ? C57 C58 1.380(3) . ? C58 C59 1.383(3) . ? C59 C60 1.390(3) . ? C61 C62 1.384(3) . ? C61 C66 1.401(3) . ? C62 C63 1.383(3) . ? C63 C64 1.378(3) . ? C64 C65 1.383(4) . ? C65 C66 1.374(3) . ? P1 F6 1.580(2) . ? P1 F3 1.584(2) . ? P1 F5 1.587(2) . ? P1 F2 1.588(2) . ? P1 F4 1.597(2) . ? P1 F1 1.598(2) . ? P1' F6' 1.580(12) . ? P1' F4' 1.583(11) . ? P1' F3' 1.588(12) . ? P1' F1' 1.589(12) . ? P1' F5' 1.592(12) . ? P1' F2' 1.593(11) . ? 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 P40 Ru P42 72.660(18) . . ? P40 Ru P15 96.313(19) . . ? P42 Ru P15 103.630(19) . . ? P40 Ru P13 101.890(19) . . ? P42 Ru P13 172.657(19) . . ? P15 Ru P13 71.696(19) . . ? P40 Ru S1 96.638(19) . . ? P42 Ru S1 90.607(19) . . ? P15 Ru S1 163.09(2) . . ? P13 Ru S1 94.975(18) . . ? P40 Ru S3 160.08(2) . . ? P42 Ru S3 91.142(19) . . ? P15 Ru S3 98.79(2) . . ? P13 Ru S3 95.152(19) . . ? S1 Ru S3 71.444(19) . . ? C2 S1 Ru 88.59(8) . . ? N4 C2 S1 122.50(18) . . ? N4 C2 S3 125.40(18) . . ? S1 C2 S3 112.03(12) . . ? C2 S3 Ru 87.92(7) . . ? C2 N4 C5 121.7(2) . . ? C2 N4 C9 119.8(2) . . ? C5 N4 C9 117.2(2) . . ? N4 C5 C6 114.4(2) . . ? O7 C6 C5 108.0(2) . . ? C6 O7 C8 109.2(2) . . ? N4 C9 C10 116.2(2) . . ? O11 C10 O11' 48.0(12) . . ? O11 C10 C9 110.2(3) . . ? O11' C10 C9 107.6(10) . . ? C10 O11 C12 114.3(3) . . ? C12' O11' C10 122(2) . . ? C16 P13 C22 102.15(9) . . ? C16 P13 C14 107.05(9) . . ? C22 P13 C14 106.85(10) . . ? C16 P13 Ru 122.96(7) . . ? C22 P13 Ru 120.98(7) . . ? C14 P13 Ru 94.92(7) . . ? P13 C14 P15 96.28(10) . . ? C34 P15 C28 102.21(10) . . ? C34 P15 C14 105.87(10) . . ? C28 P15 C14 103.88(10) . . ? C34 P15 Ru 126.48(8) . . ? C28 P15 Ru 119.64(7) . . ? C14 P15 Ru 95.43(7) . . ? C17 C16 C21 119.2(2) . . ? C17 C16 P13 119.86(16) . . ? C21 C16 P13 120.90(17) . . ? C18 C17 C16 120.1(2) . . ? C19 C18 C17 119.8(3) . . ? C20 C19 C18 120.9(2) . . ? C19 C20 C21 119.7(3) . . ? C20 C21 C16 120.2(2) . . ? C23 C22 C27 118.4(2) . . ? C23 C22 P13 118.03(17) . . ? C27 C22 P13 123.61(19) . . ? C22 C23 C24 121.0(3) . . ? C25 C24 C23 120.1(3) . . ? C26 C25 C24 119.8(3) . . ? C25 C26 C27 121.1(3) . . ? C22 C27 C26 119.6(3) . . ? C29 C28 C33 119.0(2) . . ? C29 C28 P15 118.95(18) . . ? C33 C28 P15 122.05(19) . . ? C28 C29 C30 120.0(3) . . ? C31 C30 C29 120.3(3) . . ? C32 C31 C30 120.1(3) . . ? C31 C32 C33 120.9(3) . . ? C32 C33 C28 119.7(3) . . ? C39 C34 C35 118.8(2) . . ? C39 C34 P15 120.12(18) . . ? C35 C34 P15 121.03(19) . . ? C34 C35 C36 119.8(3) . . ? C37 C36 C35 120.5(3) . . ? C36 C37 C38 120.3(3) . . ? C37 C38 C39 119.5(3) . . ? C34 C39 C38 121.0(3) . . ? C43 P40 C49 101.16(9) . . ? C43 P40 C41 106.15(9) . . ? C49 P40 C41 105.89(9) . . ? C43 P40 Ru 125.29(7) . . ? C49 P40 Ru 120.40(7) . . ? C41 P40 Ru 95.54(6) . . ? P42 C41 P40 95.85(9) . . ? C55 P42 C61 100.48(9) . . ? C55 P42 C41 107.06(9) . . ? C61 P42 C41 108.40(9) . . ? C55 P42 Ru 123.37(7) . . ? C61 P42 Ru 120.65(7) . . ? C41 P42 Ru 95.61(6) . . ? C48 C43 C44 119.23(18) . . ? C48 C43 P40 122.03(16) . . ? C44 C43 P40 118.71(15) . . ? C45 C44 C43 120.5(2) . . ? C44 C45 C46 120.0(2) . . ? C47 C46 C45 119.8(2) . . ? C46 C47 C48 120.4(2) . . ? C43 C48 C47 120.0(2) . . ? C54 C49 C50 118.38(19) . . ? C54 C49 P40 119.92(16) . . ? C50 C49 P40 121.53(16) . . ? C51 C50 C49 120.0(2) . . ? C52 C51 C50 120.7(2) . . ? C51 C52 C53 119.8(2) . . ? C52 C53 C54 120.2(2) . . ? C53 C54 C49 121.0(2) . . ? C60 C55 C56 119.6(2) . . ? C60 C55 P42 119.97(16) . . ? C56 C55 P42 120.43(17) . . ? C55 C56 C57 120.3(2) . . ? C58 C57 C56 119.9(2) . . ? C57 C58 C59 120.2(2) . . ? C58 C59 C60 119.7(2) . . ? C55 C60 C59 120.3(2) . . ? C62 C61 C66 118.5(2) . . ? C62 C61 P42 124.42(16) . . ? C66 C61 P42 117.10(16) . . ? C63 C62 C61 120.7(2) . . ? C64 C63 C62 120.5(2) . . ? C63 C64 C65 119.2(2) . . ? C66 C65 C64 120.7(2) . . ? C65 C66 C61 120.4(2) . . ? F6 P1 F3 91.48(15) . . ? F6 P1 F5 89.91(14) . . ? F3 P1 F5 178.60(19) . . ? F6 P1 F2 90.89(17) . . ? F3 P1 F2 90.58(16) . . ? F5 P1 F2 89.62(15) . . ? F6 P1 F4 90.11(17) . . ? F3 P1 F4 90.10(17) . . ? F5 P1 F4 89.68(15) . . ? F2 P1 F4 178.8(2) . . ? F6 P1 F1 179.68(19) . . ? F3 P1 F1 88.65(14) . . ? F5 P1 F1 89.97(15) . . ? F2 P1 F1 88.82(14) . . ? F4 P1 F1 90.18(14) . . ? F6' P1' F4' 90.8(7) . . ? F6' P1' F3' 89.0(8) . . ? F4' P1' F3' 90.6(7) . . ? F6' P1' F1' 179.6(10) . . ? F4' P1' F1' 89.4(7) . . ? F3' P1' F1' 90.7(8) . . ? F6' P1' F5' 90.2(7) . . ? F4' P1' F5' 90.5(7) . . ? F3' P1' F5' 178.6(10) . . ? F1' P1' F5' 90.1(7) . . ? F6' P1' F2' 89.6(7) . . ? F4' P1' F2' 179.5(10) . . ? F3' P1' F2' 89.1(7) . . ? F1' P1' F2' 90.2(7) . . ? F5' P1' F2' 89.8(7) . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.617 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.065 #===END data_15 _database_code_depnum_ccdc_archive 'CCDC 750275' #TrackingRef 'DT_Wilton-Ely_amine_terminated.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H53 N O3 P2 Ru S2, 0.3(C H2 Cl2)' _chemical_formula_sum 'C53.30 H53.60 Cl0.60 N O3 P2 Ru S2' _chemical_formula_weight 1004.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9999(3) _cell_length_b 15.2412(3) _cell_length_c 15.3608(4) _cell_angle_alpha 111.203(2) _cell_angle_beta 106.398(2) _cell_angle_gamma 95.0213(18) _cell_volume 2455.53(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23800 _cell_measurement_theta_min 3.1783 _cell_measurement_theta_max 72.3769 _exptl_crystal_description 'platy needles' _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1041 _exptl_absorpt_coefficient_mu 4.631 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.832 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33789 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 72.65 _reflns_number_total 9694 _reflns_number_gt 8842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0418P)^2^+0.8571P] 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 9694 _refine_ls_number_parameters 629 _refine_ls_number_restraints 142 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _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 0.191032(10) 0.672071(9) 0.287367(9) 0.02152(5) Uani 1 1 d . . . P1 P 0.01802(4) 0.67930(3) 0.33272(3) 0.02183(9) Uani 1 1 d . . . P2 P 0.35544(4) 0.67203(3) 0.23097(3) 0.02411(9) Uani 1 1 d . . . S1 S 0.29088(4) 0.60857(3) 0.41085(3) 0.03022(10) Uani 1 1 d . . . C2 C 0.35538(15) 0.72534(14) 0.49165(13) 0.0272(3) Uani 1 1 d . . . S3 S 0.30999(4) 0.80734(3) 0.44520(3) 0.02667(9) Uani 1 1 d . . . N4 N 0.43398(14) 0.74912(12) 0.58207(12) 0.0320(3) Uani 1 1 d D A . C5 C 0.46347(18) 0.67453(17) 0.61853(15) 0.0375(4) Uani 1 1 d D A . H5A H 0.3917 0.6227 0.5916 0.045 Uiso 1 1 calc R . . H5B H 0.4860 0.7029 0.6917 0.045 Uiso 1 1 calc R . . C6 C 0.56295(19) 0.63089(16) 0.59095(17) 0.0399(4) Uani 1 1 d D . . H6A H 0.5668 0.5722 0.6044 0.048 Uiso 0.86(3) 1 calc PR A 1 H6B H 0.5485 0.6125 0.5193 0.048 Uiso 0.86(3) 1 calc PR A 1 H6C H 0.5412 0.6034 0.5200 0.048 Uiso 0.14(3) 1 d PR A 2 H6D H 0.5734 0.5798 0.6131 0.048 Uiso 0.14(3) 1 d PR A 2 O7 O 0.6715(2) 0.6993(3) 0.6476(7) 0.0477(13) Uani 0.86(3) 1 d PDU A 1 C8 C 0.7683(4) 0.6595(3) 0.6245(10) 0.0633(19) Uani 0.86(3) 1 d PDU A 1 H8A H 0.8434 0.7055 0.6680 0.095 Uiso 0.86(3) 1 calc PR A 1 H8B H 0.7592 0.6462 0.5552 0.095 Uiso 0.86(3) 1 calc PR A 1 H8C H 0.7687 0.5995 0.6343 0.095 Uiso 0.86(3) 1 calc PR A 1 O7' O 0.6718(12) 0.692(2) 0.638(4) 0.056(8) Uiso 0.14(3) 1 d PDU A 2 C8' C 0.7747(14) 0.653(3) 0.655(2) 0.057(7) Uiso 0.14(3) 1 d PDU A 2 H8'A H 0.8457 0.7052 0.6840 0.085 Uiso 0.14(3) 1 calc PR A 2 H8'B H 0.7753 0.6056 0.5922 0.085 Uiso 0.14(3) 1 calc PR A 2 H8'C H 0.7742 0.6226 0.7010 0.085 Uiso 0.14(3) 1 calc PR A 2 C9 C 0.4942(2) 0.84966(17) 0.64554(16) 0.0427(5) Uani 1 1 d D . . H9A H 0.5103 0.8812 0.6029 0.051 Uiso 0.569(3) 1 calc PR B -1 H9B H 0.5719 0.8504 0.6908 0.051 Uiso 0.569(3) 1 calc PR B -1 H9C H 0.4889 0.8852 0.6046 0.051 Uiso 0.346(5) 1 d PR C -2 H9D H 0.5769 0.8521 0.6757 0.051 Uiso 0.346(5) 1 d PR C -2 H9E H 0.5186 0.8806 0.6075 0.051 Uiso 0.085(4) 1 d PR D -3 H9F H 0.5631 0.8533 0.6981 0.051 Uiso 0.085(4) 1 d PR D -3 C10 C 0.4278(7) 0.9093(4) 0.7075(4) 0.0523(15) Uani 0.569(3) 1 d PDU B -1 H10A H 0.4704 0.9776 0.7399 0.063 Uiso 0.569(3) 1 calc PR B -1 H10B H 0.3474 0.9053 0.6638 0.063 Uiso 0.569(3) 1 calc PR B -1 O11 O 0.4179(4) 0.8774(3) 0.7794(2) 0.0523(8) Uani 0.569(3) 1 d PDU B -1 C12 C 0.3545(6) 0.9308(5) 0.8396(4) 0.0697(15) Uani 0.569(3) 1 d PDU B -1 H12A H 0.3412 0.8994 0.8824 0.105 Uiso 0.569(3) 1 calc PR B -1 H12B H 0.2778 0.9330 0.7968 0.105 Uiso 0.569(3) 1 calc PR B -1 H12C H 0.4012 0.9965 0.8807 0.105 Uiso 0.569(3) 1 calc PR B -1 C10' C 0.4369(14) 0.8920(10) 0.7244(8) 0.085(5) Uiso 0.346(5) 1 d PDU B -2 H10C H 0.4641 0.9629 0.7556 0.102 Uiso 0.346(5) 1 calc PR C -2 H10D H 0.3495 0.8770 0.6921 0.102 Uiso 0.346(5) 1 calc PR C -2 O11' O 0.4638(6) 0.8575(5) 0.7956(5) 0.0617(19) Uiso 0.346(5) 1 d PDU B -2 C12' C 0.5811(8) 0.8894(8) 0.8659(7) 0.072(2) Uiso 0.346(5) 1 d PDU B -2 H12D H 0.5884 0.8577 0.9120 0.108 Uiso 0.346(5) 1 calc PR C -2 H12E H 0.5972 0.9593 0.9029 0.108 Uiso 0.346(5) 1 calc PR C -2 H12F H 0.6383 0.8730 0.8311 0.108 Uiso 0.346(5) 1 calc PR C -2 C10" C 0.407(2) 0.907(2) 0.6853(17) 0.051(8) Uiso 0.085(4) 1 d PDU B -3 H10E H 0.3859 0.9476 0.6477 0.061 Uiso 0.085(4) 1 calc PR D -3 H10F H 0.3334 0.8601 0.6675 0.061 Uiso 0.085(4) 1 calc PR D -3 O11" O 0.4354(15) 0.9634(12) 0.7795(11) 0.045(5) Uiso 0.085(4) 1 d PDU B -3 C12" C 0.358(3) 0.990(3) 0.832(2) 0.059(6) Uiso 0.085(4) 1 d PDU B -3 H12G H 0.4037 1.0322 0.9017 0.088 Uiso 0.085(4) 1 calc PR D -3 H12H H 0.3118 0.9321 0.8298 0.088 Uiso 0.085(4) 1 calc PR D -3 H12I H 0.3038 1.0241 0.8031 0.088 Uiso 0.085(4) 1 calc PR D -3 C13 C 0.13135(16) 0.76329(13) 0.21916(13) 0.0267(3) Uani 1 1 d . E . H13A H 0.0735 0.7333 0.1546 0.032 Uiso 1 1 calc R . . C14 C 0.16489(17) 0.85846(14) 0.25565(15) 0.0323(4) Uani 1 1 d D . . H14A H 0.2303 0.8897 0.3157 0.039 Uiso 0.670(12) 1 calc PR E 1 H14B H 0.2290 0.8857 0.3180 0.039 Uiso 0.330(12) 1 d PR E 2 C15 C 0.1026(4) 0.9213(2) 0.2052(3) 0.0355(11) Uani 0.670(12) 1 d PGDU E 1 C16 C -0.0146(4) 0.8915(3) 0.1415(3) 0.0407(9) Uani 0.670(12) 1 d PGU E 1 H16A H -0.0583 0.8291 0.1245 0.049 Uiso 0.670(12) 1 calc PR E 1 C17 C -0.0678(5) 0.9528(3) 0.1026(3) 0.0464(11) Uani 0.670(12) 1 d PGU E 1 H17A H -0.1479 0.9325 0.0591 0.056 Uiso 0.670(12) 1 calc PR E 1 C18 C -0.0037(6) 1.0441(3) 0.1275(4) 0.0461(14) Uani 0.670(12) 1 d PGDU E 1 C19 C 0.1135(6) 1.0739(2) 0.1912(4) 0.0464(13) Uani 0.670(12) 1 d PGU E 1 H19A H 0.1573 1.1362 0.2082 0.056 Uiso 0.670(12) 1 calc PR E 1 C20 C 0.1667(5) 1.0125(2) 0.2300(4) 0.0415(10) Uani 0.670(12) 1 d PGU E 1 H20A H 0.2468 1.0329 0.2736 0.050 Uiso 0.670(12) 1 calc PR E 1 C21 C -0.0633(7) 1.1139(4) 0.0881(4) 0.0617(19) Uani 0.670(12) 1 d PDU E 1 H21A H -0.0971 1.1540 0.1358 0.093 Uiso 0.670(12) 1 calc PR E 1 H21B H -0.1267 1.0771 0.0243 0.093 Uiso 0.670(12) 1 calc PR E 1 H21C H -0.0040 1.1552 0.0791 0.093 Uiso 0.670(12) 1 calc PR E 1 C15' C 0.1255(8) 0.9283(5) 0.2205(7) 0.0263(18) Uiso 0.330(12) 1 d PGDU E 2 C16' C 0.0133(8) 0.9070(4) 0.1504(7) 0.0343(19) Uiso 0.330(12) 1 d PGU E 2 H16B H -0.0367 0.8452 0.1253 0.041 Uiso 0.330(12) 1 calc PR E 2 C17' C -0.0258(8) 0.9760(5) 0.1170(5) 0.043(2) Uiso 0.330(12) 1 d PGU E 2 H17B H -0.1025 0.9615 0.0690 0.051 Uiso 0.330(12) 1 calc PR E 2 C18' C 0.0474(9) 1.0664(5) 0.1537(6) 0.036(2) Uiso 0.330(12) 1 d PGDU E 2 C19' C 0.1596(8) 1.0877(4) 0.2239(7) 0.046(2) Uiso 0.330(12) 1 d PGU E 2 H19B H 0.2096 1.1494 0.2490 0.056 Uiso 0.330(12) 1 calc PR E 2 C20' C 0.1987(7) 1.0186(5) 0.2573(7) 0.047(2) Uiso 0.330(12) 1 d PGU E 2 H20B H 0.2754 1.0332 0.3052 0.056 Uiso 0.330(12) 1 calc PR E 2 C21' C 0.0004(11) 1.1449(7) 0.1205(8) 0.055(3) Uiso 0.330(12) 1 d PDU E 2 H21D H -0.0517 1.1732 0.1570 0.082 Uiso 0.330(12) 1 calc PR E 2 H21E H -0.0443 1.1159 0.0492 0.082 Uiso 0.330(12) 1 calc PR E 2 H21F H 0.0676 1.1953 0.1345 0.082 Uiso 0.330(12) 1 calc PR E 2 C22 C 0.10991(16) 0.55918(14) 0.17654(14) 0.0290(4) Uani 1 1 d . . . O22 O 0.06178(13) 0.48960(10) 0.10965(11) 0.0393(3) Uani 1 1 d . . . C23 C 0.03692(15) 0.77164(13) 0.45475(13) 0.0260(3) Uani 1 1 d . . . C24 C 0.0263(2) 0.74942(15) 0.53233(15) 0.0390(4) Uani 1 1 d . . . H24A H 0.0072 0.6840 0.5227 0.047 Uiso 1 1 calc R . . C25 C 0.0434(3) 0.82241(19) 0.62419(18) 0.0546(6) Uani 1 1 d . . . H25A H 0.0349 0.8065 0.6767 0.065 Uiso 1 1 calc R . . C26 C 0.0729(2) 0.91796(18) 0.63978(17) 0.0490(6) Uani 1 1 d . . . H26A H 0.0830 0.9676 0.7023 0.059 Uiso 1 1 calc R . . C27 C 0.08754(19) 0.94076(15) 0.56377(16) 0.0363(4) Uani 1 1 d . . . H27A H 0.1099 1.0062 0.5746 0.044 Uiso 1 1 calc R . . C28 C 0.06959(16) 0.86823(14) 0.47182(14) 0.0292(4) Uani 1 1 d . . . H28A H 0.0796 0.8844 0.4199 0.035 Uiso 1 1 calc R . . C29 C -0.10619(15) 0.70320(13) 0.24835(13) 0.0263(3) Uani 1 1 d . . . C30 C -0.16304(16) 0.77834(14) 0.27907(15) 0.0320(4) Uani 1 1 d . . . H30A H -0.1381 0.8205 0.3473 0.038 Uiso 1 1 calc R . . C31 C -0.25604(18) 0.79247(16) 0.21112(17) 0.0400(5) Uani 1 1 d . . . H31A H -0.2935 0.8447 0.2330 0.048 Uiso 1 1 calc R . . C32 C -0.29424(18) 0.73113(18) 0.11221(16) 0.0412(5) Uani 1 1 d . . . H32A H -0.3571 0.7416 0.0657 0.049 Uiso 1 1 calc R . . C33 C -0.24075(19) 0.65428(18) 0.08078(16) 0.0416(5) Uani 1 1 d . . . H33A H -0.2683 0.6108 0.0129 0.050 Uiso 1 1 calc R . . C34 C -0.14700(17) 0.64061(15) 0.14818(15) 0.0353(4) Uani 1 1 d . . . H34A H -0.1101 0.5881 0.1260 0.042 Uiso 1 1 calc R . . C35 C -0.05897(15) 0.56996(13) 0.33394(13) 0.0262(3) Uani 1 1 d . . . C36 C -0.17318(18) 0.56485(15) 0.33956(17) 0.0366(4) Uani 1 1 d . . . H36A H -0.2111 0.6174 0.3417 0.044 Uiso 1 1 calc R . . C37 C -0.23171(19) 0.48384(17) 0.34204(19) 0.0426(5) Uani 1 1 d . . . H37A H -0.3093 0.4812 0.3462 0.051 Uiso 1 1 calc R . . C38 C -0.1777(2) 0.40684(16) 0.33844(18) 0.0420(5) Uani 1 1 d . . . H38A H -0.2172 0.3517 0.3414 0.050 Uiso 1 1 calc R . . C39 C -0.0657(2) 0.41052(17) 0.3306(2) 0.0435(5) Uani 1 1 d . . . H39A H -0.0287 0.3572 0.3266 0.052 Uiso 1 1 calc R . . C40 C -0.00678(17) 0.49200(15) 0.32834(16) 0.0346(4) Uani 1 1 d . . . H40A H 0.0702 0.4939 0.3229 0.042 Uiso 1 1 calc R . . C41 C 0.49266(16) 0.75620(14) 0.32275(14) 0.0290(4) Uani 1 1 d . . . C42 C 0.50364(19) 0.85536(15) 0.34883(16) 0.0378(4) Uani 1 1 d . . . H42A H 0.4424 0.8786 0.3147 0.045 Uiso 1 1 calc R . . C43 C 0.6030(2) 0.91994(17) 0.42396(19) 0.0476(5) Uani 1 1 d . . . H43A H 0.6110 0.9869 0.4394 0.057 Uiso 1 1 calc R . . C44 C 0.6904(2) 0.88730(19) 0.47634(17) 0.0486(6) Uani 1 1 d . . . H44A H 0.7581 0.9318 0.5282 0.058 Uiso 1 1 calc R . . C45 C 0.67974(19) 0.79025(19) 0.45352(17) 0.0444(5) Uani 1 1 d . . . H45A H 0.7398 0.7680 0.4901 0.053 Uiso 1 1 calc R . . C46 C 0.58098(17) 0.72445(15) 0.37682(15) 0.0342(4) Uani 1 1 d . . . H46A H 0.5741 0.6575 0.3615 0.041 Uiso 1 1 calc R . . C47 C 0.33137(16) 0.69872(14) 0.12013(14) 0.0285(4) Uani 1 1 d . . . C48 C 0.40938(18) 0.76573(16) 0.11211(16) 0.0366(4) Uani 1 1 d . . . H48A H 0.4808 0.8006 0.1659 0.044 Uiso 1 1 calc R . . C49 C 0.3839(2) 0.78231(17) 0.02581(18) 0.0425(5) Uani 1 1 d . . . H49A H 0.4373 0.8292 0.0217 0.051 Uiso 1 1 calc R . . C50 C 0.2819(2) 0.73134(17) -0.05336(17) 0.0412(5) Uani 1 1 d . . . H50A H 0.2647 0.7431 -0.1119 0.049 Uiso 1 1 calc R . . C51 C 0.2047(2) 0.66295(19) -0.04719(17) 0.0447(5) Uani 1 1 d . . . H51A H 0.1352 0.6264 -0.1023 0.054 Uiso 1 1 calc R . . C52 C 0.22839(19) 0.64743(16) 0.03901(15) 0.0385(4) Uani 1 1 d . . . H52A H 0.1738 0.6012 0.0430 0.046 Uiso 1 1 calc R . . C53 C 0.40584(16) 0.55809(13) 0.19082(13) 0.0283(4) Uani 1 1 d . . . C54 C 0.49608(18) 0.55045(15) 0.14878(16) 0.0357(4) Uani 1 1 d . . . H54A H 0.5283 0.6032 0.1379 0.043 Uiso 1 1 calc R . . C55 C 0.53835(19) 0.46654(17) 0.12305(17) 0.0418(5) Uani 1 1 d . . . H55A H 0.5997 0.4619 0.0948 0.050 Uiso 1 1 calc R . . C56 C 0.4916(2) 0.38917(16) 0.13837(16) 0.0400(5) Uani 1 1 d . . . H56A H 0.5219 0.3320 0.1218 0.048 Uiso 1 1 calc R . . C57 C 0.40093(19) 0.39509(15) 0.17775(15) 0.0363(4) Uani 1 1 d . . . H57A H 0.3676 0.3416 0.1869 0.044 Uiso 1 1 calc R . . C58 C 0.35851(17) 0.47953(14) 0.20406(14) 0.0311(4) Uani 1 1 d . . . H58A H 0.2964 0.4834 0.2314 0.037 Uiso 1 1 calc R . . C60 C 0.6767(7) 0.9697(5) 0.9461(5) 0.0396(15) Uani 0.30 1 d P F 1 H60A H 0.6156 0.9785 0.8929 0.047 Uiso 0.30 1 calc PR F 1 H60B H 0.7556 1.0004 0.9508 0.047 Uiso 0.30 1 calc PR F 1 Cl1 Cl 0.6529(2) 1.02644(15) 1.06001(15) 0.0523(4) Uani 0.30 1 d P F 1 Cl2 Cl 0.6699(3) 0.84678(15) 0.91552(18) 0.0659(6) Uani 0.30 1 d P F 1 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 0.01924(7) 0.02172(7) 0.02233(7) 0.00790(5) 0.00662(5) 0.00385(5) P1 0.02024(19) 0.0231(2) 0.02260(19) 0.00931(16) 0.00767(15) 0.00524(15) P2 0.0206(2) 0.0245(2) 0.0263(2) 0.00875(17) 0.00892(16) 0.00407(16) S1 0.0298(2) 0.0269(2) 0.0298(2) 0.01249(17) 0.00357(17) 0.00346(17) C2 0.0213(8) 0.0340(9) 0.0265(8) 0.0119(7) 0.0093(7) 0.0047(7) S3 0.0248(2) 0.0253(2) 0.0259(2) 0.00778(16) 0.00663(16) 0.00422(15) N4 0.0276(8) 0.0374(9) 0.0271(7) 0.0127(7) 0.0055(6) 0.0026(6) C5 0.0321(10) 0.0488(12) 0.0329(10) 0.0233(9) 0.0055(8) 0.0039(9) C6 0.0388(11) 0.0370(11) 0.0400(11) 0.0177(9) 0.0058(9) 0.0044(9) O7 0.0293(14) 0.0360(14) 0.071(3) 0.0151(12) 0.0152(9) 0.0080(7) C8 0.0443(18) 0.0448(18) 0.114(5) 0.036(2) 0.039(2) 0.0199(13) C9 0.0399(11) 0.0411(11) 0.0312(10) 0.0091(9) -0.0013(8) -0.0003(9) C10 0.088(4) 0.042(3) 0.020(2) 0.003(2) 0.023(2) 0.004(2) O11 0.073(2) 0.061(2) 0.0336(15) 0.0244(14) 0.0243(15) 0.0204(18) C12 0.082(4) 0.086(4) 0.048(3) 0.024(3) 0.036(3) 0.016(3) C13 0.0262(8) 0.0319(9) 0.0267(8) 0.0140(7) 0.0122(7) 0.0087(7) C14 0.0327(9) 0.0315(9) 0.0359(10) 0.0151(8) 0.0142(8) 0.0076(8) C15 0.045(3) 0.0322(17) 0.037(2) 0.0163(16) 0.022(2) 0.0126(16) C16 0.043(2) 0.042(2) 0.045(2) 0.0219(17) 0.0189(18) 0.0167(17) C17 0.053(3) 0.056(2) 0.048(2) 0.0312(19) 0.024(2) 0.028(2) C18 0.066(4) 0.051(2) 0.046(2) 0.030(2) 0.035(3) 0.034(3) C19 0.067(4) 0.0315(18) 0.052(3) 0.0226(17) 0.028(3) 0.015(2) C20 0.053(2) 0.0316(17) 0.049(2) 0.0219(16) 0.022(2) 0.0139(16) C21 0.098(5) 0.064(3) 0.063(3) 0.046(3) 0.047(3) 0.053(3) C22 0.0229(8) 0.0369(10) 0.0355(10) 0.0194(9) 0.0143(7) 0.0102(7) O22 0.0344(7) 0.0320(7) 0.0362(7) 0.0014(6) 0.0084(6) -0.0013(6) C23 0.0239(8) 0.0285(9) 0.0246(8) 0.0091(7) 0.0083(6) 0.0075(7) C24 0.0536(12) 0.0318(10) 0.0304(10) 0.0117(8) 0.0150(9) 0.0039(9) C25 0.0846(19) 0.0480(13) 0.0320(11) 0.0139(10) 0.0275(12) 0.0028(12) C26 0.0683(15) 0.0400(12) 0.0318(10) 0.0043(9) 0.0208(10) 0.0096(11) C27 0.0397(10) 0.0287(9) 0.0365(10) 0.0082(8) 0.0131(8) 0.0093(8) C28 0.0296(9) 0.0299(9) 0.0296(9) 0.0122(7) 0.0112(7) 0.0090(7) C29 0.0221(8) 0.0305(9) 0.0274(8) 0.0131(7) 0.0082(7) 0.0054(7) C30 0.0267(9) 0.0335(10) 0.0332(9) 0.0113(8) 0.0081(7) 0.0092(7) C31 0.0309(10) 0.0385(11) 0.0481(12) 0.0167(9) 0.0084(9) 0.0149(8) C32 0.0297(10) 0.0541(13) 0.0390(11) 0.0230(10) 0.0038(8) 0.0134(9) C33 0.0351(10) 0.0524(13) 0.0300(10) 0.0124(9) 0.0048(8) 0.0131(9) C34 0.0304(9) 0.0398(11) 0.0299(9) 0.0092(8) 0.0063(8) 0.0130(8) C35 0.0252(8) 0.0271(8) 0.0261(8) 0.0110(7) 0.0083(7) 0.0038(7) C36 0.0310(10) 0.0361(10) 0.0491(12) 0.0213(9) 0.0174(9) 0.0078(8) C37 0.0325(10) 0.0466(12) 0.0579(13) 0.0274(11) 0.0210(10) 0.0061(9) C38 0.0383(11) 0.0387(11) 0.0551(13) 0.0266(10) 0.0169(10) 0.0008(9) C39 0.0413(11) 0.0364(11) 0.0634(14) 0.0291(10) 0.0206(10) 0.0109(9) C40 0.0281(9) 0.0346(10) 0.0474(11) 0.0208(9) 0.0158(8) 0.0085(8) C41 0.0237(8) 0.0322(9) 0.0302(9) 0.0096(7) 0.0129(7) 0.0021(7) C42 0.0344(10) 0.0321(10) 0.0428(11) 0.0094(9) 0.0159(9) 0.0025(8) C43 0.0491(13) 0.0334(11) 0.0488(13) 0.0045(9) 0.0201(11) -0.0055(9) C44 0.0378(11) 0.0523(14) 0.0357(11) 0.0029(10) 0.0100(9) -0.0136(10) C45 0.0308(10) 0.0584(14) 0.0356(11) 0.0151(10) 0.0067(8) 0.0015(9) C46 0.0289(9) 0.0386(10) 0.0312(9) 0.0113(8) 0.0091(7) 0.0038(8) C47 0.0272(8) 0.0316(9) 0.0296(9) 0.0121(7) 0.0128(7) 0.0101(7) C48 0.0308(9) 0.0421(11) 0.0409(11) 0.0221(9) 0.0115(8) 0.0052(8) C49 0.0415(11) 0.0484(12) 0.0496(12) 0.0302(10) 0.0191(10) 0.0103(9) C50 0.0453(12) 0.0508(13) 0.0392(11) 0.0268(10) 0.0174(9) 0.0196(10) C51 0.0399(11) 0.0558(14) 0.0343(10) 0.0182(10) 0.0080(9) 0.0053(10) C52 0.0362(10) 0.0451(11) 0.0309(10) 0.0140(9) 0.0111(8) 0.0003(9) C53 0.0255(8) 0.0301(9) 0.0256(8) 0.0075(7) 0.0073(7) 0.0080(7) C54 0.0309(9) 0.0383(10) 0.0387(10) 0.0136(9) 0.0151(8) 0.0088(8) C55 0.0365(11) 0.0474(12) 0.0413(11) 0.0123(10) 0.0178(9) 0.0178(9) C56 0.0414(11) 0.0381(11) 0.0351(10) 0.0096(9) 0.0082(9) 0.0210(9) C57 0.0421(11) 0.0324(10) 0.0323(10) 0.0137(8) 0.0075(8) 0.0122(8) C58 0.0316(9) 0.0317(9) 0.0288(9) 0.0111(7) 0.0093(7) 0.0085(7) C60 0.040(4) 0.038(4) 0.035(3) 0.014(3) 0.006(3) 0.005(3) Cl1 0.0701(12) 0.0486(10) 0.0434(9) 0.0175(8) 0.0260(9) 0.0197(9) Cl2 0.0942(17) 0.0340(9) 0.0585(12) 0.0083(8) 0.0272(12) 0.0011(10) _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 C22 1.860(2) . ? Ru C13 2.0851(18) . ? Ru P2 2.3680(4) . ? Ru P1 2.3684(4) . ? Ru S3 2.4661(4) . ? Ru S1 2.4936(4) . ? P1 C23 1.8280(18) . ? P1 C29 1.8384(18) . ? P1 C35 1.8422(18) . ? P2 C41 1.8319(19) . ? P2 C53 1.8389(19) . ? P2 C47 1.8416(19) . ? S1 C2 1.7105(19) . ? C2 N4 1.337(2) . ? C2 S3 1.7066(19) . ? N4 C9 1.466(3) . ? N4 C5 1.466(3) . ? C5 C6 1.506(3) . ? C6 O7' 1.367(16) . ? C6 O7 1.417(4) . ? O7 C8 1.429(5) . ? O7' C8' 1.416(16) . ? C9 C10 1.515(5) . ? C9 C10' 1.530(12) . ? C9 C10" 1.541(15) . ? C10 O11 1.387(7) . ? O11 C12 1.435(6) . ? C10' O11' 1.350(12) . ? O11' C12' 1.423(10) . ? C10" O11" 1.310(15) . ? O11" C12" 1.394(15) . ? C13 C14 1.328(3) . ? C14 C15' 1.416(5) . ? C14 C15 1.553(3) . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C18 C21 1.538(4) . ? C19 C20 1.3900 . ? C15' C16' 1.3900 . ? C15' C20' 1.3900 . ? C16' C17' 1.3900 . ? C17' C18' 1.3900 . ? C18' C19' 1.3900 . ? C18' C21' 1.551(10) . ? C19' C20' 1.3900 . ? C22 O22 1.133(2) . ? C23 C24 1.386(3) . ? C23 C28 1.397(3) . ? C24 C25 1.390(3) . ? C25 C26 1.383(4) . ? C26 C27 1.383(3) . ? C27 C28 1.386(3) . ? C29 C30 1.388(3) . ? C29 C34 1.396(3) . ? C30 C31 1.389(3) . ? C31 C32 1.377(3) . ? C32 C33 1.384(3) . ? C33 C34 1.386(3) . ? C35 C40 1.378(3) . ? C35 C36 1.395(3) . ? C36 C37 1.384(3) . ? C37 C38 1.381(3) . ? C38 C39 1.381(3) . ? C39 C40 1.390(3) . ? C41 C46 1.390(3) . ? C41 C42 1.400(3) . ? C42 C43 1.385(3) . ? C43 C44 1.378(4) . ? C44 C45 1.376(4) . ? C45 C46 1.395(3) . ? C47 C48 1.387(3) . ? C47 C52 1.396(3) . ? C48 C49 1.393(3) . ? C49 C50 1.374(3) . ? C50 C51 1.380(3) . ? C51 C52 1.384(3) . ? C53 C58 1.386(3) . ? C53 C54 1.402(3) . ? C54 C55 1.382(3) . ? C55 C56 1.386(4) . ? C56 C57 1.381(3) . ? C57 C58 1.390(3) . ? C60 Cl2 1.747(8) . ? C60 Cl1 1.766(8) . ? 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 C22 Ru C13 94.86(8) . . ? C22 Ru P2 89.70(5) . . ? C13 Ru P2 88.87(5) . . ? C22 Ru P1 89.51(5) . . ? C13 Ru P1 85.49(5) . . ? P2 Ru P1 174.221(15) . . ? C22 Ru S3 172.16(6) . . ? C13 Ru S3 92.97(5) . . ? P2 Ru S3 89.961(15) . . ? P1 Ru S3 91.592(15) . . ? C22 Ru S1 101.83(6) . . ? C13 Ru S1 163.30(5) . . ? P2 Ru S1 91.725(16) . . ? P1 Ru S1 94.039(15) . . ? S3 Ru S1 70.346(15) . . ? C23 P1 C29 103.67(8) . . ? C23 P1 C35 103.13(8) . . ? C29 P1 C35 99.45(8) . . ? C23 P1 Ru 115.56(6) . . ? C29 P1 Ru 114.50(6) . . ? C35 P1 Ru 118.25(6) . . ? C41 P2 C53 102.02(8) . . ? C41 P2 C47 105.32(9) . . ? C53 P2 C47 100.80(8) . . ? C41 P2 Ru 114.88(6) . . ? C53 P2 Ru 116.98(6) . . ? C47 P2 Ru 114.95(6) . . ? C2 S1 Ru 87.54(6) . . ? N4 C2 S3 123.79(15) . . ? N4 C2 S1 122.75(15) . . ? S3 C2 S1 113.47(10) . . ? C2 S3 Ru 88.53(6) . . ? C2 N4 C9 120.73(17) . . ? C2 N4 C5 120.41(17) . . ? C9 N4 C5 118.84(16) . . ? N4 C5 C6 113.91(17) . . ? O7' C6 C5 114.1(13) . . ? O7 C6 C5 108.9(3) . . ? C6 O7 C8 110.4(5) . . ? C6 O7' C8' 118.6(19) . . ? N4 C9 C10 115.9(3) . . ? N4 C9 C10' 110.0(6) . . ? N4 C9 C10" 110.3(12) . . ? O11 C10 C9 111.3(5) . . ? C10 O11 C12 113.7(4) . . ? O11' C10' C9 112.5(9) . . ? C10' O11' C12' 118.3(9) . . ? O11" C10" C9 121.4(19) . . ? C10" O11" C12" 127.1(18) . . ? C14 C13 Ru 127.45(15) . . ? C13 C14 C15' 132.8(4) . . ? C13 C14 C15 123.4(2) . . ? C16 C15 C20 120.0 . . ? C16 C15 C14 122.5(2) . . ? C20 C15 C14 117.4(2) . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 C21 119.6(3) . . ? C17 C18 C21 120.4(3) . . ? C20 C19 C18 120.0 . . ? C19 C20 C15 120.0 . . ? C16' C15' C20' 120.0 . . ? C16' C15' C14 120.1(5) . . ? C20' C15' C14 119.9(5) . . ? C15' C16' C17' 120.0 . . ? C18' C17' C16' 120.0 . . ? C17' C18' C19' 120.0 . . ? C17' C18' C21' 119.7(6) . . ? C19' C18' C21' 120.2(6) . . ? C18' C19' C20' 120.0 . . ? C19' C20' C15' 120.0 . . ? O22 C22 Ru 178.85(18) . . ? C24 C23 C28 118.81(17) . . ? C24 C23 P1 122.59(15) . . ? C28 C23 P1 118.51(14) . . ? C23 C24 C25 120.3(2) . . ? C26 C25 C24 120.5(2) . . ? C25 C26 C27 119.6(2) . . ? C26 C27 C28 120.1(2) . . ? C27 C28 C23 120.67(18) . . ? C30 C29 C34 118.45(17) . . ? C30 C29 P1 123.73(14) . . ? C34 C29 P1 117.80(14) . . ? C29 C30 C31 120.68(19) . . ? C32 C31 C30 120.30(19) . . ? C31 C32 C33 119.76(19) . . ? C32 C33 C34 120.1(2) . . ? C33 C34 C29 120.69(19) . . ? C40 C35 C36 118.79(17) . . ? C40 C35 P1 121.49(14) . . ? C36 C35 P1 119.72(14) . . ? C37 C36 C35 120.53(19) . . ? C38 C37 C36 120.2(2) . . ? C39 C38 C37 119.53(19) . . ? C38 C39 C40 120.2(2) . . ? C35 C40 C39 120.68(18) . . ? C46 C41 C42 118.51(18) . . ? C46 C41 P2 120.70(15) . . ? C42 C41 P2 120.27(15) . . ? C43 C42 C41 120.6(2) . . ? C44 C43 C42 120.2(2) . . ? C45 C44 C43 120.0(2) . . ? C44 C45 C46 120.2(2) . . ? C41 C46 C45 120.4(2) . . ? C48 C47 C52 118.23(18) . . ? C48 C47 P2 124.16(15) . . ? C52 C47 P2 117.61(15) . . ? C47 C48 C49 120.5(2) . . ? C50 C49 C48 120.5(2) . . ? C49 C50 C51 119.6(2) . . ? C50 C51 C52 120.2(2) . . ? C51 C52 C47 120.9(2) . . ? C58 C53 C54 118.80(18) . . ? C58 C53 P2 121.06(14) . . ? C54 C53 P2 120.11(15) . . ? C55 C54 C53 120.3(2) . . ? C54 C55 C56 120.2(2) . . ? C57 C56 C55 120.02(19) . . ? C56 C57 C58 119.9(2) . . ? C53 C58 C57 120.73(18) . . ? Cl2 C60 Cl1 111.4(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 72.65 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.488 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.056 #===END