# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Antonio Tiripicchio' _publ_contact_author_address ; Dipartimento di Chimica Generale ed Inorganica, Chimica Analitica, Chimica Fisic Universita di Parma Parco Area delle Scienze 17/A Parma I-43100 ITALY ; _publ_contact_author_email TIRI@UNIPR.IT _publ_section_title ; Experimental and Computational Studies on the Solvent-controlled Cluster Isomerism of Ru3(H)(CO)9(NPPh3) and Related Dynamics ; loop_ _publ_author_name 'Carlo Mealli' 'Antonio Tiripicchio' 'Andrew D. Phillips' 'Giovanni Predieri' 'Roberto Pattacini' data_sad_1 _database_code_depnum_ccdc_archive 'CCDC 289256' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H16 N O9 P Ru3' _chemical_formula_sum 'C27 H16 N O9 P Ru3' _chemical_formula_weight 832.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 '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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.153(5) _cell_length_b 18.797(5) _cell_length_c 17.026(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.880(5) _cell_angle_gamma 90.00 _cell_volume 2929(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.888 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.634 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7091 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15690 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5731 _reflns_number_gt 3562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Platon _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^)+(0.0052P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5731 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0432 _refine_ls_wR_factor_gt 0.0390 _refine_ls_goodness_of_fit_ref 0.756 _refine_ls_restrained_S_all 0.756 _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 0.23471(4) 0.023162(19) 0.36171(2) 0.03122(9) Uani 1 1 d . . . Ru2 Ru 0.33584(3) 0.165303(19) 0.345643(19) 0.03016(9) Uani 1 1 d . . . Ru3 Ru 0.04658(3) 0.140039(19) 0.387265(19) 0.03051(9) Uani 1 1 d . . . P1 P 0.11330(11) 0.10672(6) 0.19165(6) 0.0287(3) Uani 1 1 d . . . O1 O 0.3545(4) -0.06691(19) 0.4969(2) 0.0707(11) Uani 1 1 d . . . O2 O 0.2012(4) -0.11612(18) 0.26629(19) 0.0653(10) Uani 1 1 d . . . O3 O -0.0860(3) -0.01583(16) 0.41512(17) 0.0479(8) Uani 1 1 d . . . O4 O 0.5666(3) 0.03810(17) 0.32157(18) 0.0547(9) Uani 1 1 d . . . O5 O 0.5553(3) 0.22766(18) 0.46242(19) 0.0602(10) Uani 1 1 d . . . O6 O 0.4935(3) 0.24575(18) 0.21634(18) 0.0607(10) Uani 1 1 d . . . O7 O 0.1539(3) 0.30523(16) 0.38509(19) 0.0552(9) Uani 1 1 d . . . O8 O -0.2394(3) 0.2008(2) 0.3223(2) 0.0721(11) Uani 1 1 d . . . O9 O -0.0625(3) 0.17031(17) 0.55056(18) 0.0593(9) Uani 1 1 d . . . N1 N 0.1615(3) 0.10881(17) 0.28272(17) 0.0277(8) Uani 1 1 d . . . C1 C 0.3070(5) -0.0328(2) 0.4466(3) 0.0407(12) Uani 1 1 d . . . C2 C 0.2163(4) -0.0631(2) 0.3016(3) 0.0383(11) Uani 1 1 d . . . C3 C 0.0037(4) 0.0253(2) 0.3979(2) 0.0362(11) Uani 1 1 d . . . C4 C 0.4505(5) 0.0599(2) 0.3327(2) 0.0384(11) Uani 1 1 d . . . C5 C 0.4718(4) 0.2034(2) 0.4181(2) 0.0365(11) Uani 1 1 d . . . C6 C 0.4341(4) 0.2151(2) 0.2654(2) 0.0385(11) Uani 1 1 d . . . C7 C 0.1717(4) 0.2429(3) 0.3737(2) 0.0382(12) Uani 1 1 d . . . C8 C -0.1309(4) 0.1765(2) 0.3473(2) 0.0395(11) Uani 1 1 d . . . C9 C -0.0184(4) 0.1592(2) 0.4891(3) 0.0372(11) Uani 1 1 d . . . C10 C 0.0070(4) 0.0252(2) 0.1690(2) 0.0320(10) Uani 1 1 d . . . C11 C 0.0464(5) -0.0220(3) 0.1091(3) 0.0474(13) Uani 1 1 d . . . C12 C -0.0293(6) -0.0877(3) 0.0972(3) 0.0667(17) Uani 1 1 d . . . C13 C -0.1432(7) -0.1046(3) 0.1455(4) 0.0656(17) Uani 1 1 d . . . C14 C -0.1873(5) -0.0580(3) 0.2036(3) 0.0524(14) Uani 1 1 d . . . C15 C -0.1128(5) 0.0074(3) 0.2140(3) 0.0422(12) Uani 1 1 d . . . C16 C 0.0025(4) 0.1854(2) 0.1637(2) 0.0301(10) Uani 1 1 d . . . C17 C -0.1316(5) 0.1775(3) 0.1233(3) 0.0424(12) Uani 1 1 d . . . C18 C -0.2151(5) 0.2386(3) 0.1047(3) 0.0501(14) Uani 1 1 d . . . C19 C -0.1683(5) 0.3076(3) 0.1252(3) 0.0527(14) Uani 1 1 d . . . C20 C -0.0359(5) 0.3174(3) 0.1636(3) 0.0469(13) Uani 1 1 d . . . C21 C 0.0501(5) 0.2562(3) 0.1830(3) 0.0413(12) Uani 1 1 d . . . C22 C 0.2714(4) 0.1045(2) 0.1284(2) 0.0292(10) Uani 1 1 d . . . C23 C 0.2857(5) 0.1521(2) 0.0658(3) 0.0400(12) Uani 1 1 d . . . C24 C 0.4064(5) 0.1482(3) 0.0175(3) 0.0490(13) Uani 1 1 d . . . C25 C 0.5161(5) 0.0975(3) 0.0335(3) 0.0491(14) Uani 1 1 d . . . C26 C 0.5027(5) 0.0504(3) 0.0957(3) 0.0505(14) Uani 1 1 d . . . C27 C 0.3827(5) 0.0531(3) 0.1429(3) 0.0435(13) Uani 1 1 d . . . H1 H 0.246(3) 0.1061(15) 0.4165(16) 0.015(8) Uiso 1 1 d . . . H11 H 0.125(4) -0.0035(19) 0.075(2) 0.047(3) Uiso 1 1 d . . . H12 H -0.008(4) -0.119(2) 0.055(2) 0.047(3) Uiso 1 1 d . . . H13 H -0.196(4) -0.144(2) 0.137(2) 0.047(3) Uiso 1 1 d . . . H14 H -0.262(4) -0.070(2) 0.232(2) 0.047(3) Uiso 1 1 d . . . H15 H -0.140(4) 0.041(2) 0.257(2) 0.047(3) Uiso 1 1 d . . . H17 H -0.164(4) 0.130(2) 0.110(2) 0.047(3) Uiso 1 1 d . . . H18 H -0.301(4) 0.237(2) 0.086(2) 0.047(3) Uiso 1 1 d . . . H19 H -0.220(4) 0.349(2) 0.108(2) 0.047(3) Uiso 1 1 d . . . H20 H 0.007(4) 0.368(2) 0.179(2) 0.047(3) Uiso 1 1 d . . . H21 H 0.132(4) 0.266(2) 0.208(2) 0.047(3) Uiso 1 1 d . . . H23 H 0.207(4) 0.183(2) 0.054(2) 0.047(3) Uiso 1 1 d . . . H24 H 0.415(4) 0.182(2) -0.027(2) 0.047(3) Uiso 1 1 d . . . H25 H 0.591(4) 0.095(2) 0.000(2) 0.047(3) Uiso 1 1 d . . . H26 H 0.576(4) 0.020(2) 0.104(2) 0.047(3) Uiso 1 1 d . . . H27 H 0.376(4) 0.018(2) 0.176(2) 0.047(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0343(2) 0.0303(2) 0.0291(2) 0.00193(18) -0.00152(15) 0.00334(18) Ru2 0.02818(18) 0.0347(2) 0.0276(2) -0.00095(18) 0.00017(14) -0.00253(17) Ru3 0.02819(18) 0.0340(2) 0.0294(2) 0.00028(17) 0.00400(14) 0.00211(17) P1 0.0286(6) 0.0309(7) 0.0263(6) 0.0006(5) -0.0008(5) -0.0015(5) O1 0.082(3) 0.074(3) 0.056(2) 0.021(2) -0.019(2) 0.018(2) O2 0.087(3) 0.045(2) 0.063(2) -0.015(2) -0.010(2) 0.011(2) O3 0.048(2) 0.044(2) 0.052(2) 0.0085(17) 0.0035(16) -0.0094(17) O4 0.0375(19) 0.061(2) 0.066(2) -0.0034(19) 0.0061(16) 0.0121(17) O5 0.060(2) 0.065(3) 0.054(2) -0.0077(19) -0.0162(18) -0.0192(19) O6 0.053(2) 0.082(3) 0.048(2) 0.020(2) 0.0084(17) -0.0080(19) O7 0.064(2) 0.037(2) 0.066(2) -0.0052(18) 0.0237(18) 0.0029(18) O8 0.040(2) 0.104(3) 0.073(3) 0.009(2) -0.0002(18) 0.019(2) O9 0.073(2) 0.062(2) 0.044(2) -0.008(2) 0.0210(17) -0.0018(19) N1 0.0274(18) 0.032(2) 0.0229(18) 0.0019(16) -0.0028(14) 0.0061(16) C1 0.047(3) 0.042(3) 0.033(3) -0.002(2) -0.002(2) 0.001(2) C2 0.037(3) 0.040(3) 0.038(3) -0.002(2) -0.006(2) 0.009(2) C3 0.042(3) 0.041(3) 0.025(2) 0.003(2) -0.002(2) -0.001(2) C4 0.041(3) 0.048(3) 0.026(3) 0.000(2) -0.004(2) 0.007(2) C5 0.037(3) 0.034(3) 0.039(3) 0.004(2) 0.004(2) 0.005(2) C6 0.040(3) 0.043(3) 0.033(3) -0.001(2) -0.003(2) 0.000(2) C7 0.039(3) 0.050(3) 0.026(3) -0.002(2) 0.006(2) 0.000(2) C8 0.031(3) 0.046(3) 0.041(3) -0.005(2) 0.008(2) 0.000(2) C9 0.040(3) 0.033(3) 0.039(3) 0.002(2) 0.003(2) 0.000(2) C10 0.039(3) 0.035(3) 0.022(2) 0.002(2) -0.0070(19) -0.001(2) C11 0.053(3) 0.042(3) 0.047(3) -0.009(3) 0.002(2) -0.011(3) C12 0.077(4) 0.060(4) 0.064(4) -0.024(3) 0.000(3) -0.010(3) C13 0.075(4) 0.045(4) 0.076(4) 0.000(3) -0.026(3) -0.028(3) C14 0.055(4) 0.052(4) 0.051(4) 0.009(3) -0.004(3) -0.021(3) C15 0.043(3) 0.049(3) 0.035(3) -0.004(2) -0.005(2) -0.007(3) C16 0.028(2) 0.035(3) 0.027(2) 0.002(2) -0.0029(18) -0.001(2) C17 0.037(3) 0.043(3) 0.047(3) 0.003(3) -0.009(2) -0.005(3) C18 0.034(3) 0.060(4) 0.056(3) 0.011(3) -0.017(2) 0.002(3) C19 0.046(3) 0.048(4) 0.064(4) 0.011(3) -0.004(3) 0.018(3) C20 0.049(3) 0.035(3) 0.057(3) 0.002(3) -0.007(2) 0.003(3) C21 0.038(3) 0.046(3) 0.040(3) -0.001(2) -0.007(2) -0.003(3) C22 0.032(2) 0.037(3) 0.019(2) -0.001(2) -0.0042(18) 0.004(2) C23 0.038(3) 0.043(3) 0.040(3) 0.003(2) 0.003(2) 0.000(2) C24 0.057(3) 0.055(4) 0.035(3) 0.003(3) 0.010(2) -0.014(3) C25 0.037(3) 0.066(4) 0.044(3) -0.009(3) 0.014(2) -0.003(3) C26 0.041(3) 0.062(4) 0.048(3) -0.004(3) 0.000(3) 0.019(3) C27 0.050(3) 0.053(4) 0.027(3) 0.007(2) 0.000(2) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.899(5) . ? Ru1 C2 1.923(5) . ? Ru1 C4 2.157(4) . ? Ru1 N1 2.196(3) . ? Ru1 C3 2.212(4) . ? Ru1 Ru3 2.8291(9) . ? Ru1 Ru2 2.8421(9) . ? Ru1 H1 1.82(3) . ? Ru2 C5 1.881(4) . ? Ru2 C6 1.894(5) . ? Ru2 C7 2.153(4) . ? Ru2 N1 2.184(3) . ? Ru2 C4 2.255(5) . ? Ru2 Ru3 2.7920(14) . ? Ru2 H1 1.84(3) . ? Ru3 C9 1.876(4) . ? Ru3 C8 1.880(4) . ? Ru3 N1 2.163(3) . ? Ru3 C3 2.201(5) . ? Ru3 C7 2.261(5) . ? Ru3 H1 1.99(3) . ? P1 N1 1.606(3) . ? P1 C22 1.817(4) . ? P1 C16 1.851(4) . ? P1 C10 1.852(4) . ? O1 C1 1.149(5) . ? O2 C2 1.171(5) . ? O3 C3 1.168(4) . ? O4 C4 1.157(4) . ? O5 C5 1.159(4) . ? O6 C6 1.157(5) . ? O7 C7 1.199(5) . ? O8 C8 1.168(4) . ? O9 C9 1.147(4) . ? C10 C15 1.388(5) . ? C10 C11 1.403(6) . ? C11 C12 1.430(6) . ? C11 H11 1.00(3) . ? C12 C13 1.375(7) . ? C12 H12 0.94(4) . ? C13 C14 1.386(7) . ? C13 H13 0.89(4) . ? C14 C15 1.415(6) . ? C14 H14 0.88(4) . ? C15 H15 1.00(4) . ? C16 C17 1.406(5) . ? C16 C21 1.437(5) . ? C17 C18 1.412(6) . ? C17 H17 0.97(4) . ? C18 C19 1.409(6) . ? C18 H18 0.85(3) . ? C19 C20 1.380(6) . ? C19 H19 0.96(4) . ? C20 C21 1.430(6) . ? C20 H20 1.06(4) . ? C21 H21 0.87(3) . ? C22 C23 1.401(5) . ? C22 C27 1.422(6) . ? C23 C24 1.389(6) . ? C23 H23 0.94(3) . ? C24 C25 1.408(6) . ? C24 H24 0.99(4) . ? C25 C26 1.387(7) . ? C25 H25 0.90(4) . ? C26 C27 1.373(6) . ? C26 H26 0.90(4) . ? C27 H27 0.87(4) . ? 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 C1 Ru1 C2 87.98(18) . . ? C1 Ru1 C4 92.38(17) . . ? C2 Ru1 C4 102.78(17) . . ? C1 Ru1 N1 166.40(15) . . ? C2 Ru1 N1 105.60(15) . . ? C4 Ru1 N1 84.11(14) . . ? C1 Ru1 C3 96.98(16) . . ? C2 Ru1 C3 94.97(16) . . ? C4 Ru1 C3 160.21(17) . . ? N1 Ru1 C3 82.73(13) . . ? C1 Ru1 Ru3 121.26(13) . . ? C2 Ru1 Ru3 133.46(12) . . ? C4 Ru1 Ru3 110.40(12) . . ? N1 Ru1 Ru3 49.02(8) . . ? C3 Ru1 Ru3 49.95(12) . . ? C1 Ru1 Ru2 118.93(13) . . ? C2 Ru1 Ru2 140.12(13) . . ? C4 Ru1 Ru2 51.43(12) . . ? N1 Ru1 Ru2 49.35(8) . . ? C3 Ru1 Ru2 108.92(12) . . ? Ru3 Ru1 Ru2 58.98(3) . . ? C1 Ru1 H1 93.9(9) . . ? C2 Ru1 H1 177.8(8) . . ? C4 Ru1 H1 78.4(8) . . ? N1 Ru1 H1 72.5(9) . . ? C3 Ru1 H1 83.6(8) . . ? Ru3 Ru1 H1 44.4(8) . . ? Ru2 Ru1 H1 39.4(9) . . ? C5 Ru2 C6 88.20(17) . . ? C5 Ru2 C7 93.06(17) . . ? C6 Ru2 C7 99.54(17) . . ? C5 Ru2 N1 168.02(15) . . ? C6 Ru2 N1 103.74(15) . . ? C7 Ru2 N1 86.05(14) . . ? C5 Ru2 C4 95.42(16) . . ? C6 Ru2 C4 97.87(17) . . ? C7 Ru2 C4 160.85(16) . . ? N1 Ru2 C4 82.10(13) . . ? C5 Ru2 Ru3 121.25(12) . . ? C6 Ru2 Ru3 136.84(12) . . ? C7 Ru2 Ru3 52.51(12) . . ? N1 Ru2 Ru3 49.70(8) . . ? C4 Ru2 Ru3 108.66(11) . . ? C5 Ru2 Ru1 120.55(13) . . ? C6 Ru2 Ru1 133.83(13) . . ? C7 Ru2 Ru1 112.72(12) . . ? N1 Ru2 Ru1 49.72(8) . . ? C4 Ru2 Ru1 48.39(11) . . ? Ru3 Ru2 Ru1 60.276(13) . . ? C5 Ru2 H1 95.6(8) . . ? C6 Ru2 H1 172.5(9) . . ? C7 Ru2 H1 86.8(8) . . ? N1 Ru2 H1 72.4(8) . . ? C4 Ru2 H1 75.3(8) . . ? Ru3 Ru2 H1 45.3(8) . . ? Ru1 Ru2 H1 38.8(8) . . ? C9 Ru3 C8 88.85(17) . . ? C9 Ru3 N1 167.87(14) . . ? C8 Ru3 N1 103.27(14) . . ? C9 Ru3 C3 93.02(17) . . ? C8 Ru3 C3 103.43(17) . . ? N1 Ru3 C3 83.75(13) . . ? C9 Ru3 C7 95.69(17) . . ? C8 Ru3 C7 95.03(17) . . ? N1 Ru3 C7 83.93(13) . . ? C3 Ru3 C7 159.73(15) . . ? C9 Ru3 Ru2 121.16(12) . . ? C8 Ru3 Ru2 131.57(13) . . ? N1 Ru3 Ru2 50.36(8) . . ? C3 Ru3 Ru2 111.02(11) . . ? C7 Ru3 Ru2 49.06(11) . . ? C9 Ru3 Ru1 119.57(13) . . ? C8 Ru3 Ru1 138.72(13) . . ? N1 Ru3 Ru1 50.04(8) . . ? C3 Ru3 Ru1 50.30(11) . . ? C7 Ru3 Ru1 109.75(11) . . ? Ru2 Ru3 Ru1 60.74(2) . . ? C9 Ru3 H1 97.6(8) . . ? C8 Ru3 H1 172.4(8) . . ? N1 Ru3 H1 70.3(8) . . ? C3 Ru3 H1 80.2(8) . . ? C7 Ru3 H1 80.5(8) . . ? Ru2 Ru3 H1 41.2(8) . . ? Ru1 Ru3 H1 39.8(8) . . ? N1 P1 C22 111.27(16) . . ? N1 P1 C16 111.71(17) . . ? C22 P1 C16 107.73(18) . . ? N1 P1 C10 110.91(17) . . ? C22 P1 C10 106.16(19) . . ? C16 P1 C10 108.84(18) . . ? P1 N1 Ru3 132.17(16) . . ? P1 N1 Ru2 132.33(17) . . ? Ru3 N1 Ru2 79.93(10) . . ? P1 N1 Ru1 130.55(18) . . ? Ru3 N1 Ru1 80.94(10) . . ? Ru2 N1 Ru1 80.92(10) . . ? O1 C1 Ru1 178.1(4) . . ? O2 C2 Ru1 177.9(4) . . ? O3 C3 Ru3 142.7(3) . . ? O3 C3 Ru1 137.5(4) . . ? Ru3 C3 Ru1 79.75(15) . . ? O4 C4 Ru1 140.5(4) . . ? O4 C4 Ru2 139.2(4) . . ? Ru1 C4 Ru2 80.17(15) . . ? O5 C5 Ru2 179.2(4) . . ? O6 C6 Ru2 179.6(4) . . ? O7 C7 Ru2 142.6(3) . . ? O7 C7 Ru3 138.5(3) . . ? Ru2 C7 Ru3 78.43(16) . . ? O8 C8 Ru3 178.2(4) . . ? O9 C9 Ru3 177.9(4) . . ? C15 C10 C11 117.5(4) . . ? C15 C10 P1 120.1(3) . . ? C11 C10 P1 122.3(3) . . ? C10 C11 C12 121.3(5) . . ? C10 C11 H11 114(2) . . ? C12 C11 H11 125(2) . . ? C13 C12 C11 119.0(5) . . ? C13 C12 H12 119(2) . . ? C11 C12 H12 122(3) . . ? C12 C13 C14 120.9(5) . . ? C12 C13 H13 120(3) . . ? C14 C13 H13 118(3) . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H14 119(3) . . ? C15 C14 H14 122(3) . . ? C10 C15 C14 121.6(5) . . ? C10 C15 H15 117(2) . . ? C14 C15 H15 121(2) . . ? C17 C16 C21 117.9(4) . . ? C17 C16 P1 120.9(3) . . ? C21 C16 P1 121.2(3) . . ? C16 C17 C18 119.4(4) . . ? C16 C17 H17 118(2) . . ? C18 C17 H17 122(2) . . ? C19 C18 C17 122.1(4) . . ? C19 C18 H18 114(3) . . ? C17 C18 H18 123(3) . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19 118(2) . . ? C18 C19 H19 121(2) . . ? C19 C20 C21 118.5(5) . . ? C19 C20 H20 124(2) . . ? C21 C20 H20 118(2) . . ? C20 C21 C16 122.0(4) . . ? C20 C21 H21 114(3) . . ? C16 C21 H21 124(3) . . ? C23 C22 C27 119.5(4) . . ? C23 C22 P1 121.4(3) . . ? C27 C22 P1 119.2(3) . . ? C24 C23 C22 120.1(4) . . ? C24 C23 H23 121(2) . . ? C22 C23 H23 119(2) . . ? C23 C24 C25 119.5(4) . . ? C23 C24 H24 119(2) . . ? C25 C24 H24 121(2) . . ? C26 C25 C24 120.6(4) . . ? C26 C25 H25 122(3) . . ? C24 C25 H25 117(3) . . ? C27 C26 C25 120.3(4) . . ? C27 C26 H26 122(3) . . ? C25 C26 H26 117(3) . . ? C26 C27 C22 120.1(4) . . ? C26 C27 H27 115(3) . . ? C22 C27 H27 125(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.490 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.089 _exptl_crystal_recrystallization_method 'Hexane solution evaporation' # Attachment '1b.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 289257' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H16 N O9 P Ru3' _chemical_formula_sum 'C27 H16 N O9 P Ru3' _chemical_formula_weight 832.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 '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' 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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3591(10) _cell_length_b 17.6646(10) _cell_length_c 18.1015(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.100(10) _cell_angle_gamma 90.00 _cell_volume 2946.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.624 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.885901 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13668 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.1865 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 24.81 _reflns_number_total 5036 _reflns_number_gt 2072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Platon _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5036 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1417 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0535 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 0.648 _refine_ls_restrained_S_all 0.648 _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 Ru1 Ru 0.00990(7) 0.17550(4) 0.07974(3) 0.04344(18) Uani 1 1 d . . . Ru2 Ru 0.01908(6) 0.25700(4) 0.20449(3) 0.04522(18) Uani 1 1 d . . . Ru3 Ru 0.25385(6) 0.25194(4) 0.12613(3) 0.04219(17) Uani 1 1 d . . . P1 P 0.2016(2) 0.09150(11) 0.23234(10) 0.0366(5) Uani 1 1 d . . . O1 O -0.2876(6) 0.1102(4) 0.0814(4) 0.108(3) Uani 1 1 d . . . O2 O 0.1069(6) 0.0571(3) -0.0228(3) 0.081(2) Uani 1 1 d . . . O3 O -0.1100(6) 0.2829(3) -0.0434(3) 0.095(2) Uani 1 1 d . . . O4 O -0.2405(6) 0.1803(4) 0.2504(4) 0.109(3) Uani 1 1 d . . . O5 O 0.1235(7) 0.3193(4) 0.3618(3) 0.115(3) Uani 1 1 d . . . O6 O -0.1795(6) 0.3818(4) 0.1360(3) 0.086(2) Uani 1 1 d . . . O7 O 0.5375(7) 0.3138(4) 0.2150(4) 0.124(3) Uani 1 1 d . . . O8 O 0.3906(6) 0.1672(4) 0.0127(3) 0.091(2) Uani 1 1 d . . . O9 O 0.2145(7) 0.3833(4) 0.0185(3) 0.091(2) Uani 1 1 d . . . N1 N 0.1539(5) 0.1669(3) 0.1821(3) 0.0382(16) Uani 1 1 d . . . C1 C -0.1720(9) 0.1332(5) 0.0839(5) 0.069(3) Uani 1 1 d . . . C2 C 0.0725(8) 0.1016(4) 0.0154(4) 0.048(2) Uani 1 1 d . . . C3 C -0.0651(8) 0.2408(5) 0.0051(4) 0.063(2) Uani 1 1 d . . . C4 C -0.1432(9) 0.2051(5) 0.2320(5) 0.069(3) Uani 1 1 d . . . C5 C 0.0871(9) 0.2958(4) 0.3031(5) 0.062(3) Uani 1 1 d . . . C6 C -0.1061(9) 0.3358(5) 0.1626(5) 0.060(3) Uani 1 1 d . . . C7 C 0.4300(9) 0.2877(5) 0.1865(5) 0.072(3) Uani 1 1 d . . . C8 C 0.3399(9) 0.1959(4) 0.0576(4) 0.061(3) Uani 1 1 d . . . C9 C 0.2321(9) 0.3326(5) 0.0585(5) 0.063(3) Uani 1 1 d . . . C10 C 0.0470(7) 0.0521(4) 0.2662(4) 0.0405(11) Uani 1 1 d . . . C11 C -0.0616(7) 0.0163(4) 0.2196(4) 0.0585(7) Uani 1 1 d . . . H11 H -0.0544 0.0100 0.1694 0.070 Uiso 1 1 calc R . . C12 C -0.1830(8) -0.0110(4) 0.2451(4) 0.0585(7) Uani 1 1 d . . . H12 H -0.2570 -0.0353 0.2127 0.070 Uiso 1 1 calc R . . C13 C -0.1910(8) -0.0012(5) 0.3191(4) 0.0670(15) Uani 1 1 d . . . H13 H -0.2720 -0.0189 0.3371 0.080 Uiso 1 1 calc R . . C14 C -0.0827(8) 0.0338(4) 0.3671(4) 0.0585(7) Uani 1 1 d . . . H14 H -0.0900 0.0389 0.4174 0.070 Uiso 1 1 calc R . . C15 C 0.0372(8) 0.0618(4) 0.3419(4) 0.0585(7) Uani 1 1 d . . . H15 H 0.1103 0.0866 0.3744 0.070 Uiso 1 1 calc R . . C16 C 0.3414(7) 0.1067(4) 0.3123(4) 0.0405(11) Uani 1 1 d . . . C17 C 0.4043(7) 0.0443(4) 0.3515(4) 0.0585(7) Uani 1 1 d . . . H17 H 0.3729 -0.0039 0.3358 0.070 Uiso 1 1 calc R . . C18 C 0.5114(8) 0.0522(4) 0.4127(4) 0.0585(7) Uani 1 1 d . . . H18 H 0.5521 0.0096 0.4383 0.070 Uiso 1 1 calc R . . C19 C 0.5594(7) 0.1234(5) 0.4366(4) 0.0670(15) Uani 1 1 d . . . H19 H 0.6331 0.1291 0.4780 0.080 Uiso 1 1 calc R . . C20 C 0.4978(8) 0.1856(4) 0.3989(4) 0.0585(7) Uani 1 1 d . . . H20 H 0.5278 0.2339 0.4152 0.070 Uiso 1 1 calc R . . C21 C 0.3888(7) 0.1764(4) 0.3354(4) 0.0585(7) Uani 1 1 d . . . H21 H 0.3489 0.2188 0.3090 0.070 Uiso 1 1 calc R . . C22 C 0.2756(7) 0.0194(4) 0.1805(4) 0.0405(11) Uani 1 1 d . . . C23 C 0.2240(8) -0.0530(4) 0.1724(4) 0.0585(7) Uani 1 1 d . . . H23 H 0.1456 -0.0665 0.1948 0.070 Uiso 1 1 calc R . . C24 C 0.2845(7) -0.1067(4) 0.1318(4) 0.0585(7) Uani 1 1 d . . . H24 H 0.2470 -0.1555 0.1261 0.070 Uiso 1 1 calc R . . C25 C 0.4006(7) -0.0861(5) 0.1005(4) 0.0670(15) Uani 1 1 d . . . H25 H 0.4415 -0.1212 0.0721 0.080 Uiso 1 1 calc R . . C26 C 0.4585(8) -0.0149(4) 0.1099(4) 0.0585(7) Uani 1 1 d . . . H26 H 0.5404 -0.0027 0.0897 0.070 Uiso 1 1 calc R . . C27 C 0.3963(7) 0.0382(4) 0.1489(4) 0.0585(7) Uani 1 1 d . . . H27 H 0.4345 0.0869 0.1544 0.070 Uiso 1 1 calc R . . H1 H 0.168(6) 0.320(4) 0.189(3) 0.09(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0496(4) 0.0409(4) 0.0389(4) 0.0011(4) 0.0053(3) 0.0005(4) Ru2 0.0547(4) 0.0393(4) 0.0458(4) -0.0001(4) 0.0203(3) 0.0070(4) Ru3 0.0466(4) 0.0414(4) 0.0406(4) 0.0013(4) 0.0132(3) -0.0005(4) P1 0.0422(13) 0.0326(13) 0.0362(13) -0.0020(10) 0.0107(11) 0.0021(10) O1 0.057(4) 0.152(7) 0.107(6) 0.038(5) -0.005(4) -0.039(5) O2 0.130(5) 0.052(4) 0.067(5) -0.023(3) 0.037(4) 0.003(4) O3 0.102(5) 0.093(6) 0.078(5) 0.029(4) -0.019(4) 0.020(4) O4 0.084(5) 0.088(6) 0.175(7) 0.031(5) 0.077(5) 0.006(5) O5 0.170(6) 0.123(6) 0.048(4) -0.030(5) 0.010(5) 0.021(5) O6 0.077(5) 0.078(5) 0.099(5) 0.017(4) 0.005(4) 0.032(4) O7 0.081(5) 0.154(8) 0.124(7) -0.016(5) -0.019(5) -0.033(5) O8 0.106(5) 0.090(5) 0.093(5) 0.003(4) 0.066(4) 0.023(4) O9 0.132(6) 0.067(5) 0.078(5) 0.018(4) 0.027(4) 0.010(4) N1 0.035(3) 0.021(4) 0.061(4) 0.000(3) 0.017(3) -0.003(3) C1 0.053(7) 0.093(8) 0.055(6) 0.008(5) -0.012(5) -0.011(6) C2 0.071(6) 0.039(6) 0.031(5) 0.002(4) 0.004(5) -0.005(5) C3 0.067(6) 0.058(7) 0.056(6) -0.010(5) -0.007(5) 0.010(6) C4 0.069(7) 0.041(6) 0.101(8) 0.014(5) 0.029(6) 0.005(5) C5 0.082(7) 0.048(6) 0.057(7) 0.005(5) 0.018(6) 0.014(5) C6 0.058(6) 0.060(7) 0.068(7) 0.007(6) 0.025(5) 0.013(5) C7 0.075(7) 0.090(9) 0.050(7) 0.008(5) 0.006(6) 0.013(6) C8 0.076(7) 0.037(6) 0.077(7) 0.010(5) 0.038(6) 0.014(5) C9 0.074(6) 0.056(7) 0.061(7) 0.004(5) 0.015(5) 0.014(6) C10 0.039(3) 0.040(3) 0.045(3) 0.001(2) 0.014(2) -0.001(2) C11 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C12 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C13 0.057(3) 0.089(4) 0.058(4) -0.009(3) 0.015(3) 0.008(3) C14 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C15 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C16 0.039(3) 0.040(3) 0.045(3) 0.001(2) 0.014(2) -0.001(2) C17 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C18 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C19 0.057(3) 0.089(4) 0.058(4) -0.009(3) 0.015(3) 0.008(3) C20 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C21 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C22 0.039(3) 0.040(3) 0.045(3) 0.001(2) 0.014(2) -0.001(2) C23 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C24 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C25 0.057(3) 0.089(4) 0.058(4) -0.009(3) 0.015(3) 0.008(3) C26 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(15) C27 0.0626(18) 0.0561(18) 0.0590(18) -0.0032(15) 0.0170(13) -0.0008(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 Ru1 C3 1.822(8) . ? Ru1 C1 1.872(8) . ? Ru1 C2 1.909(8) . ? Ru1 N1 2.097(5) . ? Ru1 Ru3 2.6588(9) . ? Ru1 Ru2 2.6667(9) . ? Ru2 C6 1.891(8) . ? Ru2 C4 1.913(8) . ? Ru2 C5 1.914(8) . ? Ru2 N1 2.113(5) . ? Ru2 Ru3 2.8179(8) . ? Ru2 H1 1.85(6) . ? Ru3 C9 1.867(9) . ? Ru3 C8 1.875(8) . ? Ru3 C7 1.918(9) . ? Ru3 N1 2.119(5) . ? Ru3 H1 1.92(6) . ? P1 N1 1.631(5) . ? P1 C22 1.792(7) . ? P1 C16 1.793(7) . ? P1 C10 1.807(6) . ? O1 C1 1.150(7) . ? O2 C2 1.130(7) . ? O3 C3 1.170(8) . ? O4 C4 1.113(7) . ? O5 C5 1.137(8) . ? O6 C6 1.117(8) . ? O7 C7 1.145(8) . ? O8 C8 1.130(7) . ? O9 C9 1.145(8) . ? C10 C11 1.359(8) . ? C10 C15 1.399(8) . ? C11 C12 1.386(8) . ? C11 H11 0.9300 . ? C12 C13 1.366(9) . ? C12 H12 0.9300 . ? C13 C14 1.363(8) . ? C13 H13 0.9300 . ? C14 C15 1.376(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.350(9) . ? C16 C17 1.385(9) . ? C17 C18 1.364(8) . ? C17 H17 0.9300 . ? C18 C19 1.380(9) . ? C18 H18 0.9300 . ? C19 C20 1.367(9) . ? C19 H19 0.9300 . ? C20 C21 1.406(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.365(9) . ? C22 C27 1.393(8) . ? C23 C24 1.380(8) . ? C23 H23 0.9300 . ? C24 C25 1.360(9) . ? C24 H24 0.9300 . ? C25 C26 1.369(10) . ? C25 H25 0.9300 . ? C26 C27 1.364(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? 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 C3 Ru1 C1 92.8(4) . . ? C3 Ru1 C2 95.7(3) . . ? C1 Ru1 C2 97.5(4) . . ? C3 Ru1 N1 143.7(3) . . ? C1 Ru1 N1 112.5(3) . . ? C2 Ru1 N1 105.8(3) . . ? C3 Ru1 Ru3 96.3(3) . . ? C1 Ru1 Ru3 157.8(3) . . ? C2 Ru1 Ru3 101.6(2) . . ? N1 Ru1 Ru3 51.27(14) . . ? C3 Ru1 Ru2 103.7(3) . . ? C1 Ru1 Ru2 94.3(3) . . ? C2 Ru1 Ru2 156.7(2) . . ? N1 Ru1 Ru2 50.97(14) . . ? Ru3 Ru1 Ru2 63.89(2) . . ? C6 Ru2 C4 89.6(3) . . ? C6 Ru2 C5 101.0(3) . . ? C4 Ru2 C5 94.5(4) . . ? C6 Ru2 N1 145.7(3) . . ? C4 Ru2 N1 102.5(3) . . ? C5 Ru2 N1 109.6(3) . . ? C6 Ru2 Ru1 97.6(3) . . ? C4 Ru2 Ru1 93.0(3) . . ? C5 Ru2 Ru1 159.9(2) . . ? N1 Ru2 Ru1 50.44(13) . . ? C6 Ru2 Ru3 107.7(2) . . ? C4 Ru2 Ru3 147.2(3) . . ? C5 Ru2 Ru3 108.6(2) . . ? N1 Ru2 Ru3 48.34(14) . . ? Ru1 Ru2 Ru3 57.92(2) . . ? C6 Ru2 H1 85.8(19) . . ? C4 Ru2 H1 170.2(19) . . ? C5 Ru2 H1 77.9(17) . . ? N1 Ru2 H1 86.0(19) . . ? Ru1 Ru2 H1 96.2(18) . . ? Ru3 Ru2 H1 42.6(19) . . ? C9 Ru3 C8 88.8(3) . . ? C9 Ru3 C7 96.1(4) . . ? C8 Ru3 C7 97.2(4) . . ? C9 Ru3 N1 148.0(3) . . ? C8 Ru3 N1 102.6(3) . . ? C7 Ru3 N1 111.6(3) . . ? C9 Ru3 Ru1 101.1(3) . . ? C8 Ru3 Ru1 88.1(3) . . ? C7 Ru3 Ru1 162.1(3) . . ? N1 Ru3 Ru1 50.55(13) . . ? C9 Ru3 Ru2 107.5(2) . . ? C8 Ru3 Ru2 144.4(2) . . ? C7 Ru3 Ru2 111.8(3) . . ? N1 Ru3 Ru2 48.17(14) . . ? Ru1 Ru3 Ru2 58.19(2) . . ? C9 Ru3 H1 84.3(18) . . ? C8 Ru3 H1 173.0(19) . . ? C7 Ru3 H1 82.1(16) . . ? N1 Ru3 H1 84.1(19) . . ? Ru1 Ru3 H1 94.6(17) . . ? Ru2 Ru3 H1 40.6(18) . . ? N1 P1 C22 112.5(3) . . ? N1 P1 C16 114.6(3) . . ? C22 P1 C16 103.6(3) . . ? N1 P1 C10 110.3(3) . . ? C22 P1 C10 108.1(3) . . ? C16 P1 C10 107.4(3) . . ? P1 N1 Ru1 128.5(3) . . ? P1 N1 Ru2 128.5(3) . . ? Ru1 N1 Ru2 78.59(17) . . ? P1 N1 Ru3 138.2(3) . . ? Ru1 N1 Ru3 78.19(18) . . ? Ru2 N1 Ru3 83.5(2) . . ? O1 C1 Ru1 174.7(8) . . ? O2 C2 Ru1 178.6(8) . . ? O3 C3 Ru1 178.4(8) . . ? O4 C4 Ru2 174.3(9) . . ? O5 C5 Ru2 178.0(8) . . ? O6 C6 Ru2 178.1(8) . . ? O7 C7 Ru3 171.7(9) . . ? O8 C8 Ru3 174.3(8) . . ? O9 C9 Ru3 177.2(8) . . ? C11 C10 C15 119.7(7) . . ? C11 C10 P1 121.7(6) . . ? C15 C10 P1 118.6(6) . . ? C10 C11 C12 121.5(7) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 118.2(8) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C14 C13 C12 121.3(8) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 120.7(8) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 118.6(7) . . ? C14 C15 H15 120.7 . . ? C10 C15 H15 120.7 . . ? C21 C16 C17 118.7(7) . . ? C21 C16 P1 122.7(6) . . ? C17 C16 P1 118.6(6) . . ? C18 C17 C16 121.4(8) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 120.0(8) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.4(8) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 119.8(8) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 120.7(8) . . ? C16 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C27 118.4(7) . . ? C23 C22 P1 124.1(6) . . ? C27 C22 P1 117.5(6) . . ? C22 C23 C24 122.0(8) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C25 C24 C23 118.1(8) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C24 C25 C26 121.4(8) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 120.0(8) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.0(8) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.81 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.488 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.098