Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email KBNOLAN@RCSI.IE _publ_contact_author_name 'Prof Kevin Nolan' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name K.Nolan J.Comiskey E.Farkas K.A.Krot-Lacina C.McAuliffe ; R.G.Pritchard ; data_new _database_code_CSD 210644 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 N3 O11 Ru1, 4.91(H2 O1)' _chemical_formula_sum 'C18 H31.82 N3 O15.91 Ru' _chemical_formula_weight 645.91 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' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.700(6) _cell_length_b 8.5319(9) _cell_length_c 15.292(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.264(10) _cell_angle_gamma 90.00 _cell_volume 5226.2(12) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19394 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656.8 _exptl_absorpt_coefficient_mu 0.68 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 1.056 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10672 _diffrn_reflns_av_R_equivalents 0.1962 _diffrn_reflns_av_sigmaI/netI 0.1623 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 23.59 _reflns_number_total 3739 _reflns_number_gt 2140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (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^)+(0.0300P)^2^+329.1807P] 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 SHELXL _refine_ls_extinction_coef 0.00093(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3739 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2074 _refine_ls_R_factor_gt 0.1252 _refine_ls_wR_factor_ref 0.3133 _refine_ls_wR_factor_gt 0.2490 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.256 _refine_ls_shift/su_mean 0.006 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 0.146990(11) 0.42968(6) 0.54011(3) 0.04599(12) Uani 1 1 d . . . C1 C 0.19664(12) 0.3865(8) 0.4644(3) 0.055(2) Uani 1 1 d . . . C2 C 0.21606(13) 0.3310(7) 0.4070(3) 0.0503(18) Uani 1 1 d . . . C3 C 0.20333(12) 0.1920(8) 0.3542(3) 0.055(2) Uani 1 1 d . . . H3 H 0.1846 0.1422 0.3590 0.066 Uiso 1 1 calc R . . C4 C 0.21915(15) 0.1317(9) 0.2956(4) 0.063(2) Uani 1 1 d . . . H4 H 0.2098 0.0479 0.2563 0.076 Uiso 1 1 calc R . . C5 C 0.24857(13) 0.1971(8) 0.2962(3) 0.057(2) Uani 1 1 d . . . H5 H 0.2596 0.1528 0.2594 0.068 Uiso 1 1 calc R . . C6 C 0.26236(15) 0.3268(8) 0.3500(4) 0.063(2) Uani 1 1 d . . . H6 H 0.2823 0.3696 0.3494 0.076 Uiso 1 1 calc R . . C7 C 0.24554(12) 0.3927(7) 0.4059(3) 0.0497(18) Uani 1 1 d . . . C8 C 0.29090(11) 0.5769(8) 0.4725(4) 0.0543(18) Uani 1 1 d . . . H8A H 0.3061 0.4898 0.4874 0.081 Uiso 1 1 calc R . . H8B H 0.2980 0.6530 0.5217 0.081 Uiso 1 1 calc R . . H8C H 0.2907 0.6239 0.4152 0.081 Uiso 1 1 calc R . . C9 C 0.09234(12) 0.5027(7) 0.6023(3) 0.0485(16) Uani 1 1 d . . . H9A H 0.0805 0.5721 0.5514 0.058 Uiso 1 1 calc R . . H9B H 0.0841 0.5205 0.6531 0.058 Uiso 1 1 calc R . . C10 C 0.08632(12) 0.3304(7) 0.5699(4) 0.0506(19) Uani 1 1 d . . . H10A H 0.0977 0.2604 0.6210 0.061 Uiso 1 1 calc R . . H10B H 0.0626 0.3066 0.5483 0.061 Uiso 1 1 calc R . . C11 C 0.14866(14) 0.4646(8) 0.7289(3) 0.055(2) Uani 1 1 d . . . H11A H 0.1651 0.5403 0.7644 0.066 Uiso 1 1 calc R . . H11B H 0.1335 0.4456 0.7625 0.066 Uiso 1 1 calc R . . C12 C 0.16543(13) 0.3208(8) 0.7242(4) 0.0536(19) Uani 1 1 d . . . C13 C 0.13391(14) 0.7121(7) 0.6354(3) 0.0532(19) Uani 1 1 d . . . H13A H 0.1576 0.7334 0.6531 0.064 Uiso 1 1 calc R . . H13B H 0.1232 0.7520 0.5727 0.064 Uiso 1 1 calc R . . C14 C 0.12064(14) 0.8009(7) 0.7002(4) 0.0547(19) Uani 1 1 d . . . C15 C 0.07792(13) 0.3884(8) 0.4052(4) 0.053(2) Uani 1 1 d . . . H15A H 0.0566 0.4140 0.4112 0.064 Uiso 1 1 calc R . . H15B H 0.0737 0.3142 0.3544 0.064 Uiso 1 1 calc R . . C16 C 0.09294(14) 0.5401(10) 0.3794(4) 0.070(2) Uani 1 1 d . . . C17 C 0.10429(12) 0.1438(7) 0.4794(4) 0.0504(18) Uani 1 1 d . . . H17A H 0.1141 0.1332 0.4312 0.060 Uiso 1 1 calc R . . H17B H 0.1200 0.1007 0.5365 0.060 Uiso 1 1 calc R . . C18 C 0.07347(14) 0.0523(8) 0.4528(3) 0.060(2) Uani 1 1 d . . . N1 N 0.20721(11) 0.5059(6) 0.5219(3) 0.0537(16) Uani 1 1 d . . . H1 H 0.2257 0.5524 0.5274 0.064 Uiso 1 1 calc R . . N2 N 0.12893(9) 0.5361(5) 0.6340(3) 0.0418(13) Uani 1 1 d . . . N3 N 0.09952(10) 0.3106(5) 0.4937(3) 0.0457(14) Uani 1 1 d . . . O1 O 0.16756(9) 0.3218(5) 0.4555(2) 0.0539(13) Uani 1 1 d . . . O2 O 0.18813(8) 0.5541(5) 0.5726(2) 0.0570(13) Uani 1 1 d . . . O3 O 0.25685(9) 0.5212(5) 0.4618(2) 0.0595(14) Uani 1 1 d . . . O4 O 0.16591(9) 0.2753(5) 0.6450(2) 0.0519(12) Uani 1 1 d . . . O5 O 0.17911(9) 0.2491(5) 0.7966(2) 0.0604(14) Uani 1 1 d . . . O6 O 0.12623(10) 0.9532(5) 0.6945(2) 0.0671(15) Uani 1 1 d . . . H6A H 0.1097 0.9942 0.6565 0.101 Uiso 1 1 calc R . . O7 O 0.10921(10) 0.7470(5) 0.7533(2) 0.0638(14) Uani 1 1 d . . . O8 O 0.12279(8) 0.5768(5) 0.4324(2) 0.0497(11) Uani 1 1 d . . . O9 O 0.07628(10) 0.6092(5) 0.3088(2) 0.0649(15) Uani 1 1 d . . . O10 O 0.04528(9) 0.1041(5) 0.4356(3) 0.0598(14) Uani 1 1 d . . . O11 O 0.07897(10) -0.1044(5) 0.4525(3) 0.0680(16) Uani 1 1 d . . . H11 H 0.0610 -0.1505 0.4320 0.102 Uiso 1 1 calc R . . O12 O 0.12704(11) 0.1169(6) 0.8391(3) 0.0865(17) Uani 1 1 d . . . O13 O -0.02937(13) -0.2820(7) 0.0668(5) 0.089(3) Uani 0.805(10) 1 d P . . O14A O -0.0160(2) -0.5398(12) -0.2080(5) 0.106(4) Uani 0.637(11) 1 d P . . O14B O -0.0212(2) -0.4166(15) -0.1819(6) 0.078(4) Uani 0.425(9) 1 d P . . O14C O -0.0110(3) -0.3025(19) -0.0788(9) 0.138(6) Uani 0.458(11) 1 d P . . O15A O 0.0373(2) -0.073(2) 0.1943(7) 0.333(9) Uani 1.000(18) 1 d . . . O15B O 0.0224(3) 0.1031(19) 0.1359(10) 0.040(4) Uiso 0.214(7) 1 d P . . O15C O 0.0176(5) 0.107(3) 0.1966(13) 0.132(7) Uiso 0.362(12) 1 d P . . 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 0.04841(18) 0.0503(2) 0.04283(17) 0.0002(2) 0.02026(13) -0.0007(3) C1 0.043(2) 0.097(5) 0.030(2) 0.014(3) 0.0204(16) 0.012(3) C2 0.068(3) 0.047(3) 0.046(2) -0.004(2) 0.0317(19) -0.003(3) C3 0.033(2) 0.087(5) 0.050(3) -0.007(3) 0.0199(18) 0.006(3) C4 0.067(3) 0.083(5) 0.036(3) -0.015(3) 0.013(2) -0.002(3) C5 0.055(3) 0.086(5) 0.035(2) -0.019(3) 0.0249(18) -0.013(3) C6 0.073(3) 0.062(4) 0.065(3) 0.019(3) 0.037(2) 0.018(3) C7 0.045(2) 0.060(4) 0.045(2) 0.005(3) 0.0176(19) 0.015(3) C8 0.043(2) 0.055(3) 0.071(3) 0.013(3) 0.0264(19) -0.010(3) C9 0.055(2) 0.053(3) 0.055(2) 0.014(2) 0.0413(16) 0.014(2) C10 0.040(2) 0.049(4) 0.065(3) 0.001(3) 0.021(2) -0.002(3) C11 0.056(3) 0.081(5) 0.026(2) -0.002(3) 0.0114(19) 0.003(3) C12 0.048(3) 0.073(4) 0.044(2) -0.001(3) 0.0217(19) -0.001(3) C13 0.071(3) 0.063(4) 0.030(2) 0.005(2) 0.0229(19) -0.014(3) C14 0.081(3) 0.042(3) 0.049(3) -0.001(3) 0.032(2) 0.015(3) C15 0.038(3) 0.069(4) 0.051(3) -0.003(3) 0.013(2) 0.000(3) C16 0.046(3) 0.114(6) 0.048(3) -0.014(4) 0.016(2) 0.003(4) C17 0.042(3) 0.049(3) 0.064(3) -0.001(3) 0.023(2) 0.002(3) C18 0.063(3) 0.076(4) 0.042(2) -0.007(3) 0.020(2) 0.015(3) N1 0.058(2) 0.053(3) 0.050(2) -0.020(2) 0.0179(18) -0.012(2) N2 0.047(2) 0.043(3) 0.0376(18) 0.0078(18) 0.0175(15) -0.0126(19) N3 0.058(2) 0.036(3) 0.047(2) 0.004(2) 0.0229(16) 0.001(2) O1 0.070(2) 0.065(3) 0.0306(14) 0.0001(17) 0.0235(13) -0.004(2) O2 0.0475(17) 0.071(3) 0.0583(18) -0.012(2) 0.0263(13) -0.010(2) O3 0.065(2) 0.063(3) 0.0506(19) -0.0021(19) 0.0196(16) 0.003(2) O4 0.0582(19) 0.051(2) 0.0504(17) 0.0000(18) 0.0233(14) -0.0084(19) O5 0.066(2) 0.067(3) 0.0510(18) 0.011(2) 0.0232(15) 0.007(2) O6 0.104(3) 0.046(2) 0.0588(19) 0.0076(19) 0.0374(17) 0.014(2) O7 0.081(2) 0.070(3) 0.0489(17) -0.001(2) 0.0333(15) 0.000(2) O8 0.0713(19) 0.042(2) 0.0426(15) -0.0064(17) 0.0286(13) -0.005(2) O9 0.072(2) 0.071(3) 0.0517(19) 0.023(2) 0.0212(16) 0.009(2) O10 0.0489(19) 0.048(3) 0.079(2) 0.003(2) 0.0183(17) 0.0010(19) O11 0.060(2) 0.045(3) 0.095(3) 0.012(2) 0.0214(19) -0.007(2) O12 0.119(3) 0.076(3) 0.090(2) -0.020(2) 0.0685(17) -0.008(3) O13 0.057(3) 0.065(4) 0.139(5) 0.002(4) 0.029(3) 0.016(3) O14A 0.111(6) 0.119(8) 0.084(5) -0.002(5) 0.029(4) 0.014(6) O14B 0.071(6) 0.109(9) 0.048(5) -0.015(6) 0.013(4) -0.034(6) O14C 0.080(6) 0.200(13) 0.140(9) -0.049(9) 0.047(5) -0.086(7) O15A 0.149(6) 0.65(2) 0.178(8) 0.069(12) 0.029(6) 0.169(9) _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 O2 1.964(4) . ? Ru1 O4 2.016(4) . ? Ru1 O1 2.019(4) . ? Ru1 O8 2.044(3) . ? Ru1 N2 2.060(4) . ? Ru1 N3 2.156(4) . ? C1 O1 1.323(7) . ? C1 N1 1.319(8) . ? C1 C2 1.479(8) . ? C2 C7 1.370(8) . ? C2 C3 1.432(8) . ? C3 C4 1.394(9) . ? C4 C5 1.371(9) . ? C5 C6 1.383(9) . ? C6 C7 1.409(9) . ? C7 O3 1.372(7) . ? C8 O3 1.484(7) . ? C9 N2 1.494(6) . ? C9 C10 1.544(8) . ? C10 N3 1.470(8) . ? C11 C12 1.435(9) . ? C11 N2 1.530(6) . ? C12 O5 1.222(6) . ? C12 O4 1.278(7) . ? C13 C14 1.505(9) . ? C13 N2 1.516(8) . ? C14 O7 1.177(8) . ? C14 O6 1.329(7) . ? C15 N3 1.502(6) . ? C15 C16 1.555(10) . ? C16 O9 1.220(7) . ? C16 O8 1.290(6) . ? C17 C18 1.462(8) . ? C17 N3 1.465(7) . ? C18 O10 1.222(7) . ? C18 O11 1.358(8) . ? N1 O2 1.368(7) . ? O14A O14B 1.174(16) . ? O14B O14C 1.773(18) . ? O15A O15B 1.75(2) . ? O15A O15C 1.75(3) . ? O15B O15C 1.02(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 O2 Ru1 O4 94.32(15) . . ? O2 Ru1 O1 81.89(16) . . ? O4 Ru1 O1 93.93(16) . . ? O2 Ru1 O8 91.71(15) . . ? O4 Ru1 O8 173.75(15) . . ? O1 Ru1 O8 88.54(15) . . ? O2 Ru1 N2 95.95(16) . . ? O4 Ru1 N2 82.95(16) . . ? O1 Ru1 N2 176.08(13) . . ? O8 Ru1 N2 94.80(15) . . ? O2 Ru1 N3 174.16(16) . . ? O4 Ru1 N3 91.50(15) . . ? O1 Ru1 N3 98.16(17) . . ? O8 Ru1 N3 82.46(15) . . ? N2 Ru1 N3 84.33(17) . . ? O1 C1 N1 118.9(5) . . ? O1 C1 C2 120.4(5) . . ? N1 C1 C2 120.7(5) . . ? C7 C2 C3 118.8(5) . . ? C7 C2 C1 126.2(5) . . ? C3 C2 C1 114.7(5) . . ? C4 C3 C2 119.6(6) . . ? C5 C4 C3 119.5(6) . . ? C4 C5 C6 122.0(6) . . ? C5 C6 C7 118.6(6) . . ? C2 C7 O3 115.2(5) . . ? C2 C7 C6 121.2(5) . . ? O3 C7 C6 123.6(5) . . ? N2 C9 C10 108.9(4) . . ? N3 C10 C9 107.3(5) . . ? C12 C11 N2 114.4(4) . . ? O5 C12 O4 123.2(6) . . ? O5 C12 C11 118.2(5) . . ? O4 C12 C11 118.6(5) . . ? C14 C13 N2 115.2(5) . . ? O7 C14 O6 123.7(6) . . ? O7 C14 C13 126.7(6) . . ? O6 C14 C13 109.4(5) . . ? N3 C15 C16 114.7(4) . . ? O9 C16 O8 125.8(7) . . ? O9 C16 C15 117.5(5) . . ? O8 C16 C15 116.6(5) . . ? C18 C17 N3 113.7(5) . . ? O10 C18 O11 120.9(6) . . ? O10 C18 C17 126.3(6) . . ? O11 C18 C17 112.7(5) . . ? C1 N1 O2 118.5(5) . . ? C9 N2 C13 108.6(4) . . ? C9 N2 C11 113.7(4) . . ? C13 N2 C11 110.6(4) . . ? C9 N2 Ru1 107.0(3) . . ? C13 N2 Ru1 111.3(3) . . ? C11 N2 Ru1 105.6(3) . . ? C17 N3 C10 109.9(5) . . ? C17 N3 C15 111.6(4) . . ? C10 N3 C15 112.2(4) . . ? C17 N3 Ru1 110.1(3) . . ? C10 N3 Ru1 105.1(3) . . ? C15 N3 Ru1 107.6(3) . . ? C1 O1 Ru1 110.2(3) . . ? N1 O2 Ru1 110.5(3) . . ? C7 O3 C8 116.4(5) . . ? C12 O4 Ru1 115.0(4) . . ? C16 O8 Ru1 118.1(4) . . ? O14A O14B O14C 141.0(9) . . ? O15B O15A O15C 33.8(9) . . ? O15C O15B O15A 73.3(15) . . ? O15B O15C O15A 73.0(16) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 23.59 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.197 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.166