# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1999 data_GS _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety trans-[Ru(NO)(H2O)(en)2]Cl3 _chemical_formula_sum 'C4 H18 Cl3 N5 O2 Ru' _chemical_formula_weight 375.65 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' 'Cl' 'Cl' 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 15.4564(3) _cell_length_b 8.4266(2) _cell_length_c 10.0560(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1309.74(5) _cell_formula_units_Z 4 _cell_measurement_temperature 106(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 20 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.800 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7034 _exptl_absorpt_correction_T_max 0.8642 _exptl_absorpt_process_details 'Absorption was corrected by SADABS. ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 106(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector system' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 137274 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 65.70 _reflns_number_total 22136 _reflns_number_gt 20247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT & SADABS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens 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^)+(0.0170P)^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 SHELXL _refine_ls_extinction_coef 0.0578(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(6) _refine_ls_number_reflns 22136 _refine_ls_number_parameters 209 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0322 _refine_ls_wR_factor_gt 0.0316 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 -0.107505(1) -0.280848(2) -0.303713(4) 0.00547(0) Uani 1 1 d . . . N1 N -0.00369(2) -0.35321(4) -0.33382(3) 0.00836(3) Uani 1 1 d . . . O1 O 0.06379(2) -0.40457(5) -0.35314(4) 0.01452(5) Uani 1 1 d . . . O2 O -0.229102(19) -0.19309(4) -0.26378(3) 0.00961(3) Uani 1 1 d . . . H1W H -0.2746(10) -0.2617(15) -0.2631(14) 0.017(3) Uiso 1 1 d . . . H2W H -0.2384(9) -0.1082(17) -0.3015(17) 0.029(3) Uiso 1 1 d . . . N2 N -0.16550(2) -0.49260(4) -0.37109(3) 0.00908(4) Uani 1 1 d . . . H2A H -0.1351(9) -0.5738(18) -0.3401(15) 0.025(3) Uiso 1 1 d . . . H2B H -0.2217(10) -0.4946(19) -0.3457(17) 0.033(4) Uiso 1 1 d . . . C1 C -0.16809(3) -0.48998(5) -0.51949(4) 0.01203(5) Uani 1 1 d . . . H1A H -0.2020(9) -0.5673(16) -0.5515(12) 0.019(3) Uiso 1 1 d . . . H1B H -0.1124(9) -0.5158(19) -0.5532(15) 0.024(3) Uiso 1 1 d . . . C2 C -0.19404(3) -0.32366(6) -0.56338(4) 0.01266(5) Uani 1 1 d . . . H2C H -0.1940(10) -0.3139(18) -0.6582(16) 0.029(3) Uiso 1 1 d . . . H2D H -0.2526(9) -0.2912(15) -0.5316(14) 0.019(3) Uiso 1 1 d . . . N3 N -0.13095(2) -0.20991(4) -0.50242(3) 0.00926(4) Uani 1 1 d . . . H3A H -0.1473(8) -0.1092(16) -0.5100(14) 0.019(3) Uiso 1 1 d . . . H3B H -0.0828(11) -0.2124(15) -0.5495(16) 0.020(3) Uiso 1 1 d . . . N4 N -0.06693(2) -0.06035(4) -0.22569(3) 0.00862(4) Uani 1 1 d . . . H4A H -0.0093(9) -0.0475(17) -0.2415(14) 0.023(3) Uiso 1 1 d . . . H4B H -0.0990(7) 0.0196(16) -0.2535(12) 0.012(2) Uiso 1 1 d . . . C3 C -0.07685(3) -0.06294(5) -0.07749(4) 0.01127(5) Uani 1 1 d . . . H3C H -0.1366(8) -0.0429(15) -0.0589(13) 0.015(3) Uiso 1 1 d . . . H3D H -0.0451(8) 0.0272(17) -0.0388(13) 0.020(3) Uiso 1 1 d . . . C4 C -0.05148(3) -0.22624(5) -0.02692(4) 0.01238(5) Uani 1 1 d . . . H4C H 0.0053(11) -0.2518(19) -0.0514(16) 0.029(3) Uiso 1 1 d . . . H4D H -0.0646(10) -0.2354(17) 0.0708(17) 0.025(3) Uiso 1 1 d . . . N5 N -0.10398(2) -0.34524(4) -0.10182(3) 0.00953(4) Uani 1 1 d . . . H5A H -0.1573(8) -0.3460(16) -0.0675(13) 0.016(2) Uiso 1 1 d . . . H5B H -0.0828(9) -0.4426(16) -0.1001(13) 0.018(3) Uiso 1 1 d . . . Cl1 Cl -0.230689(7) 0.114856(12) -0.402842(11) 0.01183(1) Uani 1 1 d . . . Cl2 Cl 0.032498(8) -0.314995(12) -0.675232(12) 0.01310(2) Uani 1 1 d . . . Cl3 Cl -0.361062(6) -0.443713(13) -0.259876(12) 0.01226(1) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.00541(1) 0.00492(1) 0.00609(1) -0.00007(1) 0.00034(1) 0.00015(0) N1 0.00731(8) 0.00788(8) 0.00989(8) -0.00093(7) 0.00037(7) 0.00095(6) O1 0.00851(9) 0.01540(12) 0.01965(13) -0.00184(10) 0.00222(9) 0.00391(8) O2 0.00734(7) 0.00906(8) 0.01243(9) 0.00014(7) 0.00127(7) 0.00067(6) N2 0.00910(9) 0.00749(8) 0.01065(9) -0.00067(7) -0.00022(7) -0.00062(7) C1 0.01424(13) 0.01071(12) 0.01116(11) -0.00300(10) -0.00117(10) -0.00105(10) C2 0.01391(13) 0.01351(14) 0.01058(11) -0.00033(10) -0.00367(10) -0.00022(11) N3 0.01064(10) 0.00903(9) 0.00810(8) 0.00070(7) 0.00013(7) 0.00088(7) N4 0.00896(8) 0.00701(8) 0.00988(9) -0.00054(7) 0.00039(7) -0.00065(7) C3 0.01452(13) 0.00925(11) 0.01005(10) -0.00214(9) 0.00059(10) -0.00079(10) C4 0.01553(14) 0.01201(13) 0.00959(11) -0.00034(10) -0.00253(10) 0.00023(11) N5 0.01221(10) 0.00802(8) 0.00835(8) 0.00085(7) 0.00083(8) 0.00052(8) Cl1 0.01373(3) 0.00965(3) 0.01209(3) 0.00053(2) -0.00144(3) 0.00244(2) Cl2 0.01661(4) 0.00788(3) 0.01481(3) 0.00023(3) 0.00561(3) 0.00236(3) Cl3 0.00805(3) 0.01356(3) 0.01518(3) 0.00125(3) 0.00062(2) -0.00174(2) _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 N1 1.7431(3) . ? Ru1 O2 2.0592(3) . ? Ru1 N5 2.1022(3) . ? Ru1 N2 2.1086(3) . ? Ru1 N4 2.1122(3) . ? Ru1 N3 2.1170(3) . ? N1 O1 1.1457(4) . ? N2 C1 1.4930(6) . ? C1 C2 1.5231(7) . ? C2 N3 1.4984(6) . ? N4 C3 1.4983(5) . ? C3 C4 1.5185(6) . ? C4 N5 1.4938(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 O2 178.593(15) . . ? N1 Ru1 N5 93.074(15) . . ? O2 Ru1 N5 85.871(14) . . ? N1 Ru1 N2 92.265(14) . . ? O2 Ru1 N2 88.772(13) . . ? N5 Ru1 N2 95.906(14) . . ? N1 Ru1 N4 95.674(14) . . ? O2 Ru1 N4 83.262(13) . . ? N5 Ru1 N4 81.988(13) . . ? N2 Ru1 N4 171.879(13) . . ? N1 Ru1 N3 95.303(15) . . ? O2 Ru1 N3 85.779(14) . . ? N5 Ru1 N3 171.458(14) . . ? N2 Ru1 N3 82.118(14) . . ? N4 Ru1 N3 98.805(13) . . ? O1 N1 Ru1 178.27(3) . . ? C1 N2 Ru1 108.67(2) . . ? N2 C1 C2 108.08(3) . . ? N3 C2 C1 107.38(3) . . ? C2 N3 Ru1 108.48(3) . . ? C3 N4 Ru1 109.04(2) . . ? N4 C3 C4 108.66(3) . . ? N5 C4 C3 107.41(3) . . ? C4 N5 Ru1 109.13(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Ru1 N1 O1 110.1(12) . . . . ? N5 Ru1 N1 O1 68.7(12) . . . . ? N2 Ru1 N1 O1 -27.4(12) . . . . ? N4 Ru1 N1 O1 150.9(12) . . . . ? N3 Ru1 N1 O1 -109.7(12) . . . . ? N1 Ru1 N2 C1 -80.50(3) . . . . ? O2 Ru1 N2 C1 100.46(3) . . . . ? N5 Ru1 N2 C1 -173.82(3) . . . . ? N4 Ru1 N2 C1 111.66(9) . . . . ? N3 Ru1 N2 C1 14.55(3) . . . . ? Ru1 N2 C1 C2 -41.65(4) . . . . ? N2 C1 C2 N3 55.82(4) . . . . ? C1 C2 N3 Ru1 -41.96(4) . . . . ? N1 Ru1 N3 C2 106.93(3) . . . . ? O2 Ru1 N3 C2 -73.97(3) . . . . ? N5 Ru1 N3 C2 -61.79(10) . . . . ? N2 Ru1 N3 C2 15.37(3) . . . . ? N4 Ru1 N3 C2 -156.48(3) . . . . ? N1 Ru1 N4 C3 -104.13(3) . . . . ? O2 Ru1 N4 C3 74.95(3) . . . . ? N5 Ru1 N4 C3 -11.81(3) . . . . ? N2 Ru1 N4 C3 63.67(10) . . . . ? N3 Ru1 N4 C3 159.59(3) . . . . ? Ru1 N4 C3 C4 38.55(4) . . . . ? N4 C3 C4 N5 -53.97(5) . . . . ? C3 C4 N5 Ru1 42.74(4) . . . . ? N1 Ru1 N5 C4 78.05(3) . . . . ? O2 Ru1 N5 C4 -101.02(3) . . . . ? N2 Ru1 N5 C4 170.65(3) . . . . ? N4 Ru1 N5 C4 -17.25(3) . . . . ? N3 Ru1 N5 C4 -113.20(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 65.70 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.510 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.103 #===END data_428nm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H18 Cl3 N5 O2 Ru' _chemical_formula_weight 375.65 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' 'Cl' 'Cl' 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 15.4889(3) _cell_length_b 8.4263(2) _cell_length_c 10.0578(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1312.68(5) _cell_formula_units_Z 4 _cell_measurement_temperature 106(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 20 _exptl_crystal_description block _exptl_crystal_colour 'brownish yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.796 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.7549 _exptl_absorpt_correction_T_max 0.8766 _exptl_absorpt_process_details 'Absorption was corrected by SADABS. ' _exptl_special_details ; ? ; _diffrn_ambient_temperature 106(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD area detector' _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 137867 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 65.65 _reflns_number_total 22032 _reflns_number_gt 19518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT & SADABS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material 'Siemens 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^)+(0.0192P)^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 SHELXL _refine_ls_extinction_coef 0.0125(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(7) _refine_ls_number_reflns 22032 _refine_ls_number_parameters 86 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0238 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0375 _refine_ls_wR_factor_gt 0.0367 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.003 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 0.107954(2) 0.280017(3) 0.303671(5) 0.00545(0) Uani 1 1 d G . . N1 N 0.004414(9) 0.35258(4) 0.33393(3) 0.008 Uani 0.920(4) 1 d PG A 1 O1 O -0.062873(15) 0.40408(7) 0.35334(5) 0.015 Uani 0.920(4) 1 d PG A 1 O2 O 0.229217(11) 0.19202(5) 0.26356(4) 0.010 Uani 0.920(4) 1 d PG A 1 H1W H 0.2747 0.2606 0.2628 0.017 Uiso 0.920(4) 1 d PG A 1 H2W H 0.2385 0.1071 0.3012 0.029 Uiso 0.920(4) 1 d PG A 1 N2 N 0.16599(2) 0.49165(3) 0.37097(4) 0.009 Uani 0.920(4) 1 d PG A 1 H2A H 0.1356 0.5729 0.3400 0.025 Uiso 0.920(4) 1 d PG A 1 H2B H 0.2220 0.4935 0.3455 0.033 Uiso 0.920(4) 1 d PG A 1 C1 C 0.16867(3) 0.48901(6) 0.51934(4) 0.012 Uani 0.920(4) 1 d PG A 1 H1A H 0.2025 0.5663 0.5513 0.019 Uiso 0.920(4) 1 d PG A 1 H1B H 0.1131 0.5150 0.5531 0.024 Uiso 0.920(4) 1 d PG A 1 C2 C 0.19449(3) 0.32262(8) 0.56317(3) 0.013 Uani 0.920(4) 1 d PG A 1 H2C H 0.1945 0.3129 0.6579 0.029 Uiso 0.920(4) 1 d PG A 1 H2D H 0.2529 0.2900 0.5313 0.019 Uiso 0.920(4) 1 d PG A 1 N3 N 0.13143(3) 0.20901(5) 0.502304(15) 0.009 Uani 0.920(4) 1 d PG A 1 H3A H 0.1477 0.1083 0.5098 0.019 Uiso 0.920(4) 1 d PG A 1 H3B H 0.0834 0.2116 0.5494 0.021 Uiso 0.920(4) 1 d PG A 1 N4 N 0.06728(3) 0.05960(3) 0.22570(4) 0.009 Uani 0.920(4) 1 d PG A 1 H4A H 0.0098 0.0469 0.2415 0.023 Uiso 0.920(4) 1 d PG A 1 H4B H 0.0993 -0.0204 0.2534 0.012 Uiso 0.920(4) 1 d PG A 1 C3 C 0.07709(3) 0.06220(6) 0.07752(4) 0.011 Uani 0.920(4) 1 d PG A 1 H3C H 0.1367 0.0420 0.0589 0.015 Uiso 0.920(4) 1 d PG A 1 H3D H 0.0453 -0.0279 0.0388 0.020 Uiso 0.920(4) 1 d PG A 1 C4 C 0.05184(3) 0.22555(8) 0.02701(2) 0.012 Uani 0.920(4) 1 d PG A 1 H4C H -0.0048 0.2512 0.0515 0.029 Uiso 0.920(4) 1 d PG A 1 H4D H 0.0649 0.2347 -0.0708 0.025 Uiso 0.920(4) 1 d PG A 1 N5 N 0.10436(3) 0.34444(5) 0.101824(13) 0.010 Uani 0.920(4) 1 d PG A 1 H5A H 0.1576 0.3451 0.0675 0.016 Uiso 0.920(4) 1 d PG A 1 H5B H 0.0833 0.4418 0.1002 0.018 Uiso 0.920(4) 1 d PG A 1 O1E O -0.0014(3) 0.3543(5) 0.3357(4) 0.0022(5) Uiso 0.080(4) 1 d P A 2 N1E N -0.0702(4) 0.4067(8) 0.3551(6) 0.0070(6) Uiso 0.080(4) 1 d P A 2 O2E O 0.2281(3) 0.1930(8) 0.2648(6) 0.0083(5) Uiso 0.080(4) 1 d P A 2 N2E N 0.1625(3) 0.4961(5) 0.3705(5) 0.0037(5) Uiso 0.080(4) 1 d P A 2 C1E C 0.1645(4) 0.4958(7) 0.5204(6) 0.0058(6) Uiso 0.080(4) 1 d P A 2 C2E C 0.1914(4) 0.3292(8) 0.5658(6) 0.0064(6) Uiso 0.080(4) 1 d P A 2 N3E N 0.1291(4) 0.2148(7) 0.5041(4) 0.0053(5) Uiso 0.080(4) 1 d P A 2 N4E N 0.0637(4) 0.0585(6) 0.2280(6) 0.0053(5) Uiso 0.080(4) 1 d P A 2 C3E C 0.0739(5) 0.0605(8) 0.0775(6) 0.0069(6) Uiso 0.080(4) 1 d P A 2 C4E C 0.0480(4) 0.2237(9) 0.0280(6) 0.0072(6) Uiso 0.080(4) 1 d P A 2 N5E N 0.1010(4) 0.3436(7) 0.1014(4) 0.0055(5) Uiso 0.080(4) 1 d P A 2 Cl1 Cl 0.230695(9) -0.115499(16) 0.402965(13) 0.01146(2) Uani 1 1 d . . . Cl2 Cl -0.032056(10) 0.316004(16) 0.675337(15) 0.01294(2) Uani 1 1 d . . . Cl3 Cl 0.361183(8) 0.442330(16) 0.260103(15) 0.01183(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.00577(1) 0.00512(1) 0.00547(1) -0.00005(1) 0.00025(1) -0.00008(1) N1 0.007 0.008 0.010 -0.001 0.000 0.001 O1 0.009 0.015 0.020 -0.002 0.002 0.004 O2 0.007 0.009 0.012 0.000 0.001 0.001 N2 0.009 0.007 0.011 -0.001 0.000 -0.001 C1 0.014 0.011 0.011 -0.003 -0.001 -0.001 C2 0.014 0.014 0.011 0.000 -0.004 0.000 N3 0.011 0.009 0.008 0.001 0.000 0.001 N4 0.009 0.007 0.010 -0.001 0.000 -0.001 C3 0.015 0.009 0.010 -0.002 0.001 -0.001 C4 0.016 0.012 0.010 0.000 -0.003 0.000 N5 0.012 0.008 0.008 0.001 0.001 0.001 Cl1 0.01358(4) 0.00964(3) 0.01117(4) 0.00054(3) -0.00135(3) 0.00239(3) Cl2 0.01661(5) 0.00793(3) 0.01430(4) 0.00027(3) 0.00588(4) 0.00252(3) Cl3 0.00785(3) 0.01359(4) 0.01406(4) 0.00111(4) 0.00061(3) -0.00173(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 N1 1.7431 . ? Ru1 O1E 1.834(4) . ? Ru1 O2E 2.039(5) . ? Ru1 O2 2.0592 . ? Ru1 N5 2.1022 . ? Ru1 N5E 2.107(4) . ? Ru1 N2 2.1086 . ? Ru1 N4 2.1122 . ? Ru1 N3E 2.115(4) . ? Ru1 N2E 2.116(4) . ? Ru1 N3 2.1169 . ? Ru1 N4E 2.129(4) . ? N1 O1 1.1457 . ? N2 C1 1.4930 . ? C1 C2 1.5231 . ? C2 N3 1.4984 . ? N4 C3 1.4983 . ? C3 C4 1.5185 . ? C4 N5 1.4938 . ? O1E N1E 1.169(6) . ? N2E C1E 1.507(6) . ? C1E C2E 1.533(7) . ? C2E N3E 1.499(7) . ? N4E C3E 1.523(7) . ? C3E C4E 1.516(8) . ? C4E N5E 1.496(7) . ? 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 N1 Ru1 O1E 0.57(13) . . ? N1 Ru1 O2E 178.83(17) . . ? O1E Ru1 O2E 178.49(17) . . ? N1 Ru1 O2 178.6 . . ? O1E Ru1 O2 178.29(12) . . ? O2E Ru1 O2 0.25(18) . . ? N1 Ru1 N5 93.1 . . ? O1E Ru1 N5 93.26(12) . . ? O2E Ru1 N5 86.09(18) . . ? O2 Ru1 N5 85.9 . . ? N1 Ru1 N5E 91.85(16) . . ? O1E Ru1 N5E 92.03(16) . . ? O2E Ru1 N5E 87.30(18) . . ? O2 Ru1 N5E 87.08(16) . . ? N5 Ru1 N5E 1.43(16) . . ? N1 Ru1 N2 92.3 . . ? O1E Ru1 N2 92.78(12) . . ? O2E Ru1 N2 88.64(19) . . ? O2 Ru1 N2 88.8 . . ? N5 Ru1 N2 95.9 . . ? N5E Ru1 N2 96.70(17) . . ? N1 Ru1 N4 95.7 . . ? O1E Ru1 N4 95.16(12) . . ? O2E Ru1 N4 83.40(19) . . ? O2 Ru1 N4 83.3 . . ? N5 Ru1 N4 82.0 . . ? N5E Ru1 N4 81.37(17) . . ? N2 Ru1 N4 171.9 . . ? N1 Ru1 N3E 93.85(16) . . ? O1E Ru1 N3E 93.70(17) . . ? O2E Ru1 N3E 87.02(18) . . ? O2 Ru1 N3E 87.24(16) . . ? N5 Ru1 N3E 172.61(17) . . ? N5E Ru1 N3E 174.01(19) . . ? N2 Ru1 N3E 81.26(17) . . ? N4 Ru1 N3E 99.87(17) . . ? N1 Ru1 N2E 90.56(14) . . ? O1E Ru1 N2E 91.08(15) . . ? O2E Ru1 N2E 90.34(19) . . ? O2 Ru1 N2E 90.47(15) . . ? N5 Ru1 N2E 95.47(15) . . ? N5E Ru1 N2E 96.23(16) . . ? N2 Ru1 N2E 1.78(14) . . ? N4 Ru1 N2E 173.37(15) . . ? N3E Ru1 N2E 81.89(16) . . ? N1 Ru1 N3 95.3 . . ? O1E Ru1 N3 95.14(12) . . ? O2E Ru1 N3 85.56(18) . . ? O2 Ru1 N3 85.8 . . ? N5 Ru1 N3 171.5 . . ? N5E Ru1 N3 172.79(16) . . ? N2 Ru1 N3 82.1 . . ? N4 Ru1 N3 98.8 . . ? N3E Ru1 N3 1.71(17) . . ? N2E Ru1 N3 82.80(15) . . ? N1 Ru1 N4E 94.23(17) . . ? O1E Ru1 N4E 93.72(17) . . ? O2E Ru1 N4E 84.85(19) . . ? O2 Ru1 N4E 84.72(17) . . ? N5 Ru1 N4E 82.69(17) . . ? N5E Ru1 N4E 82.04(17) . . ? N2 Ru1 N4E 173.42(18) . . ? N4 Ru1 N4E 1.58(18) . . ? N3E Ru1 N4E 99.35(17) . . ? N2E Ru1 N4E 174.9(2) . . ? N3 Ru1 N4E 98.32(17) . . ? O1 N1 Ru1 178.3 . . ? C1 N2 Ru1 108.7 . . ? N2 C1 C2 108.1 . . ? N3 C2 C1 107.4 . . ? C2 N3 Ru1 108.5 . . ? C3 N4 Ru1 109.0 . . ? N4 C3 C4 108.7 . . ? N5 C4 C3 107.4 . . ? C4 N5 Ru1 109.1 . . ? N1E O1E Ru1 177.8(3) . . ? C1E N2E Ru1 108.9(3) . . ? N2E C1E C2E 107.8(4) . . ? N3E C2E C1E 106.9(4) . . ? C2E N3E Ru1 109.1(3) . . ? C3E N4E Ru1 108.2(3) . . ? C4E C3E N4E 108.0(4) . . ? N5E C4E C3E 107.8(4) . . ? C4E N5E Ru1 109.4(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 65.65 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.584 _refine_diff_density_min -1.740 _refine_diff_density_rms 0.110