# Copyright The Royal Society of Chemistry, 1998 data_rtruacac _audit_creation_method SHELXL _chemical_name_systematic 'Tris(acetylacetonato)ruthenium (III)' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural Ru(acac)3 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H21 O6 Ru' _chemical_formula_weight 398.39 _chemical_melting_point ? _chemical_compound_source ? 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' '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 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 14.071(4) _cell_length_b 7.534(2) _cell_length_c 16.363(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.05(2) _cell_angle_gamma 90.00 _cell_volume 1713.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Rectangular Prism' _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method ? _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens P3/P4' _diffrn_measurement_method omega/2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 3141 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3023 _reflns_number_observed 2539 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3/P4-PC software, rev. 4.27, 1991' _computing_cell_refinement 'Siemens P3/P4-PC software, rev. 4.27, 1991' _computing_data_reduction 'PROFIT (Streltsov & Zavodnik, 1989)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1983)' _computing_publication_material 'SHELXTL (Sheldrick, 1983)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.4672P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3018 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_obs 0.0278 _refine_ls_wR_factor_all 0.0705 _refine_ls_wR_factor_obs 0.0626 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.054 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.054 _refine_ls_shift/esd_max 1.005 _refine_ls_shift/esd_mean 0.104 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.23758(2) 0.26852(3) 0.472470(14) 0.04866(11) Uani 1 d . . O1A O 0.1806(24) 0.2110(31) 0.5673(18) 0.055(4) Uani 0.50 d P 1 O2A O 0.1181(14) 0.3539(31) 0.4019(10) 0.056(3) Uani 0.50 d P 1 C1A C 0.0867(25) 0.2181(25) 0.5747(21) 0.079(6) Uani 0.50 d P 1 C2A C 0.0192(15) 0.2810(26) 0.5042(15) 0.085(5) Uani 0.50 d P 1 H2A H -0.0443(120) 0.2468(202) 0.5238(94) 0.128(62) Uiso 0.50 d P 1 C3A C 0.0288(28) 0.3388(35) 0.4360(26) 0.073(6) Uani 0.50 d P 1 C4A C 0.0581(23) 0.1558(44) 0.6488(20) 0.108(8) Uani 0.50 d P 1 H41A H -0.0015(116) 0.1231(275) 0.6471(93) 0.156(35) Uiso 0.50 d P 1 H42A H 0.0508(111) 0.2590(164) 0.6922(95) 0.156(35) Uiso 0.50 d P 1 H43A H 0.1069(119) 0.0789(277) 0.7065(105) 0.156(35) Uiso 0.50 d P 1 C5A C -0.0484(16) 0.3997(37) 0.3704(16) 0.088(6) Uani 0.50 d P 1 H51A H -0.0946(69) 0.4487(103) 0.3858(51) 0.060(15) Uiso 0.50 d P 1 H52A H -0.0476(60) 0.3596(140) 0.3200(61) 0.060(15) Uiso 0.50 d P 1 H53A H -0.0340(62) 0.4892(109) 0.3473(55) 0.060(15) Uiso 0.50 d P 1 O1B O 0.1808(24) 0.1688(31) 0.5763(19) 0.054(3) Uani 0.50 d P 2 O2B O 0.1031(13) 0.3350(28) 0.4209(10) 0.055(3) Uani 0.50 d P 2 C1B C 0.0944(22) 0.1561(23) 0.5732(18) 0.060(4) Uani 0.50 d P 2 C2B C 0.0192(14) 0.1969(25) 0.5135(14) 0.073(4) Uani 0.50 d P 2 H2B H -0.0268(126) 0.1772(176) 0.5230(75) 0.092(44) Uiso 0.50 d P 2 C3B C 0.0339(30) 0.2856(38) 0.4351(25) 0.086(7) Uani 0.50 d P 2 C4B C 0.0735(22) 0.0854(47) 0.6611(19) 0.101(7) Uani 0.50 d P 2 H41B H 0.0170(104) 0.0540(136) 0.6529(66) 0.076(18) Uiso 0.50 d P 2 H42B H 0.1064(81) 0.1664(149) 0.6994(80) 0.076(18) Uiso 0.50 d P 2 H43B H 0.1073(70) 0.0077(122) 0.6691(70) 0.076(18) Uiso 0.50 d P 2 C5B C -0.0689(22) 0.3252(42) 0.3817(21) 0.109(9) Uani 0.50 d P 2 H51B H -0.1161(87) 0.3909(205) 0.4220(71) 0.151(31) Uiso 0.50 d P 2 H52B H -0.1146(94) 0.2071(165) 0.3766(86) 0.151(31) Uiso 0.50 d P 2 H53B H -0.0772(128) 0.2820(231) 0.3432(132) 0.151(31) Uiso 0.50 d P 2 O3 O 0.2130(2) 0.0234(3) 0.42632(13) 0.0587(5) Uani 1 d . . O4 O 0.2978(2) 0.3525(3) 0.37617(12) 0.0586(5) Uani 1 d . . C6 C 0.2326(2) -0.0253(4) 0.3565(2) 0.0546(8) Uani 1 d . . C7 C 0.2733(3) 0.0820(5) 0.3022(2) 0.0628(9) Uani 1 d . . C8 C 0.3042(2) 0.2562(4) 0.3133(2) 0.0566(8) Uani 1 d . . C9 C 0.2086(4) -0.2151(6) 0.3351(3) 0.0731(11) Uani 1 d . . C10 C 0.3509(5) 0.3460(8) 0.2480(3) 0.0823(13) Uani 1 d . . O5 O 0.3681(2) 0.1877(3) 0.52724(13) 0.0548(5) Uani 1 d . . O6 O 0.2572(2) 0.5132(3) 0.52262(12) 0.0611(6) Uani 1 d . . C11 C 0.4328(2) 0.2924(5) 0.5632(2) 0.0576(8) Uani 1 d . . C12 C 0.4198(3) 0.4700(5) 0.5793(2) 0.0687(9) Uani 1 d . . C13 C 0.3354(3) 0.5690(4) 0.5624(2) 0.0592(8) Uani 1 d . . C14 C 0.5284(3) 0.2051(9) 0.5918(4) 0.0872(13) Uani 1 d . . C15 C 0.3332(6) 0.7566(6) 0.5937(4) 0.0883(15) Uani 1 d . . H7 H 0.2834(25) 0.0308(52) 0.2585(22) 0.076(12) Uiso 1 d . . H91 H 0.2252(44) -0.2857(73) 0.3765(39) 0.137(24) Uiso 1 d . . H92 H 0.1458(45) -0.2316(63) 0.3252(35) 0.121(20) Uiso 1 d . . H93 H 0.2268(46) -0.2409(68) 0.2894(40) 0.136(24) Uiso 1 d . . H101 H 0.3793(36) 0.4494(74) 0.2639(29) 0.124(19) Uiso 1 d . . H102 H 0.4022(52) 0.2822(82) 0.2369(44) 0.159(29) Uiso 1 d . . H103 H 0.3128(35) 0.3395(66) 0.2051(30) 0.108(18) Uiso 1 d . . H12 H 0.4702(25) 0.5263(50) 0.6043(21) 0.077(11) Uiso 1 d . . H141 H 0.5418(34) 0.1289(67) 0.5521(29) 0.118(19) Uiso 1 d . . H142 H 0.5770(37) 0.2942(62) 0.5983(30) 0.107(17) Uiso 1 d . . H143 H 0.5324(40) 0.1814(79) 0.6422(38) 0.134(24) Uiso 1 d . . H151 H 0.2949(40) 0.8139(74) 0.5632(35) 0.118(23) Uiso 1 d . . H152 H 0.2830(62) 0.7620(89) 0.6270(54) 0.203(39) Uiso 1 d . . H153 H 0.3902(45) 0.7890(75) 0.6117(38) 0.136(25) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0540(2) 0.0501(2) 0.0418(2) -0.00129(10) 0.00727(10) 0.00648(11) O1A 0.070(5) 0.056(10) 0.040(6) 0.011(6) 0.010(4) -0.008(7) O2A 0.058(6) 0.080(5) 0.033(6) 0.001(5) 0.015(4) 0.005(4) C1A 0.079(11) 0.084(14) 0.081(8) -0.031(12) 0.035(7) -0.015(12) C2A 0.059(8) 0.105(12) 0.091(11) -0.005(12) 0.014(7) -0.010(9) C3A 0.059(10) 0.085(13) 0.074(9) -0.032(11) 0.005(6) 0.026(10) C4A 0.085(13) 0.161(23) 0.078(12) 0.023(13) 0.015(8) -0.034(15) C5A 0.051(9) 0.122(18) 0.086(13) -0.026(12) -0.009(7) 0.014(10) O1B 0.063(5) 0.053(9) 0.048(6) 0.016(5) 0.017(4) 0.003(6) O2B 0.053(7) 0.079(6) 0.036(6) 0.010(4) 0.017(4) 0.020(6) C1B 0.058(7) 0.063(10) 0.061(7) -0.011(8) 0.019(5) 0.001(8) C2B 0.049(7) 0.092(10) 0.079(8) 0.002(9) 0.015(5) -0.006(9) C3B 0.082(10) 0.105(18) 0.060(8) -0.038(13) -0.023(6) 0.043(13) C4B 0.088(14) 0.145(21) 0.075(11) 0.045(11) 0.034(10) -0.002(13) C5B 0.076(13) 0.135(22) 0.105(13) -0.006(14) -0.024(10) 0.007(11) O3 0.0692(13) 0.0534(12) 0.0523(12) -0.0012(10) 0.0056(10) -0.0023(11) O4 0.0800(15) 0.0516(12) 0.0456(11) 0.0016(10) 0.0141(10) 0.0002(11) C6 0.051(2) 0.054(2) 0.053(2) -0.0073(15) -0.0082(14) 0.0096(14) C7 0.076(2) 0.066(2) 0.046(2) -0.013(2) 0.008(2) 0.004(2) C8 0.057(2) 0.066(2) 0.045(2) 0.0019(15) 0.0036(14) 0.009(2) C9 0.079(3) 0.061(2) 0.072(3) -0.014(2) -0.010(2) -0.001(2) C10 0.107(4) 0.093(3) 0.050(2) -0.001(2) 0.022(2) -0.016(3) O5 0.0557(12) 0.0536(12) 0.0553(12) 0.0007(10) 0.0094(10) 0.0076(10) O6 0.0762(15) 0.0542(12) 0.0529(13) -0.0058(10) 0.0104(11) 0.0113(11) C11 0.053(2) 0.069(2) 0.052(2) 0.011(2) 0.0133(15) 0.002(2) C12 0.069(2) 0.066(2) 0.069(2) -0.001(2) 0.002(2) -0.013(2) C13 0.088(2) 0.050(2) 0.040(2) 0.0013(14) 0.013(2) -0.007(2) C14 0.056(2) 0.112(4) 0.092(4) -0.002(3) 0.006(2) 0.009(2) C15 0.130(5) 0.056(2) 0.077(3) -0.009(2) 0.012(3) -0.004(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 Ru O1A 1.91(3) . ? Ru O2A 1.99(2) . ? Ru O5 2.007(2) . ? Ru O4 2.006(2) . ? Ru O3 2.005(2) . ? Ru O6 2.019(2) . ? Ru O2B 2.01(2) . ? Ru O1B 2.13(3) . ? O1A C1A 1.35(4) . ? O2A C3A 1.46(4) . ? C1A C4A 1.42(4) . ? C1A C2A 1.45(4) . ? C2A C3A 1.22(5) . ? C3A C5A 1.48(4) . ? O1B C1B 1.21(4) . ? O2B C3B 1.10(5) . ? C1B C2B 1.36(4) . ? C1B C4B 1.60(4) . ? C2B C3B 1.49(5) . ? C3B C5B 1.60(4) . ? O3 C6 1.271(4) . ? O4 C8 1.273(4) . ? C6 C7 1.390(5) . ? C6 C9 1.498(5) . ? C7 C8 1.385(5) . ? C8 C10 1.501(5) . ? O5 C11 1.276(4) . ? O6 C13 1.260(4) . ? C11 C12 1.382(5) . ? C11 C14 1.505(6) . ? C12 C13 1.393(5) . ? C13 C15 1.505(5) . ? 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 O1A Ru O2A 96.9(10) . . ? O1A Ru O5 92.3(9) . . ? O2A Ru O5 170.7(3) . . ? O1A Ru O4 174.7(8) . . ? O2A Ru O4 82.3(3) . . ? O5 Ru O4 88.63(9) . . ? O1A Ru O3 91.6(8) . . ? O2A Ru O3 90.0(7) . . ? O5 Ru O3 88.87(9) . . ? O4 Ru O3 93.66(9) . . ? O1A Ru O6 85.7(8) . . ? O2A Ru O6 89.4(7) . . ? O5 Ru O6 92.20(9) . . ? O4 Ru O6 89.07(9) . . ? O3 Ru O6 177.09(8) . . ? O5 Ru O2B 176.1(5) . . ? O4 Ru O2B 94.5(3) . . ? O3 Ru O2B 88.6(6) . . ? O6 Ru O2B 90.1(6) . . ? O5 Ru O1B 88.2(9) . . ? O4 Ru O1B 176.5(8) . . ? O3 Ru O1B 84.9(8) . . ? O6 Ru O1B 92.4(8) . . ? O2B Ru O1B 88.7(9) . . ? C1A O1A Ru 127.5(23) . . ? C3A O2A Ru 117.0(18) . . ? O1A C1A C4A 118.6(30) . . ? O1A C1A C2A 118.1(27) . . ? C4A C1A C2A 123.3(29) . . ? C3A C2A C1A 133.4(27) . . ? C2A C3A O2A 126.9(29) . . ? C2A C3A C5A 126.9(35) . . ? O2A C3A C5A 106.1(32) . . ? C1B O1B Ru 119.7(23) . . ? C3B O2B Ru 129.3(22) . . ? O1B C1B C2B 132.4(28) . . ? O1B C1B C4B 108.2(27) . . ? C2B C1B C4B 119.3(25) . . ? C1B C2B C3B 121.6(24) . . ? O2B C3B C2B 125.4(29) . . ? O2B C3B C5B 125.2(38) . . ? C2B C3B C5B 108.6(34) . . ? C6 O3 Ru 123.7(2) . . ? C8 O4 Ru 123.2(2) . . ? O3 C6 C7 125.2(3) . . ? O3 C6 C9 114.4(3) . . ? C7 C6 C9 120.4(4) . . ? C6 C7 C8 128.2(3) . . ? O4 C8 C7 125.9(3) . . ? O4 C8 C10 114.4(3) . . ? C7 C8 C10 119.7(3) . . ? C11 O5 Ru 123.7(2) . . ? C13 O6 Ru 124.6(2) . . ? O5 C11 C12 125.5(3) . . ? O5 C11 C14 114.3(4) . . ? C12 C11 C14 120.2(4) . . ? C11 C12 C13 127.9(3) . . ? O6 C13 C12 124.9(3) . . ? O6 C13 C15 115.3(4) . . ? C12 C13 C15 119.9(4) . . ? _refine_diff_density_max 0.473 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.069 #=END #********************************************** data_ltruacac _audit_creation_method SHELXL _chemical_name_systematic 'Tris(acetylacetonato)ruthenium (III)' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural Ru(acac)3 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H21 O6 Ru' _chemical_formula_weight 398.39 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 .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 13.819(4) _cell_length_b 7.442(2) _cell_length_c 16.137(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.25(2) _cell_angle_gamma 90.00 _cell_volume 1638.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 14.0 _cell_measurement_theta_max 15.3 _exptl_crystal_description 'Rectangular Prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method ? _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8062 _exptl_absorpt_correction_T_max 0.8370 _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(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 'Siemens P4' _diffrn_measurement_method 2theta/omega _diffrn_standards_number 6 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.0 _diffrn_reflns_number 7433 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 30.0 _reflns_number_total 3782 _reflns_number_observed 3338 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'PROFIT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+2.2712P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3782 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_obs 0.0364 _refine_ls_wR_factor_all 0.0723 _refine_ls_wR_factor_obs 0.0688 _refine_ls_goodness_of_fit_all 1.107 _refine_ls_goodness_of_fit_obs 1.129 _refine_ls_restrained_S_all 1.107 _refine_ls_restrained_S_obs 1.129 _refine_ls_shift/esd_max -0.378 _refine_ls_shift/esd_mean 0.022 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.23618(2) 0.26899(3) 0.471581(14) 0.02273(9) Uani 1 d . . O1A O 0.1800(12) 0.2174(11) 0.5734(9) 0.025(2) Uani 0.50 d P 1 O2A O 0.1144(7) 0.3765(10) 0.4064(6) 0.023(2) Uani 0.50 d P 1 C1A C 0.0847(6) 0.2289(12) 0.5714(5) 0.033(2) Uani 0.50 d P 1 C2A C 0.0130(6) 0.2955(15) 0.5055(5) 0.041(2) Uani 0.50 d P 1 H2A H -0.0348(67) 0.2709(119) 0.5231(51) 0.039(23) Uiso 0.50 d P 1 C3A C 0.0302(6) 0.3631(12) 0.4308(5) 0.034(2) Uani 0.50 d P 1 C4A C 0.0533(7) 0.1720(17) 0.6542(6) 0.044(2) Uani 0.50 d P 1 H41A H -0.0085(66) 0.0953(114) 0.6460(48) 0.034(14) Uiso 0.50 d P 1 H42A H 0.0434(57) 0.2609(103) 0.6919(49) 0.034(14) Uiso 0.50 d P 1 H43A H 0.0930(116) 0.1109(215) 0.6841(72) 0.034(14) Uiso 0.50 d P 1 C5A C -0.0538(7) 0.4329(18) 0.3674(7) 0.045(2) Uani 0.50 d P 1 H51A H -0.1153(96) 0.4642(151) 0.3947(76) 0.084(25) Uiso 0.50 d P 1 H52A H -0.0764(96) 0.3023(172) 0.3258(93) 0.084(25) Uiso 0.50 d P 1 H53A H -0.0396(80) 0.5335(158) 0.3428(69) 0.084(25) Uiso 0.50 d P 1 O1B O 0.1777(11) 0.1618(10) 0.5715(8) 0.018(2) Uani 0.50 d P 2 O2B O 0.0990(7) 0.3209(9) 0.4145(6) 0.0205(15) Uani 0.50 d P 2 C1B C 0.0894(6) 0.1371(10) 0.5760(5) 0.024(2) Uani 0.50 d P 2 C2B C 0.0135(6) 0.1814(14) 0.5130(5) 0.029(2) Uani 0.50 d P 2 H2B H -0.0323(72) 0.1510(120) 0.5124(55) 0.040(27) Uiso 0.50 d P 2 C3B C 0.0194(5) 0.2698(10) 0.4385(4) 0.0217(14) Uani 0.50 d P 2 C4B C 0.0701(8) 0.0518(18) 0.6560(6) 0.042(2) Uani 0.50 d P 2 H41B H 0.0100(76) 0.0008(118) 0.6570(54) 0.045(16) Uiso 0.50 d P 2 H42B H 0.0981(97) 0.1453(172) 0.7043(62) 0.045(16) Uiso 0.50 d P 2 H43B H 0.1183(65) -0.0278(115) 0.6772(51) 0.045(16) Uiso 0.50 d P 2 C5B C -0.0723(7) 0.3163(15) 0.3797(6) 0.034(2) Uani 0.50 d P 2 H51B H -0.1152(71) 0.3766(121) 0.4030(55) 0.035(15) Uiso 0.50 d P 2 H52B H -0.0968(61) 0.2277(112) 0.3724(53) 0.035(15) Uiso 0.50 d P 2 H53B H -0.0577(72) 0.3832(133) 0.3297(69) 0.035(15) Uiso 0.50 d P 2 O3 O 0.2107(2) 0.0215(3) 0.42506(12) 0.0251(5) Uani 1 d . . O4 O 0.2976(2) 0.3552(3) 0.37439(12) 0.0248(5) Uani 1 d . . C6 C 0.2315(2) -0.0286(4) 0.3542(2) 0.0221(6) Uani 1 d . . C7 C 0.2739(2) 0.0785(4) 0.2988(2) 0.0238(7) Uani 1 d . . C8 C 0.3056(2) 0.2565(4) 0.3109(2) 0.0208(6) Uani 1 d . . C9 C 0.2068(3) -0.2214(5) 0.3327(2) 0.0334(8) Uani 1 d . . C10 C 0.3546(3) 0.3459(5) 0.2448(2) 0.0290(8) Uani 1 d . . O5 O 0.3695(2) 0.1874(3) 0.52659(12) 0.0208(4) Uani 1 d . . O6 O 0.2571(2) 0.5163(3) 0.52290(13) 0.0308(5) Uani 1 d . . C11 C 0.4369(2) 0.2930(4) 0.5620(2) 0.0215(6) Uani 1 d . . C12 C 0.4245(3) 0.4748(4) 0.5790(2) 0.0268(7) Uani 1 d . . C13 C 0.3379(3) 0.5732(4) 0.5624(2) 0.0270(7) Uani 1 d . . C14 C 0.5342(3) 0.2058(5) 0.5899(2) 0.0311(8) Uani 1 d . . C15 C 0.3357(4) 0.7635(5) 0.5943(2) 0.0387(10) Uani 1 d . . H7 H 0.2846(27) 0.0225(49) 0.2507(22) 0.037(10) Uiso 1 d . . H91 H 0.2236(28) -0.2980(49) 0.3810(23) 0.038(10) Uiso 1 d . . H92 H 0.1396(34) -0.2345(55) 0.3206(26) 0.052(13) Uiso 1 d . . H93 H 0.2328(30) -0.2537(53) 0.2885(26) 0.048(12) Uiso 1 d . . H101 H 0.3796(29) 0.4643(56) 0.2624(23) 0.045(11) Uiso 1 d . . H102 H 0.4132(32) 0.2849(55) 0.2402(25) 0.052(12) Uiso 1 d . . H103 H 0.3116(34) 0.3520(59) 0.1976(27) 0.058(14) Uiso 1 d . . H12 H 0.4775(28) 0.5244(51) 0.6059(22) 0.037(11) Uiso 1 d . . H141 H 0.5501(29) 0.1266(55) 0.5499(24) 0.048(12) Uiso 1 d . . H142 H 0.5848(31) 0.2874(56) 0.6009(25) 0.050(12) Uiso 1 d . . H143 H 0.5314(32) 0.1386(61) 0.6384(28) 0.064(14) Uiso 1 d . . H151 H 0.3029(31) 0.8410(55) 0.5527(25) 0.050(12) Uiso 1 d . . H152 H 0.3049(36) 0.7646(64) 0.6405(31) 0.075(15) Uiso 1 d . . H153 H 0.3942(38) 0.8006(65) 0.6112(29) 0.064(17) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01796(15) 0.03596(14) 0.01459(11) -0.00121(9) 0.00363(10) 0.00817(11) O1A 0.025(4) 0.032(5) 0.021(3) -0.016(4) 0.009(3) -0.021(5) O2A 0.019(4) 0.031(4) 0.018(3) -0.003(3) -0.002(3) 0.004(3) C1A 0.026(5) 0.050(5) 0.027(4) -0.013(4) 0.012(4) -0.020(5) C2A 0.018(5) 0.070(7) 0.036(4) -0.017(4) 0.012(4) -0.011(4) C3A 0.017(4) 0.050(5) 0.031(4) -0.021(4) -0.002(3) 0.006(4) C4A 0.030(5) 0.070(7) 0.037(5) -0.023(4) 0.021(4) -0.027(5) C5A 0.022(5) 0.072(8) 0.037(4) -0.021(5) -0.009(4) 0.014(5) O1B 0.014(4) 0.021(4) 0.018(3) -0.001(3) 0.003(3) -0.007(4) O2B 0.023(4) 0.018(4) 0.021(3) 0.004(3) 0.005(3) 0.002(3) C1B 0.013(4) 0.033(4) 0.027(3) 0.011(3) 0.001(3) -0.006(3) C2B 0.015(4) 0.043(4) 0.030(4) 0.011(3) 0.006(3) -0.002(4) C3B 0.012(4) 0.028(3) 0.023(3) -0.001(3) -0.004(3) 0.002(3) C4B 0.033(6) 0.063(7) 0.032(4) 0.019(4) 0.010(4) -0.005(5) C5B 0.022(5) 0.042(5) 0.037(4) 0.005(4) 0.000(4) 0.014(4) O3 0.0197(13) 0.0352(11) 0.0198(9) -0.0004(8) 0.0010(9) -0.0039(9) O4 0.0331(14) 0.0253(10) 0.0167(9) 0.0005(8) 0.0060(10) 0.0064(9) C6 0.015(2) 0.0289(15) 0.0198(13) 0.0004(11) -0.0049(13) 0.0020(12) C7 0.026(2) 0.0269(15) 0.0183(13) -0.0034(11) 0.0020(14) 0.0026(13) C8 0.016(2) 0.0312(15) 0.0145(11) 0.0023(11) 0.0004(12) 0.0075(12) C9 0.030(2) 0.035(2) 0.031(2) 0.0018(14) -0.007(2) -0.008(2) C10 0.033(2) 0.036(2) 0.0194(14) 0.0019(12) 0.007(2) 0.002(2) O5 0.0185(12) 0.0241(10) 0.0202(9) 0.0035(8) 0.0046(9) 0.0029(8) O6 0.034(2) 0.0388(12) 0.0183(9) -0.0050(9) 0.0003(10) 0.0178(11) C11 0.018(2) 0.0288(14) 0.0192(12) 0.0050(11) 0.0087(13) -0.0012(12) C12 0.026(2) 0.027(2) 0.0265(15) 0.0016(12) 0.003(2) -0.0023(14) C13 0.041(2) 0.0283(15) 0.0129(12) 0.0024(11) 0.0086(14) 0.0052(14) C14 0.019(2) 0.038(2) 0.037(2) -0.0018(15) 0.005(2) -0.0002(15) C15 0.065(3) 0.028(2) 0.024(2) 0.0007(13) 0.008(2) 0.010(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 Ru O1A 1.965(13) . ? Ru O3 1.999(2) . ? Ru O2B 2.007(11) . ? Ru O4 2.005(2) . ? Ru O5 2.007(2) . ? Ru O2A 2.003(10) . ? Ru O6 2.020(2) . ? Ru O1B 2.076(12) . ? O1A C1A 1.32(2) . ? O2A C3A 1.291(12) . ? C1A C2A 1.421(14) . ? C1A C4A 1.529(11) . ? C2A C3A 1.362(12) . ? C3A C5A 1.511(13) . ? O1B C1B 1.25(2) . ? O2B C3B 1.282(10) . ? C1B C2B 1.378(12) . ? C1B C4B 1.501(10) . ? C2B C3B 1.385(10) . ? C3B C5B 1.496(11) . ? O3 C6 1.279(3) . ? O4 C8 1.280(3) . ? C6 C7 1.394(4) . ? C6 C9 1.503(5) . ? C7 C8 1.399(4) . ? C8 C10 1.508(4) . ? O5 C11 1.280(4) . ? O6 C13 1.266(4) . ? C11 C12 1.396(4) . ? C11 C14 1.495(5) . ? C12 C13 1.392(5) . ? C13 C15 1.509(5) . ? 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 O1A Ru O3 93.7(2) . . ? O3 Ru O2B 84.8(2) . . ? O1A Ru O4 172.1(2) . . ? O3 Ru O4 94.15(8) . . ? O2B Ru O4 93.8(2) . . ? O1A Ru O5 91.7(5) . . ? O3 Ru O5 88.93(9) . . ? O2B Ru O5 173.5(2) . . ? O4 Ru O5 88.21(8) . . ? O1A Ru O2A 96.1(5) . . ? O3 Ru O2A 95.1(2) . . ? O4 Ru O2A 83.5(2) . . ? O5 Ru O2A 171.0(2) . . ? O1A Ru O6 83.4(2) . . ? O3 Ru O6 177.00(9) . . ? O2B Ru O6 94.3(2) . . ? O4 Ru O6 88.76(9) . . ? O5 Ru O6 91.92(9) . . ? O2A Ru O6 84.5(3) . . ? O3 Ru O1B 82.6(2) . . ? O2B Ru O1B 88.5(5) . . ? O4 Ru O1B 175.8(3) . . ? O5 Ru O1B 89.1(4) . . ? O6 Ru O1B 94.6(2) . . ? C1A O1A Ru 119.7(10) . . ? C3A O2A Ru 122.1(7) . . ? O1A C1A C2A 128.1(9) . . ? O1A C1A C4A 112.6(10) . . ? C2A C1A C4A 119.2(8) . . ? C3A C2A C1A 126.2(7) . . ? O2A C3A C2A 126.4(9) . . ? O2A C3A C5A 113.5(9) . . ? C2A C3A C5A 120.1(8) . . ? C1B O1B Ru 127.4(10) . . ? C3B O2B Ru 126.7(6) . . ? O1B C1B C2B 123.9(9) . . ? O1B C1B C4B 115.0(9) . . ? C2B C1B C4B 121.1(8) . . ? C1B C2B C3B 127.6(8) . . ? O2B C3B C2B 125.2(8) . . ? O2B C3B C5B 114.9(7) . . ? C2B C3B C5B 119.9(7) . . ? C6 O3 Ru 123.6(2) . . ? C8 O4 Ru 123.0(2) . . ? O3 C6 C7 125.7(3) . . ? O3 C6 C9 114.1(3) . . ? C7 C6 C9 120.1(3) . . ? C6 C7 C8 127.3(3) . . ? O4 C8 C7 126.1(2) . . ? O4 C8 C10 114.8(3) . . ? C7 C8 C10 119.0(3) . . ? C11 O5 Ru 124.2(2) . . ? C13 O6 Ru 124.6(2) . . ? O5 C11 C12 125.4(3) . . ? O5 C11 C14 115.0(3) . . ? C12 C11 C14 119.6(3) . . ? C13 C12 C11 127.0(3) . . ? O6 C13 C12 125.6(3) . . ? O6 C13 C15 115.0(3) . . ? C12 C13 C15 119.5(4) . . ? _refine_diff_density_max .842 _refine_diff_density_min -1.570 _refine_diff_density_rms .079 #=END #********************************************************** data_heruacac _audit_creation_method SHELXL _chemical_name_systematic 'Tris(acetylacetonato)ruthenium (III)' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural Ru(acac)3 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H21 O6 Ru' _chemical_formula_weight 398.39 _chemical_melting_point ? _chemical_compound_source ? 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' '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 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 13.758(2) _cell_length_b 7.4100(10) _cell_length_c 16.095(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.340(10) _cell_angle_gamma 90.00 _cell_volume 1619.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 10.5(5) _cell_measurement_reflns_used 12 _cell_measurement_theta_min 14 _cell_measurement_theta_max 15.45 _exptl_crystal_description 'Rectangular Prism' _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method ? _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.7519 _exptl_absorpt_correction_T_max 0.8295 _exptl_special_details ; ? ; _diffrn_ambient_temperature 10.5(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator none _diffrn_measurement_device 'Huber 512' _diffrn_measurement_method omega/2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 12357 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 48.75 _reflns_number_total 6359 _reflns_number_observed 5798 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Locally written program' _computing_cell_refinement 'Siemens P3/P4-PC software, rev. 4.27, 1991' _computing_data_reduction 'PROFIT (Streltsov & Zavodnik, 1989)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL, 1981, Rev. 3' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+1.2931P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00051(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6350 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_obs 0.0280 _refine_ls_wR_factor_all 0.0677 _refine_ls_wR_factor_obs 0.0640 _refine_ls_goodness_of_fit_all 1.163 _refine_ls_goodness_of_fit_obs 1.173 _refine_ls_restrained_S_all 1.181 _refine_ls_restrained_S_obs 1.173 _refine_ls_shift/esd_max 0.328 _refine_ls_shift/esd_mean 0.035 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1A Ru 0.239182(15) 0.28852(3) 0.470345(13) 0.00793(4) Uani 0.50 d P 1 O1A O 0.1757(2) 0.2188(3) 0.57024(13) 0.0134(4) Uani 0.50 d P 1 O2A O 0.1140(2) 0.3793(3) 0.40494(14) 0.0146(4) Uani 0.50 d P 1 C1A C 0.0832(2) 0.2336(5) 0.5712(2) 0.0194(6) Uani 0.50 d P 1 C2A C 0.0121(2) 0.3002(6) 0.5052(2) 0.0230(7) Uani 0.50 d P 1 H2A H -0.0532(2) 0.2980(6) 0.5136(2) 0.035 Uiso 0.50 calc PR 1 C3A C 0.0302(2) 0.3687(5) 0.4289(2) 0.0189(6) Uani 0.50 d P 1 C4A C 0.0505(3) 0.1763(6) 0.6528(2) 0.0272(8) Uani 0.50 d P 1 H4A1 H 0.1007(10) 0.1028(34) 0.6847(9) 0.028(7) Uiso 0.50 calc PR 1 H4A2 H -0.0095(12) 0.1084(36) 0.6404(2) 0.028(7) Uiso 0.50 calc PR 1 H4A3 H 0.0397(22) 0.2814(6) 0.6849(9) 0.028(7) Uiso 0.50 calc PR 1 C5A C -0.0537(2) 0.4421(6) 0.3652(2) 0.0245(8) Uani 0.50 d P 1 H5A1 H -0.0335(9) 0.5526(26) 0.3420(17) 0.044(9) Uiso 0.50 calc PR 1 H5A2 H -0.1097(9) 0.4645(46) 0.3924(5) 0.044(9) Uiso 0.50 calc PR 1 H5A3 H -0.0710(18) 0.3555(21) 0.3209(12) 0.044(9) Uiso 0.50 calc PR 1 O3A O 0.20926(15) 0.0390(3) 0.42558(13) 0.0126(4) Uani 0.50 d P 1 O4A O 0.30437(15) 0.3681(3) 0.37381(12) 0.0089(3) Uani 0.50 d P 1 C6A C 0.2310(2) -0.0135(4) 0.3530(2) 0.0118(5) Uani 0.50 d P 1 C7A C 0.2743(2) 0.0839(4) 0.2957(2) 0.0111(4) Uani 0.50 d P 1 H7A H 0.2825(2) 0.0287(4) 0.2455(2) 0.017 Uiso 0.50 calc PR 1 C8A C 0.3070(2) 0.2642(3) 0.3100(2) 0.0086(4) Uani 0.50 d P 1 C9A C 0.2004(2) -0.2102(5) 0.3369(2) 0.0166(5) Uani 0.50 d P 1 H9A1 H 0.2277(17) -0.2821(8) 0.3846(7) 0.016(6) Uiso 0.50 calc PR 1 H9A2 H 0.2245(17) -0.2531(12) 0.2878(10) 0.016(6) Uiso 0.50 calc PR 1 H9A3 H 0.1299(2) -0.2189(7) 0.3282(17) 0.016(6) Uiso 0.50 calc PR 1 C10A C 0.3573(2) 0.3611(3) 0.2447(2) 0.0084(4) Uani 0.50 d P 1 H10A H 0.3798(19) 0.4775(16) 0.2659(8) 0.023(7) Uiso 0.50 calc PR 1 H10B H 0.3112(6) 0.3757(35) 0.1935(6) 0.023(7) Uiso 0.50 calc PR 1 H10C H 0.4124(13) 0.2910(19) 0.2336(14) 0.023(7) Uiso 0.50 calc PR 1 O5A O 0.36966(14) 0.2014(3) 0.52874(12) 0.0085(3) Uani 0.50 d P 1 O6A O 0.26352(15) 0.5386(3) 0.52087(12) 0.0103(3) Uani 0.50 d P 1 C11A C 0.4408(2) 0.2992(5) 0.5634(2) 0.0161(6) Uani 0.50 d P 1 C12A C 0.4322(2) 0.4864(4) 0.5806(2) 0.0096(4) Uani 0.50 d P 1 H12A H 0.4885(2) 0.5468(4) 0.6059(2) 0.014 Uiso 0.50 calc PR 1 C13A C 0.3470(2) 0.5839(5) 0.5625(2) 0.0145(5) Uani 0.50 d P 1 C14A C 0.5337(2) 0.2218(3) 0.5890(2) 0.0104(4) Uani 0.50 d P 1 H14A H 0.5459(10) 0.1328(30) 0.5486(10) 0.032(8) Uiso 0.50 calc PR 1 H14B H 0.5355(8) 0.1657(37) 0.6430(9) 0.032(8) Uiso 0.50 calc PR 1 H14C H 0.5833(3) 0.3140(7) 0.5930(19) 0.032(8) Uiso 0.50 calc PR 1 C15A C 0.3474(2) 0.7741(4) 0.5961(2) 0.0137(5) Uani 0.50 d P 1 H15A H 0.3063(19) 0.8490(10) 0.5562(9) 0.031(8) Uiso 0.50 calc PR 1 H15B H 0.4134(4) 0.8202(16) 0.6049(19) 0.031(8) Uiso 0.50 calc PR 1 H15C H 0.3225(22) 0.7740(7) 0.6485(10) 0.031(8) Uiso 0.50 calc PR 1 Ru1B Ru 0.232278(14) 0.25355(3) 0.470749(12) 0.00504(4) Uani 0.50 d P 2 O1B O 0.18110(14) 0.1629(3) 0.57316(12) 0.0088(3) Uani 0.50 d P 2 O2B O 0.09713(14) 0.3236(3) 0.41280(12) 0.0078(3) Uani 0.50 d P 2 C1B C 0.0894(2) 0.1359(5) 0.5750(2) 0.0147(5) Uani 0.50 d P 2 C2B C 0.0110(2) 0.1792(5) 0.5117(2) 0.0173(6) Uani 0.50 d P 2 H2B H -0.0515(2) 0.1422(5) 0.5196(2) 0.026 Uiso 0.50 calc PR 2 C3B C 0.0175(2) 0.2729(4) 0.4374(2) 0.0121(5) Uani 0.50 d P 2 C4B C 0.0699(2) 0.0483(6) 0.6549(2) 0.0260(8) Uani 0.50 d P 2 H4B1 H 0.1150(14) -0.0498(24) 0.6692(9) 0.018(6) Uiso 0.50 calc PR 2 H4B2 H 0.0036(7) 0.0034(33) 0.6469(6) 0.018(6) Uiso 0.50 calc PR 2 H4B3 H 0.0785(20) 0.1355(11) 0.6996(5) 0.018(6) Uiso 0.50 calc PR 2 C5B C -0.0758(2) 0.3178(5) 0.3787(2) 0.0182(6) Uani 0.50 d P 2 H5B1 H -0.0601(3) 0.3843(40) 0.3314(11) 0.038(9) Uiso 0.50 calc PR 2 H5B2 H -0.1176(11) 0.3896(39) 0.4079(6) 0.038(9) Uiso 0.50 calc PR 2 H5B3 H -0.1093(13) 0.2083(5) 0.3593(17) 0.038(9) Uiso 0.50 calc PR 2 O3B O 0.21068(15) 0.0060(3) 0.42274(13) 0.0095(3) Uani 0.50 d P 2 O4B O 0.29118(15) 0.3443(3) 0.37259(12) 0.0096(3) Uani 0.50 d P 2 C6B C 0.2315(2) -0.0442(4) 0.3531(2) 0.0083(4) Uani 0.50 d P 2 C7B C 0.2754(2) 0.0722(4) 0.3002(2) 0.0149(5) Uani 0.50 d P 2 H7B H 0.2862(2) 0.0196(4) 0.2500(2) 0.022 Uiso 0.50 calc PR 2 C8B C 0.3050(2) 0.2483(4) 0.3098(2) 0.0129(5) Uani 0.50 d P 2 C9B C 0.2126(2) -0.2332(4) 0.3277(2) 0.0110(4) Uani 0.50 d P 2 H9B1 H 0.2236(22) -0.3092(6) 0.3766(3) 0.029(8) Uiso 0.50 calc PR 2 H9B2 H 0.2563(16) -0.2681(13) 0.2897(15) 0.029(8) Uiso 0.50 calc PR 2 H9B3 H 0.1456(7) -0.2457(9) 0.3002(17) 0.029(8) Uiso 0.50 calc PR 2 C10B C 0.3542(2) 0.3282(4) 0.2427(2) 0.0113(4) Uani 0.50 d P 2 H10D H 0.3748(19) 0.4491(14) 0.2582(9) 0.023(7) Uiso 0.50 calc PR 2 H10E H 0.3090(7) 0.3302(36) 0.1906(4) 0.023(7) Uiso 0.50 calc PR 2 H10F H 0.4107(13) 0.2568(23) 0.2361(13) 0.023(7) Uiso 0.50 calc PR 2 O5B O 0.37001(13) 0.1744(3) 0.52308(12) 0.0073(3) Uani 0.50 d P 2 O6B O 0.2502(2) 0.4999(2) 0.52276(12) 0.0085(3) Uani 0.50 d P 2 C11B C 0.4343(2) 0.2904(3) 0.5594(2) 0.0073(4) Uani 0.50 d P 2 C12B C 0.4194(2) 0.4674(4) 0.5776(2) 0.0125(5) Uani 0.50 d P 2 H12B H 0.4745(2) 0.5301(4) 0.6038(2) 0.019 Uiso 0.50 calc PR 2 C13B C 0.3297(2) 0.5684(3) 0.5615(2) 0.0083(4) Uani 0.50 d P 2 C14B C 0.5376(2) 0.1904(4) 0.5895(2) 0.0111(4) Uani 0.50 d P 2 H14D H 0.5548(10) 0.1203(28) 0.5439(5) 0.015(6) Uiso 0.50 calc PR 2 H14E H 0.5319(6) 0.1124(27) 0.6361(11) 0.015(6) Uiso 0.50 calc PR 2 H14F H 0.5879(4) 0.2788(4) 0.6066(16) 0.015(6) Uiso 0.50 calc PR 2 C15B C 0.3238(2) 0.7580(4) 0.5927(2) 0.0135(5) Uani 0.50 d P 2 H15D H 0.2963(19) 0.8348(8) 0.5468(4) 0.020(7) Uiso 0.50 calc PR 2 H15E H 0.3886(3) 0.7996(14) 0.6158(16) 0.020(7) Uiso 0.50 calc PR 2 H15F H 0.2826(17) 0.7612(7) 0.6354(12) 0.020(7) Uiso 0.50 calc PR 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 Ru1A 0.00505(7) 0.01337(9) 0.00531(8) -0.00020(6) 0.00070(5) 0.00112(6) O1A 0.0081(8) 0.0234(11) 0.0092(8) -0.0013(7) 0.0026(6) -0.0034(7) O2A 0.0074(8) 0.0236(11) 0.0121(9) -0.0024(8) -0.0002(6) 0.0039(7) C1A 0.0114(12) 0.031(2) 0.0178(14) -0.0091(12) 0.0070(10) -0.0068(11) C2A 0.0060(10) 0.043(2) 0.0203(15) -0.0134(14) 0.0029(10) -0.0025(12) C3A 0.0092(11) 0.033(2) 0.0137(12) -0.0127(12) -0.0007(9) 0.0016(11) C4A 0.021(2) 0.042(2) 0.022(2) -0.014(2) 0.0151(13) -0.0159(15) C5A 0.0104(12) 0.039(2) 0.021(2) -0.0112(14) -0.0039(11) 0.0077(12) O3A 0.0087(8) 0.0206(10) 0.0086(8) 0.0013(7) 0.0022(6) -0.0006(7) O4A 0.0128(8) 0.0086(7) 0.0057(7) -0.0001(5) 0.0030(6) -0.0007(6) C6A 0.0100(10) 0.0102(10) 0.0126(11) -0.0006(8) -0.0059(8) -0.0026(8) C7A 0.0069(9) 0.0229(13) 0.0040(9) 0.0018(8) 0.0020(7) -0.0016(9) C8A 0.0063(8) 0.0061(9) 0.0132(11) 0.0018(7) 0.0007(7) 0.0001(7) C9A 0.0121(11) 0.028(2) 0.0094(11) -0.0039(10) 0.0016(9) 0.0036(11) C10A 0.0135(10) 0.0032(8) 0.0094(10) 0.0008(7) 0.0043(8) 0.0003(7) O5A 0.0093(7) 0.0076(7) 0.0086(7) -0.0007(6) 0.0018(6) 0.0017(6) O6A 0.0125(8) 0.0098(8) 0.0083(8) 0.0000(6) 0.0005(6) 0.0012(6) C11A 0.0101(11) 0.031(2) 0.0071(10) 0.0000(10) 0.0013(8) -0.0083(11) C12A 0.0052(9) 0.0112(10) 0.0127(11) 0.0009(8) 0.0020(8) 0.0001(7) C13A 0.0091(10) 0.028(2) 0.0063(10) 0.0015(9) 0.0017(8) -0.0024(10) C14A 0.0094(9) 0.0035(8) 0.0186(12) 0.0010(8) 0.0034(8) 0.0046(7) C15A 0.0081(10) 0.0216(14) 0.0111(11) 0.0010(10) 0.0005(8) 0.0009(9) Ru1B 0.00544(7) 0.00383(6) 0.00620(8) -0.00024(5) 0.00199(5) 0.00056(5) O1B 0.0063(7) 0.0109(8) 0.0095(8) 0.0030(6) 0.0023(6) 0.0004(6) O2B 0.0064(7) 0.0098(7) 0.0075(7) 0.0016(6) 0.0018(5) 0.0016(6) C1B 0.0064(9) 0.0267(15) 0.0117(11) 0.0085(10) 0.0030(8) 0.0002(10) C2B 0.0069(10) 0.033(2) 0.0128(12) 0.0099(11) 0.0024(9) 0.0021(10) C3B 0.0071(9) 0.0195(13) 0.0101(11) 0.0041(9) 0.0023(8) 0.0037(9) C4B 0.0107(12) 0.051(2) 0.0157(14) 0.0158(15) 0.0006(10) -0.0039(14) C5B 0.0074(10) 0.038(2) 0.0092(11) 0.0062(11) 0.0003(8) 0.0087(11) O3B 0.0095(7) 0.0075(7) 0.0106(8) -0.0019(6) -0.0007(6) 0.0001(6) O4B 0.0113(8) 0.0089(8) 0.0087(8) -0.0016(6) 0.0021(6) -0.0041(6) C6B 0.0077(9) 0.0093(9) 0.0073(9) 0.0025(7) -0.0003(7) 0.0027(7) C7B 0.0239(14) 0.0102(11) 0.0096(11) -0.0005(8) -0.0002(10) 0.0068(10) C8B 0.0122(10) 0.0256(14) 0.0010(8) -0.0003(8) 0.0015(7) 0.0111(10) C9B 0.0124(11) 0.0072(10) 0.0124(11) -0.0048(8) -0.0013(8) -0.0001(8) C10B 0.0195(12) 0.0043(9) 0.0100(10) -0.0012(7) 0.0022(9) -0.0002(8) O5B 0.0049(6) 0.0074(7) 0.0094(7) -0.0032(6) 0.0004(5) 0.0015(5) O6B 0.0156(8) 0.0012(6) 0.0083(7) -0.0010(5) 0.0007(6) -0.0005(5) C11B 0.0050(8) 0.0066(9) 0.0113(10) 0.0027(7) 0.0044(7) 0.0048(7) C12B 0.0118(10) 0.0127(11) 0.0134(11) -0.0020(9) 0.0027(9) -0.0104(9) C13B 0.0121(10) 0.0082(9) 0.0059(9) 0.0007(7) 0.0049(7) 0.0033(8) C14B 0.0053(8) 0.0071(9) 0.0201(12) -0.0019(8) -0.0004(8) 0.0047(7) C15B 0.0145(11) 0.0130(11) 0.0124(11) 0.0000(9) 0.0003(9) 0.0019(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 Ru1A O2A 1.984(2) . ? Ru1A O5A 1.994(2) . ? Ru1A O4A 2.005(2) . ? Ru1A O3A 2.003(2) . ? Ru1A O1A 2.017(2) . ? Ru1A O6A 2.030(2) . ? O1A C1A 1.281(4) . ? O2A C3A 1.277(4) . ? C1A C2A 1.411(5) . ? C1A C4A 1.516(5) . ? C2A C3A 1.388(5) . ? C3A C5A 1.514(5) . ? O3A C6A 1.311(4) . ? O4A C8A 1.288(3) . ? C6A C7A 1.380(4) . ? C6A C9A 1.528(4) . ? C7A C8A 1.416(4) . ? C8A C10A 1.529(4) . ? O5A C11A 1.271(4) . ? O6A C13A 1.277(3) . ? C11A C14A 1.400(4) . ? C11A C12A 1.423(5) . ? C12A C13A 1.367(4) . ? C13A C15A 1.509(5) . ? Ru1B O3B 1.994(2) . ? Ru1B O4B 2.005(2) . ? Ru1B O2B 2.008(2) . ? Ru1B O6B 2.007(2) . ? Ru1B O1B 2.010(2) . ? Ru1B O5B 2.031(2) . ? O1B C1B 1.282(3) . ? O2B C3B 1.280(3) . ? C1B C2B 1.397(4) . ? C1B C4B 1.503(4) . ? C2B C3B 1.398(4) . ? C3B C5B 1.503(4) . ? O3B C6B 1.257(3) . ? O4B C8B 1.275(3) . ? C6B C7B 1.415(4) . ? C6B C9B 1.470(4) . ? C7B C8B 1.368(5) . ? C8B C10B 1.487(4) . ? O5B C11B 1.302(3) . ? O6B C13B 1.274(3) . ? C11B C12B 1.367(4) . ? C11B C14B 1.607(3) . ? C12B C13B 1.430(4) . ? C13B C15B 1.499(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 O2A Ru1A O5A 175.78(9) . . ? O2A Ru1A O4A 87.02(9) . . ? O5A Ru1A O4A 88.78(8) . . ? O2A Ru1A O3A 90.70(9) . . ? O5A Ru1A O3A 89.29(8) . . ? O4A Ru1A O3A 94.84(8) . . ? O2A Ru1A O1A 93.39(9) . . ? O5A Ru1A O1A 90.82(9) . . ? O4A Ru1A O1A 177.42(9) . . ? O3A Ru1A O1A 87.71(9) . . ? O2A Ru1A O6A 88.60(9) . . ? O5A Ru1A O6A 91.68(8) . . ? O4A Ru1A O6A 88.65(8) . . ? O3A Ru1A O6A 176.39(8) . . ? O1A Ru1A O6A 88.81(9) . . ? C1A O1A Ru1A 123.2(2) . . ? C3A O2A Ru1A 124.6(2) . . ? O1A C1A C2A 126.2(3) . . ? O1A C1A C4A 114.9(3) . . ? C2A C1A C4A 118.9(3) . . ? C3A C2A C1A 126.3(3) . . ? O2A C3A C2A 126.1(3) . . ? O2A C3A C5A 113.6(3) . . ? C2A C3A C5A 120.3(3) . . ? C6A O3A Ru1A 122.1(2) . . ? C8A O4A Ru1A 121.1(2) . . ? O3A C6A C7A 128.8(3) . . ? O3A C6A C9A 109.7(3) . . ? C7A C6A C9A 121.5(3) . . ? C6A C7A C8A 123.0(3) . . ? O4A C8A C7A 130.1(2) . . ? O4A C8A C10A 110.0(2) . . ? C7A C8A C10A 119.9(2) . . ? C11A O5A Ru1A 126.3(2) . . ? C13A O6A Ru1A 121.7(2) . . ? O5A C11A C14A 119.8(3) . . ? O5A C11A C12A 123.9(3) . . ? C14A C11A C12A 116.3(3) . . ? C13A C12A C11A 124.7(3) . . ? O6A C13A C12A 129.8(3) . . ? O6A C13A C15A 112.5(3) . . ? C12A C13A C15A 117.7(3) . . ? O3B Ru1B O4B 93.27(8) . . ? O3B Ru1B O2B 89.38(8) . . ? O4B Ru1B O2B 90.54(8) . . ? O3B Ru1B O6B 177.48(8) . . ? O4B Ru1B O6B 89.19(8) . . ? O2B Ru1B O6B 90.01(8) . . ? O3B Ru1B O1B 87.73(8) . . ? O4B Ru1B O1B 176.67(8) . . ? O2B Ru1B O1B 92.64(8) . . ? O6B Ru1B O1B 89.86(8) . . ? O3B Ru1B O5B 88.01(8) . . ? O4B Ru1B O5B 87.39(8) . . ? O2B Ru1B O5B 176.58(7) . . ? O6B Ru1B O5B 92.68(8) . . ? O1B Ru1B O5B 89.47(8) . . ? C1B O1B Ru1B 123.2(2) . . ? C3B O2B Ru1B 123.7(2) . . ? O1B C1B C2B 126.4(3) . . ? O1B C1B C4B 113.6(2) . . ? C2B C1B C4B 120.0(3) . . ? C3B C2B C1B 126.1(3) . . ? O2B C3B C2B 126.0(3) . . ? O2B C3B C5B 115.3(2) . . ? C2B C3B C5B 118.7(3) . . ? C6B O3B Ru1B 125.2(2) . . ? C8B O4B Ru1B 124.7(2) . . ? O3B C6B C7B 122.5(3) . . ? O3B C6B C9B 118.3(2) . . ? C7B C6B C9B 119.1(2) . . ? C8B C7B C6B 131.4(3) . . ? O4B C8B C7B 122.8(3) . . ? O4B C8B C10B 119.8(3) . . ? C7B C8B C10B 117.4(2) . . ? C11B O5B Ru1B 121.0(2) . . ? C13B O6B Ru1B 127.1(2) . . ? O5B C11B C12B 128.0(2) . . ? O5B C11B C14B 109.5(2) . . ? C12B C11B C14B 122.3(2) . . ? C11B C12B C13B 128.2(2) . . ? O6B C13B C12B 121.9(2) . . ? O6B C13B C15B 116.6(2) . . ? C12B C13B C15B 121.5(2) . . ? _refine_diff_density_max 0.598 _refine_diff_density_min -1.096 _refine_diff_density_rms 0.084