# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 ---------- X-Sun-Data-Type: ciffile X-Sun-Data-Name: 159433-4 X-Sun-Charset: us-ascii X-Sun-Content-Lines: 1150 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Zhang Yu-Hua' 'Yuan Jian-Chao' 'Yin Yuan-Qi' 'Zhou Zhong-Yuan' 'Albert S. C. Chan' data_zhy1.cif _database_code_CSD 159433 _audit_creation_date 04-SEP-97 _audit_creation_method 'from_GCIF_by_our_laboratory' _audit_creation_record ; ; _chemical_name_systematic ; ; _chemical_compound_source ; ; _chemical_formula_sum 'Ru1 Mo1 Co1 S1 O10 C16 H9' _chemical_formula_moiety 'Ru1 Mo1 Co1 S1 O10 C16 H9' _chemical_formula_weight 649.24 _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n' _cell_length_a 10.075(1) _cell_length_b 9.034(2) _cell_length_c 22.973(7) _cell_angle_alpha 90 _cell_angle_beta 92.70(2) _cell_angle_gamma 90 _cell_volume 2088.7(8) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_meas ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.11 _cell_measurement_theta_max 14.46 _exptl_absorpt_coefficient_mu 2.207 _cell_measurement_temperature 296 _exptl_crystal_description '' _exptl_crystal_colour '' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method '\w/2\q' _exptl_absorpt_correction_type 'Empirical psi scans(TEXSAN)' _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 4470 _reflns_number_total 4378 _reflns_number_observed 3686 _reflns_observed_criterion refl_observed_if_I_>2.0_sigma(I) _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 26.0 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% 6.4 _refine_ls_structure_factor_coef 'F' _refine_ls_R_factor_obs .030 _refine_ls_wR_factor_obs .042 _refine_ls_goodness_of_fit_obs 1.23 _refine_ls_number_reflns 3686 _refine_ls_number_parameters 271 _refine_ls_hydrogen_treatment 'Not Refined' _refine_ls_weight_scheme 'w=1/(\s^2^(F))' _refine_ls_shift/esd_max 0.003 _refine_diff_density_max 0.41 _refine_diff_density_min -0.83 _atom_type_scat_source 'International Tables for X-Ray Crystallography Vol.IV ' _refine_ls_abs_structure_details ; ; _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CAD4 (Enraf-Nonius)' _computing_data_reduction 'PROCESS(TEXSAN)' _computing_structure_solution 'MITHRIL' _computing_structure_refinement 'LS(TEXSAN)' _computing_molecular_graphics 'ORTEP (1989)' _computing_publication_material 'GCIF_by_Our_laboratory' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type RU 0.24987(3) -0.05295(3) 0.14536(1) 1.0000 0.03473(9) Uani MO 0.35513(3) 0.19301(3) 0.08385(1) 1.0000 0.03245(9) Uani CO 0.08969(5) 0.12876(6) 0.08875(2) 1.0000 0.0384(1) Uani S 0.2325(1) -0.0128(1) 0.04535(4) 1.0000 0.0401(2) Uani O1 0.5976(3) -0.0236(4) 0.0811(2) 1.0000 0.074(1) Uani O2 0.4256(3) 0.2293(4) 0.2160(1) 1.0000 0.0582(9) Uani O3 0.0802(4) -0.3296(4) 0.1431(2) 1.0000 0.079(1) Uani O4 0.4997(4) -0.2222(4) 0.1794(2) 1.0000 0.084(1) Uani O5 0.1904(4) 0.0402(4) 0.2686(1) 1.0000 0.067(1) Uani O6 -0.1320(4) -0.0702(5) 0.1091(2) 1.0000 0.100(2) Uani O7 0.0796(4) 0.3325(4) 0.1868(2) 1.0000 0.074(1) Uani O8 -0.0202(4) 0.3112(4) -0.0076(2) 1.0000 0.074(1) Uani O9 0.6350(3) 0.4581(4) 0.1471(2) 1.0000 0.082(1) Uani O10 0.7323(3) 0.3215(5) 0.0801(2) 1.0000 0.095(2) Uani C1 0.5081(4) 0.0531(4) 0.0829(2) 1.0000 0.048(1) Uani C2 0.3891(4) 0.2030(4) 0.1693(2) 1.0000 0.040(1) Uani C3 0.1425(4) -0.2253(5) 0.1442(2) 1.0000 0.050(1) Uani C4 0.4062(4) -0.1606(5) 0.1668(2) 1.0000 0.051(1) Uani C5 0.2141(4) 0.0032(4) 0.2234(2) 1.0000 0.044(1) Uani C6 -0.0468(4) 0.0087(6) 0.1010(2) 1.0000 0.060(1) Uani C7 0.0867(4) 0.2528(5) 0.1483(2) 1.0000 0.052(1) Uani C8 0.0208(4) 0.2402(5) 0.0295(2) 1.0000 0.052(1) Uani C9 0.5042(4) 0.3775(4) 0.0690(2) 1.0000 0.045(1) Uani C10 0.4746(5) 0.3060(5) 0.0139(2) 1.0000 0.054(1) Uani C11 0.3424(5) 0.3346(5) -0.0019(2) 1.0000 0.059(1) Uani C12 0.2884(4) 0.4236(5) 0.0418(2) 1.0000 0.054(1) Uani C13 0.3876(4) 0.4484(4) 0.0860(2) 1.0000 0.047(1) Uani C14 0.6370(5) 0.3808(5) 0.0989(2) 1.0000 0.062(1) Uani C15 0.7610(7) 0.464(1) 0.1819(4) 1.0000 0.131(4) Uani C16 0.739(1) 0.525(2) 0.2350(6) 1.0000 0.222(6) Uani H1 0.53291 0.24276 -0.01265 1.0000 0.06599 Uiso H2 0.28967 0.30884 -0.03761 1.0000 0.07019 Uiso H3 0.20777 0.45348 0.04475 1.0000 0.06509 Uiso H4 0.38624 0.51887 0.12598 1.0000 0.05603 Uiso H5 0.79465 0.36656 0.18756 1.0000 0.15686 Uiso H6 0.82328 0.52192 0.16226 1.0000 0.15686 Uiso H7 0.82140 0.53267 0.25680 1.0000 0.26401 Uiso H8 0.70325 0.62228 0.22907 1.0000 0.26401 Uiso H9 0.67920 0.46642 0.25491 1.0000 0.26401 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 RU .0390(2) .0319(2) .0333(2) -.0015(1) .0020(1) .0044(1) MO .0352(2) .0307(2) .0319(2) -.0028(1) .0057(1) .0015(1) CO .0341(3) .0434(3) .0374(3) -.0002(2) -.0030(2) .0041(2) S .0482(5) .0410(5) .0311(4) -.0064(4) .0031(4) -.0048(4) O1 .056(2) .071(2) .097(3) .019(2) .028(2) -.002(2) O2 .074(2) .060(2) .040(2) -.008(2) -.006(1) -.006(1) O3 .097(3) .061(2) .076(2) -.037(2) -.019(2) .016(2) O4 .062(2) .076(2) .113(3) .031(2) .002(2) .029(2) O5 .098(3) .062(2) .042(2) -.004(2) .020(2) -.000(1) O6 .050(2) .109(3) .140(4) -.023(2) -.003(2) .045(3) O7 .076(2) .078(2) .069(2) .020(2) .001(2) -.023(2) O8 .077(2) .076(2) .067(2) .005(2) -.023(2) .021(2) O9 .051(2) .089(3) .104(3) -.003(2) -.015(2) -.033(2) O10 .048(2) .101(3) .138(4) .001(2) .027(2) -.016(3) C1 .046(2) .049(2) .050(2) -.004(2) .018(2) -.003(2) C2 .039(2) .037(2) .045(2) .001(2) .006(2) -.000(2) C3 .056(2) .047(2) .047(2) -.007(2) -.001(2) .009(2) C4 .054(3) .043(2) .056(3) .004(2) .003(2) .008(2) C5 .053(2) .037(2) .042(2) -.004(2) .003(2) .006(2) C6 .039(2) .067(3) .072(3) -.004(2) -.004(2) .013(2) C7 .048(2) .054(3) .052(2) .008(2) -.000(2) .001(2) C8 .048(2) .056(3) .052(2) .002(2) -.009(2) .001(2) C9 .043(2) .038(2) .055(2) -.010(2) .011(2) .007(2) C10 .068(3) .048(2) .048(2) -.018(2) .023(2) .007(2) C11 .086(3) .045(2) .044(2) -.017(2) -.001(2) .016(2) C12 .059(3) .039(2) .064(3) -.007(2) -.003(2) .017(2) C13 .055(2) .029(2) .058(2) -.010(2) .007(2) .003(2) C14 .053(3) .050(3) .085(3) -.011(2) .012(2) .003(2) C15 .061(4) .157(8) .171(9) -.012(4) -.042(5) -.046(7) C16 .15(1) .24(1) .26(1) .066(9) -.13(1) -.11(1) loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_frag RU MO 2.8632(7) . 1_555 Yes RU CO 2.6060(8) . 1_555 Yes RU S 2.324(1) . 1_555 Yes RU C3 1.896(4) . 1_555 Yes RU C4 1.897(4) . 1_555 Yes RU C5 1.914(4) . 1_555 Yes MO CO 2.7440(7) . 1_555 Yes MO S 2.380(1) . 1_555 Yes MO C1 1.994(4) . 1_555 Yes MO C2 1.978(4) . 1_555 Yes MO C9 2.280(4) . 1_555 Yes MO C10 2.293(5) . 1_555 Yes MO C11 2.346(4) . 1_555 Yes MO C12 2.380(4) . 1_555 Yes MO C13 2.331(4) . 1_555 Yes CO S 2.199(1) . 1_555 Yes CO C6 1.784(5) . 1_555 Yes CO C7 1.771(5) . 1_555 Yes CO C8 1.806(4) . 1_555 Yes O1 C1 1.139(5) . 1_555 Yes O2 C2 1.144(5) . 1_555 Yes O3 C3 1.132(6) . 1_555 Yes O4 C4 1.120(6) . 1_555 Yes O5 C5 1.128(5) . 1_555 Yes O6 C6 1.137(6) . 1_555 Yes O7 C7 1.144(6) . 1_555 Yes O8 C8 1.128(6) . 1_555 Yes O9 C14 1.310(7) . 1_555 Yes O9 C15 1.468(8) . 1_555 Yes O10 C14 1.197(6) . 1_555 Yes C9 C10 1.440(6) . 1_555 Yes C9 C13 1.410(6) . 1_555 Yes C9 C14 1.476(6) . 1_555 Yes C10 C11 1.388(7) . 1_555 Yes C11 C12 1.414(6) . 1_555 Yes C12 C13 1.409(6) . 1_555 Yes C15 C16 1.37(2) . 1_555 Yes 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_falg MO RU CO 60.01(2) 1_555 . 1_555 Yes MO RU S 53.39(3) 1_555 . 1_555 Yes MO RU C3 148.7(1) 1_555 . 1_555 Yes MO RU C4 101.8(1) 1_555 . 1_555 Yes MO RU C5 110.3(1) 1_555 . 1_555 Yes CO RU S 52.59(3) 1_555 . 1_555 Yes CO RU C3 99.8(1) 1_555 . 1_555 Yes CO RU C4 160.0(1) 1_555 . 1_555 Yes CO RU C5 99.2(1) 1_555 . 1_555 Yes S RU C3 95.6(1) 1_555 . 1_555 Yes S RU C4 111.1(1) 1_555 . 1_555 Yes S RU C5 151.1(1) 1_555 . 1_555 Yes C3 RU C4 92.8(2) 1_555 . 1_555 Yes C3 RU C5 95.7(2) 1_555 . 1_555 Yes C4 RU C5 94.8(2) 1_555 . 1_555 Yes RU MO CO 55.34(2) 1_555 . 1_555 Yes RU MO S 51.63(3) 1_555 . 1_555 Yes RU MO C1 79.5(1) 1_555 . 1_555 Yes RU MO C2 66.2(1) 1_555 . 1_555 Yes RU MO C9 154.6(1) 1_555 . 1_555 Yes RU MO C10 155.5(1) 1_555 . 1_555 Yes RU MO C11 146.1(1) 1_555 . 1_555 Yes RU MO C12 140.9(1) 1_555 . 1_555 Yes RU MO C13 144.3(1) 1_555 . 1_555 Yes CO MO S 50.21(3) 1_555 . 1_555 Yes CO MO C1 128.5(1) 1_555 . 1_555 Yes CO MO C2 95.3(1) 1_555 . 1_555 Yes CO MO C9 144.2(1) 1_555 . 1_555 Yes CO MO C10 131.9(1) 1_555 . 1_555 Yes CO MO C11 97.8(1) 1_555 . 1_555 Yes CO MO C12 86.8(1) 1_555 . 1_555 Yes CO MO C13 110.1(1) 1_555 . 1_555 Yes S MO C1 83.6(1) 1_555 . 1_555 Yes S MO C2 117.8(1) 1_555 . 1_555 Yes S MO C9 148.2(1) 1_555 . 1_555 Yes S MO C10 111.6(1) 1_555 . 1_555 Yes S MO C11 96.1(1) 1_555 . 1_555 Yes S MO C12 113.7(1) 1_555 . 1_555 Yes S MO C13 148.4(1) 1_555 . 1_555 Yes C1 MO C2 86.7(2) 1_555 . 1_555 Yes C1 MO C9 86.9(2) 1_555 . 1_555 Yes C1 MO C10 80.9(2) 1_555 . 1_555 Yes C1 MO C11 110.3(2) 1_555 . 1_555 Yes C1 MO C12 138.9(2) 1_555 . 1_555 Yes C1 MO C13 121.3(2) 1_555 . 1_555 Yes C2 MO C9 91.8(1) 1_555 . 1_555 Yes C2 MO C10 127.1(2) 1_555 . 1_555 Yes C2 MO C11 143.9(2) 1_555 . 1_555 Yes C2 MO C12 113.3(2) 1_555 . 1_555 Yes C2 MO C13 85.2(2) 1_555 . 1_555 Yes C9 MO C10 36.7(2) 1_555 . 1_555 Yes C9 MO C11 59.1(2) 1_555 . 1_555 Yes C9 MO C12 58.3(1) 1_555 . 1_555 Yes C9 MO C13 35.6(1) 1_555 . 1_555 Yes C10 MO C11 34.8(2) 1_555 . 1_555 Yes C10 MO C12 58.2(2) 1_555 . 1_555 Yes C10 MO C13 59.8(2) 1_555 . 1_555 Yes C11 MO C12 34.8(2) 1_555 . 1_555 Yes C11 MO C13 58.7(2) 1_555 . 1_555 Yes C12 MO C13 34.8(1) 1_555 . 1_555 Yes RU CO MO 64.65(2) 1_555 . 1_555 Yes RU CO S 57.11(3) 1_555 . 1_555 Yes RU CO C6 90.1(2) 1_555 . 1_555 Yes RU CO C7 92.6(1) 1_555 . 1_555 Yes RU CO C8 159.1(1) 1_555 . 1_555 Yes MO CO S 56.27(3) 1_555 . 1_555 Yes MO CO C6 153.5(2) 1_555 . 1_555 Yes MO CO C7 87.1(1) 1_555 . 1_555 Yes MO CO C8 101.1(1) 1_555 . 1_555 Yes S CO C6 104.1(2) 1_555 . 1_555 Yes S CO C7 139.0(1) 1_555 . 1_555 Yes S CO C8 102.6(1) 1_555 . 1_555 Yes C6 CO C7 102.8(2) 1_555 . 1_555 Yes C6 CO C8 100.7(2) 1_555 . 1_555 Yes C7 CO C8 102.1(2) 1_555 . 1_555 Yes RU S MO 74.97(3) 1_555 . 1_555 Yes RU S CO 70.30(4) 1_555 . 1_555 Yes MO S CO 73.52(4) 1_555 . 1_555 Yes C14 O9 C15 115.5(5) 1_555 . 1_555 Yes MO C1 O1 177.7(4) 1_555 . 1_555 Yes MO C2 O2 166.9(3) 1_555 . 1_555 Yes RU C3 O3 178.7(4) 1_555 . 1_555 Yes RU C4 O4 178.9(4) 1_555 . 1_555 Yes RU C5 O5 177.6(4) 1_555 . 1_555 Yes CO C6 O6 178.5(4) 1_555 . 1_555 Yes CO C7 O7 177.4(4) 1_555 . 1_555 Yes CO C8 O8 178.8(4) 1_555 . 1_555 Yes MO C9 C10 72.1(2) 1_555 . 1_555 Yes MO C9 C13 74.2(2) 1_555 . 1_555 Yes MO C9 C14 122.3(3) 1_555 . 1_555 Yes C10 C9 C13 107.9(4) 1_555 . 1_555 Yes C10 C9 C14 124.3(4) 1_555 . 1_555 Yes C13 C9 C14 127.6(4) 1_555 . 1_555 Yes MO C10 C9 71.2(2) 1_555 . 1_555 Yes MO C10 C11 74.7(3) 1_555 . 1_555 Yes C9 C10 C11 107.6(4) 1_555 . 1_555 Yes MO C11 C10 70.5(3) 1_555 . 1_555 Yes MO C11 C12 73.9(3) 1_555 . 1_555 Yes C10 C11 C12 108.5(4) 1_555 . 1_555 Yes MO C12 C11 71.3(2) 1_555 . 1_555 Yes MO C12 C13 70.7(2) 1_555 . 1_555 Yes C11 C12 C13 108.6(4) 1_555 . 1_555 Yes MO C13 C9 70.2(2) 1_555 . 1_555 Yes MO C13 C12 74.5(2) 1_555 . 1_555 Yes C9 C13 C12 107.4(4) 1_555 . 1_555 Yes O9 C14 O10 126.0(5) 1_555 . 1_555 Yes O9 C14 C9 110.8(4) 1_555 . 1_555 Yes O10 C14 C9 123.2(5) 1_555 . 1_555 Yes O9 C15 C16 109.1(7) 1_555 . 1_555 Yes _publ_section_references ; Enraf-Nonius (1977). CAD4 Operations Manual. Enraf-Nonius, Delft, The Netherlands. Cromer,D.T. & Waber,J.T.(1974). International Tables for X-ray Crystallography, Vol.IV, Tables 2.2A,2.3.1. Birmingham:Kynoch Press. Gilmore G.J., MITHRIL, (1983). A Computer Program for the Automatic Solution of Crystal Structures from X-Ray Data. University of Glasgow, Scotland. Moleculer Structure Corporation, TEXSAN, TEXRAY Structure Analysis Package, Revised(1987), MSC, 3200A Research Forest Drive, The Woodlands, TX77381, USA. Rogers,D.(1981). Acta Cryst. A37, 734-741 ; data_yin8 _database_code_CSD 159434 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H11 Co Mo O11 Ru S' _chemical_formula_weight 691.27 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 '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' 'S' 'S' 0.1246 0.1234 '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 7.670(3) _cell_length_b 22.001(10) _cell_length_c 13.392(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.230(9) _cell_angle_gamma 90.00 _cell_volume 2258.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used CCD _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description PRISM _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.082 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.6809 _exptl_absorpt_correction_T_max 0.7883 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14867 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5166 _reflns_number_gt 3455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 0.00000(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5166 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1659 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.010 _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 0.22125(4) 0.526099(12) 0.17119(2) 0.04308(8) Uani 1 1 d . . . Mo1 Mo 0.15939(3) 0.645508(11) 0.249965(18) 0.03051(6) Uani 1 1 d . . . Co1 Co 0.04042(6) 0.539528(19) 0.33174(3) 0.03752(12) Uani 1 1 d . . . S1 S -0.04814(11) 0.57324(4) 0.18334(6) 0.0391(2) Uani 1 1 d . . . O1 O 0.5523(3) 0.75933(12) 0.29666(18) 0.0532(7) Uani 1 1 d . . . O2 O 0.5695(3) 0.73749(12) 0.0606(2) 0.0589(8) Uani 1 1 d . . . O3 O 0.8218(4) 0.78755(15) 0.0809(2) 0.0761(10) Uani 1 1 d . . . O4 O 0.1783(4) 0.68387(12) 0.02499(17) 0.0641(9) Uani 1 1 d . . . O5 O 0.5577(3) 0.62065(12) 0.2522(2) 0.0603(8) Uani 1 1 d . . . O6 O 0.3587(5) 0.55387(16) -0.0322(2) 0.1014(12) Uani 1 1 d . . . O7 O 0.5596(4) 0.47368(14) 0.2618(3) 0.0821(11) Uani 1 1 d . . . O8 O 0.0749(5) 0.40460(14) 0.1029(3) 0.1061(14) Uani 1 1 d . . . O9 O -0.0356(4) 0.40971(13) 0.3420(3) 0.0860(11) Uani 1 1 d . . . O10 O 0.3443(4) 0.55193(14) 0.4696(2) 0.0734(10) Uani 1 1 d . . . O11 O -0.2495(4) 0.58348(14) 0.4477(2) 0.0721(9) Uani 1 1 d . . . C1 C 0.2517(5) 0.70389(15) 0.3854(2) 0.0432(9) Uani 1 1 d . . . H1A H 0.3537 0.6951 0.4294 0.052 Uiso 1 1 calc R . . C2 C 0.0795(5) 0.68831(15) 0.4050(2) 0.0469(10) Uani 1 1 d . . . H2A H 0.0410 0.6658 0.4633 0.056 Uiso 1 1 calc R . . C3 C -0.0307(5) 0.71405(15) 0.3277(3) 0.0520(10) Uani 1 1 d . . . H3A H -0.1584 0.7123 0.3240 0.062 Uiso 1 1 calc R . . C4 C 0.0727(4) 0.74576(15) 0.2635(3) 0.0470(10) Uani 1 1 d . . . H4A H 0.0293 0.7712 0.2079 0.056 Uiso 1 1 calc R . . C5 C 0.2529(4) 0.74072(14) 0.2974(2) 0.0385(9) Uani 1 1 d . . . C6 C 0.4089(4) 0.77027(14) 0.2600(2) 0.0416(9) Uani 1 1 d . . . C7 C 0.3853(5) 0.81460(16) 0.1725(3) 0.0536(11) Uani 1 1 d . . . H7A H 0.3222 0.8501 0.1942 0.064 Uiso 1 1 calc R . . H7B H 0.3164 0.7953 0.1191 0.064 Uiso 1 1 calc R . . C8 C 0.5605(5) 0.83429(17) 0.1331(3) 0.0599(12) Uani 1 1 d . . . H8A H 0.5394 0.8654 0.0827 0.072 Uiso 1 1 calc R . . H8B H 0.6287 0.8527 0.1876 0.072 Uiso 1 1 calc R . . C9 C 0.6669(5) 0.78506(17) 0.0888(3) 0.0512(10) Uani 1 1 d . . . C10 C 0.6611(6) 0.6866(2) 0.0188(3) 0.0788(16) Uani 1 1 d . . . H10A H 0.5791 0.6551 0.0005 0.118 Uiso 1 1 calc R . . H10B H 0.7449 0.6711 0.0675 0.118 Uiso 1 1 calc R . . H10C H 0.7201 0.6996 -0.0394 0.118 Uiso 1 1 calc R . . C11 C 0.1728(5) 0.66941(15) 0.1059(3) 0.0449(10) Uani 1 1 d . . . C12 C 0.4056(4) 0.62136(14) 0.2467(2) 0.0401(9) Uani 1 1 d . . . C13 C 0.3095(6) 0.54372(18) 0.0448(3) 0.0647(13) Uani 1 1 d . . . C14 C 0.4366(5) 0.49321(18) 0.2266(3) 0.0573(12) Uani 1 1 d . . . C15 C 0.1280(6) 0.44964(18) 0.1287(3) 0.0672(14) Uani 1 1 d . . . C16 C -0.0040(5) 0.45969(17) 0.3359(3) 0.0567(12) Uani 1 1 d . . . C17 C 0.2273(5) 0.54743(15) 0.4125(3) 0.0487(10) Uani 1 1 d . . . C18 C -0.1400(5) 0.56675(16) 0.4032(3) 0.0468(10) 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 0.04443(15) 0.04478(14) 0.04022(14) -0.00645(11) 0.00397(12) 0.00776(12) Mo1 0.02694(13) 0.03766(12) 0.02695(12) -0.00106(10) 0.00127(10) 0.00290(10) Co1 0.0330(2) 0.0438(2) 0.0357(2) 0.00372(17) 0.00104(18) -0.00226(18) S1 0.0338(4) 0.0459(4) 0.0369(4) -0.0013(3) -0.0062(3) 0.0008(3) O1 0.0360(13) 0.0748(16) 0.0480(14) 0.0063(12) -0.0078(11) -0.0059(12) O2 0.0424(14) 0.0676(15) 0.0668(16) -0.0011(13) 0.0009(13) 0.0024(12) O3 0.0426(16) 0.115(2) 0.0705(18) 0.0223(17) 0.0020(14) -0.0067(16) O4 0.090(2) 0.0701(16) 0.0314(12) 0.0091(11) -0.0050(13) -0.0101(15) O5 0.0388(14) 0.0614(15) 0.0806(18) -0.0014(14) 0.0008(13) 0.0063(12) O6 0.142(3) 0.111(2) 0.0537(16) 0.0039(16) 0.0450(16) 0.037(2) O7 0.0565(18) 0.085(2) 0.104(2) 0.0138(17) -0.0058(18) 0.0231(15) O8 0.130(3) 0.0705(19) 0.117(3) -0.0364(18) -0.010(2) -0.008(2) O9 0.087(2) 0.0562(16) 0.115(2) 0.0154(16) 0.002(2) -0.0162(15) O10 0.0597(18) 0.091(2) 0.0681(18) 0.0155(15) -0.0221(15) -0.0185(15) O11 0.0562(17) 0.091(2) 0.0705(17) -0.0037(16) 0.0213(14) 0.0005(16) C1 0.0470(19) 0.0548(18) 0.0278(14) -0.0097(13) 0.0014(14) -0.0068(15) C2 0.053(2) 0.0516(18) 0.0370(16) -0.0109(14) 0.0163(15) -0.0086(15) C3 0.0409(19) 0.0454(17) 0.071(2) -0.0168(16) 0.0178(17) -0.0002(15) C4 0.0398(18) 0.0394(16) 0.062(2) -0.0079(15) 0.0099(16) 0.0072(14) C5 0.0351(17) 0.0452(16) 0.0351(16) -0.0072(13) -0.0004(13) -0.0014(13) C6 0.0362(17) 0.0408(16) 0.0476(18) -0.0040(14) 0.0013(15) 0.0013(14) C7 0.050(2) 0.0443(18) 0.067(2) 0.0094(17) 0.0015(19) 0.0043(16) C8 0.057(2) 0.056(2) 0.068(2) 0.0192(17) 0.013(2) -0.0087(18) C9 0.0368(19) 0.075(2) 0.0415(17) 0.0230(16) 0.0014(15) -0.0008(17) C10 0.081(3) 0.086(3) 0.071(3) 0.007(2) 0.016(2) 0.023(2) C11 0.049(2) 0.0454(17) 0.0400(17) 0.0006(14) -0.0059(16) -0.0035(15) C12 0.0427(18) 0.0397(15) 0.0382(16) 0.0066(13) 0.0053(14) 0.0037(14) C13 0.084(3) 0.069(2) 0.0416(19) -0.0147(17) 0.0069(19) 0.023(2) C14 0.048(2) 0.052(2) 0.073(2) -0.0056(18) 0.012(2) -0.0004(17) C15 0.074(3) 0.052(2) 0.075(3) -0.0208(19) -0.001(2) 0.005(2) C16 0.053(2) 0.058(2) 0.059(2) 0.0111(18) -0.0027(19) -0.0045(18) C17 0.051(2) 0.0458(17) 0.0496(19) 0.0119(15) 0.0030(17) -0.0081(16) C18 0.044(2) 0.0551(19) 0.0417(17) -0.0021(15) 0.0072(15) -0.0028(16) _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 C13 1.887(4) . ? Ru1 C15 1.906(4) . ? Ru1 C14 1.926(4) . ? Ru1 S1 2.3234(12) . ? Ru1 Co1 2.6203(10) . ? Ru1 Mo1 2.8773(11) . ? Mo1 C12 1.964(4) . ? Mo1 C11 2.006(4) . ? Mo1 C5 2.296(3) . ? Mo1 C1 2.311(3) . ? Mo1 C4 2.313(3) . ? Mo1 C3 2.367(4) . ? Mo1 C2 2.382(3) . ? Mo1 S1 2.3973(11) . ? Mo1 Co1 2.7471(10) . ? Co1 C17 1.770(4) . ? Co1 C16 1.790(4) . ? Co1 C18 1.815(4) . ? Co1 S1 2.2037(12) . ? O1 C6 1.211(4) . ? O2 C9 1.332(5) . ? O2 C10 1.447(5) . ? O3 C9 1.198(4) . ? O4 C11 1.132(4) . ? O5 C12 1.167(4) . ? O6 C13 1.134(5) . ? O7 C14 1.124(5) . ? O8 C15 1.121(5) . ? O9 C16 1.130(5) . ? O10 C17 1.161(4) . ? O11 C18 1.111(5) . ? C1 C2 1.400(5) . ? C1 C5 1.430(4) . ? C2 C3 1.428(5) . ? C3 C4 1.381(5) . ? C4 C5 1.442(5) . ? C5 C6 1.467(5) . ? C6 C7 1.530(5) . ? C7 C8 1.526(5) . ? C8 C9 1.493(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 C13 Ru1 C15 93.30(18) . . ? C13 Ru1 C14 95.16(19) . . ? C15 Ru1 C14 95.14(18) . . ? C13 Ru1 S1 108.80(14) . . ? C15 Ru1 S1 95.19(14) . . ? C14 Ru1 S1 153.24(13) . . ? C13 Ru1 Co1 158.82(13) . . ? C15 Ru1 Co1 98.03(14) . . ? C14 Ru1 Co1 101.54(13) . . ? S1 Ru1 Co1 52.53(3) . . ? C13 Ru1 Mo1 102.19(12) . . ? C15 Ru1 Mo1 148.19(14) . . ? C14 Ru1 Mo1 110.68(12) . . ? S1 Ru1 Mo1 53.62(2) . . ? Co1 Ru1 Mo1 59.741(15) . . ? C12 Mo1 C11 87.95(14) . . ? C12 Mo1 C5 87.86(13) . . ? C11 Mo1 C5 90.00(12) . . ? C12 Mo1 C1 84.39(13) . . ? C11 Mo1 C1 125.69(13) . . ? C5 Mo1 C1 36.16(11) . . ? C12 Mo1 C4 122.64(13) . . ? C11 Mo1 C4 81.44(13) . . ? C5 Mo1 C4 36.47(12) . . ? C1 Mo1 C4 59.24(12) . . ? C12 Mo1 C3 142.32(13) . . ? C11 Mo1 C3 108.15(14) . . ? C5 Mo1 C3 59.21(12) . . ? C1 Mo1 C3 58.39(13) . . ? C4 Mo1 C3 34.31(12) . . ? C12 Mo1 C2 113.99(13) . . ? C11 Mo1 C2 139.40(13) . . ? C5 Mo1 C2 59.07(11) . . ? C1 Mo1 C2 34.66(12) . . ? C4 Mo1 C2 57.99(12) . . ? C3 Mo1 C2 34.99(12) . . ? C12 Mo1 S1 115.94(10) . . ? C11 Mo1 S1 82.76(10) . . ? C5 Mo1 S1 154.68(9) . . ? C1 Mo1 S1 147.09(9) . . ? C4 Mo1 S1 118.23(9) . . ? C3 Mo1 S1 100.08(9) . . ? C2 Mo1 S1 113.40(9) . . ? C12 Mo1 Co1 96.54(9) . . ? C11 Mo1 Co1 129.50(10) . . ? C5 Mo1 Co1 140.27(8) . . ? C1 Mo1 Co1 104.80(9) . . ? C4 Mo1 Co1 132.62(9) . . ? C3 Mo1 Co1 98.37(9) . . ? C2 Mo1 Co1 83.54(9) . . ? S1 Mo1 Co1 50.16(3) . . ? C12 Mo1 Ru1 64.68(9) . . ? C11 Mo1 Ru1 82.61(10) . . ? C5 Mo1 Ru1 151.68(9) . . ? C1 Mo1 Ru1 138.19(9) . . ? C4 Mo1 Ru1 162.09(9) . . ? C3 Mo1 Ru1 148.90(9) . . ? C2 Mo1 Ru1 137.09(8) . . ? S1 Mo1 Ru1 51.29(3) . . ? Co1 Mo1 Ru1 55.48(3) . . ? C17 Co1 C16 103.18(17) . . ? C17 Co1 C18 105.19(17) . . ? C16 Co1 C18 99.06(17) . . ? C17 Co1 S1 137.02(12) . . ? C16 Co1 S1 107.80(13) . . ? C18 Co1 S1 98.61(12) . . ? C17 Co1 Ru1 94.02(12) . . ? C16 Co1 Ru1 91.27(13) . . ? C18 Co1 Ru1 155.34(11) . . ? S1 Co1 Ru1 56.80(4) . . ? C17 Co1 Mo1 83.48(11) . . ? C16 Co1 Mo1 155.72(13) . . ? C18 Co1 Mo1 101.66(11) . . ? S1 Co1 Mo1 56.65(3) . . ? Ru1 Co1 Mo1 64.78(2) . . ? Co1 S1 Ru1 70.68(3) . . ? Co1 S1 Mo1 73.18(3) . . ? Ru1 S1 Mo1 75.09(4) . . ? C9 O2 C10 116.3(3) . . ? C2 C1 C5 109.3(3) . . ? C2 C1 Mo1 75.44(19) . . ? C5 C1 Mo1 71.36(18) . . ? C1 C2 C3 107.6(3) . . ? C1 C2 Mo1 69.90(18) . . ? C3 C2 Mo1 71.94(19) . . ? C4 C3 C2 108.3(3) . . ? C4 C3 Mo1 70.7(2) . . ? C2 C3 Mo1 73.07(19) . . ? C3 C4 C5 109.4(3) . . ? C3 C4 Mo1 75.0(2) . . ? C5 C4 Mo1 71.13(18) . . ? C1 C5 C4 105.4(3) . . ? C1 C5 C6 124.3(3) . . ? C4 C5 C6 130.0(3) . . ? C1 C5 Mo1 72.48(18) . . ? C4 C5 Mo1 72.40(18) . . ? C6 C5 Mo1 124.0(2) . . ? O1 C6 C5 120.8(3) . . ? O1 C6 C7 121.1(3) . . ? C5 C6 C7 118.1(3) . . ? C6 C7 C8 111.5(3) . . ? C9 C8 C7 115.7(3) . . ? O3 C9 O2 123.9(4) . . ? O3 C9 C8 124.1(4) . . ? O2 C9 C8 112.0(3) . . ? O4 C11 Mo1 178.6(3) . . ? O5 C12 Mo1 164.3(3) . . ? O6 C13 Ru1 178.3(4) . . ? O7 C14 Ru1 177.6(4) . . ? O8 C15 Ru1 179.1(4) . . ? O9 C16 Co1 177.1(4) . . ? O10 C17 Co1 176.3(3) . . ? O11 C18 Co1 179.4(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 C13 Ru1 Mo1 C12 -73.36(17) . . . . ? C15 Ru1 Mo1 C12 169.3(3) . . . . ? C14 Ru1 Mo1 C12 27.01(16) . . . . ? S1 Ru1 Mo1 C12 -177.85(10) . . . . ? Co1 Ru1 Mo1 C12 118.58(10) . . . . ? C13 Ru1 Mo1 C11 17.87(18) . . . . ? C15 Ru1 Mo1 C11 -99.5(3) . . . . ? C14 Ru1 Mo1 C11 118.24(17) . . . . ? S1 Ru1 Mo1 C11 -86.62(11) . . . . ? Co1 Ru1 Mo1 C11 -150.19(11) . . . . ? C13 Ru1 Mo1 C5 -58.2(2) . . . . ? C15 Ru1 Mo1 C5 -175.6(3) . . . . ? C14 Ru1 Mo1 C5 42.2(2) . . . . ? S1 Ru1 Mo1 C5 -162.70(17) . . . . ? Co1 Ru1 Mo1 C5 133.73(17) . . . . ? C13 Ru1 Mo1 C1 -119.64(19) . . . . ? C15 Ru1 Mo1 C1 123.0(3) . . . . ? C14 Ru1 Mo1 C1 -19.27(18) . . . . ? S1 Ru1 Mo1 C1 135.87(13) . . . . ? Co1 Ru1 Mo1 C1 72.30(13) . . . . ? C13 Ru1 Mo1 C4 45.1(3) . . . . ? C15 Ru1 Mo1 C4 -72.3(4) . . . . ? C14 Ru1 Mo1 C4 145.5(3) . . . . ? S1 Ru1 Mo1 C4 -59.4(3) . . . . ? Co1 Ru1 Mo1 C4 -123.0(3) . . . . ? C13 Ru1 Mo1 C3 131.0(2) . . . . ? C15 Ru1 Mo1 C3 13.6(3) . . . . ? C14 Ru1 Mo1 C3 -128.6(2) . . . . ? S1 Ru1 Mo1 C3 26.54(18) . . . . ? Co1 Ru1 Mo1 C3 -37.03(18) . . . . ? C13 Ru1 Mo1 C2 -172.09(19) . . . . ? C15 Ru1 Mo1 C2 70.5(3) . . . . ? C14 Ru1 Mo1 C2 -71.72(18) . . . . ? S1 Ru1 Mo1 C2 83.42(13) . . . . ? Co1 Ru1 Mo1 C2 19.85(13) . . . . ? C13 Ru1 Mo1 S1 104.49(14) . . . . ? C15 Ru1 Mo1 S1 -12.9(2) . . . . ? C14 Ru1 Mo1 S1 -155.14(13) . . . . ? Co1 Ru1 Mo1 S1 -63.57(3) . . . . ? C13 Ru1 Mo1 Co1 168.06(14) . . . . ? C15 Ru1 Mo1 Co1 50.7(2) . . . . ? C14 Ru1 Mo1 Co1 -91.57(13) . . . . ? S1 Ru1 Mo1 Co1 63.57(3) . . . . ? C13 Ru1 Co1 C17 -114.9(4) . . . . ? C15 Ru1 Co1 C17 123.46(17) . . . . ? C14 Ru1 Co1 C17 26.50(16) . . . . ? S1 Ru1 Co1 C17 -146.15(11) . . . . ? Mo1 Ru1 Co1 C17 -80.85(11) . . . . ? C13 Ru1 Co1 C16 141.8(4) . . . . ? C15 Ru1 Co1 C16 20.15(18) . . . . ? C14 Ru1 Co1 C16 -76.81(17) . . . . ? S1 Ru1 Co1 C16 110.54(13) . . . . ? Mo1 Ru1 Co1 C16 175.83(13) . . . . ? C13 Ru1 Co1 C18 26.6(5) . . . . ? C15 Ru1 Co1 C18 -95.1(3) . . . . ? C14 Ru1 Co1 C18 168.0(3) . . . . ? S1 Ru1 Co1 C18 -4.7(3) . . . . ? Mo1 Ru1 Co1 C18 60.6(3) . . . . ? C13 Ru1 Co1 S1 31.3(4) . . . . ? C15 Ru1 Co1 S1 -90.39(14) . . . . ? C14 Ru1 Co1 S1 172.64(12) . . . . ? Mo1 Ru1 Co1 S1 65.29(3) . . . . ? C13 Ru1 Co1 Mo1 -34.0(4) . . . . ? C15 Ru1 Co1 Mo1 -155.69(13) . . . . ? C14 Ru1 Co1 Mo1 107.35(12) . . . . ? S1 Ru1 Co1 Mo1 -65.29(3) . . . . ? C12 Mo1 Co1 C17 44.54(15) . . . . ? C11 Mo1 Co1 C17 137.28(18) . . . . ? C5 Mo1 Co1 C17 -49.99(18) . . . . ? C1 Mo1 Co1 C17 -41.36(15) . . . . ? C4 Mo1 Co1 C17 -102.95(17) . . . . ? C3 Mo1 Co1 C17 -100.75(15) . . . . ? C2 Mo1 Co1 C17 -68.97(15) . . . . ? S1 Mo1 Co1 C17 163.08(12) . . . . ? Ru1 Mo1 Co1 C17 97.58(12) . . . . ? C12 Mo1 Co1 C16 -63.2(3) . . . . ? C11 Mo1 Co1 C16 29.5(3) . . . . ? C5 Mo1 Co1 C16 -157.7(3) . . . . ? C1 Mo1 Co1 C16 -149.1(3) . . . . ? C4 Mo1 Co1 C16 149.3(3) . . . . ? C3 Mo1 Co1 C16 151.5(3) . . . . ? C2 Mo1 Co1 C16 -176.7(3) . . . . ? S1 Mo1 Co1 C16 55.3(3) . . . . ? Ru1 Mo1 Co1 C16 -10.2(3) . . . . ? C12 Mo1 Co1 C18 148.76(15) . . . . ? C11 Mo1 Co1 C18 -118.50(18) . . . . ? C5 Mo1 Co1 C18 54.23(17) . . . . ? C1 Mo1 Co1 C18 62.86(15) . . . . ? C4 Mo1 Co1 C18 1.27(17) . . . . ? C3 Mo1 Co1 C18 3.47(15) . . . . ? C2 Mo1 Co1 C18 35.25(14) . . . . ? S1 Mo1 Co1 C18 -92.71(12) . . . . ? Ru1 Mo1 Co1 C18 -158.21(11) . . . . ? C12 Mo1 Co1 S1 -118.54(10) . . . . ? C11 Mo1 Co1 S1 -25.79(14) . . . . ? C5 Mo1 Co1 S1 146.93(13) . . . . ? C1 Mo1 Co1 S1 155.57(9) . . . . ? C4 Mo1 Co1 S1 93.98(13) . . . . ? C3 Mo1 Co1 S1 96.17(10) . . . . ? C2 Mo1 Co1 S1 127.96(9) . . . . ? Ru1 Mo1 Co1 S1 -65.50(4) . . . . ? C12 Mo1 Co1 Ru1 -53.04(9) . . . . ? C11 Mo1 Co1 Ru1 39.71(14) . . . . ? C5 Mo1 Co1 Ru1 -147.57(13) . . . . ? C1 Mo1 Co1 Ru1 -138.93(9) . . . . ? C4 Mo1 Co1 Ru1 159.47(12) . . . . ? C3 Mo1 Co1 Ru1 161.67(9) . . . . ? C2 Mo1 Co1 Ru1 -166.55(9) . . . . ? S1 Mo1 Co1 Ru1 65.50(4) . . . . ? C17 Co1 S1 Ru1 54.59(18) . . . . ? C16 Co1 S1 Ru1 -79.50(14) . . . . ? C18 Co1 S1 Ru1 178.03(11) . . . . ? Mo1 Co1 S1 Ru1 79.70(4) . . . . ? C17 Co1 S1 Mo1 -25.10(17) . . . . ? C16 Co1 S1 Mo1 -159.19(14) . . . . ? C18 Co1 S1 Mo1 98.34(12) . . . . ? Ru1 Co1 S1 Mo1 -79.70(4) . . . . ? C13 Ru1 S1 Co1 -168.57(13) . . . . ? C15 Ru1 S1 Co1 96.16(13) . . . . ? C14 Ru1 S1 Co1 -16.2(3) . . . . ? Mo1 Ru1 S1 Co1 -77.06(3) . . . . ? C13 Ru1 S1 Mo1 -91.51(14) . . . . ? C15 Ru1 S1 Mo1 173.22(13) . . . . ? C14 Ru1 S1 Mo1 60.9(3) . . . . ? Co1 Ru1 S1 Mo1 77.06(3) . . . . ? C12 Mo1 S1 Co1 76.06(10) . . . . ? C11 Mo1 S1 Co1 160.22(11) . . . . ? C5 Mo1 S1 Co1 -125.36(19) . . . . ? C1 Mo1 S1 Co1 -47.40(16) . . . . ? C4 Mo1 S1 Co1 -123.58(11) . . . . ? C3 Mo1 S1 Co1 -92.54(10) . . . . ? C2 Mo1 S1 Co1 -58.62(10) . . . . ? Ru1 Mo1 S1 Co1 73.90(3) . . . . ? C12 Mo1 S1 Ru1 2.16(10) . . . . ? C11 Mo1 S1 Ru1 86.31(11) . . . . ? C5 Mo1 S1 Ru1 160.73(19) . . . . ? C1 Mo1 S1 Ru1 -121.30(16) . . . . ? C4 Mo1 S1 Ru1 162.52(10) . . . . ? C3 Mo1 S1 Ru1 -166.44(9) . . . . ? C2 Mo1 S1 Ru1 -132.52(9) . . . . ? Co1 Mo1 S1 Ru1 -73.90(3) . . . . ? C12 Mo1 C1 C2 -149.4(2) . . . . ? C11 Mo1 C1 C2 127.2(2) . . . . ? C5 Mo1 C1 C2 116.6(3) . . . . ? C4 Mo1 C1 C2 77.1(2) . . . . ? C3 Mo1 C1 C2 36.7(2) . . . . ? S1 Mo1 C1 C2 -18.3(3) . . . . ? Co1 Mo1 C1 C2 -54.1(2) . . . . ? Ru1 Mo1 C1 C2 -108.3(2) . . . . ? C12 Mo1 C1 C5 94.1(2) . . . . ? C11 Mo1 C1 C5 10.7(3) . . . . ? C4 Mo1 C1 C5 -39.50(19) . . . . ? C3 Mo1 C1 C5 -79.8(2) . . . . ? C2 Mo1 C1 C5 -116.6(3) . . . . ? S1 Mo1 C1 C5 -134.87(17) . . . . ? Co1 Mo1 C1 C5 -170.64(17) . . . . ? Ru1 Mo1 C1 C5 135.09(17) . . . . ? C5 C1 C2 C3 1.4(4) . . . . ? Mo1 C1 C2 C3 -62.4(2) . . . . ? C5 C1 C2 Mo1 63.9(2) . . . . ? C12 Mo1 C2 C1 33.7(2) . . . . ? C11 Mo1 C2 C1 -83.6(3) . . . . ? C5 Mo1 C2 C1 -37.97(19) . . . . ? C4 Mo1 C2 C1 -81.0(2) . . . . ? C3 Mo1 C2 C1 -117.3(3) . . . . ? S1 Mo1 C2 C1 169.29(17) . . . . ? Co1 Mo1 C2 C1 128.01(19) . . . . ? Ru1 Mo1 C2 C1 111.66(19) . . . . ? C12 Mo1 C2 C3 151.0(2) . . . . ? C11 Mo1 C2 C3 33.7(3) . . . . ? C5 Mo1 C2 C3 79.4(2) . . . . ? C1 Mo1 C2 C3 117.3(3) . . . . ? C4 Mo1 C2 C3 36.3(2) . . . . ? S1 Mo1 C2 C3 -73.4(2) . . . . ? Co1 Mo1 C2 C3 -114.67(19) . . . . ? Ru1 Mo1 C2 C3 -131.02(17) . . . . ? C1 C2 C3 C4 -1.2(4) . . . . ? Mo1 C2 C3 C4 -62.3(2) . . . . ? C1 C2 C3 Mo1 61.1(2) . . . . ? C12 Mo1 C3 C4 70.6(3) . . . . ? C11 Mo1 C3 C4 -40.7(2) . . . . ? C5 Mo1 C3 C4 38.1(2) . . . . ? C1 Mo1 C3 C4 80.6(2) . . . . ? C2 Mo1 C3 C4 117.0(3) . . . . ? S1 Mo1 C3 C4 -126.3(2) . . . . ? Co1 Mo1 C3 C4 -177.1(2) . . . . ? Ru1 Mo1 C3 C4 -147.03(18) . . . . ? C12 Mo1 C3 C2 -46.4(3) . . . . ? C11 Mo1 C3 C2 -157.7(2) . . . . ? C5 Mo1 C3 C2 -78.9(2) . . . . ? C1 Mo1 C3 C2 -36.40(19) . . . . ? C4 Mo1 C3 C2 -117.0(3) . . . . ? S1 Mo1 C3 C2 116.72(19) . . . . ? Co1 Mo1 C3 C2 65.88(19) . . . . ? Ru1 Mo1 C3 C2 96.0(2) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? Mo1 C3 C4 C5 -63.3(2) . . . . ? C2 C3 C4 Mo1 63.9(2) . . . . ? C12 Mo1 C4 C3 -136.8(2) . . . . ? C11 Mo1 C4 C3 141.2(2) . . . . ? C5 Mo1 C4 C3 -117.0(3) . . . . ? C1 Mo1 C4 C3 -77.9(2) . . . . ? C2 Mo1 C4 C3 -37.1(2) . . . . ? S1 Mo1 C4 C3 64.3(2) . . . . ? Co1 Mo1 C4 C3 3.9(3) . . . . ? Ru1 Mo1 C4 C3 113.9(3) . . . . ? C12 Mo1 C4 C5 -19.8(2) . . . . ? C11 Mo1 C4 C5 -101.7(2) . . . . ? C1 Mo1 C4 C5 39.16(19) . . . . ? C3 Mo1 C4 C5 117.0(3) . . . . ? C2 Mo1 C4 C5 80.0(2) . . . . ? S1 Mo1 C4 C5 -178.72(15) . . . . ? Co1 Mo1 C4 C5 120.89(17) . . . . ? Ru1 Mo1 C4 C5 -129.1(3) . . . . ? C2 C1 C5 C4 -1.1(4) . . . . ? Mo1 C1 C5 C4 65.4(2) . . . . ? C2 C1 C5 C6 173.8(3) . . . . ? Mo1 C1 C5 C6 -119.7(3) . . . . ? C2 C1 C5 Mo1 -66.5(2) . . . . ? C3 C4 C5 C1 0.3(4) . . . . ? Mo1 C4 C5 C1 -65.5(2) . . . . ? C3 C4 C5 C6 -174.2(3) . . . . ? Mo1 C4 C5 C6 120.0(3) . . . . ? C3 C4 C5 Mo1 65.8(2) . . . . ? C12 Mo1 C5 C1 -83.4(2) . . . . ? C11 Mo1 C5 C1 -171.4(2) . . . . ? C4 Mo1 C5 C1 113.1(3) . . . . ? C3 Mo1 C5 C1 77.4(2) . . . . ? C2 Mo1 C5 C1 36.4(2) . . . . ? S1 Mo1 C5 C1 115.8(2) . . . . ? Co1 Mo1 C5 C1 14.2(3) . . . . ? Ru1 Mo1 C5 C1 -97.1(2) . . . . ? C12 Mo1 C5 C4 163.5(2) . . . . ? C11 Mo1 C5 C4 75.5(2) . . . . ? C1 Mo1 C5 C4 -113.1(3) . . . . ? C3 Mo1 C5 C4 -35.8(2) . . . . ? C2 Mo1 C5 C4 -76.8(2) . . . . ? S1 Mo1 C5 C4 2.6(3) . . . . ? Co1 Mo1 C5 C4 -98.9(2) . . . . ? Ru1 Mo1 C5 C4 149.77(18) . . . . ? C12 Mo1 C5 C6 36.6(3) . . . . ? C11 Mo1 C5 C6 -51.3(3) . . . . ? C1 Mo1 C5 C6 120.1(4) . . . . ? C4 Mo1 C5 C6 -126.8(4) . . . . ? C3 Mo1 C5 C6 -162.6(3) . . . . ? C2 Mo1 C5 C6 156.4(3) . . . . ? S1 Mo1 C5 C6 -124.2(2) . . . . ? Co1 Mo1 C5 C6 134.3(2) . . . . ? Ru1 Mo1 C5 C6 23.0(4) . . . . ? C1 C5 C6 O1 8.3(5) . . . . ? C4 C5 C6 O1 -178.2(3) . . . . ? Mo1 C5 C6 O1 -83.0(4) . . . . ? C1 C5 C6 C7 -172.5(3) . . . . ? C4 C5 C6 C7 1.1(5) . . . . ? Mo1 C5 C6 C7 96.3(3) . . . . ? O1 C6 C7 C8 7.4(5) . . . . ? C5 C6 C7 C8 -171.9(3) . . . . ? C6 C7 C8 C9 64.0(4) . . . . ? C10 O2 C9 O3 0.4(5) . . . . ? C10 O2 C9 C8 -178.6(3) . . . . ? C7 C8 C9 O3 -157.7(4) . . . . ? C7 C8 C9 O2 21.3(5) . . . . ? C12 Mo1 C11 O4 -141(15) . . . . ? C5 Mo1 C11 O4 -54(15) . . . . ? C1 Mo1 C11 O4 -60(15) . . . . ? C4 Mo1 C11 O4 -18(15) . . . . ? C3 Mo1 C11 O4 4(15) . . . . ? C2 Mo1 C11 O4 -16(15) . . . . ? S1 Mo1 C11 O4 102(15) . . . . ? Co1 Mo1 C11 O4 122(15) . . . . ? Ru1 Mo1 C11 O4 154(15) . . . . ? C11 Mo1 C12 O5 92.1(10) . . . . ? C5 Mo1 C12 O5 2.0(10) . . . . ? C1 Mo1 C12 O5 -34.1(10) . . . . ? C4 Mo1 C12 O5 13.6(11) . . . . ? C3 Mo1 C12 O5 -25.5(11) . . . . ? C2 Mo1 C12 O5 -52.5(10) . . . . ? S1 Mo1 C12 O5 173.0(10) . . . . ? Co1 Mo1 C12 O5 -138.4(10) . . . . ? Ru1 Mo1 C12 O5 174.9(11) . . . . ? C15 Ru1 C13 O6 46(13) . . . . ? C14 Ru1 C13 O6 142(13) . . . . ? S1 Ru1 C13 O6 -51(13) . . . . ? Co1 Ru1 C13 O6 -76(13) . . . . ? Mo1 Ru1 C13 O6 -106(13) . . . . ? C13 Ru1 C14 O7 180(100) . . . . ? C15 Ru1 C14 O7 -86(9) . . . . ? S1 Ru1 C14 O7 26(9) . . . . ? Co1 Ru1 C14 O7 13(9) . . . . ? Mo1 Ru1 C14 O7 75(9) . . . . ? C13 Ru1 C15 O8 32(29) . . . . ? C14 Ru1 C15 O8 -63(29) . . . . ? S1 Ru1 C15 O8 141(29) . . . . ? Co1 Ru1 C15 O8 -166(29) . . . . ? Mo1 Ru1 C15 O8 152(28) . . . . ? C17 Co1 C16 O9 83(8) . . . . ? C18 Co1 C16 O9 -25(8) . . . . ? S1 Co1 C16 O9 -127(8) . . . . ? Ru1 Co1 C16 O9 177(100) . . . . ? Mo1 Co1 C16 O9 -174(7) . . . . ? C16 Co1 C17 O10 -70(5) . . . . ? C18 Co1 C17 O10 33(5) . . . . ? S1 Co1 C17 O10 154(5) . . . . ? Ru1 Co1 C17 O10 -163(5) . . . . ? Mo1 Co1 C17 O10 133(5) . . . . ? C17 Co1 C18 O11 -5(30) . . . . ? C16 Co1 C18 O11 101(30) . . . . ? S1 Co1 C18 O11 -149(100) . . . . ? Ru1 Co1 C18 O11 -145(100) . . . . ? Mo1 Co1 C18 O11 -92(30) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.955 _refine_diff_density_min -0.817 _refine_diff_density_rms 0.186