# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M Whittlesey' _publ_contact_author_email M.K.WHITTLESEY@BATH.AC.UK _publ_section_title ; Abnormal Coordination of Arduengo's Carbene Upon Reaction with M3(CO)12 (M = Ru, Os) ; loop_ _publ_author_name 'M Whittlesey' 'Matthew R Crittall' 'Charles E Ellul' 'Mary Mahon' 'Olly Saker' # Attachment '1_k07mkw32.cif' data_k07mkw32 _database_code_depnum_ccdc_archive 'CCDC 687171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H40 N2 O12 Ru3' _chemical_formula_weight 1019.93 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' N N 0.0061 0.0033 '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 P21/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 14.7010(1) _cell_length_b 18.5170(2) _cell_length_c 15.1150(1) _cell_angle_alpha 90.00 _cell_angle_beta 105.924(1) _cell_angle_gamma 90.00 _cell_volume 3956.69(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68733 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.194 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79718 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9050 _reflns_number_gt 7727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+3.5296P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9050 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.731331(13) 0.029777(10) 0.715314(12) 0.01847(5) Uani 1 1 d . . . Ru2 Ru 0.805868(14) -0.034334(11) 0.890884(13) 0.02328(6) Uani 1 1 d . A . Ru3 Ru 0.810389(14) -0.114591(10) 0.730383(13) 0.02189(6) Uani 1 1 d . A . O1 O 0.54693(14) -0.05575(12) 0.65574(15) 0.0414(5) Uani 1 1 d . . . O2 O 0.63803(17) 0.13578(11) 0.81337(13) 0.0438(5) Uani 1 1 d . . . O3 O 0.90451(15) 0.12785(11) 0.73365(15) 0.0418(5) Uani 1 1 d . . . O4 O 0.82061(16) 0.09567(12) 1.01769(14) 0.0423(5) Uani 1 1 d . A . O5 O 0.59420(15) -0.05455(12) 0.87744(15) 0.0429(5) Uani 1 1 d . A . O6 O 0.8740(2) -0.15635(13) 1.03046(15) 0.0631(7) Uani 1 1 d . A . O7 O 1.00521(15) 0.00573(15) 0.88094(14) 0.0506(6) Uani 1 1 d . A . O8 O 0.64115(17) -0.19424(11) 0.76981(17) 0.0496(6) Uani 1 1 d . A . O9 O 0.96395(19) -0.21620(15) 0.84051(17) 0.0637(7) Uani 1 1 d . A . O10 O 0.77456(15) -0.19090(11) 0.54579(14) 0.0402(5) Uani 1 1 d . A . O11 O 0.95093(14) -0.02094(11) 0.66399(14) 0.0356(4) Uani 1 1 d . A . O12 O 0.81689(17) 0.19022(16) 0.41658(19) 0.0644(7) Uani 1 1 d . . . N1 N 0.65747(13) 0.10957(10) 0.51055(12) 0.0170(4) Uani 1 1 d . . . N2 N 0.70026(14) 0.02958(10) 0.42412(13) 0.0188(4) Uani 1 1 d . . . C1 C 0.6187(2) -0.02810(14) 0.68130(17) 0.0273(5) Uani 1 1 d . A . C2 C 0.6734(2) 0.09786(14) 0.77252(17) 0.0284(6) Uani 1 1 d . A . C3 C 0.8440(2) 0.08911(14) 0.73029(17) 0.0285(6) Uani 1 1 d . A . C4 C 0.81151(19) 0.04696(15) 0.97014(17) 0.0290(6) Uani 1 1 d . . . C5 C 0.6720(2) -0.04856(15) 0.87885(18) 0.0315(6) Uani 1 1 d . . . C6 C 0.8493(2) -0.11155(16) 0.97835(19) 0.0394(7) Uani 1 1 d . . . C7 C 0.9301(2) -0.01075(17) 0.88001(17) 0.0339(6) Uani 1 1 d . . . C8 C 0.7027(2) -0.16141(15) 0.7582(2) 0.0350(6) Uani 1 1 d . . . C9 C 0.9058(2) -0.17881(16) 0.8010(2) 0.0377(7) Uani 1 1 d . . . C10 C 0.78649(18) -0.16183(13) 0.61432(18) 0.0270(5) Uani 1 1 d . . . C11 C 0.89490(19) -0.04868(14) 0.69262(17) 0.0267(5) Uani 1 1 d . . . C12 C 0.66072(16) 0.09382(12) 0.42495(15) 0.0180(4) Uani 1 1 d . A . H12 H 0.6381 0.1241 0.3728 0.022 Uiso 1 1 calc R . . C13 C 0.69846(17) 0.05249(12) 0.57047(15) 0.0202(5) Uani 1 1 d . A 1 C14 C 0.72340(18) 0.00372(13) 0.51358(15) 0.0223(5) Uani 1 1 d . A 1 H14 H 0.7525 -0.0416 0.5326 0.027 Uiso 1 1 calc R A 1 C15 C 0.61173(16) 0.17800(12) 0.53024(15) 0.0180(4) Uani 1 1 d . A . C16 C 0.52720(17) 0.15887(12) 0.56719(16) 0.0216(5) Uani 1 1 d . . . H16A H 0.5490 0.1293 0.6237 0.026 Uiso 1 1 calc R A . H16B H 0.4805 0.1303 0.5208 0.026 Uiso 1 1 calc R . . C17 C 0.48066(18) 0.22873(13) 0.58888(17) 0.0254(5) Uani 1 1 d . A . H17 H 0.4265 0.2164 0.6141 0.030 Uiso 1 1 calc R . . C18 C 0.55352(19) 0.27396(13) 0.65957(17) 0.0277(5) Uani 1 1 d . . . H18A H 0.5233 0.3187 0.6737 0.033 Uiso 1 1 calc R A . H18B H 0.5769 0.2462 0.7173 0.033 Uiso 1 1 calc R . . C19 C 0.63646(18) 0.29338(13) 0.62103(17) 0.0253(5) Uani 1 1 d . A . H19 H 0.6835 0.3229 0.6672 0.030 Uiso 1 1 calc R . . C20 C 0.59950(19) 0.33716(13) 0.53225(18) 0.0273(5) Uani 1 1 d . . . H20A H 0.5693 0.3822 0.5454 0.033 Uiso 1 1 calc R A . H20B H 0.6527 0.3504 0.5071 0.033 Uiso 1 1 calc R . . C21 C 0.52751(18) 0.29174(13) 0.46219(16) 0.0241(5) Uani 1 1 d . A . H21 H 0.5037 0.3200 0.4041 0.029 Uiso 1 1 calc R . . C22 C 0.57542(17) 0.22237(12) 0.44163(15) 0.0210(5) Uani 1 1 d . . . H22A H 0.5296 0.1934 0.3949 0.025 Uiso 1 1 calc R A . H22B H 0.6289 0.2350 0.4166 0.025 Uiso 1 1 calc R . . C23 C 0.44468(18) 0.27263(14) 0.50011(18) 0.0279(5) Uani 1 1 d . . . H23A H 0.3975 0.2441 0.4541 0.034 Uiso 1 1 calc R A . H23B H 0.4137 0.3173 0.5130 0.034 Uiso 1 1 calc R . . C24 C 0.68428(17) 0.22393(13) 0.60013(16) 0.0220(5) Uani 1 1 d . . . H24A H 0.7376 0.2365 0.5748 0.026 Uiso 1 1 calc R A . H24B H 0.7096 0.1961 0.6576 0.026 Uiso 1 1 calc R . . C25 C 0.71601(17) -0.00953(12) 0.34374(15) 0.0184(4) Uani 1 1 d . A . C26 C 0.65144(18) -0.07601(13) 0.32428(16) 0.0241(5) Uani 1 1 d . . . H26A H 0.5844 -0.0608 0.3101 0.029 Uiso 1 1 calc R A . H26B H 0.6653 -0.1076 0.3792 0.029 Uiso 1 1 calc R . . C27 C 0.6684(2) -0.11736(14) 0.24228(17) 0.0299(6) Uani 1 1 d . A . H27 H 0.6266 -0.1609 0.2294 0.036 Uiso 1 1 calc R . . C28 C 0.7720(2) -0.14088(14) 0.26517(19) 0.0342(6) Uani 1 1 d . . . H28A H 0.7830 -0.1686 0.2130 0.041 Uiso 1 1 calc R A . H28B H 0.7870 -0.1726 0.3200 0.041 Uiso 1 1 calc R . . C29 C 0.8363(2) -0.07434(15) 0.28399(18) 0.0322(6) Uani 1 1 d . A . H29 H 0.9040 -0.0898 0.2984 0.039 Uiso 1 1 calc R . . C30 C 0.8128(2) -0.02498(15) 0.19989(19) 0.0347(6) Uani 1 1 d . . . H30A H 0.8543 0.0181 0.2124 0.042 Uiso 1 1 calc R A . H30B H 0.8243 -0.0509 0.1467 0.042 Uiso 1 1 calc R . . C31 C 0.7098(2) -0.00158(14) 0.17731(16) 0.0285(6) Uani 1 1 d . A . H31 H 0.6948 0.0305 0.1220 0.034 Uiso 1 1 calc R . . C32 C 0.69257(19) 0.03985(13) 0.25960(16) 0.0236(5) Uani 1 1 d . . . H32A H 0.7330 0.0835 0.2723 0.028 Uiso 1 1 calc R A . H32B H 0.6257 0.0554 0.2452 0.028 Uiso 1 1 calc R . . C33 C 0.81971(18) -0.03270(14) 0.36600(17) 0.0264(5) Uani 1 1 d . . . H33A H 0.8356 -0.0638 0.4214 0.032 Uiso 1 1 calc R A . H33B H 0.8611 0.0104 0.3789 0.032 Uiso 1 1 calc R . . C34 C 0.6450(2) -0.06803(15) 0.15776(17) 0.0326(6) Uani 1 1 d . . . H34A H 0.5780 -0.0526 0.1433 0.039 Uiso 1 1 calc R A . H34B H 0.6542 -0.0946 0.1040 0.039 Uiso 1 1 calc R . . C35 C 0.8908(2) 0.16664(19) 0.4926(2) 0.0478(8) Uani 1 1 d . . . H35A H 0.8777 0.1173 0.5110 0.057 Uiso 1 1 calc R . . H35B H 0.8969 0.1994 0.5457 0.057 Uiso 1 1 calc R . . C36 C 0.9810(2) 0.1674(2) 0.4624(2) 0.0519(9) Uani 1 1 d . . . H36A H 1.0313 0.1952 0.5061 0.062 Uiso 1 1 calc R . . H36B H 1.0039 0.1177 0.4574 0.062 Uiso 1 1 calc R . . C37 C 0.9514(3) 0.2037(3) 0.3697(3) 0.0735(12) Uani 1 1 d . . . H37A H 0.9979 0.2410 0.3646 0.088 Uiso 1 1 calc R . . H37B H 0.9456 0.1680 0.3197 0.088 Uiso 1 1 calc R . . C38 C 0.8583(3) 0.2369(2) 0.3650(3) 0.0624(10) Uani 1 1 d . . . H38A H 0.8663 0.2860 0.3920 0.075 Uiso 1 1 calc R . . H38B H 0.8188 0.2400 0.3005 0.075 Uiso 1 1 calc R . . 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 0.02250(11) 0.01931(10) 0.01384(9) 0.00003(6) 0.00536(7) 0.00300(7) Ru2 0.02527(11) 0.02923(11) 0.01555(10) 0.00339(7) 0.00595(8) 0.00407(8) Ru3 0.02516(11) 0.02018(10) 0.02172(10) 0.00257(7) 0.00878(8) 0.00373(7) O1 0.0296(11) 0.0451(12) 0.0463(12) -0.0053(10) 0.0051(9) -0.0066(9) O2 0.0670(15) 0.0415(12) 0.0297(10) 0.0015(9) 0.0245(10) 0.0239(11) O3 0.0352(12) 0.0367(11) 0.0545(13) -0.0048(10) 0.0140(10) -0.0101(10) O4 0.0453(13) 0.0435(12) 0.0380(11) -0.0094(10) 0.0114(9) 0.0049(10) O5 0.0357(12) 0.0544(13) 0.0453(12) -0.0001(10) 0.0222(10) -0.0075(10) O6 0.106(2) 0.0433(13) 0.0370(12) 0.0169(11) 0.0147(13) 0.0230(14) O7 0.0251(12) 0.0948(19) 0.0305(11) -0.0073(11) 0.0051(9) -0.0036(12) O8 0.0536(14) 0.0346(11) 0.0746(16) -0.0019(11) 0.0412(13) -0.0090(10) O9 0.0638(17) 0.0674(16) 0.0568(15) 0.0257(13) 0.0115(13) 0.0377(14) O10 0.0460(13) 0.0388(11) 0.0373(11) -0.0128(9) 0.0139(9) -0.0058(9) O11 0.0364(11) 0.0354(10) 0.0414(11) -0.0058(9) 0.0214(9) -0.0065(9) O12 0.0348(13) 0.0808(19) 0.0753(17) 0.0202(15) 0.0113(12) -0.0138(12) N1 0.0185(10) 0.0169(9) 0.0167(9) -0.0011(7) 0.0064(7) 0.0002(7) N2 0.0226(10) 0.0189(9) 0.0151(9) -0.0002(7) 0.0054(8) 0.0012(8) C1 0.0305(15) 0.0297(13) 0.0224(12) 0.0003(10) 0.0083(10) 0.0042(11) C2 0.0370(15) 0.0270(13) 0.0213(12) 0.0039(10) 0.0082(11) 0.0052(11) C3 0.0313(15) 0.0305(14) 0.0223(12) -0.0010(10) 0.0048(10) 0.0051(12) C4 0.0259(14) 0.0380(15) 0.0238(12) 0.0043(11) 0.0077(10) 0.0049(11) C5 0.0411(17) 0.0316(14) 0.0240(13) 0.0038(11) 0.0123(11) 0.0019(12) C6 0.054(2) 0.0383(16) 0.0258(13) 0.0000(12) 0.0114(13) 0.0102(14) C7 0.0300(16) 0.0534(17) 0.0153(12) -0.0017(11) 0.0013(10) 0.0070(13) C8 0.0436(17) 0.0255(13) 0.0422(16) -0.0016(11) 0.0225(13) 0.0041(12) C9 0.0434(17) 0.0382(16) 0.0341(15) 0.0073(12) 0.0148(13) 0.0106(14) C10 0.0269(13) 0.0231(12) 0.0332(14) 0.0003(11) 0.0116(11) -0.0024(10) C11 0.0305(14) 0.0274(12) 0.0211(12) -0.0043(10) 0.0052(10) 0.0016(11) C12 0.0199(12) 0.0182(11) 0.0161(10) 0.0012(8) 0.0052(9) -0.0011(9) C13 0.0244(12) 0.0196(11) 0.0163(10) 0.0016(9) 0.0052(9) 0.0023(9) C14 0.0299(13) 0.0207(11) 0.0162(11) 0.0009(9) 0.0062(9) 0.0052(10) C15 0.0192(11) 0.0164(10) 0.0188(10) -0.0003(8) 0.0060(9) 0.0012(9) C16 0.0239(12) 0.0201(11) 0.0234(11) -0.0001(9) 0.0109(9) -0.0005(9) C17 0.0251(13) 0.0235(12) 0.0322(13) 0.0015(10) 0.0156(10) 0.0020(10) C18 0.0372(15) 0.0222(12) 0.0265(12) -0.0017(10) 0.0136(11) 0.0083(11) C19 0.0250(13) 0.0218(12) 0.0271(12) -0.0066(10) 0.0036(10) -0.0005(10) C20 0.0308(14) 0.0180(11) 0.0357(14) 0.0001(10) 0.0133(11) -0.0002(10) C21 0.0264(13) 0.0217(12) 0.0245(12) 0.0039(9) 0.0073(10) 0.0044(10) C22 0.0235(12) 0.0204(11) 0.0196(11) 0.0020(9) 0.0069(9) 0.0035(9) C23 0.0234(13) 0.0261(13) 0.0345(14) 0.0013(10) 0.0083(11) 0.0064(10) C24 0.0215(12) 0.0215(11) 0.0226(11) -0.0042(9) 0.0055(9) -0.0007(9) C25 0.0231(12) 0.0173(10) 0.0155(10) -0.0027(8) 0.0066(9) -0.0003(9) C26 0.0285(13) 0.0224(12) 0.0219(11) -0.0025(9) 0.0080(10) -0.0044(10) C27 0.0390(16) 0.0234(12) 0.0258(13) -0.0056(10) 0.0062(11) -0.0067(11) C28 0.0498(18) 0.0255(13) 0.0282(13) -0.0070(11) 0.0124(12) 0.0076(12) C29 0.0294(14) 0.0383(15) 0.0313(14) -0.0065(11) 0.0127(11) 0.0084(12) C30 0.0425(17) 0.0377(15) 0.0318(14) -0.0069(12) 0.0236(13) -0.0043(12) C31 0.0444(16) 0.0278(13) 0.0155(11) -0.0010(10) 0.0119(10) 0.0010(11) C32 0.0315(14) 0.0212(12) 0.0196(11) -0.0004(9) 0.0096(10) 0.0002(10) C33 0.0228(13) 0.0304(13) 0.0257(12) -0.0048(10) 0.0059(10) 0.0009(10) C34 0.0423(16) 0.0317(14) 0.0212(12) -0.0079(10) 0.0045(11) -0.0006(12) C35 0.048(2) 0.054(2) 0.0428(17) -0.0074(15) 0.0148(15) -0.0140(16) C36 0.0379(18) 0.067(2) 0.0512(19) -0.0102(17) 0.0131(15) 0.0075(16) C37 0.070(3) 0.087(3) 0.075(3) 0.008(2) 0.039(2) -0.001(2) C38 0.052(2) 0.062(2) 0.072(3) 0.016(2) 0.0149(19) -0.0048(18) _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 C2 1.862(3) . ? Ru1 C1 1.920(3) . ? Ru1 C3 1.948(3) . ? Ru1 C13 2.150(2) . ? Ru1 Ru2 2.8384(3) . ? Ru1 Ru3 2.8989(3) . ? Ru2 C4 1.912(3) . ? Ru2 C7 1.928(3) . ? Ru2 C6 1.933(3) . ? Ru2 C5 1.944(3) . ? Ru2 Ru3 2.8613(3) . ? Ru3 C10 1.905(3) . ? Ru3 C9 1.923(3) . ? Ru3 C11 1.936(3) . ? Ru3 C8 1.949(3) . ? O1 C1 1.141(3) . ? O2 C2 1.149(3) . ? O3 C3 1.133(3) . ? O4 C4 1.138(3) . ? O5 C5 1.144(3) . ? O6 C6 1.133(4) . ? O7 C7 1.142(4) . ? O8 C8 1.143(4) . ? O9 C9 1.134(4) . ? O10 C10 1.137(3) . ? O11 C11 1.151(3) . ? O12 C38 1.409(4) . ? O12 C35 1.417(4) . ? N1 C12 1.340(3) . ? N1 C13 1.415(3) . ? N1 C15 1.502(3) . ? N2 C12 1.325(3) . ? N2 C14 1.386(3) . ? N2 C25 1.486(3) . ? C13 C14 1.365(3) . ? C15 C24 1.536(3) . ? C15 C16 1.537(3) . ? C15 C22 1.537(3) . ? C16 C17 1.540(3) . ? C17 C23 1.533(3) . ? C17 C18 1.537(4) . ? C18 C19 1.531(4) . ? C19 C20 1.534(3) . ? C19 C24 1.539(3) . ? C20 C21 1.528(3) . ? C21 C23 1.523(4) . ? C21 C22 1.537(3) . ? C25 C32 1.527(3) . ? C25 C33 1.530(3) . ? C25 C26 1.533(3) . ? C26 C27 1.534(3) . ? C27 C28 1.530(4) . ? C27 C34 1.531(4) . ? C28 C29 1.532(4) . ? C29 C30 1.526(4) . ? C29 C33 1.535(3) . ? C30 C31 1.521(4) . ? C31 C34 1.534(4) . ? C31 C32 1.540(3) . ? C35 C36 1.515(5) . ? C36 C37 1.506(5) . ? C37 C38 1.484(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 C2 Ru1 C1 91.81(12) . . ? C2 Ru1 C3 92.69(12) . . ? C1 Ru1 C3 171.46(10) . . ? C2 Ru1 C13 109.68(10) . . ? C1 Ru1 C13 84.27(10) . . ? C3 Ru1 C13 87.39(10) . . ? C2 Ru1 Ru2 87.56(7) . . ? C1 Ru1 Ru2 95.75(7) . . ? C3 Ru1 Ru2 91.69(7) . . ? C13 Ru1 Ru2 162.76(6) . . ? C2 Ru1 Ru3 144.34(8) . . ? C1 Ru1 Ru3 78.69(8) . . ? C3 Ru1 Ru3 101.61(8) . . ? C13 Ru1 Ru3 103.51(6) . . ? Ru2 Ru1 Ru3 59.818(6) . . ? C4 Ru2 C7 89.76(12) . . ? C4 Ru2 C6 101.80(12) . . ? C7 Ru2 C6 94.77(13) . . ? C4 Ru2 C5 91.96(11) . . ? C7 Ru2 C5 168.80(11) . . ? C6 Ru2 C5 95.71(13) . . ? C4 Ru2 Ru1 101.29(8) . . ? C7 Ru2 Ru1 87.55(8) . . ? C6 Ru2 Ru1 156.80(9) . . ? C5 Ru2 Ru1 81.25(8) . . ? C4 Ru2 Ru3 158.96(8) . . ? C7 Ru2 Ru3 78.61(8) . . ? C6 Ru2 Ru3 96.64(8) . . ? C5 Ru2 Ru3 96.24(8) . . ? Ru1 Ru2 Ru3 61.141(6) . . ? C10 Ru3 C9 98.58(12) . . ? C10 Ru3 C11 89.38(10) . . ? C9 Ru3 C11 97.12(12) . . ? C10 Ru3 C8 92.22(11) . . ? C9 Ru3 C8 96.74(13) . . ? C11 Ru3 C8 165.65(11) . . ? C10 Ru3 Ru2 167.99(8) . . ? C9 Ru3 Ru2 91.94(9) . . ? C11 Ru3 Ru2 95.08(7) . . ? C8 Ru3 Ru2 80.74(8) . . ? C10 Ru3 Ru1 112.49(8) . . ? C9 Ru3 Ru1 146.04(9) . . ? C11 Ru3 Ru1 70.81(8) . . ? C8 Ru3 Ru1 95.46(8) . . ? Ru2 Ru3 Ru1 59.041(6) . . ? C38 O12 C35 106.6(3) . . ? C12 N1 C13 109.50(18) . . ? C12 N1 C15 120.76(18) . . ? C13 N1 C15 129.69(18) . . ? C12 N2 C14 106.96(19) . . ? C12 N2 C25 127.75(19) . . ? C14 N2 C25 125.28(19) . . ? O1 C1 Ru1 172.2(2) . . ? O2 C2 Ru1 174.4(2) . . ? O3 C3 Ru1 173.8(2) . . ? O4 C4 Ru2 175.8(2) . . ? O5 C5 Ru2 175.3(2) . . ? O6 C6 Ru2 179.0(3) . . ? O7 C7 Ru2 174.1(2) . . ? O8 C8 Ru3 173.6(2) . . ? O9 C9 Ru3 177.6(3) . . ? O10 C10 Ru3 178.1(2) . . ? O11 C11 Ru3 167.3(2) . . ? N2 C12 N1 109.66(19) . . ? C14 C13 N1 103.40(19) . . ? C14 C13 Ru1 119.21(17) . . ? N1 C13 Ru1 137.34(16) . . ? C13 C14 N2 110.5(2) . . ? N1 C15 C24 109.83(18) . . ? N1 C15 C16 109.15(18) . . ? C24 C15 C16 110.84(18) . . ? N1 C15 C22 110.22(17) . . ? C24 C15 C22 108.25(18) . . ? C16 C15 C22 108.54(19) . . ? C15 C16 C17 109.53(19) . . ? C23 C17 C18 109.1(2) . . ? C23 C17 C16 109.0(2) . . ? C18 C17 C16 109.9(2) . . ? C19 C18 C17 109.82(19) . . ? C18 C19 C20 109.2(2) . . ? C18 C19 C24 109.7(2) . . ? C20 C19 C24 109.5(2) . . ? C21 C20 C19 109.10(19) . . ? C23 C21 C20 109.9(2) . . ? C23 C21 C22 109.9(2) . . ? C20 C21 C22 109.4(2) . . ? C15 C22 C21 109.83(18) . . ? C21 C23 C17 109.4(2) . . ? C15 C24 C19 109.49(19) . . ? N2 C25 C32 109.81(18) . . ? N2 C25 C33 109.04(18) . . ? C32 C25 C33 109.6(2) . . ? N2 C25 C26 108.73(18) . . ? C32 C25 C26 109.55(19) . . ? C33 C25 C26 110.14(19) . . ? C25 C26 C27 109.1(2) . . ? C28 C27 C34 109.9(2) . . ? C28 C27 C26 109.4(2) . . ? C34 C27 C26 109.1(2) . . ? C27 C28 C29 109.8(2) . . ? C30 C29 C28 109.9(2) . . ? C30 C29 C33 108.8(2) . . ? C28 C29 C33 109.1(2) . . ? C31 C30 C29 110.0(2) . . ? C30 C31 C34 110.0(2) . . ? C30 C31 C32 109.5(2) . . ? C34 C31 C32 108.9(2) . . ? C25 C32 C31 108.95(19) . . ? C25 C33 C29 109.4(2) . . ? C27 C34 C31 109.4(2) . . ? O12 C35 C36 107.0(3) . . ? C37 C36 C35 103.3(3) . . ? C38 C37 C36 104.9(3) . . ? O12 C38 C37 104.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.899 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.112 # Attachment '2_k08mkw6.cif' data_k08mkw6 _database_code_depnum_ccdc_archive 'CCDC 687172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 N2 O11 Os3' _chemical_formula_weight 1215.22 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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.8360(2) _cell_length_b 12.6320(2) _cell_length_c 22.3790(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3345.94(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 154870 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 11.430 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.46 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7652 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7652 _reflns_number_gt 6440 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0578P)^2^+13.9620P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.499(17) _refine_ls_number_reflns 7652 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.50042(6) 0.27909(3) 0.106355(16) 0.02106(10) Uani 1 1 d . . . Os2 Os 0.37821(6) 0.08179(5) 0.122810(19) 0.02409(14) Uani 1 1 d . . . Os3 Os 0.62203(6) 0.08590(5) 0.130217(19) 0.02384(14) Uani 1 1 d . . . O1 O 0.4263(8) 0.2390(8) -0.0230(4) 0.039(2) Uani 1 1 d . . . O2 O 0.7174(7) 0.3821(8) 0.0638(4) 0.038(2) Uani 1 1 d . . . O3 O 0.5311(8) 0.3527(9) 0.2365(4) 0.049(3) Uani 1 1 d . . . O4 O 0.4190(8) 0.0003(8) -0.0051(4) 0.038(2) Uani 1 1 d . . . O5 O 0.1510(8) 0.1727(8) 0.0828(5) 0.049(3) Uani 1 1 d . . . O6 O 0.3220(12) -0.1468(10) 0.1538(5) 0.048(3) Uani 1 1 d . . . O7 O 0.3537(8) 0.1707(9) 0.2507(5) 0.047(3) Uani 1 1 d . . . O8 O 0.6502(8) 0.0986(10) -0.0067(4) 0.049(3) Uani 1 1 d . . . O9 O 0.8671(9) 0.1598(9) 0.1381(5) 0.050(3) Uani 1 1 d . . . O10 O 0.6624(12) -0.1502(10) 0.1455(6) 0.051(3) Uani 1 1 d . . . O11 O 0.5995(9) 0.1134(11) 0.2665(4) 0.056(3) Uani 1 1 d . . . N1 N 0.3517(8) 0.4990(8) 0.0862(4) 0.027(2) Uani 1 1 d . . . N2 N 0.2069(8) 0.4694(8) 0.1428(4) 0.026(2) Uani 1 1 d . . . C1 C 0.4545(10) 0.2469(10) 0.0254(6) 0.032(3) Uani 1 1 d . . . C2 C 0.6326(10) 0.3467(10) 0.0815(5) 0.029(3) Uani 1 1 d . . . C3 C 0.5212(14) 0.3208(10) 0.1895(5) 0.039(4) Uani 1 1 d . . . C4 C 0.4081(10) 0.0321(10) 0.0419(5) 0.029(3) Uani 1 1 d . . . C5 C 0.2335(12) 0.1375(11) 0.0984(6) 0.038(3) Uani 1 1 d . . . C6 C 0.3463(12) -0.0600(12) 0.1430(6) 0.029(3) Uani 1 1 d . . . C7 C 0.3682(12) 0.1400(11) 0.2022(6) 0.036(3) Uani 1 1 d . . . C8 C 0.6351(12) 0.0924(13) 0.0436(6) 0.042(3) Uani 1 1 d . . . C9 C 0.7732(11) 0.1332(11) 0.1352(6) 0.030(3) Uani 1 1 d . . . C10 C 0.6462(15) -0.0627(11) 0.1393(7) 0.035(4) Uani 1 1 d . . . C11 C 0.6019(13) 0.1042(13) 0.2161(6) 0.041(4) Uani 1 1 d . . . C12 C 0.3699(9) 0.3948(9) 0.1097(5) 0.025(2) Uani 1 1 d . . . C13 C 0.2769(9) 0.3826(10) 0.1456(5) 0.027(2) Uani 1 1 d . . . H13 H 0.2625 0.3218 0.1693 0.032 Uiso 1 1 calc R . . C14 C 0.2545(8) 0.5409(10) 0.1057(5) 0.023(2) Uani 1 1 d . . . H14 H 0.2247 0.6083 0.0954 0.027 Uiso 1 1 calc R . . C15 C 0.4262(10) 0.5661(11) 0.0452(5) 0.029(3) Uani 1 1 d . . . C16 C 0.3591(12) 0.6623(11) 0.0246(6) 0.033(3) Uani 1 1 d . . . H16A H 0.3363 0.7051 0.0596 0.039 Uiso 1 1 calc R . . H16B H 0.2898 0.6390 0.0036 0.039 Uiso 1 1 calc R . . C17 C 0.4339(11) 0.7317(11) -0.0188(6) 0.032(3) Uani 1 1 d . . . H17 H 0.3901 0.7949 -0.0324 0.039 Uiso 1 1 calc R . . C18 C 0.4709(9) 0.6653(10) -0.0732(5) 0.031(3) Uani 1 1 d . . . H18A H 0.4038 0.6432 -0.0965 0.037 Uiso 1 1 calc R . . H18B H 0.5203 0.7080 -0.0995 0.037 Uiso 1 1 calc R . . C19 C 0.5338(10) 0.5692(11) -0.0512(6) 0.036(3) Uani 1 1 d . . . H19 H 0.5581 0.5261 -0.0865 0.044 Uiso 1 1 calc R . . C20 C 0.4627(9) 0.4991(9) -0.0095(5) 0.023(2) Uani 1 1 d . . . H20A H 0.5076 0.4374 0.0038 0.027 Uiso 1 1 calc R . . H20B H 0.3951 0.4727 -0.0310 0.027 Uiso 1 1 calc R . . C21 C 0.5309(9) 0.6045(10) 0.0804(5) 0.031(3) Uani 1 1 d . . . H21A H 0.5069 0.6478 0.1150 0.037 Uiso 1 1 calc R . . H21B H 0.5742 0.5430 0.0955 0.037 Uiso 1 1 calc R . . C22 C 0.6050(12) 0.6710(11) 0.0381(6) 0.033(3) Uani 1 1 d . . . H22 H 0.6733 0.6965 0.0601 0.040 Uiso 1 1 calc R . . C23 C 0.5363(10) 0.7666(11) 0.0159(6) 0.035(3) Uani 1 1 d . . . H23A H 0.5120 0.8097 0.0505 0.042 Uiso 1 1 calc R . . H23B H 0.5846 0.8114 -0.0099 0.042 Uiso 1 1 calc R . . C24 C 0.6415(10) 0.6050(11) -0.0156(5) 0.031(3) Uani 1 1 d . . . H24A H 0.6842 0.5421 -0.0019 0.038 Uiso 1 1 calc R . . H24B H 0.6914 0.6475 -0.0418 0.038 Uiso 1 1 calc R . . C25 C 0.0937(11) 0.4833(11) 0.1730(6) 0.031(3) Uani 1 1 d . . . C26 C 0.0152(14) 0.3958(11) 0.1514(6) 0.040(3) Uani 1 1 d . . . H26A H 0.0480 0.3255 0.1605 0.048 Uiso 1 1 calc R . . H26B H 0.0039 0.4012 0.1077 0.048 Uiso 1 1 calc R . . C27 C -0.1008(12) 0.4098(15) 0.1849(8) 0.054(4) Uani 1 1 d . . . H27 H -0.1544 0.3536 0.1714 0.065 Uiso 1 1 calc R . . C28 C -0.0796(14) 0.3976(13) 0.2510(8) 0.057(4) Uani 1 1 d . . . H28A H -0.0429 0.3286 0.2589 0.068 Uiso 1 1 calc R . . H28B H -0.1524 0.3992 0.2728 0.068 Uiso 1 1 calc R . . C29 C -0.005(2) 0.4861(11) 0.2727(5) 0.046(3) Uani 1 1 d . . . H29 H 0.0062 0.4796 0.3169 0.055 Uiso 1 1 calc R . . C30 C 0.1121(11) 0.4724(12) 0.2406(5) 0.036(3) Uani 1 1 d . . . H30A H 0.1657 0.5272 0.2547 0.043 Uiso 1 1 calc R . . H30B H 0.1443 0.4020 0.2499 0.043 Uiso 1 1 calc R . . C31 C 0.0446(11) 0.5926(13) 0.1597(6) 0.039(3) Uani 1 1 d . . . H31A H 0.0354 0.6017 0.1160 0.046 Uiso 1 1 calc R . . H31B H 0.0965 0.6482 0.1744 0.046 Uiso 1 1 calc R . . C32 C -0.0731(11) 0.6028(11) 0.1916(6) 0.035(3) Uani 1 1 d . . . H32 H -0.1070 0.6734 0.1823 0.042 Uiso 1 1 calc R . . C33 C -0.1477(15) 0.5175(13) 0.1681(8) 0.053(4) Uani 1 1 d . . . H33A H -0.1529 0.5232 0.1241 0.063 Uiso 1 1 calc R . . H33B H -0.2246 0.5256 0.1848 0.063 Uiso 1 1 calc R . . C34 C -0.0515(12) 0.5944(11) 0.2584(6) 0.040(3) Uani 1 1 d . . . H34A H 0.0031 0.6496 0.2709 0.048 Uiso 1 1 calc R . . H34B H -0.1228 0.6058 0.2806 0.048 Uiso 1 1 calc R . . 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 Os1 0.01781(17) 0.02719(19) 0.01819(18) -0.00018(14) -0.0002(3) 0.0012(3) Os2 0.0192(3) 0.0295(3) 0.0235(2) 0.00082(19) -0.00029(19) -0.0006(3) Os3 0.0203(3) 0.0310(3) 0.0203(2) 0.00058(19) -0.00089(19) 0.0041(3) O1 0.042(6) 0.043(6) 0.031(5) 0.006(4) -0.015(4) -0.008(4) O2 0.023(5) 0.048(6) 0.045(5) 0.009(4) 0.002(4) -0.001(4) O3 0.051(8) 0.060(7) 0.036(5) -0.011(5) -0.007(4) -0.002(5) O4 0.045(6) 0.036(6) 0.032(5) -0.003(4) 0.001(4) -0.003(4) O5 0.036(6) 0.048(6) 0.062(7) -0.003(5) -0.017(5) 0.008(5) O6 0.050(8) 0.045(8) 0.048(7) 0.006(5) 0.000(5) -0.007(6) O7 0.034(6) 0.071(7) 0.037(6) -0.010(5) 0.002(4) -0.006(5) O8 0.037(5) 0.091(9) 0.019(5) 0.000(5) -0.003(4) 0.013(5) O9 0.037(6) 0.069(7) 0.045(6) 0.012(5) -0.002(5) -0.011(5) O10 0.066(9) 0.038(7) 0.048(7) 0.000(5) -0.005(6) -0.001(6) O11 0.051(7) 0.095(9) 0.021(5) -0.007(5) -0.006(4) 0.028(6) N1 0.021(5) 0.038(6) 0.021(5) 0.005(4) 0.004(4) -0.008(4) N2 0.028(5) 0.034(6) 0.018(4) -0.004(4) 0.010(4) -0.003(4) C1 0.021(6) 0.034(8) 0.041(8) -0.002(6) 0.001(5) -0.002(5) C2 0.025(7) 0.034(7) 0.027(6) 0.004(5) -0.007(5) 0.000(5) C3 0.056(13) 0.036(7) 0.024(6) -0.007(5) -0.010(6) -0.003(6) C4 0.027(7) 0.033(7) 0.028(7) 0.007(5) -0.003(5) -0.002(5) C5 0.042(8) 0.041(8) 0.031(7) -0.010(6) -0.004(6) 0.003(6) C6 0.027(8) 0.030(8) 0.028(7) 0.005(6) 0.002(5) 0.004(6) C7 0.024(7) 0.045(9) 0.039(7) -0.011(6) 0.006(6) 0.001(6) C8 0.033(8) 0.061(10) 0.032(7) 0.005(7) 0.002(5) 0.019(7) C9 0.025(7) 0.039(8) 0.026(6) 0.000(5) 0.004(5) 0.000(5) C10 0.055(11) 0.008(7) 0.042(8) 0.008(6) 0.002(7) -0.001(6) C11 0.031(9) 0.059(10) 0.033(7) -0.006(6) -0.004(5) 0.027(7) C12 0.020(6) 0.030(6) 0.026(5) -0.014(5) 0.003(5) -0.005(5) C13 0.018(6) 0.036(7) 0.027(6) 0.004(5) 0.001(4) -0.003(5) C14 0.016(5) 0.039(7) 0.013(5) -0.002(5) 0.002(4) 0.004(4) C15 0.022(6) 0.043(8) 0.022(6) 0.005(5) 0.010(4) -0.006(5) C16 0.026(8) 0.030(7) 0.042(8) 0.006(6) 0.002(6) 0.006(6) C17 0.031(7) 0.034(7) 0.032(7) -0.006(6) -0.001(5) 0.004(6) C18 0.028(8) 0.041(7) 0.024(6) -0.001(5) 0.006(4) 0.000(5) C19 0.039(9) 0.041(8) 0.029(6) -0.004(6) 0.002(5) -0.006(5) C20 0.024(6) 0.024(6) 0.021(5) -0.004(4) 0.001(4) -0.003(4) C21 0.037(9) 0.033(7) 0.021(5) 0.000(5) 0.001(4) 0.010(5) C22 0.031(9) 0.042(8) 0.028(6) 0.001(6) -0.010(6) -0.007(6) C23 0.036(8) 0.034(7) 0.036(7) 0.009(6) 0.005(5) 0.000(5) C24 0.025(7) 0.042(8) 0.028(6) 0.008(5) 0.011(5) 0.001(5) C25 0.030(8) 0.035(8) 0.028(6) -0.003(5) 0.010(5) 0.008(6) C26 0.032(9) 0.053(8) 0.036(6) -0.007(6) 0.011(6) -0.006(7) C27 0.028(8) 0.073(12) 0.061(10) -0.017(9) 0.013(6) -0.015(8) C28 0.050(10) 0.044(9) 0.077(11) 0.012(9) 0.035(8) 0.014(7) C29 0.043(7) 0.061(8) 0.034(6) -0.004(6) 0.020(9) -0.004(11) C30 0.033(7) 0.048(8) 0.026(6) -0.001(5) -0.003(5) 0.012(6) C31 0.020(6) 0.063(10) 0.033(7) 0.011(7) 0.003(5) 0.003(6) C32 0.031(7) 0.040(8) 0.036(7) 0.006(6) 0.000(5) -0.001(6) C33 0.058(11) 0.050(10) 0.051(9) -0.022(8) 0.005(8) -0.004(8) C34 0.045(7) 0.043(8) 0.032(7) -0.010(6) 0.007(6) -0.005(6) _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 Os1 C2 1.867(12) . ? Os1 C1 1.934(13) . ? Os1 C3 1.949(12) . ? Os1 C12 2.128(12) . ? Os1 Os3 2.8831(8) . ? Os1 Os2 2.9051(8) . ? Os2 C6 1.886(15) . ? Os2 C7 1.926(13) . ? Os2 C5 1.931(14) . ? Os2 C4 1.949(13) . ? Os2 Os3 2.8911(5) . ? Os3 C9 1.890(13) . ? Os3 C10 1.910(14) . ? Os3 C8 1.946(13) . ? Os3 C11 1.950(13) . ? O1 C1 1.137(15) . ? O2 C2 1.168(15) . ? O3 C3 1.133(15) . ? O4 C4 1.133(15) . ? O5 C5 1.128(16) . ? O6 C6 1.158(17) . ? O7 C7 1.166(17) . ? O8 C8 1.143(16) . ? O9 C9 1.163(15) . ? O10 C10 1.130(17) . ? O11 C11 1.135(16) . ? N1 C14 1.340(14) . ? N1 C12 1.435(16) . ? N1 C15 1.529(14) . ? N2 C14 1.349(15) . ? N2 C13 1.375(16) . ? N2 C25 1.511(15) . ? C12 C13 1.371(16) . ? C15 C16 1.523(19) . ? C15 C21 1.546(16) . ? C15 C20 1.550(16) . ? C16 C17 1.579(19) . ? C17 C23 1.506(17) . ? C17 C18 1.542(16) . ? C18 C19 1.507(18) . ? C19 C20 1.537(16) . ? C19 C24 1.571(17) . ? C21 C22 1.539(18) . ? C22 C24 1.526(18) . ? C22 C23 1.538(19) . ? C25 C26 1.52(2) . ? C25 C31 1.53(2) . ? C25 C30 1.534(17) . ? C26 C27 1.573(19) . ? C27 C28 1.51(3) . ? C27 C33 1.52(3) . ? C28 C29 1.51(3) . ? C29 C34 1.51(2) . ? C29 C30 1.57(2) . ? C31 C32 1.572(17) . ? C32 C33 1.49(2) . ? C32 C34 1.521(18) . ? 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 C2 Os1 C1 93.0(5) . . ? C2 Os1 C3 93.2(6) . . ? C1 Os1 C3 170.4(6) . . ? C2 Os1 C12 107.7(5) . . ? C1 Os1 C12 88.5(5) . . ? C3 Os1 C12 82.6(6) . . ? C2 Os1 Os3 91.4(4) . . ? C1 Os1 Os3 97.8(4) . . ? C3 Os1 Os3 89.4(4) . . ? C12 Os1 Os3 159.6(3) . . ? C2 Os1 Os2 147.9(4) . . ? C1 Os1 Os2 78.4(4) . . ? C3 Os1 Os2 100.0(4) . . ? C12 Os1 Os2 102.9(3) . . ? Os3 Os1 Os2 59.930(13) . . ? C6 Os2 C7 97.4(6) . . ? C6 Os2 C5 103.7(6) . . ? C7 Os2 C5 93.8(6) . . ? C6 Os2 C4 87.3(6) . . ? C7 Os2 C4 172.3(6) . . ? C5 Os2 C4 90.9(5) . . ? C6 Os2 Os3 101.7(4) . . ? C7 Os2 Os3 90.1(4) . . ? C5 Os2 Os3 153.6(5) . . ? C4 Os2 Os3 83.0(4) . . ? C6 Os2 Os1 160.9(4) . . ? C7 Os2 Os1 79.6(4) . . ? C5 Os2 Os1 95.4(4) . . ? C4 Os2 Os1 93.9(4) . . ? Os3 Os2 Os1 59.66(2) . . ? C9 Os3 C10 99.4(7) . . ? C9 Os3 C8 88.3(6) . . ? C10 Os3 C8 97.8(7) . . ? C9 Os3 C11 91.2(6) . . ? C10 Os3 C11 91.7(7) . . ? C8 Os3 C11 170.4(7) . . ? C9 Os3 Os1 102.5(4) . . ? C10 Os3 Os1 157.9(5) . . ? C8 Os3 Os1 79.6(4) . . ? C11 Os3 Os1 91.2(4) . . ? C9 Os3 Os2 162.6(4) . . ? C10 Os3 Os2 97.9(5) . . ? C8 Os3 Os2 91.3(4) . . ? C11 Os3 Os2 86.4(4) . . ? Os1 Os3 Os2 60.41(2) . . ? C14 N1 C12 111.8(9) . . ? C14 N1 C15 118.2(10) . . ? C12 N1 C15 130.0(10) . . ? C14 N2 C13 108.0(9) . . ? C14 N2 C25 124.6(10) . . ? C13 N2 C25 127.3(10) . . ? O1 C1 Os1 172.9(12) . . ? O2 C2 Os1 175.0(12) . . ? O3 C3 Os1 174.8(12) . . ? O4 C4 Os2 175.7(11) . . ? O5 C5 Os2 177.3(14) . . ? O6 C6 Os2 176.7(14) . . ? O7 C7 Os2 174.3(13) . . ? O8 C8 Os3 175.3(13) . . ? O9 C9 Os3 178.4(12) . . ? O10 C10 Os3 178.5(16) . . ? O11 C11 Os3 174.3(13) . . ? C13 C12 N1 101.4(10) . . ? C13 C12 Os1 121.8(9) . . ? N1 C12 Os1 136.6(8) . . ? C12 C13 N2 111.6(11) . . ? N1 C14 N2 107.2(10) . . ? C16 C15 N1 108.8(10) . . ? C16 C15 C21 108.7(11) . . ? N1 C15 C21 109.3(9) . . ? C16 C15 C20 110.0(10) . . ? N1 C15 C20 109.4(10) . . ? C21 C15 C20 110.5(9) . . ? C15 C16 C17 109.7(11) . . ? C23 C17 C18 109.7(10) . . ? C23 C17 C16 107.2(10) . . ? C18 C17 C16 110.1(11) . . ? C19 C18 C17 108.7(10) . . ? C18 C19 C20 113.1(10) . . ? C18 C19 C24 109.6(11) . . ? C20 C19 C24 107.6(10) . . ? C19 C20 C15 108.5(10) . . ? C22 C21 C15 108.3(9) . . ? C24 C22 C23 108.9(11) . . ? C24 C22 C21 110.3(11) . . ? C23 C22 C21 109.0(11) . . ? C17 C23 C22 111.2(12) . . ? C22 C24 C19 109.1(10) . . ? N2 C25 C26 108.3(10) . . ? N2 C25 C31 110.8(11) . . ? C26 C25 C31 111.2(12) . . ? N2 C25 C30 107.7(10) . . ? C26 C25 C30 109.5(11) . . ? C31 C25 C30 109.1(11) . . ? C25 C26 C27 107.4(11) . . ? C28 C27 C33 113.4(14) . . ? C28 C27 C26 108.1(13) . . ? C33 C27 C26 107.6(14) . . ? C27 C28 C29 109.7(13) . . ? C28 C29 C34 112.8(17) . . ? C28 C29 C30 106.8(11) . . ? C34 C29 C30 109.0(11) . . ? C25 C30 C29 108.5(11) . . ? C25 C31 C32 108.8(11) . . ? C33 C32 C34 113.4(12) . . ? C33 C32 C31 107.8(12) . . ? C34 C32 C31 106.9(11) . . ? C32 C33 C27 110.2(14) . . ? C29 C34 C32 109.5(11) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 2.266 _refine_diff_density_min -1.784 _refine_diff_density_rms 0.237 # Attachment '3_k07mkw38.cif' data_k07mkw38 _database_code_depnum_ccdc_archive 'CCDC 687173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H34 Cl2 N2 O9 Ru3' _chemical_formula_weight 976.73 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9540(1) _cell_length_b 22.9860(2) _cell_length_c 13.3710(1) _cell_angle_alpha 90.00 _cell_angle_beta 107.636(1) _cell_angle_gamma 90.00 _cell_volume 3501.33(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 71731 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 1.486 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.76 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73592 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 30.04 _reflns_number_total 10224 _reflns_number_gt 8575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0302P)^2^+3.6507P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10224 _refine_ls_number_parameters 446 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.637244(15) 0.397138(7) 0.608037(14) 0.01753(5) Uani 1 1 d D . . Ru2 Ru 0.615113(15) 0.282088(8) 0.700350(14) 0.01798(5) Uani 1 1 d D . . Ru3 Ru 0.825507(15) 0.332969(8) 0.719833(14) 0.01798(5) Uani 1 1 d . . . Cl1 Cl 0.79956(7) 0.13941(5) 0.19077(7) 0.0612(3) Uani 1 1 d . . . Cl2 Cl 0.61442(10) 0.21519(5) 0.06902(11) 0.0819(4) Uani 1 1 d . . . O1 O 0.54021(19) 0.45754(9) 0.76797(17) 0.0402(5) Uani 1 1 d . . . O2 O 0.79061(18) 0.50130(8) 0.59817(18) 0.0405(5) Uani 1 1 d . . . O3 O 0.42492(18) 0.42316(10) 0.41758(16) 0.0431(5) Uani 1 1 d . . . O4 O 0.5423(2) 0.33049(10) 0.88560(16) 0.0433(5) Uani 1 1 d . . . O5 O 0.72694(19) 0.18063(8) 0.84042(15) 0.0359(4) Uani 1 1 d . . . O6 O 0.38463(17) 0.23435(9) 0.55350(17) 0.0388(5) Uani 1 1 d . . . O7 O 0.81207(19) 0.39410(9) 0.91708(15) 0.0396(5) Uani 1 1 d . . . O8 O 0.99502(18) 0.23841(9) 0.83468(17) 0.0430(5) Uani 1 1 d . . . O9 O 1.02286(17) 0.40825(9) 0.69067(15) 0.0361(4) Uani 1 1 d . . . N1 N 0.73833(16) 0.23330(8) 0.52478(14) 0.0167(3) Uani 1 1 d . . . N2 N 0.75690(16) 0.31870(8) 0.45584(14) 0.0179(4) Uani 1 1 d . . . C1 C 0.5796(2) 0.43723(10) 0.7090(2) 0.0255(5) Uani 1 1 d . . . C2 C 0.7354(2) 0.46123(11) 0.5999(2) 0.0269(5) Uani 1 1 d . . . C3 C 0.5033(2) 0.41372(11) 0.4884(2) 0.0255(5) Uani 1 1 d . . . C4 C 0.5684(2) 0.31208(11) 0.8170(2) 0.0277(5) Uani 1 1 d . . . C5 C 0.6862(2) 0.21843(11) 0.78567(19) 0.0242(5) Uani 1 1 d . . . C6 C 0.4689(2) 0.25021(10) 0.6126(2) 0.0247(5) Uani 1 1 d . . . C7 C 0.8156(2) 0.37076(11) 0.84244(19) 0.0261(5) Uani 1 1 d . . . C8 C 0.9296(2) 0.27237(11) 0.7884(2) 0.0265(5) Uani 1 1 d . . . C9 C 0.9480(2) 0.37936(11) 0.69876(19) 0.0249(5) Uani 1 1 d . . . C10 C 0.70370(18) 0.27604(9) 0.58732(17) 0.0160(4) Uani 1 1 d . . . C11 C 0.71476(19) 0.33053(9) 0.54270(17) 0.0171(4) Uani 1 1 d . . . C12 C 0.76816(19) 0.26142(9) 0.44977(17) 0.0183(4) Uani 1 1 d . . . H12 H 0.7945 0.2427 0.3977 0.022 Uiso 1 1 calc R . . C13 C 0.7818(2) 0.36036(9) 0.37878(17) 0.0190(4) Uani 1 1 d . . . C14 C 0.8819(2) 0.40099(11) 0.4384(2) 0.0280(5) Uani 1 1 d . . . H14A H 0.8597 0.4214 0.4948 0.034 Uiso 1 1 calc R . . H14B H 0.9535 0.3779 0.4712 0.034 Uiso 1 1 calc R . . C15 C 0.9066(2) 0.44563(12) 0.3625(2) 0.0348(6) Uani 1 1 d . . . H15 H 0.9706 0.4725 0.4018 0.042 Uiso 1 1 calc R . . C16 C 0.7955(2) 0.48039(11) 0.3112(2) 0.0289(5) Uani 1 1 d . . . H16A H 0.7711 0.5013 0.3659 0.035 Uiso 1 1 calc R . . H16B H 0.8116 0.5096 0.2630 0.035 Uiso 1 1 calc R . . C17 C 0.6970(2) 0.44042(11) 0.2504(2) 0.0277(5) Uani 1 1 d . . . H17 H 0.6249 0.4639 0.2172 0.033 Uiso 1 1 calc R . . C18 C 0.6713(2) 0.39621(11) 0.32711(19) 0.0253(5) Uani 1 1 d . . . H18A H 0.6464 0.4170 0.3817 0.030 Uiso 1 1 calc R . . H18B H 0.6067 0.3701 0.2888 0.030 Uiso 1 1 calc R . . C19 C 0.8198(3) 0.32860(12) 0.2950(2) 0.0416(8) Uani 1 1 d . . . H19A H 0.7566 0.3020 0.2557 0.050 Uiso 1 1 calc R . . H19B H 0.8907 0.3051 0.3282 0.050 Uiso 1 1 calc R . . C20 C 0.7333(3) 0.40839(13) 0.1659(2) 0.0433(8) Uani 1 1 d . . . H20A H 0.7475 0.4366 0.1151 0.052 Uiso 1 1 calc R . . H20B H 0.6699 0.3816 0.1275 0.052 Uiso 1 1 calc R . . C21 C 0.9437(3) 0.41432(15) 0.2785(3) 0.0508(9) Uani 1 1 d . . . H21A H 1.0163 0.3918 0.3110 0.061 Uiso 1 1 calc R . . H21B H 0.9604 0.4430 0.2296 0.061 Uiso 1 1 calc R . . C22 C 0.8466(4) 0.37354(13) 0.2185(3) 0.0508(9) Uani 1 1 d . . . H22 H 0.8718 0.3526 0.1635 0.061 Uiso 1 1 calc R . . C23 C 0.74243(19) 0.16807(9) 0.53512(17) 0.0171(4) Uani 1 1 d . . . C24 C 0.8442(2) 0.15057(9) 0.63128(17) 0.0193(4) Uani 1 1 d . . . H24A H 0.8336 0.1684 0.6952 0.023 Uiso 1 1 calc R . . H24B H 0.9193 0.1648 0.6234 0.023 Uiso 1 1 calc R . . C26 C 0.8477(2) 0.08388(10) 0.64191(18) 0.0228(5) Uani 1 1 d . . . H26 H 0.9135 0.0726 0.7053 0.027 Uiso 1 1 calc R . . C27 C 0.7315(2) 0.06195(10) 0.65410(18) 0.0240(5) Uani 1 1 d . . . H27A H 0.7186 0.0794 0.7174 0.029 Uiso 1 1 calc R . . H27B H 0.7344 0.0191 0.6627 0.029 Uiso 1 1 calc R . . C28 C 0.6305(2) 0.07867(10) 0.55649(18) 0.0228(5) Uani 1 1 d . . . H28 H 0.5547 0.0642 0.5642 0.027 Uiso 1 1 calc R . . C29 C 0.62539(19) 0.14545(9) 0.54486(18) 0.0198(4) Uani 1 1 d . . . H29A H 0.5607 0.1565 0.4817 0.024 Uiso 1 1 calc R . . H29B H 0.6099 0.1632 0.6068 0.024 Uiso 1 1 calc R . . C30 C 0.7621(2) 0.14084(9) 0.43693(18) 0.0216(5) Uani 1 1 d . . . H30A H 0.8368 0.1552 0.4286 0.026 Uiso 1 1 calc R . . H30B H 0.6976 0.1523 0.3739 0.026 Uiso 1 1 calc R . . C31 C 0.8683(2) 0.05697(10) 0.5443(2) 0.0272(5) Uani 1 1 d . . . H31A H 0.8729 0.0141 0.5513 0.033 Uiso 1 1 calc R . . H31B H 0.9434 0.0712 0.5366 0.033 Uiso 1 1 calc R . . C32 C 0.6506(2) 0.05143(10) 0.45886(19) 0.0271(5) Uani 1 1 d . . . H32A H 0.6535 0.0085 0.4656 0.033 Uiso 1 1 calc R . . H32B H 0.5850 0.0618 0.3958 0.033 Uiso 1 1 calc R . . C33 C 0.7662(2) 0.07404(10) 0.44736(19) 0.0255(5) Uani 1 1 d . . . H33 H 0.7792 0.0566 0.3833 0.031 Uiso 1 1 calc R . . C34 C 0.6999(3) 0.15298(19) 0.0689(3) 0.0582(10) Uani 1 1 d . . . H34A H 0.6475 0.1189 0.0472 0.070 Uiso 1 1 calc R . . H34B H 0.7429 0.1582 0.0168 0.070 Uiso 1 1 calc R . . H1 H 0.538(3) 0.3408(7) 0.620(2) 0.039(9) Uiso 1 1 d 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 0.01826(9) 0.01298(8) 0.02125(9) -0.00105(6) 0.00581(7) 0.00152(6) Ru2 0.02025(9) 0.01630(9) 0.01884(9) 0.00064(6) 0.00810(7) 0.00095(6) Ru3 0.01738(9) 0.01727(9) 0.01754(9) -0.00201(6) 0.00266(7) 0.00068(6) Cl1 0.0410(4) 0.1006(8) 0.0367(4) 0.0137(4) 0.0040(3) -0.0228(5) Cl2 0.0615(6) 0.0565(6) 0.1085(9) 0.0090(6) -0.0033(6) -0.0199(5) O1 0.0455(12) 0.0329(10) 0.0492(12) -0.0184(9) 0.0247(10) -0.0046(9) O2 0.0390(11) 0.0251(10) 0.0640(14) -0.0050(9) 0.0256(10) -0.0081(8) O3 0.0304(10) 0.0558(13) 0.0375(11) 0.0077(10) 0.0018(9) 0.0148(10) O4 0.0515(13) 0.0518(13) 0.0343(11) -0.0031(9) 0.0247(10) 0.0119(10) O5 0.0536(12) 0.0311(10) 0.0254(9) 0.0090(8) 0.0155(9) 0.0130(9) O6 0.0276(10) 0.0339(10) 0.0484(12) 0.0012(9) 0.0021(9) -0.0050(8) O7 0.0442(12) 0.0445(12) 0.0285(10) -0.0137(9) 0.0089(9) 0.0044(9) O8 0.0380(11) 0.0302(10) 0.0449(12) -0.0042(9) -0.0115(9) 0.0119(9) O9 0.0295(10) 0.0443(11) 0.0320(10) -0.0025(8) 0.0055(8) -0.0135(8) N1 0.0201(9) 0.0130(8) 0.0169(9) 0.0014(7) 0.0057(7) 0.0004(7) N2 0.0222(9) 0.0149(8) 0.0181(9) 0.0021(7) 0.0081(7) 0.0013(7) C1 0.0256(11) 0.0192(11) 0.0322(13) -0.0080(9) 0.0092(10) -0.0026(9) C2 0.0266(12) 0.0200(11) 0.0362(14) -0.0024(10) 0.0126(11) 0.0028(9) C3 0.0260(12) 0.0222(11) 0.0291(13) 0.0011(9) 0.0099(10) 0.0045(9) C4 0.0306(13) 0.0272(12) 0.0276(13) 0.0004(10) 0.0125(11) 0.0043(10) C5 0.0295(12) 0.0242(12) 0.0220(11) -0.0011(9) 0.0126(10) 0.0010(9) C6 0.0255(12) 0.0196(11) 0.0319(13) 0.0043(9) 0.0133(10) 0.0020(9) C7 0.0245(11) 0.0264(12) 0.0250(12) -0.0025(10) 0.0037(10) 0.0028(9) C8 0.0235(11) 0.0246(12) 0.0257(12) -0.0072(9) -0.0013(10) 0.0013(9) C9 0.0219(11) 0.0288(12) 0.0203(11) -0.0032(9) 0.0008(9) -0.0001(9) C10 0.0164(9) 0.0146(9) 0.0169(10) -0.0006(8) 0.0048(8) 0.0005(7) C11 0.0170(10) 0.0155(10) 0.0186(10) -0.0005(8) 0.0050(8) 0.0010(8) C12 0.0202(10) 0.0166(10) 0.0183(10) 0.0009(8) 0.0061(8) 0.0023(8) C13 0.0251(11) 0.0152(10) 0.0190(10) 0.0054(8) 0.0100(9) 0.0018(8) C14 0.0192(11) 0.0313(13) 0.0314(13) 0.0120(10) 0.0045(10) -0.0013(9) C15 0.0264(12) 0.0359(14) 0.0407(15) 0.0160(12) 0.0081(12) -0.0093(11) C16 0.0362(13) 0.0198(11) 0.0302(13) 0.0080(10) 0.0092(11) -0.0022(10) C17 0.0269(12) 0.0257(12) 0.0273(12) 0.0119(10) 0.0036(10) 0.0009(10) C18 0.0210(11) 0.0269(12) 0.0244(12) 0.0086(9) 0.0016(9) -0.0018(9) C19 0.080(2) 0.0204(12) 0.0377(16) 0.0064(11) 0.0375(16) 0.0097(13) C20 0.076(2) 0.0317(15) 0.0224(13) 0.0065(11) 0.0148(14) -0.0104(14) C21 0.0453(17) 0.0501(19) 0.070(2) 0.0358(17) 0.0377(17) 0.0162(15) C22 0.100(3) 0.0273(14) 0.0447(18) 0.0095(13) 0.052(2) 0.0181(16) C23 0.0202(10) 0.0110(9) 0.0190(10) 0.0003(7) 0.0043(8) 0.0003(7) C24 0.0215(10) 0.0153(10) 0.0189(10) -0.0007(8) 0.0029(9) 0.0004(8) C26 0.0278(12) 0.0157(10) 0.0213(11) 0.0016(8) 0.0021(9) 0.0044(9) C27 0.0355(13) 0.0147(10) 0.0203(11) 0.0031(8) 0.0064(10) 0.0005(9) C28 0.0268(11) 0.0158(10) 0.0246(12) 0.0009(8) 0.0060(9) -0.0034(9) C29 0.0192(10) 0.0170(10) 0.0213(11) 0.0017(8) 0.0034(9) 0.0000(8) C30 0.0314(12) 0.0153(10) 0.0182(11) -0.0012(8) 0.0075(9) 0.0008(9) C31 0.0364(13) 0.0158(11) 0.0296(13) 0.0005(9) 0.0104(11) 0.0064(10) C32 0.0389(14) 0.0162(11) 0.0213(11) -0.0014(9) 0.0018(10) -0.0041(10) C33 0.0417(14) 0.0151(10) 0.0195(11) -0.0025(8) 0.0090(10) 0.0025(10) C34 0.0471(19) 0.088(3) 0.0323(17) 0.0052(17) 0.0005(15) -0.0131(19) _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 C2 1.907(3) . ? Ru1 C1 1.927(2) . ? Ru1 C3 1.928(3) . ? Ru1 C11 2.111(2) . ? Ru1 Ru3 2.7270(2) . ? Ru1 Ru2 2.9639(2) . ? Ru2 C5 1.891(2) . ? Ru2 C6 1.931(3) . ? Ru2 C4 1.936(3) . ? Ru2 C10 2.096(2) . ? Ru2 Ru3 2.7137(2) . ? Ru3 C7 1.890(2) . ? Ru3 C9 1.900(3) . ? Ru3 C8 1.908(2) . ? Ru3 C10 2.326(2) . ? Ru3 C11 2.338(2) . ? Cl1 C34 1.731(3) . ? Cl2 C34 1.758(5) . ? O1 C1 1.134(3) . ? O2 C2 1.137(3) . ? O3 C3 1.133(3) . ? O4 C4 1.136(3) . ? O5 C5 1.145(3) . ? O6 C6 1.135(3) . ? O7 C7 1.145(3) . ? O8 C8 1.144(3) . ? O9 C9 1.146(3) . ? N1 C12 1.329(3) . ? N1 C10 1.430(3) . ? N1 C23 1.505(3) . ? N2 C12 1.328(3) . ? N2 C11 1.425(3) . ? N2 C13 1.501(3) . ? C10 C11 1.411(3) . ? C13 C19 1.518(3) . ? C13 C18 1.532(3) . ? C13 C14 1.537(3) . ? C14 C15 1.534(3) . ? C15 C21 1.510(5) . ? C15 C16 1.524(4) . ? C16 C17 1.521(4) . ? C17 C20 1.517(4) . ? C17 C18 1.539(3) . ? C19 C22 1.553(4) . ? C20 C22 1.547(5) . ? C21 C22 1.518(5) . ? C23 C24 1.532(3) . ? C23 C29 1.535(3) . ? C23 C30 1.536(3) . ? C24 C26 1.539(3) . ? C26 C31 1.530(3) . ? C26 C27 1.532(3) . ? C27 C28 1.534(3) . ? C28 C32 1.531(3) . ? C28 C29 1.542(3) . ? C30 C33 1.541(3) . ? C31 C33 1.538(3) . ? C32 C33 1.528(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 C2 Ru1 C1 91.58(10) . . ? C2 Ru1 C3 99.81(11) . . ? C1 Ru1 C3 95.95(10) . . ? C2 Ru1 C11 100.47(9) . . ? C1 Ru1 C11 158.76(10) . . ? C3 Ru1 C11 99.10(9) . . ? C2 Ru1 Ru3 91.67(8) . . ? C1 Ru1 Ru3 106.60(8) . . ? C3 Ru1 Ru3 154.40(7) . . ? C11 Ru1 Ru3 56.06(6) . . ? C2 Ru1 Ru2 147.90(8) . . ? C1 Ru1 Ru2 92.23(8) . . ? C3 Ru1 Ru2 111.45(8) . . ? C11 Ru1 Ru2 68.34(6) . . ? Ru3 Ru1 Ru2 56.776(6) . . ? C5 Ru2 C6 103.40(10) . . ? C5 Ru2 C4 88.63(10) . . ? C6 Ru2 C4 101.30(11) . . ? C5 Ru2 C10 98.67(9) . . ? C6 Ru2 C10 95.65(9) . . ? C4 Ru2 C10 159.48(10) . . ? C5 Ru2 Ru3 92.38(8) . . ? C6 Ru2 Ru3 149.77(7) . . ? C4 Ru2 Ru3 104.74(8) . . ? C10 Ru2 Ru3 56.07(6) . . ? C5 Ru2 Ru1 149.43(8) . . ? C6 Ru2 Ru1 105.31(7) . . ? C4 Ru2 Ru1 95.84(8) . . ? C10 Ru2 Ru1 68.32(6) . . ? Ru3 Ru2 Ru1 57.206(6) . . ? C7 Ru3 C9 97.13(11) . . ? C7 Ru3 C8 96.99(11) . . ? C9 Ru3 C8 93.52(11) . . ? C7 Ru3 C10 136.89(9) . . ? C9 Ru3 C10 122.38(9) . . ? C8 Ru3 C10 97.02(9) . . ? C7 Ru3 C11 136.44(9) . . ? C9 Ru3 C11 95.08(9) . . ? C8 Ru3 C11 123.80(9) . . ? C10 Ru3 C11 35.21(7) . . ? C7 Ru3 Ru2 88.95(8) . . ? C9 Ru3 Ru2 163.95(7) . . ? C8 Ru3 Ru2 100.50(8) . . ? C10 Ru3 Ru2 48.41(5) . . ? C11 Ru3 Ru2 70.64(5) . . ? C7 Ru3 Ru1 88.21(7) . . ? C9 Ru3 Ru1 99.21(7) . . ? C8 Ru3 Ru1 165.56(7) . . ? C10 Ru3 Ru1 70.40(5) . . ? C11 Ru3 Ru1 48.52(5) . . ? Ru2 Ru3 Ru1 66.018(7) . . ? C12 N1 C10 107.37(17) . . ? C12 N1 C23 123.02(18) . . ? C10 N1 C23 129.61(18) . . ? C12 N2 C11 107.84(18) . . ? C12 N2 C13 123.07(18) . . ? C11 N2 C13 129.05(18) . . ? O1 C1 Ru1 175.0(2) . . ? O2 C2 Ru1 176.0(2) . . ? O3 C3 Ru1 179.5(3) . . ? O4 C4 Ru2 178.8(3) . . ? O5 C5 Ru2 177.1(2) . . ? O6 C6 Ru2 173.6(2) . . ? O7 C7 Ru3 178.5(2) . . ? O8 C8 Ru3 175.7(2) . . ? O9 C9 Ru3 176.9(2) . . ? C11 C10 N1 106.36(18) . . ? C11 C10 Ru2 112.25(15) . . ? N1 C10 Ru2 140.00(15) . . ? C11 C10 Ru3 72.86(12) . . ? N1 C10 Ru3 127.34(14) . . ? Ru2 C10 Ru3 75.52(7) . . ? C10 C11 N2 106.07(18) . . ? C10 C11 Ru1 111.09(15) . . ? N2 C11 Ru1 141.58(15) . . ? C10 C11 Ru3 71.92(12) . . ? N2 C11 Ru3 126.78(14) . . ? Ru1 C11 Ru3 75.42(7) . . ? N2 C12 N1 112.36(19) . . ? N2 C13 C19 111.45(18) . . ? N2 C13 C18 109.28(18) . . ? C19 C13 C18 109.6(2) . . ? N2 C13 C14 108.44(18) . . ? C19 C13 C14 108.4(2) . . ? C18 C13 C14 109.66(19) . . ? C15 C14 C13 109.8(2) . . ? C21 C15 C16 109.1(2) . . ? C21 C15 C14 109.4(2) . . ? C16 C15 C14 109.4(2) . . ? C17 C16 C15 110.6(2) . . ? C20 C17 C16 110.0(2) . . ? C20 C17 C18 109.6(2) . . ? C16 C17 C18 108.7(2) . . ? C13 C18 C17 109.7(2) . . ? C13 C19 C22 109.5(2) . . ? C17 C20 C22 108.7(2) . . ? C15 C21 C22 109.7(2) . . ? C21 C22 C20 110.2(2) . . ? C21 C22 C19 109.9(3) . . ? C20 C22 C19 108.5(3) . . ? N1 C23 C24 109.51(17) . . ? N1 C23 C29 109.89(17) . . ? C24 C23 C29 110.65(18) . . ? N1 C23 C30 109.67(17) . . ? C24 C23 C30 108.79(18) . . ? C29 C23 C30 108.30(18) . . ? C23 C24 C26 109.36(18) . . ? C31 C26 C27 110.1(2) . . ? C31 C26 C24 109.32(19) . . ? C27 C26 C24 109.71(19) . . ? C26 C27 C28 109.41(19) . . ? C32 C28 C27 109.7(2) . . ? C32 C28 C29 109.44(19) . . ? C27 C28 C29 109.40(18) . . ? C23 C29 C28 109.66(18) . . ? C23 C30 C33 109.74(18) . . ? C26 C31 C33 108.9(2) . . ? C33 C32 C28 109.09(19) . . ? C32 C33 C31 109.9(2) . . ? C32 C33 C30 110.1(2) . . ? C31 C33 C30 109.02(19) . . ? Cl1 C34 Cl2 112.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.127 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.126 # Attachment '4_h08mkw2.cif' data_h08mkw2 _database_code_depnum_ccdc_archive 'CCDC 687174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H20 N2 O11 Os3' _chemical_formula_weight 1059.00 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.92700(10) _cell_length_b 13.3980(2) _cell_length_c 16.7890(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.085(1) _cell_angle_gamma 90.00 _cell_volume 2779.47(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 51445 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 13.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.65 _exptl_absorpt_process_details ; Sortav & Blessing ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43466 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6343 _reflns_number_gt 6000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0357P)^2^+17.6399P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6343 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0364 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.71184(2) 0.400964(17) 0.917444(14) 0.01805(8) Uani 1 1 d . . . Os2 Os 0.687340(18) 0.188431(16) 0.918637(14) 0.01363(7) Uani 1 1 d . . . Os3 Os 0.518578(19) 0.311252(18) 0.810362(15) 0.01902(8) Uani 1 1 d . . . O1 O 0.7778(5) 0.3926(5) 0.7559(4) 0.0478(16) Uani 1 1 d . . . O2 O 0.6439(6) 0.6185(4) 0.8823(4) 0.0441(15) Uani 1 1 d . . . O3 O 0.9488(5) 0.4032(5) 1.0233(4) 0.0446(14) Uani 1 1 d . . . O4 O 0.6366(6) 0.3911(4) 1.0754(3) 0.0426(15) Uani 1 1 d . . . O5 O 0.8328(5) 0.1575(5) 0.8046(4) 0.0470(15) Uani 1 1 d . . . O6 O 0.8803(5) 0.1780(4) 1.0719(4) 0.0435(15) Uani 1 1 d . . . O7 O 0.5311(5) 0.1752(5) 1.0243(4) 0.0408(14) Uani 1 1 d . . . O8 O 0.6190(5) 0.2208(5) 0.6821(4) 0.0455(15) Uani 1 1 d . . . O9 O 0.4650(6) 0.5079(5) 0.7159(4) 0.059(2) Uani 1 1 d . . . O10 O 0.3159(5) 0.1898(5) 0.7287(6) 0.057(2) Uani 1 1 d . . . O11 O 0.4153(5) 0.3719(5) 0.9467(4) 0.0480(16) Uani 1 1 d . . . N1 N 0.5226(4) -0.0800(4) 0.8059(3) 0.0161(10) Uani 1 1 d . . . N2 N 0.6660(4) -0.0574(4) 0.9110(3) 0.0147(9) Uani 1 1 d . . . C1 C 0.7521(6) 0.3927(5) 0.8147(5) 0.0296(15) Uani 1 1 d . . . C2 C 0.6699(6) 0.5385(5) 0.8961(4) 0.0289(15) Uani 1 1 d . . . C3 C 0.8589(6) 0.4045(5) 0.9844(4) 0.0266(14) Uani 1 1 d . . . C4 C 0.6602(6) 0.3928(5) 1.0159(5) 0.0301(15) Uani 1 1 d . . . C5 C 0.7774(6) 0.1731(6) 0.8447(4) 0.0267(14) Uani 1 1 d . . . C6 C 0.8063(5) 0.1794(5) 1.0123(4) 0.0230(13) Uani 1 1 d . . . C7 C 0.5873(6) 0.1862(5) 0.9842(4) 0.0243(14) Uani 1 1 d . . . C8 C 0.5893(6) 0.2528(6) 0.7334(4) 0.0281(14) Uani 1 1 d . . . C9 C 0.4844(6) 0.4349(6) 0.7515(5) 0.0334(16) Uani 1 1 d . . . C10 C 0.3936(6) 0.2353(6) 0.7588(5) 0.0340(16) Uani 1 1 d . . . C11 C 0.4575(6) 0.3486(6) 0.8988(5) 0.0315(15) Uani 1 1 d . . . C12 C 0.6310(5) 0.0388(4) 0.8817(4) 0.0156(11) Uani 1 1 d . . . C13 C 0.5423(5) 0.0219(5) 0.8161(4) 0.0199(12) Uani 1 1 d . . . H45 H 0.4998 0.0724 0.7820 0.024 Uiso 1 1 calc R . . C14 C 0.5995(5) -0.1253(5) 0.8640(4) 0.0175(11) Uani 1 1 d . . . H29 H 0.6067 -0.1956 0.8713 0.021 Uiso 1 1 calc R . . C15 C 0.7582(5) -0.0886(5) 0.9841(4) 0.0188(12) Uani 1 1 d . . . C16 C 0.8646(5) -0.0496(5) 0.9728(5) 0.0280(14) Uani 1 1 d . . . H40A H 0.8813 -0.0866 0.9277 0.042 Uiso 1 1 calc R . . H40B H 0.9232 -0.0590 1.0246 0.042 Uiso 1 1 calc R . . H40C H 0.8573 0.0215 0.9587 0.042 Uiso 1 1 calc R . . C17 C 0.7349(6) -0.0467(5) 1.0629(4) 0.0269(14) Uani 1 1 d . . . H25A H 0.7348 0.0264 1.0610 0.040 Uiso 1 1 calc R . . H25B H 0.7910 -0.0696 1.1126 0.040 Uiso 1 1 calc R . . H25C H 0.6641 -0.0704 1.0651 0.040 Uiso 1 1 calc R . . C18 C 0.7667(6) -0.2000(5) 0.9916(5) 0.0306(16) Uani 1 1 d . . . H26A H 0.6990 -0.2272 0.9976 0.046 Uiso 1 1 calc R . . H26B H 0.8267 -0.2179 1.0405 0.046 Uiso 1 1 calc R . . H26C H 0.7798 -0.2279 0.9414 0.046 Uiso 1 1 calc R . . C19 C 0.4288(5) -0.1260(5) 0.7420(4) 0.0254(14) Uani 1 1 d . . . C20 C 0.4333(9) -0.0933(7) 0.6564(5) 0.052(3) Uani 1 1 d . . . H46A H 0.4949 -0.1254 0.6441 0.077 Uiso 1 1 calc R . . H46B H 0.4416 -0.0207 0.6556 0.077 Uiso 1 1 calc R . . H46C H 0.3661 -0.1129 0.6143 0.077 Uiso 1 1 calc R . . C21 C 0.3249(6) -0.0864(6) 0.7579(6) 0.0397(19) Uani 1 1 d . . . H33A H 0.2617 -0.1150 0.7167 0.060 Uiso 1 1 calc R . . H33B H 0.3228 -0.0135 0.7529 0.060 Uiso 1 1 calc R . . H33C H 0.3241 -0.1055 0.8140 0.060 Uiso 1 1 calc R . . C22 C 0.4352(6) -0.2379(5) 0.7509(5) 0.0285(14) Uani 1 1 d . . . H44A H 0.5030 -0.2616 0.7427 0.043 Uiso 1 1 calc R . . H44B H 0.3739 -0.2683 0.7090 0.043 Uiso 1 1 calc R . . H44C H 0.4328 -0.2566 0.8067 0.043 Uiso 1 1 calc R . . 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 Os1 0.02150(13) 0.01551(13) 0.01658(12) -0.00094(8) 0.00472(9) -0.00506(9) Os2 0.01208(12) 0.01422(12) 0.01372(12) -0.00037(7) 0.00246(9) -0.00171(7) Os3 0.01547(13) 0.01831(13) 0.02028(14) 0.00313(8) 0.00061(10) -0.00016(8) O1 0.050(4) 0.069(4) 0.035(3) -0.006(3) 0.029(3) -0.022(3) O2 0.071(5) 0.018(3) 0.042(3) 0.002(2) 0.013(3) 0.000(3) O3 0.032(3) 0.042(3) 0.051(4) -0.008(3) -0.002(3) -0.010(2) O4 0.068(4) 0.043(3) 0.025(3) -0.007(2) 0.027(3) -0.007(3) O5 0.040(3) 0.058(4) 0.058(4) 0.003(3) 0.037(3) 0.007(3) O6 0.039(3) 0.035(3) 0.039(3) 0.000(2) -0.015(3) -0.001(2) O7 0.042(3) 0.047(3) 0.046(3) 0.006(3) 0.033(3) 0.000(3) O8 0.043(3) 0.069(4) 0.025(3) -0.012(3) 0.011(3) -0.002(3) O9 0.064(4) 0.033(3) 0.055(4) 0.022(3) -0.021(3) -0.005(3) O10 0.017(3) 0.039(4) 0.105(6) -0.022(3) 0.002(3) -0.006(2) O11 0.038(3) 0.065(4) 0.050(4) 0.005(3) 0.026(3) 0.014(3) N1 0.016(2) 0.015(2) 0.016(2) -0.0035(18) 0.0034(19) -0.0062(19) N2 0.012(2) 0.018(2) 0.014(2) 0.0024(18) 0.0045(18) -0.0021(19) C1 0.030(4) 0.028(4) 0.035(4) -0.001(3) 0.015(3) -0.012(3) C2 0.043(4) 0.022(4) 0.023(3) -0.001(3) 0.011(3) -0.010(3) C3 0.035(4) 0.018(3) 0.023(3) -0.002(2) 0.001(3) -0.007(3) C4 0.037(4) 0.024(4) 0.030(4) 0.001(3) 0.011(3) -0.002(3) C5 0.023(3) 0.032(4) 0.024(3) -0.003(3) 0.006(3) -0.005(3) C6 0.021(3) 0.020(3) 0.024(3) -0.009(2) 0.000(3) -0.005(2) C7 0.027(3) 0.024(3) 0.024(3) 0.004(2) 0.010(3) 0.003(2) C8 0.023(3) 0.035(4) 0.023(3) 0.000(3) 0.001(3) -0.004(3) C9 0.029(4) 0.030(4) 0.031(4) 0.002(3) -0.007(3) -0.003(3) C10 0.021(3) 0.027(4) 0.049(5) -0.008(3) 0.002(3) 0.004(3) C11 0.023(3) 0.031(4) 0.040(4) 0.008(3) 0.009(3) 0.008(3) C12 0.012(2) 0.017(3) 0.019(3) -0.004(2) 0.006(2) -0.004(2) C13 0.019(3) 0.017(3) 0.020(3) -0.003(2) 0.000(2) 0.000(2) C14 0.020(3) 0.017(3) 0.016(3) 0.001(2) 0.005(2) -0.004(2) C15 0.016(3) 0.015(3) 0.020(3) 0.004(2) -0.003(2) -0.003(2) C16 0.017(3) 0.022(3) 0.042(4) 0.006(3) 0.005(3) 0.001(3) C17 0.031(3) 0.032(4) 0.014(3) 0.001(2) 0.000(3) -0.005(3) C18 0.032(4) 0.019(3) 0.031(4) 0.005(3) -0.006(3) -0.001(3) C19 0.021(3) 0.028(3) 0.022(3) -0.003(3) -0.002(3) -0.009(3) C20 0.076(7) 0.051(5) 0.019(4) -0.007(3) 0.000(4) -0.036(5) C21 0.020(3) 0.029(4) 0.058(5) -0.014(4) -0.008(3) -0.002(3) C22 0.023(3) 0.025(4) 0.034(4) -0.004(3) 0.003(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 Os1 C3 1.903(7) . ? Os1 C2 1.925(7) . ? Os1 C1 1.946(7) . ? Os1 C4 1.960(7) . ? Os1 Os2 2.8658(3) . ? Os1 Os3 2.8773(3) . ? Os2 C6 1.852(7) . ? Os2 C7 1.929(7) . ? Os2 C5 1.946(7) . ? Os2 C12 2.161(6) . ? Os2 Os3 2.9054(3) . ? Os3 C10 1.890(7) . ? Os3 C9 1.913(8) . ? Os3 C11 1.940(8) . ? Os3 C8 1.953(7) . ? O1 C1 1.130(9) . ? O2 C2 1.127(9) . ? O3 C3 1.154(9) . ? O4 C4 1.126(9) . ? O5 C5 1.138(9) . ? O6 C6 1.164(9) . ? O7 C7 1.136(8) . ? O8 C8 1.125(9) . ? O9 C9 1.135(10) . ? O10 C10 1.157(9) . ? O11 C11 1.141(9) . ? N1 C14 1.319(8) . ? N1 C13 1.391(8) . ? N1 C19 1.495(8) . ? N2 C14 1.338(8) . ? N2 C12 1.407(8) . ? N2 C15 1.497(8) . ? C12 C13 1.355(8) . ? C13 H45 0.9500 . ? C14 H29 0.9500 . ? C15 C18 1.500(9) . ? C15 C16 1.533(9) . ? C15 C17 1.547(9) . ? C16 H40A 0.9800 . ? C16 H40B 0.9800 . ? C16 H40C 0.9800 . ? C17 H25A 0.9800 . ? C17 H25B 0.9800 . ? C17 H25C 0.9800 . ? C18 H26A 0.9800 . ? C18 H26B 0.9800 . ? C18 H26C 0.9800 . ? C19 C22 1.506(10) . ? C19 C20 1.519(10) . ? C19 C21 1.538(11) . ? C20 H46A 0.9800 . ? C20 H46B 0.9800 . ? C20 H46C 0.9800 . ? C21 H33A 0.9800 . ? C21 H33B 0.9800 . ? C21 H33C 0.9800 . ? C22 H44A 0.9800 . ? C22 H44B 0.9800 . ? C22 H44C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Os1 C2 105.3(3) . . ? C3 Os1 C1 92.6(3) . . ? C2 Os1 C1 91.4(3) . . ? C3 Os1 C4 91.8(3) . . ? C2 Os1 C4 93.6(3) . . ? C1 Os1 C4 172.3(3) . . ? C3 Os1 Os2 96.5(2) . . ? C2 Os1 Os2 158.0(2) . . ? C1 Os1 Os2 90.5(2) . . ? C4 Os1 Os2 82.7(2) . . ? C3 Os1 Os3 155.8(2) . . ? C2 Os1 Os3 97.9(2) . . ? C1 Os1 Os3 80.3(2) . . ? C4 Os1 Os3 93.2(2) . . ? Os2 Os1 Os3 60.781(8) . . ? C6 Os2 C7 92.5(3) . . ? C6 Os2 C5 91.8(3) . . ? C7 Os2 C5 171.6(3) . . ? C6 Os2 C12 108.0(3) . . ? C7 Os2 C12 85.6(3) . . ? C5 Os2 C12 86.2(3) . . ? C6 Os2 Os1 90.3(2) . . ? C7 Os2 Os1 96.5(2) . . ? C5 Os2 Os1 90.7(2) . . ? C12 Os2 Os1 161.53(16) . . ? C6 Os2 Os3 148.4(2) . . ? C7 Os2 Os3 81.9(2) . . ? C5 Os2 Os3 98.1(2) . . ? C12 Os2 Os3 102.59(16) . . ? Os1 Os2 Os3 59.806(8) . . ? C10 Os3 C9 101.1(3) . . ? C10 Os3 C11 90.2(3) . . ? C9 Os3 C11 95.1(3) . . ? C10 Os3 C8 89.1(3) . . ? C9 Os3 C8 95.0(3) . . ? C11 Os3 C8 169.9(3) . . ? C10 Os3 Os1 168.3(3) . . ? C9 Os3 Os1 89.3(2) . . ? C11 Os3 Os1 83.6(2) . . ? C8 Os3 Os1 95.3(2) . . ? C10 Os3 Os2 111.4(2) . . ? C9 Os3 Os2 146.2(2) . . ? C11 Os3 Os2 93.8(2) . . ? C8 Os3 Os2 77.0(2) . . ? Os1 Os3 Os2 59.413(8) . . ? C14 N1 C13 106.9(5) . . ? C14 N1 C19 128.1(5) . . ? C13 N1 C19 125.0(5) . . ? C14 N2 C12 109.4(5) . . ? C14 N2 C15 120.8(5) . . ? C12 N2 C15 129.7(5) . . ? O1 C1 Os1 176.4(7) . . ? O2 C2 Os1 178.7(7) . . ? O3 C3 Os1 177.2(6) . . ? O4 C4 Os1 175.5(7) . . ? O5 C5 Os2 174.8(7) . . ? O6 C6 Os2 177.0(6) . . ? O7 C7 Os2 173.2(6) . . ? O8 C8 Os3 172.0(6) . . ? O9 C9 Os3 179.1(9) . . ? O10 C10 Os3 178.3(8) . . ? O11 C11 Os3 175.4(7) . . ? C13 C12 N2 103.9(5) . . ? C13 C12 Os2 121.4(5) . . ? N2 C12 Os2 134.7(4) . . ? C12 C13 N1 110.1(5) . . ? C12 C13 H45 124.9 . . ? N1 C13 H45 124.9 . . ? N1 C14 N2 109.7(5) . . ? N1 C14 H29 125.1 . . ? N2 C14 H29 125.1 . . ? N2 C15 C18 111.5(5) . . ? N2 C15 C16 109.3(5) . . ? C18 C15 C16 107.7(6) . . ? N2 C15 C17 107.0(5) . . ? C18 C15 C17 108.5(6) . . ? C16 C15 C17 113.0(5) . . ? C15 C16 H40A 109.5 . . ? C15 C16 H40B 109.5 . . ? H40A C16 H40B 109.5 . . ? C15 C16 H40C 109.5 . . ? H40A C16 H40C 109.5 . . ? H40B C16 H40C 109.5 . . ? C15 C17 H25A 109.5 . . ? C15 C17 H25B 109.5 . . ? H25A C17 H25B 109.5 . . ? C15 C17 H25C 109.5 . . ? H25A C17 H25C 109.5 . . ? H25B C17 H25C 109.5 . . ? C15 C18 H26A 109.5 . . ? C15 C18 H26B 109.5 . . ? H26A C18 H26B 109.5 . . ? C15 C18 H26C 109.5 . . ? H26A C18 H26C 109.5 . . ? H26B C18 H26C 109.5 . . ? N1 C19 C22 109.3(5) . . ? N1 C19 C20 108.2(6) . . ? C22 C19 C20 111.3(6) . . ? N1 C19 C21 107.4(5) . . ? C22 C19 C21 110.6(6) . . ? C20 C19 C21 110.0(7) . . ? C19 C20 H46A 109.5 . . ? C19 C20 H46B 109.5 . . ? H46A C20 H46B 109.5 . . ? C19 C20 H46C 109.5 . . ? H46A C20 H46C 109.5 . . ? H46B C20 H46C 109.5 . . ? C19 C21 H33A 109.5 . . ? C19 C21 H33B 109.5 . . ? H33A C21 H33B 109.5 . . ? C19 C21 H33C 109.5 . . ? H33A C21 H33C 109.5 . . ? H33B C21 H33C 109.5 . . ? C19 C22 H44A 109.5 . . ? C19 C22 H44B 109.5 . . ? H44A C22 H44B 109.5 . . ? C19 C22 H44C 109.5 . . ? H44A C22 H44C 109.5 . . ? H44B C22 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.645 _refine_diff_density_min -2.509 _refine_diff_density_rms 0.253