# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email bhtclau@cityu.edu.hk _publ_contact_author_name 'Tai-Chu Lau' _publ_author_name 'Wai-Lun Man' data_1 _database_code_depnum_ccdc_archive 'CCDC 821916' #TrackingRef '- CIF 1-3.cif' _audit_creation_date 2011-02-25 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C10 H6 N2 O Ru0.5), 2(C12 H10 P0.5)' _chemical_formula_sum 'C44 H32 N4 O2 P Ru' _chemical_formula_weight 780.78 _chemical_melting_point ? 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' 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' P P 0.1023 0.0942 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.4737(10) _cell_length_b 7.4234(5) _cell_length_c 28.4371(16) _cell_angle_alpha 90.0 _cell_angle_beta 93.451(5) _cell_angle_gamma 90.0 _cell_volume 3471.3(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4434 _cell_measurement_temperature 173.15 _cell_measurement_theta_max 28.0577 _cell_measurement_theta_min 3.1737 _cell_oxdiff_angle_alpha 89.982(4) _cell_oxdiff_angle_beta 117.488(6) _cell_oxdiff_angle_gamma 89.978(5) _cell_oxdiff_length_a 31.989(2) _cell_oxdiff_length_b 7.4239(4) _cell_oxdiff_length_c 16.4812(9) _cell_oxdiff_measurement_reflns_used 4364 _cell_oxdiff_volume 3472.1(3) _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1596 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_unetI/netI 0.1447 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 17636 _diffrn_reflns_theta_full 25.09 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.09 _diffrn_ambient_temperature 173.15 _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -92.00 -60.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - -15.4471 179.0000 270.0000 64 #__ type_ start__ end____ width___ exp.time_ 2 omega -37.00 10.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - -15.4471 77.0000 300.0000 94 #__ type_ start__ end____ width___ exp.time_ 3 omega -88.00 58.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - -15.4471 0.0000 90.0000 292 #__ type_ start__ end____ width___ exp.time_ 4 omega -41.00 57.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - -15.4471 37.0000 180.0000 196 #__ type_ start__ end____ width___ exp.time_ 5 omega -86.00 15.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - -15.4471 -77.0000 60.0000 202 #__ type_ start__ end____ width___ exp.time_ 6 omega -86.00 -16.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - -15.4471 -77.0000 270.0000 140 #__ type_ start__ end____ width___ exp.time_ 7 omega -11.00 55.00 0.5000 17.0000 omega____ theta____ kappa____ phi______ frames - 15.9940 -93.0000 321.0000 132 ; _diffrn_measurement_device_type 'Goniometer Xcalibur, detector: Sapphire3 (Gemini ultra Mo)' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0039162258 _diffrn_orient_matrix_UB_12 0.0842129867 _diffrn_orient_matrix_UB_13 -0.0117391235 _diffrn_orient_matrix_UB_21 0.0296922266 _diffrn_orient_matrix_UB_22 -0.0271844167 _diffrn_orient_matrix_UB_23 -0.0155999604 _diffrn_orient_matrix_UB_31 -0.0310288357 _diffrn_orient_matrix_UB_32 -0.0364923832 _diffrn_orient_matrix_UB_33 -0.0156060540 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 1963 _reflns_number_total 3080 _reflns_odcompleteness_completeness ' 99.43' _reflns_odcompleteness_iscentric ' 1' _reflns_odcompleteness_theta ' 24.97' _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.617 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.067 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 237 _refine_ls_number_reflns 3080 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.0736 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.5000 0.5000 0.0000 0.02765(14) Uani 1 2 d S . . P1 P 0.5000 0.23891(17) 0.2500 0.0201(3) Uani 1 2 d S . . O1 O 0.58225(15) 0.6295(4) 0.04231(9) 0.0412(7) Uani 1 1 d . . . N1 N 0.4098(2) 0.3837(6) 0.09241(13) 0.0621(11) Uani 1 1 d . . . N2 N 0.58456(18) 0.2928(5) 0.01090(11) 0.0383(8) Uani 1 1 d . . . C1 C 0.4418(2) 0.4223(5) 0.05944(14) 0.0370(10) Uani 1 1 d . . . C2 C 0.5849(2) 0.1327(6) -0.00823(15) 0.0450(11) Uani 1 1 d . . . H2 H 0.5426 0.1005 -0.0309 0.054 Uiso 1 1 calc R . . C3 C 0.6462(2) 0.0075(7) 0.00387(13) 0.0463(10) Uani 1 1 d . . . H3 H 0.6443 -0.1093 -0.0098 0.056 Uiso 1 1 calc R . . C4 C 0.7097(3) 0.0532(6) 0.03571(15) 0.0471(13) Uani 1 1 d . . . H4 H 0.7521 -0.0302 0.0435 0.056 Uiso 1 1 calc R . . C5 C 0.7103(2) 0.2265(6) 0.05656(13) 0.0372(10) Uani 1 1 d . . . C6 C 0.7692(3) 0.2921(7) 0.08881(15) 0.0519(12) Uani 1 1 d . . . H6 H 0.8128 0.2160 0.0996 0.062 Uiso 1 1 calc R . . C7 C 0.7659(3) 0.4604(8) 0.10509(16) 0.0604(15) Uani 1 1 d . . . H7 H 0.8076 0.4997 0.1272 0.073 Uiso 1 1 calc R . . C8 C 0.7041(2) 0.5820(6) 0.09120(14) 0.0478(12) Uani 1 1 d . . . H8 H 0.7042 0.7009 0.1036 0.057 Uiso 1 1 calc R . . C9 C 0.6428(2) 0.5261(6) 0.05918(12) 0.0390(11) Uani 1 1 d . . . C10 C 0.6460(2) 0.3438(6) 0.04246(13) 0.0322(9) Uani 1 1 d . . . C11 C 0.50612(19) 0.0925(5) 0.20029(11) 0.0208(8) Uani 1 1 d . . . C12 C 0.5615(2) 0.1143(5) 0.16616(12) 0.0328(9) Uani 1 1 d . . . H12 H 0.5969 0.2153 0.1671 0.039 Uiso 1 1 calc R . . C13 C 0.5648(2) -0.0118(7) 0.13076(12) 0.0447(10) Uani 1 1 d . . . H13 H 0.6027 0.0037 0.1072 0.054 Uiso 1 1 calc R . . C14 C 0.5145(2) -0.1593(6) 0.12889(13) 0.0404(10) Uani 1 1 d . . . H14 H 0.5183 -0.2463 0.1046 0.048 Uiso 1 1 calc R . . C15 C 0.4588(2) -0.1800(5) 0.16214(13) 0.0326(9) Uani 1 1 d . . . H15 H 0.4234 -0.2812 0.1609 0.039 Uiso 1 1 calc R . . C16 C 0.4538(2) -0.0547(4) 0.19748(12) 0.0259(9) Uani 1 1 d . . . H16 H 0.4143 -0.0688 0.2202 0.031 Uiso 1 1 calc R . . C17 C 0.58704(18) 0.3839(4) 0.25719(11) 0.0192(8) Uani 1 1 d . . . C18 C 0.60139(18) 0.5072(6) 0.22222(11) 0.0302(8) Uani 1 1 d . . . H18 H 0.5663 0.5124 0.1945 0.036 Uiso 1 1 calc R . . C19 C 0.6670(2) 0.6228(5) 0.22773(14) 0.0371(10) Uani 1 1 d . . . H19 H 0.6777 0.7061 0.2035 0.045 Uiso 1 1 calc R . . C20 C 0.7169(2) 0.6171(5) 0.26846(15) 0.0374(10) Uani 1 1 d . . . H20 H 0.7618 0.6973 0.2722 0.045 Uiso 1 1 calc R . . C21 C 0.70223(17) 0.4963(6) 0.30369(12) 0.0323(8) Uani 1 1 d . . . H21 H 0.7368 0.4940 0.3316 0.039 Uiso 1 1 calc R . . C22 C 0.63710(19) 0.3780(5) 0.29854(12) 0.0241(8) Uani 1 1 d . . . H22 H 0.6267 0.2945 0.3228 0.029 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 0.0324(2) 0.0321(3) 0.0186(2) -0.0012(3) 0.00307(16) 0.0075(3) P1 0.0188(7) 0.0200(8) 0.0218(7) 0.000 0.0047(5) 0.000 O1 0.0449(16) 0.0460(18) 0.0326(16) -0.0057(14) 0.0019(13) 0.0052(15) N1 0.073(3) 0.078(3) 0.037(2) 0.009(2) 0.021(2) 0.014(2) N2 0.045(2) 0.043(2) 0.0277(19) 0.0091(17) 0.0158(16) 0.0137(17) C1 0.041(2) 0.043(3) 0.027(2) 0.004(2) 0.0028(18) 0.0092(19) C2 0.056(3) 0.026(3) 0.056(3) 0.011(2) 0.032(2) 0.015(2) C3 0.067(3) 0.033(2) 0.042(2) -0.001(3) 0.023(2) 0.002(3) C4 0.048(3) 0.042(4) 0.054(3) 0.023(2) 0.032(2) 0.015(2) C5 0.031(2) 0.053(3) 0.029(2) 0.015(2) 0.0106(18) 0.002(2) C6 0.054(3) 0.057(3) 0.044(3) 0.013(3) 0.008(2) 0.008(3) C7 0.041(3) 0.089(5) 0.050(3) 0.006(3) -0.008(2) 0.002(3) C8 0.044(3) 0.060(3) 0.038(3) -0.006(2) -0.004(2) -0.001(2) C9 0.032(2) 0.057(4) 0.029(2) 0.020(2) 0.0110(16) 0.021(2) C10 0.028(2) 0.046(3) 0.023(2) 0.009(2) 0.0113(17) 0.003(2) C11 0.0235(19) 0.022(2) 0.0169(18) 0.0033(16) 0.0017(15) 0.0037(16) C12 0.036(2) 0.034(2) 0.030(2) -0.005(2) 0.0129(17) -0.0085(18) C13 0.054(2) 0.053(3) 0.030(2) -0.006(3) 0.0257(17) -0.001(3) C14 0.058(3) 0.037(3) 0.026(2) -0.011(2) 0.004(2) 0.002(2) C15 0.036(2) 0.027(2) 0.034(2) -0.0011(19) -0.0055(18) -0.0041(18) C16 0.0252(19) 0.028(3) 0.025(2) -0.0013(16) 0.0054(15) -0.0009(15) C17 0.0182(17) 0.016(2) 0.024(2) 0.0008(16) 0.0059(15) 0.0028(15) C18 0.0269(17) 0.027(2) 0.037(2) 0.005(3) -0.0015(14) -0.003(2) C19 0.036(2) 0.031(2) 0.045(3) 0.007(2) 0.0077(19) -0.0114(19) C20 0.026(2) 0.036(3) 0.051(3) -0.010(2) 0.0072(19) -0.0120(19) C21 0.0223(17) 0.037(2) 0.038(2) -0.014(3) -0.0001(15) 0.003(2) C22 0.0258(19) 0.017(2) 0.031(2) -0.0029(17) 0.0077(16) 0.0026(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 O1 2.003(2) . ? Ru1 O1 2.003(2) 5_665 ? Ru1 N2 2.086(3) 5_665 ? Ru1 N2 2.086(3) . ? Ru1 C1 2.075(4) 5_665 ? Ru1 C1 2.075(4) . ? P1 C11 1.791(3) 2_655 ? P1 C11 1.791(3) . ? P1 C17 1.795(3) 2_655 ? P1 C17 1.795(3) . ? O1 C9 1.326(4) . ? N1 C1 1.140(4) . ? N2 C2 1.307(5) . ? N2 C10 1.366(4) . ? C2 H2 0.9500 . ? C2 C3 1.400(5) . ? C3 H3 0.9500 . ? C3 C4 1.383(5) . ? C4 H4 0.9500 . ? C4 C5 1.416(5) . ? C5 C6 1.383(5) . ? C5 C10 1.410(5) . ? C6 H6 0.9500 . ? C6 C7 1.334(6) . ? C7 H7 0.9500 . ? C7 C8 1.400(6) . ? C8 H8 0.9500 . ? C8 C9 1.381(5) . ? C9 C10 1.437(6) . ? C11 C12 1.381(4) . ? C11 C16 1.390(4) . ? C12 H12 0.9500 . ? C12 C13 1.378(5) . ? C13 H13 0.9500 . ? C13 C14 1.373(5) . ? C14 H14 0.9500 . ? C14 C15 1.365(5) . ? C15 H15 0.9500 . ? C15 C16 1.376(4) . ? C16 H16 0.9500 . ? C17 C18 1.383(5) . ? C17 C22 1.396(4) . ? C18 H18 0.9500 . ? C18 C19 1.381(5) . ? C19 H19 0.9500 . ? C19 C20 1.380(5) . ? C20 H20 0.9500 . ? C20 C21 1.377(5) . ? C21 H21 0.9500 . ? C21 C22 1.387(5) . ? C22 H22 0.9500 . ? 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 O1 Ru1 O1 180.00(12) 5_665 . ? O1 Ru1 N2 99.03(13) . 5_665 ? O1 Ru1 N2 80.97(13) 5_665 5_665 ? O1 Ru1 N2 99.03(13) 5_665 . ? O1 Ru1 N2 80.97(13) . . ? O1 Ru1 C1 91.53(13) . 5_665 ? O1 Ru1 C1 88.47(13) 5_665 5_665 ? O1 Ru1 C1 91.53(13) 5_665 . ? O1 Ru1 C1 88.47(13) . . ? N2 Ru1 N2 180.00(17) 5_665 . ? C1 Ru1 N2 89.36(13) 5_665 . ? C1 Ru1 N2 90.64(13) . . ? C1 Ru1 N2 89.36(13) . 5_665 ? C1 Ru1 N2 90.64(13) 5_665 5_665 ? C1 Ru1 C1 180.0(2) 5_665 . ? C11 P1 C11 105.3(2) . 2_655 ? C11 P1 C17 110.89(14) . 2_655 ? C11 P1 C17 111.80(15) 2_655 2_655 ? C11 P1 C17 110.89(14) 2_655 . ? C11 P1 C17 111.80(15) . . ? C17 P1 C17 106.3(2) . 2_655 ? C9 O1 Ru1 114.0(3) . . ? C2 N2 Ru1 128.9(3) . . ? C2 N2 C10 120.3(3) . . ? C10 N2 Ru1 110.8(3) . . ? N1 C1 Ru1 178.4(4) . . ? N2 C2 H2 119.3 . . ? N2 C2 C3 121.5(4) . . ? C3 C2 H2 119.3 . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 120.6 . . ? C3 C4 C5 118.9(4) . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 125.8(4) . . ? C6 C5 C10 117.1(4) . . ? C10 C5 C4 117.1(4) . . ? C5 C6 H6 119.4 . . ? C7 C6 C5 121.2(4) . . ? C7 C6 H6 119.4 . . ? C6 C7 H7 118.3 . . ? C6 C7 C8 123.4(4) . . ? C8 C7 H7 118.3 . . ? C7 C8 H8 120.6 . . ? C9 C8 C7 118.8(4) . . ? C9 C8 H8 120.6 . . ? O1 C9 C8 124.7(4) . . ? O1 C9 C10 117.9(3) . . ? C8 C9 C10 117.5(3) . . ? N2 C10 C5 122.0(4) . . ? N2 C10 C9 116.0(3) . . ? C5 C10 C9 122.0(4) . . ? C12 C11 P1 123.7(3) . . ? C12 C11 C16 119.0(3) . . ? C16 C11 P1 117.3(2) . . ? C11 C12 H12 120.3 . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3 . . ? C12 C13 H13 119.4 . . ? C14 C13 C12 121.3(3) . . ? C14 C13 H13 119.4 . . ? C13 C14 H14 120.2 . . ? C15 C14 C13 119.5(4) . . ? C15 C14 H14 120.2 . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.1(4) . . ? C16 C15 H15 120.0 . . ? C11 C16 H16 119.7 . . ? C15 C16 C11 120.6(3) . . ? C15 C16 H16 119.7 . . ? C18 C17 P1 119.0(2) . . ? C18 C17 C22 120.6(3) . . ? C22 C17 P1 120.3(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 C17 119.7(3) . . ? C19 C18 H18 120.1 . . ? C18 C19 H19 120.0 . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19 120.0 . . ? C19 C20 H20 119.7 . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H20 119.7 . . ? C20 C21 H21 119.9 . . ? C20 C21 C22 120.3(3) . . ? C22 C21 H21 119.9 . . ? C17 C22 H22 120.5 . . ? C21 C22 C17 118.9(3) . . ? C21 C22 H22 120.5 . . ? data_2 _database_code_depnum_ccdc_archive 'CCDC 821917' #TrackingRef '- CIF 1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H72 Co N8 O16 Ru2' _chemical_formula_weight 1326.25 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.8324(2) _cell_length_b 12.7196(4) _cell_length_c 27.7063(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.2018(14) _cell_angle_gamma 90.00 _cell_volume 3110.35(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7614 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description rod _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1366 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ? _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 'NONUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15480 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5463 _reflns_number_gt 4529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.1037P)^2^+18.8713P] 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 SHELXL _refine_ls_extinction_coef 0.0140(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5463 _refine_ls_number_parameters 326 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.2700 _refine_ls_wR_factor_gt 0.2569 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.227 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 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 Ru Ru 0.13939(7) 0.43869(7) 0.18358(2) 0.0497(4) Uani 1 1 d . . . Co Co 0.0000 0.5000 0.0000 0.0622(6) Uani 1 2 d S . . N1 N 0.0330(9) 0.4660(8) 0.0725(3) 0.065(2) Uani 1 1 d . A . N2 N 0.2694(9) 0.4244(7) 0.2931(3) 0.058(2) Uani 1 1 d . . . C1 C 0.0621(10) 0.4552(9) 0.1127(3) 0.056(2) Uani 1 1 d . A . C2 C 0.2230(9) 0.4260(7) 0.2543(3) 0.046(2) Uani 1 1 d . A . O3 O 0.1489(15) 0.3706(11) -0.0167(4) 0.081(4) Uiso 0.683(6) 1 d PD A 1 H3B H 0.2039 0.3929 -0.0389 0.097 Uiso 0.683(6) 1 d PR A 1 O4 O -0.1720(12) 0.3904(10) -0.0022(4) 0.065(3) Uiso 0.683(6) 1 d PD A 1 H4B H -0.1501 0.3305 0.0097 0.078 Uiso 0.683(6) 1 d PR A 1 C21 C 0.2553(19) 0.3204(15) 0.0171(6) 0.078(5) Uiso 0.683(6) 1 d PD A 1 H21A H 0.3108 0.2654 0.0004 0.117 Uiso 0.683(6) 1 calc PR A 1 H21B H 0.2001 0.2889 0.0435 0.117 Uiso 0.683(6) 1 calc PR A 1 H21C H 0.3270 0.3728 0.0302 0.117 Uiso 0.683(6) 1 calc PR A 1 C22 C -0.3212(18) 0.3976(17) -0.0237(7) 0.085(6) Uiso 0.683(6) 1 d PD A 1 H22A H -0.3754 0.3315 -0.0186 0.127 Uiso 0.683(6) 1 calc PR A 1 H22B H -0.3149 0.4108 -0.0584 0.127 Uiso 0.683(6) 1 calc PR A 1 H22C H -0.3757 0.4555 -0.0088 0.127 Uiso 0.683(6) 1 calc PR A 1 O3' O 0.189(3) 0.416(2) -0.0135(9) 0.069(7) Uiso 0.317(6) 1 d PD A 2 H3'B H 0.1940 0.3668 -0.0338 0.083 Uiso 0.317(6) 1 d PR A 2 O4' O -0.125(4) 0.350(3) -0.0164(12) 0.099(10) Uiso 0.317(6) 1 d PD A 2 H4'B H -0.1184 0.3055 0.0062 0.119 Uiso 0.317(6) 1 d PR A 2 C21' C 0.324(5) 0.465(4) 0.0099(19) 0.120 Uiso 0.317(6) 1 d PD A 2 H21D H 0.4143 0.4258 0.0010 0.180 Uiso 0.317(6) 1 calc PR A 2 H21E H 0.3150 0.4627 0.0451 0.180 Uiso 0.317(6) 1 calc PR A 2 H21F H 0.3320 0.5380 -0.0007 0.180 Uiso 0.317(6) 1 calc PR A 2 C22' C -0.282(4) 0.357(5) -0.034(2) 0.120 Uiso 0.317(6) 1 d PD A 2 H22D H -0.3326 0.2895 -0.0286 0.180 Uiso 0.317(6) 1 calc PR A 2 H22E H -0.2862 0.3738 -0.0683 0.180 Uiso 0.317(6) 1 calc PR A 2 H22F H -0.3338 0.4123 -0.0161 0.180 Uiso 0.317(6) 1 calc PR A 2 O1 O 0.0461(10) 0.5738(6) 0.1972(3) 0.052(2) Uani 0.683(6) 1 d PD A 1 N3 N -0.0681(10) 0.3806(9) 0.2076(3) 0.048(3) Uani 0.683(6) 1 d PD A 1 C3 C -0.1180(16) 0.2856(11) 0.2112(6) 0.044(4) Uiso 0.683(6) 1 d PD A 1 H3A H -0.0576 0.2296 0.1999 0.053 Uiso 0.683(6) 1 calc PR A 1 C4 C -0.2583(16) 0.2611(12) 0.2313(5) 0.059(4) Uiso 0.683(6) 1 d PD A 1 H4A H -0.2905 0.1901 0.2336 0.071 Uiso 0.683(6) 1 calc PR A 1 C5 C -0.352(2) 0.3450(14) 0.2484(8) 0.058(5) Uiso 0.683(6) 1 d PD A 1 H5A H -0.4475 0.3309 0.2617 0.070 Uiso 0.683(6) 1 calc PR A 1 C6 C -0.2964(13) 0.4505(10) 0.2444(5) 0.040(3) Uiso 0.683(6) 1 d PD A 1 C7 C -0.368(2) 0.5400(13) 0.2583(8) 0.060(5) Uiso 0.683(6) 1 d PD A 1 H7A H -0.4634 0.5333 0.2728 0.072 Uiso 0.683(6) 1 calc PR A 1 C8 C -0.3148(18) 0.6308(12) 0.2530(6) 0.067(4) Uiso 0.683(6) 1 d PD A 1 H8A H -0.3700 0.6900 0.2637 0.081 Uiso 0.683(6) 1 calc PR A 1 C9 C -0.1743(16) 0.6459(12) 0.2315(5) 0.064(4) Uiso 0.683(6) 1 d PD A 1 H9A H -0.1386 0.7156 0.2272 0.077 Uiso 0.683(6) 1 calc PR A 1 C10 C -0.0888(15) 0.5652(12) 0.2166(6) 0.047(4) Uiso 0.683(6) 1 d PD A 1 C11 C -0.1517(12) 0.4616(8) 0.2237(4) 0.040(3) Uiso 0.683(6) 1 d PD A 1 O1' O 0.0411(17) 0.3108(13) 0.1868(6) 0.045(4) Uiso 0.317(6) 1 d PD A 2 N3' N -0.0687(19) 0.4973(13) 0.2124(7) 0.035(5) Uiso 0.317(6) 1 d PD A 2 C3' C -0.113(3) 0.5902(16) 0.2245(10) 0.039(8) Uiso 0.317(6) 1 d PD A 2 H3'A H -0.0482 0.6483 0.2193 0.047 Uiso 0.317(6) 1 calc PR A 2 C4' C -0.254(3) 0.6082(18) 0.2448(11) 0.053(7) Uiso 0.317(6) 1 d PD A 2 H4'A H -0.2880 0.6776 0.2508 0.063 Uiso 0.317(6) 1 calc PR A 2 C5' C -0.345(4) 0.5177(19) 0.2563(16) 0.060(12) Uiso 0.317(6) 1 d PD A 2 H5'A H -0.4391 0.5266 0.2714 0.073 Uiso 0.317(6) 1 calc PR A 2 C6' C -0.292(2) 0.4144(16) 0.2447(11) 0.043(8) Uiso 0.317(6) 1 d PD A 2 C7' C -0.362(4) 0.320(2) 0.2519(17) 0.063(14) Uiso 0.317(6) 1 d PD A 2 H7'A H -0.4561 0.3226 0.2672 0.075 Uiso 0.317(6) 1 calc PR A 2 C8' C -0.314(3) 0.2312(19) 0.2406(11) 0.059(8) Uiso 0.317(6) 1 d PD A 2 H8'A H -0.3712 0.1700 0.2473 0.071 Uiso 0.317(6) 1 calc PR A 2 C9' C -0.174(3) 0.2229(18) 0.2176(10) 0.055(7) Uiso 0.317(6) 1 d PD A 2 H9'A H -0.1361 0.1552 0.2102 0.066 Uiso 0.317(6) 1 calc PR A 2 C10' C -0.095(3) 0.3088(18) 0.2059(16) 0.062(13) Uiso 0.317(6) 1 d PD A 2 C11' C -0.151(2) 0.4096(13) 0.2213(8) 0.032(5) Uiso 0.317(6) 1 d PD A 2 O2 O 0.2294(9) 0.2938(8) 0.1663(3) 0.056(2) Uani 0.683(6) 1 d PD A 1 N4 N 0.3461(12) 0.4842(9) 0.1593(4) 0.061(3) Uani 0.683(6) 1 d PD A 1 C12 C 0.397(2) 0.5785(12) 0.1567(7) 0.065(5) Uiso 0.683(6) 1 d PD A 1 H12A H 0.3341 0.6331 0.1679 0.079 Uiso 0.683(6) 1 calc PR A 1 C13 C 0.538(2) 0.6089(14) 0.1390(7) 0.090(6) Uiso 0.683(6) 1 d PD A 1 H13A H 0.5710 0.6799 0.1395 0.108 Uiso 0.683(6) 1 calc PR A 1 C14 C 0.626(2) 0.5257(14) 0.1203(7) 0.074(5) Uiso 0.683(6) 1 d PD A 1 H14A H 0.7190 0.5411 0.1055 0.089 Uiso 0.683(6) 1 calc PR A 1 C15 C 0.5760(14) 0.4190(10) 0.1238(5) 0.054(3) Uiso 0.683(6) 1 d PD A 1 C16 C 0.647(2) 0.3296(14) 0.1082(7) 0.082(5) Uiso 0.683(6) 1 d PD A 1 H16A H 0.7425 0.3376 0.0943 0.098 Uiso 0.683(6) 1 calc PR A 1 C17 C 0.594(2) 0.2378(14) 0.1110(7) 0.091(6) Uiso 0.683(6) 1 d PD A 1 H17A H 0.6506 0.1800 0.0995 0.110 Uiso 0.683(6) 1 calc PR A 1 C18 C 0.4506(17) 0.2204(12) 0.1311(6) 0.073(4) Uiso 0.683(6) 1 d PD A 1 H18A H 0.4133 0.1506 0.1330 0.088 Uiso 0.683(6) 1 calc PR A 1 C19 C 0.366(2) 0.2993(13) 0.1476(8) 0.066(6) Uiso 0.683(6) 1 d PD A 1 C20 C 0.4297(15) 0.4033(10) 0.1430(5) 0.060(4) Uiso 0.683(6) 1 d PD A 1 O2' O 0.2352(17) 0.5942(13) 0.1818(6) 0.046(5) Uiso 0.317(6) 1 d PD A 2 N4' N 0.347(2) 0.4108(13) 0.1550(10) 0.056(7) Uiso 0.317(6) 1 d PD A 2 C12' C 0.394(3) 0.3169(14) 0.1455(13) 0.039(8) Uiso 0.317(6) 1 d PD A 2 H12B H 0.3298 0.2591 0.1524 0.047 Uiso 0.317(6) 1 calc PR A 2 C13' C 0.535(3) 0.2965(18) 0.1254(11) 0.062(8) Uiso 0.317(6) 1 d PD A 2 H13B H 0.5688 0.2267 0.1201 0.075 Uiso 0.317(6) 1 calc PR A 2 C14' C 0.627(2) 0.3856(16) 0.1134(9) 0.038(6) Uiso 0.317(6) 1 d PD A 2 H14B H 0.7221 0.3765 0.0989 0.045 Uiso 0.317(6) 1 calc PR A 2 C15' C 0.571(2) 0.4888(14) 0.1242(9) 0.044(6) Uiso 0.317(6) 1 d PD A 2 C16' C 0.643(3) 0.5824(17) 0.1178(11) 0.059(8) Uiso 0.317(6) 1 d PD A 2 H16B H 0.7435 0.5802 0.1071 0.071 Uiso 0.317(6) 1 calc PR A 2 C17' C 0.587(2) 0.6707(17) 0.1246(9) 0.048(7) Uiso 0.317(6) 1 d PD A 2 H17B H 0.6383 0.7313 0.1137 0.058 Uiso 0.317(6) 1 calc PR A 2 C18' C 0.448(2) 0.6839(15) 0.1482(9) 0.047(6) Uiso 0.317(6) 1 d PD A 2 H18B H 0.4126 0.7526 0.1548 0.056 Uiso 0.317(6) 1 calc PR A 2 C19' C 0.367(2) 0.6002(15) 0.1612(9) 0.026(6) Uiso 0.317(6) 1 d PD A 2 C20' C 0.429(2) 0.4999(13) 0.1462(9) 0.044(6) Uiso 0.317(6) 1 d PD A 2 O5 O 0.0538(12) 0.1625(8) 0.1150(4) 0.102(3) Uani 1 1 d . . . H5 H 0.1389 0.1818 0.1059 0.153 Uiso 1 1 d R . . C23 C 0.055(2) 0.0621(12) 0.1331(6) 0.115(5) Uani 1 1 d . . . H23A H 0.1262 0.0580 0.1610 0.172 Uiso 1 1 calc R . . H23B H 0.0866 0.0131 0.1081 0.172 Uiso 1 1 calc R . . H23C H -0.0468 0.0434 0.1430 0.172 Uiso 1 1 calc R . . O6 O 0.8754(16) 0.2018(12) 0.0382(5) 0.152(5) Uiso 1 1 d D . . H6 H 0.7901 0.2145 0.0491 0.228 Uiso 1 1 d R . . C24 C 0.852(4) 0.104(2) 0.0121(11) 0.255(16) Uiso 1 1 d D . . H24A H 0.7629 0.0681 0.0240 0.382 Uiso 1 1 calc R . . H24B H 0.9414 0.0591 0.0170 0.382 Uiso 1 1 calc R . . H24C H 0.8362 0.1190 -0.0225 0.382 Uiso 1 1 calc R . . O7 O 0.097(2) 0.2250(14) -0.0791(6) 0.200 Uiso 1 1 d . . . H7 H 0.1670 0.2690 -0.0827 0.300 Uiso 1 1 d R . . C25 C -0.022(2) 0.2364(15) -0.1184(7) 0.129(6) Uiso 1 1 d . . . H25A H -0.0991 0.1821 -0.1149 0.194 Uiso 1 1 calc R . . H25B H 0.0244 0.2287 -0.1498 0.194 Uiso 1 1 calc R . . H25C H -0.0686 0.3060 -0.1164 0.194 Uiso 1 1 calc R . . O8 O 0.328(2) 0.3987(16) 0.3890(5) 0.204(8) Uani 1 1 d . . . H8 H 0.2872 0.4495 0.3742 0.306 Uiso 1 1 d R . . C26 C 0.479(4) 0.426(3) 0.3990(12) 0.232(14) Uiso 1 1 d . . . H26A H 0.4887 0.4990 0.4070 0.348 Uiso 1 1 d R . . H26B H 0.5233 0.4173 0.3683 0.348 Uiso 1 1 d R . . H26C H 0.5241 0.3803 0.4231 0.348 Uiso 1 1 d 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 Ru 0.0345(4) 0.0782(6) 0.0362(4) 0.0050(3) -0.0006(3) -0.0066(4) Co 0.0412(9) 0.1090(17) 0.0361(9) 0.0102(10) -0.0035(7) -0.0104(10) N1 0.048(4) 0.102(7) 0.046(5) 0.013(4) -0.002(4) -0.011(4) N2 0.057(5) 0.073(6) 0.044(4) 0.004(4) -0.003(4) -0.007(4) C1 0.038(5) 0.089(8) 0.040(5) 0.008(5) 0.002(4) -0.004(5) C2 0.034(4) 0.062(6) 0.043(5) 0.003(4) 0.005(4) -0.001(4) O1 0.050(5) 0.038(5) 0.068(6) 0.008(4) -0.006(4) 0.001(4) N3 0.040(6) 0.067(8) 0.036(5) -0.003(5) -0.003(4) -0.001(5) O2 0.042(5) 0.074(7) 0.051(5) -0.005(5) 0.005(4) 0.001(4) N4 0.054(7) 0.093(11) 0.035(6) 0.000(6) -0.006(5) -0.030(7) O5 0.117(8) 0.087(7) 0.100(7) -0.005(5) -0.004(5) -0.007(6) C23 0.137(14) 0.082(10) 0.123(13) -0.025(9) -0.023(11) -0.008(10) O8 0.219(17) 0.28(2) 0.109(10) 0.079(12) -0.020(10) -0.076(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 Ru O1' 1.848(17) . ? Ru O1 1.948(9) . ? Ru N4 2.053(10) . ? Ru N4' 2.054(19) . ? Ru C1 2.065(9) . ? Ru O2 2.070(9) . ? Ru C2 2.073(9) . ? Ru N3 2.108(10) . ? Ru O2' 2.152(16) . ? Ru N3' 2.165(16) . ? Co O3' 2.02(3) 3_565 ? Co O3' 2.02(3) . ? Co O4 2.061(11) . ? Co O4 2.061(11) 3_565 ? Co N1 2.065(8) 3_565 ? Co N1 2.065(8) . ? Co O3 2.168(13) 3_565 ? Co O3 2.168(13) . ? Co O4' 2.24(3) 3_565 ? Co O4' 2.24(3) . ? N1 C1 1.142(12) . ? N2 C2 1.136(11) . ? O3 C21 1.450(15) . ? O4 C22 1.428(15) . ? O3' C21' 1.470(19) . ? O4' C22' 1.458(19) . ? O1 C10 1.331(15) . ? N3 C3 1.291(16) . ? N3 C11 1.354(13) . ? C3 C4 1.412(18) . ? C4 C5 1.442(18) . ? C5 C6 1.44(2) . ? C6 C7 1.365(18) . ? C6 C11 1.429(13) . ? C7 C8 1.258(18) . ? C8 C9 1.411(18) . ? C9 C10 1.348(18) . ? C10 C11 1.446(16) . ? O1' C10' 1.329(19) . ? N3' C3' 1.292(19) . ? N3' C11' 1.358(16) . ? C3' C4' 1.40(2) . ? C4' C5' 1.45(2) . ? C5' C6' 1.44(2) . ? C6' C7' 1.36(2) . ? C6' C11' 1.428(16) . ? C7' C8' 1.25(2) . ? C8' C9' 1.41(2) . ? C9' C10' 1.35(2) . ? C10' C11' 1.445(19) . ? O2 C19 1.334(16) . ? N4 C12 1.285(16) . ? N4 C20 1.355(14) . ? C12 C13 1.404(19) . ? C13 C14 1.426(19) . ? C14 C15 1.433(19) . ? C15 C16 1.374(18) . ? C15 C20 1.430(15) . ? C16 C17 1.259(19) . ? C17 C18 1.422(18) . ? C18 C19 1.340(18) . ? C19 C20 1.445(17) . ? O2' C19' 1.322(18) . ? N4' C12' 1.294(18) . ? N4' C20' 1.372(16) . ? C12' C13' 1.42(2) . ? C13' C14' 1.44(2) . ? C14' C15' 1.44(2) . ? C15' C16' 1.36(2) . ? C15' C20' 1.428(17) . ? C16' C17' 1.24(2) . ? C17' C18' 1.42(2) . ? C18' C19' 1.34(2) . ? C19' C20' 1.454(19) . ? O5 C23 1.371(17) . ? O6 C24 1.449(17) . ? O7 C25 1.49(2) . ? O8 C26 1.40(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Ru O1 124.3(5) . . ? O1' Ru N4 133.6(6) . . ? O1 Ru N4 101.7(4) . . ? O1' Ru N4' 107.1(6) . . ? O1 Ru N4' 128.1(5) . . ? N4 Ru N4' 26.5(6) . . ? O1' Ru C1 89.8(6) . . ? O1 Ru C1 88.1(4) . . ? N4 Ru C1 85.7(4) . . ? N4' Ru C1 85.3(8) . . ? O1' Ru O2 54.0(5) . . ? O1 Ru O2 176.9(4) . . ? N4 Ru O2 79.7(4) . . ? N4' Ru O2 53.2(5) . . ? C1 Ru O2 89.2(4) . . ? O1' Ru C2 92.1(6) . . ? O1 Ru C2 91.4(4) . . ? N4 Ru C2 92.4(4) . . ? N4' Ru C2 93.5(8) . . ? C1 Ru C2 177.9(4) . . ? O2 Ru C2 91.3(4) . . ? O1' Ru N3 42.3(5) . . ? O1 Ru N3 82.5(4) . . ? N4 Ru N3 175.8(4) . . ? N4' Ru N3 149.3(6) . . ? C1 Ru N3 94.4(4) . . ? O2 Ru N3 96.1(4) . . ? C2 Ru N3 87.5(3) . . ? O1' Ru O2' 174.8(5) . . ? O1 Ru O2' 50.5(5) . . ? N4 Ru O2' 51.5(5) . . ? N4' Ru O2' 78.1(6) . . ? C1 Ru O2' 90.1(6) . . ? O2 Ru O2' 131.1(5) . . ? C2 Ru O2' 88.1(5) . . ? N3 Ru O2' 132.6(5) . . ? O1' Ru N3' 83.0(6) . . ? O1 Ru N3' 41.7(5) . . ? N4 Ru N3' 143.3(6) . . ? N4' Ru N3' 169.8(6) . . ? C1 Ru N3' 93.5(6) . . ? O2 Ru N3' 137.0(5) . . ? C2 Ru N3' 87.4(6) . . ? N3 Ru N3' 40.8(5) . . ? O2' Ru N3' 91.8(6) . . ? O3' Co O3' 180.0(14) 3_565 . ? O3' Co O4 75.5(9) 3_565 . ? O3' Co O4 104.5(9) . . ? O3' Co O4 104.5(9) 3_565 3_565 ? O3' Co O4 75.5(9) . 3_565 ? O4 Co O4 180.000(1) . 3_565 ? O3' Co N1 89.0(8) 3_565 3_565 ? O3' Co N1 91.0(8) . 3_565 ? O4 Co N1 92.1(4) . 3_565 ? O4 Co N1 87.9(4) 3_565 3_565 ? O3' Co N1 91.0(8) 3_565 . ? O3' Co N1 89.0(8) . . ? O4 Co N1 87.9(4) . . ? O4 Co N1 92.1(4) 3_565 . ? N1 Co N1 180.00(11) 3_565 . ? O3' Co O3 18.4(8) 3_565 3_565 ? O3' Co O3 161.6(8) . 3_565 ? O4 Co O3 93.9(5) . 3_565 ? O4 Co O3 86.1(5) 3_565 3_565 ? N1 Co O3 89.1(4) 3_565 3_565 ? N1 Co O3 90.9(4) . 3_565 ? O3' Co O3 161.6(8) 3_565 . ? O3' Co O3 18.4(7) . . ? O4 Co O3 86.1(5) . . ? O4 Co O3 93.9(5) 3_565 . ? N1 Co O3 90.9(4) 3_565 . ? N1 Co O3 89.1(4) . . ? O3 Co O3 180.0(6) 3_565 . ? O3' Co O4' 85.3(12) 3_565 3_565 ? O3' Co O4' 94.7(12) . 3_565 ? O4 Co O4' 159.7(8) . 3_565 ? O4 Co O4' 20.3(8) 3_565 3_565 ? N1 Co O4' 94.0(9) 3_565 3_565 ? N1 Co O4' 86.0(9) . 3_565 ? O3 Co O4' 66.9(9) 3_565 3_565 ? O3 Co O4' 113.1(9) . 3_565 ? O3' Co O4' 94.7(12) 3_565 . ? O3' Co O4' 85.3(12) . . ? O4 Co O4' 20.3(8) . . ? O4 Co O4' 159.7(8) 3_565 . ? N1 Co O4' 86.0(9) 3_565 . ? N1 Co O4' 94.0(9) . . ? O3 Co O4' 113.1(9) 3_565 . ? O3 Co O4' 66.9(9) . . ? O4' Co O4' 180.0(17) 3_565 . ? C1 N1 Co 173.0(9) . . ? N1 C1 Ru 173.7(8) . . ? N2 C2 Ru 176.5(9) . . ? C21 O3 Co 125.5(11) . . ? C22 O4 Co 129.5(11) . . ? C21' O3' Co 111(3) . . ? C22' O4' Co 118(3) . . ? C10 O1 Ru 113.5(8) . . ? C3 N3 C11 119.7(10) . . ? C3 N3 Ru 131.0(9) . . ? C11 N3 Ru 109.2(7) . . ? N3 C3 C4 123.0(12) . . ? C3 C4 C5 119.4(13) . . ? C6 C5 C4 117.6(13) . . ? C7 C6 C11 117.6(11) . . ? C7 C6 C5 126.4(10) . . ? C11 C6 C5 116.0(10) . . ? C8 C7 C6 123.6(16) . . ? C7 C8 C9 120.9(16) . . ? C10 C9 C8 122.6(14) . . ? O1 C10 C9 125.7(13) . . ? O1 C10 C11 118.9(12) . . ? C9 C10 C11 115.4(11) . . ? N3 C11 C6 124.4(10) . . ? N3 C11 C10 115.6(10) . . ? C6 C11 C10 120.0(10) . . ? C10' O1' Ru 118.0(13) . . ? C3' N3' C11' 122.3(15) . . ? C3' N3' Ru 132.9(14) . . ? C11' N3' Ru 104.5(10) . . ? N3' C3' C4' 122.4(18) . . ? C3' C4' C5' 117.9(19) . . ? C6' C5' C4' 119.2(19) . . ? C7' C6' C11' 115.9(15) . . ? C7' C6' C5' 128.0(16) . . ? C11' C6' C5' 116.1(15) . . ? C8' C7' C6' 127(2) . . ? C7' C8' C9' 119(2) . . ? C10' C9' C8' 121.4(19) . . ? O1' C10' C9' 126.8(19) . . ? O1' C10' C11' 115.2(17) . . ? C9' C10' C11' 117.4(17) . . ? N3' C11' C6' 121.9(14) . . ? N3' C11' C10' 118.9(15) . . ? C6' C11' C10' 119.2(14) . . ? C19 O2 Ru 113.9(9) . . ? C12 N4 C20 119.5(12) . . ? C12 N4 Ru 127.0(11) . . ? C20 N4 Ru 113.5(8) . . ? N4 C12 C13 126.4(16) . . ? C12 C13 C14 115.3(16) . . ? C13 C14 C15 120.1(14) . . ? C16 C15 C20 115.4(11) . . ? C16 C15 C14 128.1(12) . . ? C20 C15 C14 116.4(11) . . ? C17 C16 C15 125.2(16) . . ? C16 C17 C18 120.2(17) . . ? C19 C18 C17 122.3(15) . . ? O2 C19 C18 128.1(14) . . ? O2 C19 C20 116.3(12) . . ? C18 C19 C20 115.6(13) . . ? N4 C20 C15 122.0(11) . . ? N4 C20 C19 116.6(11) . . ? C15 C20 C19 121.4(11) . . ? C19' O2' Ru 114.7(12) . . ? C12' N4' C20' 123.5(15) . . ? C12' N4' Ru 122.3(14) . . ? C20' N4' Ru 114.2(11) . . ? N4' C12' C13' 122.9(17) . . ? C12' C13' C14' 117.5(18) . . ? C15' C14' C13' 118.0(16) . . ? C16' C15' C20' 112.9(15) . . ? C16' C15' C14' 127.4(16) . . ? C20' C15' C14' 119.7(14) . . ? C17' C16' C15' 126(2) . . ? C16' C17' C18' 122(2) . . ? C19' C18' C17' 120.6(18) . . ? O2' C19' C18' 130.7(17) . . ? O2' C19' C20' 114.7(15) . . ? C18' C19' C20' 114.3(15) . . ? N4' C20' C15' 118.3(13) . . ? N4' C20' C19' 118.0(14) . . ? C15' C20' C19' 123.6(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.024 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.218 data_3 _database_code_depnum_ccdc_archive 'CCDC 821918' #TrackingRef '- CIF 1-3.cif' _audit_creation_date 2011-02-25 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C13 H13 Cl0.5 Co0.5 N3 O2 Ru0.5)' _chemical_formula_sum 'C26 H26 Cl Co N6 O4 Ru' _chemical_formula_weight 681.98 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4733(3) _cell_length_b 10.41624(18) _cell_length_c 17.8260(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.0942(15) _cell_angle_gamma 90.00 _cell_volume 2683.48(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7330 _cell_measurement_temperature 133.15 _cell_measurement_theta_max 71.5548 _cell_measurement_theta_min 4.9792 _exptl_absorpt_coefficient_mu 10.695 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.30473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) (compiled Aug 27 2009,17:19:36) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour violet _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rect. Prism' _exptl_crystal_F_000 1376 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_unetI/netI 0.0203 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 8064 _diffrn_reflns_theta_full 66.98 _diffrn_reflns_theta_max 66.98 _diffrn_reflns_theta_min 4.97 _diffrn_ambient_temperature 133.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2282 _reflns_number_total 2408 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.539 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.100 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 2408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0364 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+11.9175P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.0960 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.5000 0.5000 0.5000 0.01905(14) Uani 1 2 d S . . Co1 Co 0.5000 0.76616(7) 0.2500 0.01925(19) Uani 1 2 d S . . Cl1 Cl 0.5000 0.98602(12) 0.2500 0.0454(4) Uani 1 2 d S . . O1 O 0.38333(18) 0.4080(3) 0.46566(15) 0.0332(6) Uani 1 1 d . . . O2 O 0.35565(17) 0.7526(2) 0.22836(15) 0.0284(6) Uani 1 1 d . . . N1 N 0.4925(2) 0.6693(3) 0.34905(16) 0.0232(6) Uani 1 1 d . . . N2 N 0.4049(2) 0.6189(3) 0.54852(18) 0.0327(7) Uani 1 1 d . . . N3 N 0.2098(2) 0.8274(3) 0.21208(18) 0.0277(7) Uani 1 1 d . . . C1 C 0.4948(2) 0.6102(3) 0.4024(2) 0.0235(7) Uani 1 1 d . . . C2 C 0.4186(3) 0.7235(4) 0.5856(2) 0.0328(9) Uani 1 1 d . . . H2 H 0.4800 0.7551 0.5922 0.039 Uiso 1 1 calc R . . C3 C 0.3467(3) 0.7942(4) 0.6170(2) 0.0386(10) Uani 1 1 d . . . H3 H 0.3602 0.8715 0.6438 0.046 Uiso 1 1 calc R . . C4 C 0.2559(3) 0.7495(4) 0.6085(2) 0.0392(10) Uani 1 1 d . . . H4 H 0.2064 0.7954 0.6288 0.047 Uiso 1 1 calc R . . C5 C 0.2398(3) 0.6319(4) 0.5681(2) 0.0326(9) Uani 1 1 d . . . C6 C 0.1528(3) 0.5743(5) 0.5551(2) 0.0416(10) Uani 1 1 d . . . H6 H 0.1000 0.6103 0.5765 0.050 Uiso 1 1 calc R . . C7 C 0.1440(3) 0.4677(5) 0.5122(3) 0.0443(11) Uani 1 1 d . . . H7 H 0.0842 0.4316 0.5031 0.053 Uiso 1 1 calc R . . C8 C 0.2189(3) 0.4087(4) 0.4807(2) 0.0368(9) Uani 1 1 d . . . H8 H 0.2091 0.3345 0.4503 0.044 Uiso 1 1 calc R . . C9 C 0.3064(3) 0.4563(4) 0.4931(2) 0.0302(8) Uani 1 1 d . . . C10 C 0.3180(3) 0.5727(4) 0.5386(2) 0.0309(8) Uani 1 1 d . . . C11 C 0.2976(2) 0.8389(4) 0.2341(2) 0.0260(8) Uani 1 1 d . . . H11 H 0.3177 0.9181 0.2556 0.031 Uiso 1 1 calc R . . C12 C 0.1429(3) 0.9284(4) 0.2250(3) 0.0404(10) Uani 1 1 d . . . H12A H 0.1023 0.9012 0.2643 0.061 Uiso 1 1 calc R . . H12B H 0.1058 0.9452 0.1785 0.061 Uiso 1 1 calc R . . H12C H 0.1757 1.0069 0.2411 0.061 Uiso 1 1 calc R . . C13 C 0.1748(3) 0.7099(4) 0.1770(2) 0.0357(9) Uani 1 1 d . . . H13A H 0.2264 0.6513 0.1694 0.054 Uiso 1 1 calc R . . H13B H 0.1432 0.7302 0.1285 0.054 Uiso 1 1 calc R . . H13C H 0.1310 0.6689 0.2097 0.054 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 0.0181(2) 0.0219(2) 0.0173(2) 0.00097(13) 0.00153(13) 0.00217(13) Co1 0.0223(4) 0.0193(4) 0.0162(4) 0.000 0.0018(3) 0.000 Cl1 0.0250(7) 0.0218(6) 0.0897(12) 0.000 0.0051(7) 0.000 O1 0.0279(14) 0.0354(15) 0.0362(15) -0.0012(12) 0.0006(11) 0.0017(11) O2 0.0229(13) 0.0285(13) 0.0334(14) 0.0000(11) -0.0012(11) -0.0001(11) N1 0.0239(15) 0.0277(16) 0.0178(14) 0.0032(12) 0.0002(11) -0.0015(12) N2 0.0336(18) 0.0350(18) 0.0294(17) 0.0051(14) 0.0016(14) 0.0056(14) N3 0.0251(15) 0.0271(16) 0.0304(16) 0.0040(13) -0.0028(12) 0.0007(12) C1 0.0190(16) 0.0283(19) 0.0231(18) -0.0042(15) -0.0010(13) 0.0002(13) C2 0.037(2) 0.036(2) 0.0260(19) 0.0034(16) 0.0017(16) 0.0077(17) C3 0.055(3) 0.034(2) 0.027(2) 0.0016(17) 0.0012(18) 0.0040(19) C4 0.045(2) 0.048(3) 0.0250(19) 0.0094(18) 0.0097(17) 0.017(2) C5 0.030(2) 0.043(2) 0.0257(19) 0.0090(17) 0.0086(15) 0.0130(17) C6 0.037(2) 0.049(3) 0.040(2) 0.013(2) 0.0069(18) 0.007(2) C7 0.034(2) 0.047(3) 0.052(3) 0.014(2) 0.005(2) 0.004(2) C8 0.032(2) 0.037(2) 0.041(2) 0.0088(18) -0.0027(17) -0.0037(17) C9 0.0288(19) 0.035(2) 0.0268(19) 0.0117(16) 0.0047(15) 0.0114(16) C10 0.029(2) 0.037(2) 0.0265(19) 0.0113(16) 0.0035(15) 0.0084(16) C11 0.0271(18) 0.0265(19) 0.0243(18) 0.0010(14) 0.0006(14) 0.0005(15) C12 0.031(2) 0.041(2) 0.048(3) 0.003(2) -0.0047(18) 0.0116(18) C13 0.031(2) 0.034(2) 0.041(2) 0.0018(18) -0.0113(17) -0.0033(17) _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 O1 2.008(3) . ? Ru1 O1 2.008(3) 5_666 ? Ru1 N2 2.075(3) 5_666 ? Ru1 N2 2.075(3) . ? Ru1 C1 2.082(4) . ? Ru1 C1 2.082(4) 5_666 ? Co1 Cl1 2.2901(15) . ? Co1 O2 2.109(2) 2_655 ? Co1 O2 2.109(2) . ? Co1 N1 2.041(3) 2_655 ? Co1 N1 2.041(3) . ? O1 C9 1.339(5) . ? O2 C11 1.238(4) . ? N1 C1 1.133(5) . ? N2 C2 1.284(5) . ? N2 C10 1.349(5) . ? N3 C11 1.315(5) . ? N3 C12 1.457(5) . ? N3 C13 1.453(5) . ? C2 H2 0.9500 . ? C2 C3 1.415(6) . ? C3 H3 0.9500 . ? C3 C4 1.395(7) . ? C4 H4 0.9500 . ? C4 C5 1.433(6) . ? C5 C6 1.402(6) . ? C5 C10 1.416(5) . ? C6 H6 0.9500 . ? C6 C7 1.350(7) . ? C7 H7 0.9500 . ? C7 C8 1.390(6) . ? C8 H8 0.9500 . ? C8 C9 1.367(6) . ? C9 C10 1.463(6) . ? C11 H11 0.9500 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 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 O1 Ru1 O1 180.00(8) 5_666 . ? O1 Ru1 N2 81.14(12) 5_666 5_666 ? O1 Ru1 N2 98.86(12) . 5_666 ? O1 Ru1 N2 98.86(12) 5_666 . ? O1 Ru1 N2 81.14(12) . . ? O1 Ru1 C1 89.04(12) 5_666 . ? O1 Ru1 C1 89.04(12) . 5_666 ? O1 Ru1 C1 90.96(12) . . ? O1 Ru1 C1 90.96(12) 5_666 5_666 ? N2 Ru1 N2 180.00(16) . 5_666 ? N2 Ru1 C1 88.60(13) 5_666 . ? N2 Ru1 C1 91.40(13) . . ? N2 Ru1 C1 88.60(13) . 5_666 ? N2 Ru1 C1 91.40(13) 5_666 5_666 ? C1 Ru1 C1 180.000(1) 5_666 . ? O2 Co1 Cl1 93.84(7) . . ? O2 Co1 Cl1 93.84(7) 2_655 . ? O2 Co1 O2 172.32(15) . 2_655 ? N1 Co1 Cl1 119.61(9) . . ? N1 Co1 Cl1 119.61(9) 2_655 . ? N1 Co1 O2 84.67(11) 2_655 . ? N1 Co1 O2 91.53(11) . . ? N1 Co1 O2 91.53(11) 2_655 2_655 ? N1 Co1 O2 84.67(11) . 2_655 ? N1 Co1 N1 120.77(17) . 2_655 ? C9 O1 Ru1 114.3(3) . . ? C11 O2 Co1 127.3(2) . . ? C1 N1 Co1 174.2(3) . . ? C2 N2 Ru1 129.3(3) . . ? C2 N2 C10 119.2(4) . . ? C10 N2 Ru1 111.5(3) . . ? C11 N3 C12 121.8(3) . . ? C11 N3 C13 120.9(3) . . ? C13 N3 C12 117.2(3) . . ? N1 C1 Ru1 179.4(3) . . ? N2 C2 H2 118.3 . . ? N2 C2 C3 123.3(4) . . ? C3 C2 H2 118.3 . . ? C2 C3 H3 120.3 . . ? C4 C3 C2 119.4(4) . . ? C4 C3 H3 120.3 . . ? C3 C4 H4 121.1 . . ? C3 C4 C5 117.9(4) . . ? C5 C4 H4 121.1 . . ? C6 C5 C4 124.7(4) . . ? C6 C5 C10 118.8(4) . . ? C10 C5 C4 116.6(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 C5 120.1(4) . . ? C7 C6 H6 120.0 . . ? C6 C7 H7 118.6 . . ? C6 C7 C8 122.8(4) . . ? C8 C7 H7 118.6 . . ? C7 C8 H8 119.7 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? O1 C9 C8 125.9(4) . . ? O1 C9 C10 116.2(3) . . ? C8 C9 C10 117.9(4) . . ? N2 C10 C5 123.7(4) . . ? N2 C10 C9 116.6(3) . . ? C5 C10 C9 119.8(4) . . ? O2 C11 N3 124.0(3) . . ? O2 C11 H11 118.0 . . ? N3 C11 H11 118.0 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ?