# Electronic Supplementary Material (ESI) for Green Chemistry # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Green Chemistry' _journal_coden_cambridge 1048 _publ_contact_author_name 'Professor Jimenez-Aparicio' _publ_contact_author_address ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; _publ_contact_author_email reyesja@quim.ucm.es _publ_contact_author_phone '+34 91 3944334' _publ_contact_author_fax ;+34 91 3944352 ; loop_ _publ_author_name _publ_author_address R.Jimenez-Aparicio ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; S.Herrero ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; J.Perles ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; J.L.Priego ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; S.Saguar ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; ; F.Urbanos ; ;Facultad de CC. Quimicas Universidad Complutense de Madrid Madrid Spain ; data_jru20 _database_code_depnum_ccdc_archive 'CCDC 814431' #TrackingRef '4376_web_deposit_cif_file_0_JosefinaPerles_1298468827.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 N12 O Ru2' _chemical_formula_sum 'C52 H48 N12 O Ru2' _chemical_formula_weight 1059.16 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' Ru Ru -1.2594 0.8363 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.7033(13) _cell_length_b 25.8907(18) _cell_length_c 9.8896(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4789.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8699 _exptl_absorpt_correction_T_max 0.9474 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45141 _diffrn_reflns_av_R_equivalents 0.1485 _diffrn_reflns_av_sigmaI/netI 0.1768 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 29.12 _reflns_number_total 11341 _reflns_number_gt 4788 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0004(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(7) _refine_ls_number_reflns 11341 _refine_ls_number_parameters 509 _refine_ls_number_restraints 385 _refine_ls_R_factor_all 0.2126 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2572 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.123 _refine_ls_shift/su_mean 0.006 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 C1 C 0.2984(6) 0.1710(4) 0.3289(9) 0.074(4) Uani 1 1 d GU . . C2 C 0.2716(5) 0.1641(4) 0.4589(11) 0.083(4) Uani 1 1 d GU . . H2 H 0.2347 0.1408 0.4742 0.100 Uiso 1 1 calc R . . C3 C 0.3001(6) 0.1922(4) 0.5659(9) 0.099(5) Uani 1 1 d GU . . H3 H 0.2822 0.1877 0.6528 0.119 Uiso 1 1 calc R . . C4 C 0.3552(6) 0.2271(4) 0.5430(10) 0.107(5) Uani 1 1 d GU . . H4 H 0.3742 0.2459 0.6146 0.128 Uiso 1 1 calc R . . C5 C 0.3819(6) 0.2340(5) 0.4131(12) 0.164(8) Uani 1 1 d GU . . H5 H 0.4188 0.2573 0.3977 0.196 Uiso 1 1 calc R . . C6 C 0.3535(7) 0.2059(5) 0.3060(9) 0.152(8) Uani 1 1 d GU . . H6 H 0.3714 0.2104 0.2191 0.182 Uiso 1 1 calc R . . C7 C 0.1187(4) 0.0728(3) 0.1751(10) 0.068(3) Uani 1 1 d GU . . C8 C 0.0741(5) 0.0985(3) 0.2651(11) 0.086(4) Uani 1 1 d GU . . H8 H 0.0896 0.1287 0.3068 0.103 Uiso 1 1 calc R . . C9 C 0.0063(4) 0.0792(4) 0.2927(10) 0.102(5) Uani 1 1 d GU . . H9 H -0.0235 0.0964 0.3529 0.122 Uiso 1 1 calc R . . C10 C -0.0168(4) 0.0340(4) 0.2304(11) 0.103(5) Uani 1 1 d GU . . H10 H -0.0622 0.0211 0.2489 0.124 Uiso 1 1 calc R . . C11 C 0.0278(5) 0.0083(3) 0.1404(11) 0.089(4) Uani 1 1 d GU . . H11 H 0.0123 -0.0219 0.0987 0.107 Uiso 1 1 calc R . . C12 C 0.0955(4) 0.0276(3) 0.1128(10) 0.079(4) Uani 1 1 d GU . . H12 H 0.1254 0.0104 0.0526 0.095 Uiso 1 1 calc R . . C13 C 0.4275(6) 0.0587(4) 0.2194(13) 0.086(4) Uani 1 1 d GU . . C14 C 0.4601(7) 0.0122(3) 0.2527(16) 0.145(7) Uani 1 1 d GU . . H14 H 0.4430 -0.0186 0.2163 0.174 Uiso 1 1 calc R . . C15 C 0.5181(8) 0.0116(4) 0.3404(17) 0.156(8) Uani 1 1 d GU . . H15 H 0.5399 -0.0195 0.3627 0.187 Uiso 1 1 calc R . . C16 C 0.5436(7) 0.0575(5) 0.3948(15) 0.148(8) Uani 1 1 d GU . . H16 H 0.5825 0.0572 0.4535 0.178 Uiso 1 1 calc R . . C17 C 0.5110(8) 0.1041(4) 0.3615(17) 0.156(8) Uani 1 1 d GU . . H17 H 0.5281 0.1348 0.3979 0.188 Uiso 1 1 calc R . . C18 C 0.4529(7) 0.1047(3) 0.2738(16) 0.160(8) Uani 1 1 d GU . . H18 H 0.4311 0.1358 0.2515 0.192 Uiso 1 1 calc R . . C19 C 0.2561(5) -0.0343(2) 0.0112(9) 0.059(3) Uani 1 1 d GU . . C20 C 0.2607(5) -0.0709(3) 0.1135(8) 0.084(4) Uani 1 1 d GU . . H20 H 0.2839 -0.0629 0.1941 0.101 Uiso 1 1 calc R . . C21 C 0.2308(6) -0.1196(3) 0.0954(11) 0.102(5) Uani 1 1 d GU . . H21 H 0.2340 -0.1441 0.1639 0.122 Uiso 1 1 calc R . . C22 C 0.1963(6) -0.1316(3) -0.0250(12) 0.102(5) Uani 1 1 d GU . . H22 H 0.1763 -0.1642 -0.0371 0.123 Uiso 1 1 calc R . . C23 C 0.1916(5) -0.0950(4) -0.1273(9) 0.094(4) Uani 1 1 d GU . . H23 H 0.1685 -0.1030 -0.2078 0.113 Uiso 1 1 calc R . . C24 C 0.2215(5) -0.0463(3) -0.1092(8) 0.083(4) Uani 1 1 d GU . . H24 H 0.2184 -0.0218 -0.1777 0.099 Uiso 1 1 calc R . . C25 C 0.4588(5) 0.1265(5) -0.1530(13) 0.097(5) Uani 1 1 d GU . . C26 C 0.4828(7) 0.1408(7) -0.2806(12) 0.169(8) Uani 1 1 d GU . . H26 H 0.4510 0.1418 -0.3529 0.203 Uiso 1 1 calc R . . C27 C 0.5542(8) 0.1535(7) -0.3001(13) 0.191(9) Uani 1 1 d GU . . H27 H 0.5703 0.1631 -0.3855 0.230 Uiso 1 1 calc R . . C28 C 0.6017(5) 0.1519(7) -0.1920(17) 0.171(8) Uani 1 1 d GU . . H28 H 0.6495 0.1604 -0.2051 0.205 Uiso 1 1 calc R . . C29 C 0.5777(6) 0.1376(6) -0.0644(15) 0.154(7) Uani 1 1 d GU . . H29 H 0.6094 0.1365 0.0080 0.185 Uiso 1 1 calc R . . C30 C 0.5062(6) 0.1249(5) -0.0449(11) 0.131(6) Uani 1 1 d GU . . H30 H 0.4901 0.1153 0.0405 0.157 Uiso 1 1 calc R . . C31 C 0.2670(5) 0.0488(4) -0.3379(8) 0.064(3) Uani 1 1 d GU . . C32 C 0.3135(4) 0.0196(4) -0.4163(11) 0.108(6) Uani 1 1 d GU . . H32 H 0.3619 0.0186 -0.3954 0.130 Uiso 1 1 calc R . . C33 C 0.2875(5) -0.0083(5) -0.5259(11) 0.134(7) Uani 1 1 d GU . . H33 H 0.3186 -0.0279 -0.5784 0.161 Uiso 1 1 calc R . . C34 C 0.2151(5) -0.0069(4) -0.5572(10) 0.102(5) Uani 1 1 d GU . . H34 H 0.1977 -0.0256 -0.6305 0.122 Uiso 1 1 calc R . . C35 C 0.1686(4) 0.0223(4) -0.4788(10) 0.083(4) Uani 1 1 d GU . . H35 H 0.1201 0.0233 -0.4996 0.100 Uiso 1 1 calc R . . C36 C 0.1945(4) 0.0502(3) -0.3691(9) 0.065(3) Uani 1 1 d GU . . H36 H 0.1634 0.0698 -0.3167 0.078 Uiso 1 1 calc R . . C37 C 0.3202(5) 0.2430(3) -0.0383(14) 0.085(4) Uani 1 1 d GU . . C38 C 0.2772(5) 0.2868(4) -0.0374(18) 0.122(5) Uani 1 1 d GU . . H38 H 0.2280 0.2836 -0.0476 0.147 Uiso 1 1 calc R . . C39 C 0.3078(7) 0.3353(3) -0.0214(19) 0.145(7) Uani 1 1 d GU . . H39 H 0.2790 0.3646 -0.0208 0.174 Uiso 1 1 calc R . . C40 C 0.3814(7) 0.3401(3) -0.0062(19) 0.161(8) Uani 1 1 d GU . . H40 H 0.4019 0.3726 0.0045 0.194 Uiso 1 1 calc R . . C41 C 0.4244(5) 0.2963(5) -0.007(2) 0.167(8) Uani 1 1 d GU . . H41 H 0.4736 0.2995 0.0031 0.200 Uiso 1 1 calc R . . C42 C 0.3938(5) 0.2478(4) -0.0231(18) 0.139(7) Uani 1 1 d GU . . H42 H 0.4226 0.2185 -0.0237 0.166 Uiso 1 1 calc R . . C43 C 0.1275(4) 0.1541(4) -0.1779(9) 0.059(3) Uani 1 1 d GU . . C44 C 0.1178(6) 0.1907(4) -0.2792(12) 0.113(6) Uani 1 1 d GU . . H44 H 0.1534 0.2147 -0.2972 0.136 Uiso 1 1 calc R . . C45 C 0.0547(7) 0.1913(5) -0.3535(11) 0.143(7) Uani 1 1 d GU . . H45 H 0.0482 0.2157 -0.4213 0.171 Uiso 1 1 calc R . . C46 C 0.0013(5) 0.1553(5) -0.3265(11) 0.117(6) Uani 1 1 d GU . . H46 H -0.0409 0.1557 -0.3762 0.140 Uiso 1 1 calc R . . C47 C 0.0111(4) 0.1188(4) -0.2252(12) 0.091(4) Uani 1 1 d GU . . H47 H -0.0246 0.0947 -0.2071 0.110 Uiso 1 1 calc R . . C48 C 0.0742(5) 0.1182(3) -0.1509(9) 0.078(4) Uani 1 1 d GU . . H48 H 0.0807 0.0937 -0.0831 0.094 Uiso 1 1 calc R . . C50 C 0.5788(19) 0.2299(13) 0.375(3) 0.150(11) Uani 1 1 d . . . H50A H 0.5731 0.2599 0.4323 0.180 Uiso 1 1 calc R . . H50B H 0.5490 0.2029 0.4128 0.180 Uiso 1 1 calc R . . C51 C 0.6492(18) 0.2137(15) 0.389(3) 0.190(14) Uani 1 1 d . . . H51A H 0.6784 0.2376 0.4402 0.228 Uiso 1 1 calc R . . H51B H 0.6533 0.1790 0.4252 0.228 Uiso 1 1 calc R . . C52 C 0.662(2) 0.216(2) 0.257(5) 0.28(3) Uani 1 1 d . . . H52A H 0.6591 0.1807 0.2234 0.335 Uiso 1 1 calc R . . H52B H 0.7107 0.2270 0.2459 0.335 Uiso 1 1 calc R . . C53 C 0.618(3) 0.2478(12) 0.164(4) 0.25(3) Uani 1 1 d . . . H53A H 0.6347 0.2832 0.1578 0.300 Uiso 1 1 calc R . . H53B H 0.6137 0.2329 0.0743 0.300 Uiso 1 1 calc R . . N1 N 0.2774(6) 0.1407(4) 0.2143(11) 0.063(3) Uani 1 1 d . . . N2 N 0.2145(5) 0.1205(4) 0.2380(11) 0.058(3) Uani 1 1 d . . . N3 N 0.1880(5) 0.0924(4) 0.1395(11) 0.057(3) Uani 1 1 d . . . N4 N 0.3695(5) 0.0624(4) 0.1241(12) 0.059(3) Uani 1 1 d . . . N5 N 0.3406(5) 0.0169(4) 0.1051(11) 0.061(3) Uani 1 1 d . . . N6 N 0.2827(5) 0.0175(3) 0.0258(11) 0.057(3) Uani 1 1 d . . . N7 N 0.3858(5) 0.1142(4) -0.1285(12) 0.064(3) Uani 1 1 d . . . N8 N 0.3566(6) 0.0902(4) -0.2360(12) 0.064(3) Uani 1 1 d . . . N9 N 0.2920(6) 0.0759(4) -0.2170(12) 0.063(3) Uani 1 1 d . . . N10 N 0.2896(5) 0.1936(3) -0.0389(14) 0.064(3) Uani 1 1 d . . . N11 N 0.2270(6) 0.1943(4) -0.1007(11) 0.067(3) Uani 1 1 d . . . N12 N 0.1940(5) 0.1497(4) -0.1064(10) 0.054(3) Uani 1 1 d . . . Ru1 Ru 0.33456(5) 0.12951(3) 0.04486(11) 0.0508(3) Uani 1 1 d . . . Ru2 Ru 0.23472(5) 0.08150(3) -0.04374(11) 0.0521(3) Uani 1 1 d . . . O1 O 0.5490(18) 0.2428(14) 0.247(6) 0.34(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.084(9) 0.085(9) 0.053(6) -0.016(7) 0.011(7) -0.015(7) C2 0.095(9) 0.100(9) 0.054(7) 0.006(9) 0.002(8) -0.032(7) C3 0.129(12) 0.117(12) 0.050(8) -0.016(8) -0.001(9) -0.020(8) C4 0.121(11) 0.109(11) 0.091(9) -0.064(11) 0.018(10) -0.025(8) C5 0.210(18) 0.175(17) 0.106(12) -0.057(12) 0.030(12) -0.108(13) C6 0.140(15) 0.241(19) 0.074(10) -0.052(12) 0.043(10) -0.108(12) C7 0.044(7) 0.085(9) 0.076(10) 0.005(6) 0.008(6) -0.016(6) C8 0.047(7) 0.116(11) 0.095(12) -0.014(8) 0.009(7) 0.000(6) C9 0.059(8) 0.166(14) 0.080(10) -0.029(9) 0.016(7) -0.022(9) C10 0.063(8) 0.156(13) 0.091(12) -0.011(9) 0.008(7) -0.028(8) C11 0.062(8) 0.083(9) 0.122(12) 0.001(8) 0.013(8) -0.020(6) C12 0.047(6) 0.084(8) 0.105(11) 0.000(7) -0.008(7) -0.004(6) C13 0.083(10) 0.056(7) 0.121(13) -0.002(8) -0.024(8) -0.004(6) C14 0.129(14) 0.108(9) 0.199(18) 0.017(13) -0.087(13) 0.014(10) C15 0.157(16) 0.110(9) 0.20(2) 0.030(13) -0.102(13) 0.004(12) C16 0.173(16) 0.092(10) 0.180(19) 0.007(11) -0.092(13) 0.021(10) C17 0.165(16) 0.108(9) 0.196(19) -0.012(13) -0.116(14) 0.016(11) C18 0.153(16) 0.115(9) 0.21(2) -0.038(14) -0.121(14) 0.007(12) C19 0.061(7) 0.045(6) 0.072(8) 0.000(5) -0.004(6) 0.001(5) C20 0.083(9) 0.073(8) 0.095(10) 0.019(7) -0.028(8) -0.015(7) C21 0.130(13) 0.054(7) 0.121(11) 0.031(8) -0.034(10) -0.012(7) C22 0.099(10) 0.063(8) 0.145(13) 0.008(8) -0.031(10) -0.028(7) C23 0.086(9) 0.089(9) 0.108(11) 0.001(7) -0.026(9) -0.036(8) C24 0.100(11) 0.069(7) 0.079(8) 0.005(7) -0.014(8) -0.022(7) C25 0.071(9) 0.122(12) 0.097(10) -0.015(10) 0.008(7) -0.029(9) C26 0.110(11) 0.31(2) 0.091(10) -0.051(14) 0.021(9) -0.094(15) C27 0.111(13) 0.33(2) 0.133(14) 0.007(19) 0.042(10) -0.080(17) C28 0.079(11) 0.27(2) 0.166(16) -0.028(19) 0.026(9) -0.025(14) C29 0.077(9) 0.23(2) 0.150(13) -0.033(16) -0.002(10) -0.006(12) C30 0.093(10) 0.192(17) 0.109(10) -0.040(13) -0.001(9) -0.031(11) C31 0.066(6) 0.075(8) 0.050(8) 0.009(6) 0.006(6) -0.008(6) C32 0.082(8) 0.121(12) 0.121(15) -0.056(10) -0.010(8) 0.014(8) C33 0.102(9) 0.179(16) 0.121(14) -0.076(12) -0.027(11) 0.019(11) C34 0.103(9) 0.138(12) 0.065(10) -0.037(9) -0.011(8) 0.002(9) C35 0.079(8) 0.093(10) 0.078(10) -0.019(8) 0.004(7) -0.022(7) C36 0.059(6) 0.074(8) 0.064(8) -0.013(6) 0.001(6) -0.010(6) C37 0.084(7) 0.060(6) 0.112(11) 0.041(8) -0.026(10) -0.004(6) C38 0.137(10) 0.059(7) 0.170(15) -0.003(12) -0.040(14) 0.006(6) C39 0.146(11) 0.059(7) 0.23(2) -0.016(12) 0.021(17) 0.000(8) C40 0.154(12) 0.076(8) 0.25(2) 0.015(14) -0.015(17) -0.032(8) C41 0.129(11) 0.092(9) 0.28(2) 0.025(15) -0.051(16) -0.036(7) C42 0.118(8) 0.086(8) 0.213(19) 0.019(12) -0.068(14) -0.019(7) C43 0.061(7) 0.068(8) 0.050(7) -0.007(5) -0.002(6) 0.003(5) C44 0.111(11) 0.118(12) 0.111(13) 0.049(9) -0.048(10) -0.018(9) C45 0.121(13) 0.194(18) 0.113(14) 0.058(12) -0.043(11) -0.007(11) C46 0.082(10) 0.173(16) 0.096(13) -0.009(9) -0.036(9) 0.012(9) C47 0.061(7) 0.125(12) 0.089(11) -0.024(8) -0.017(7) -0.005(8) C48 0.056(7) 0.102(10) 0.076(10) 0.012(7) -0.006(6) -0.003(6) C50 0.15(3) 0.19(3) 0.105(18) -0.037(18) 0.042(18) -0.04(2) C51 0.14(3) 0.33(4) 0.10(2) -0.01(2) -0.013(18) -0.03(3) C52 0.21(4) 0.47(9) 0.16(4) 0.05(4) 0.01(3) -0.12(4) C53 0.37(6) 0.16(3) 0.22(4) -0.04(3) 0.21(4) -0.09(3) N1 0.074(8) 0.060(6) 0.056(7) -0.020(5) -0.002(6) -0.008(5) N2 0.051(7) 0.065(7) 0.057(8) -0.003(6) 0.003(5) -0.007(5) N3 0.042(6) 0.066(7) 0.063(7) -0.006(6) 0.003(5) -0.009(5) N4 0.051(6) 0.053(6) 0.072(7) -0.003(6) -0.028(6) -0.006(5) N5 0.061(6) 0.054(6) 0.069(8) -0.008(5) -0.004(6) 0.006(5) N6 0.060(6) 0.054(5) 0.059(7) -0.013(5) -0.004(5) -0.007(4) N7 0.056(6) 0.063(7) 0.072(8) -0.009(6) 0.009(6) -0.008(5) N8 0.067(8) 0.065(7) 0.061(8) 0.002(6) 0.005(6) -0.015(6) N9 0.065(7) 0.064(7) 0.061(7) -0.009(5) 0.004(6) 0.000(5) N10 0.056(6) 0.059(6) 0.078(7) -0.006(7) 0.018(7) -0.004(5) N11 0.070(7) 0.065(7) 0.067(8) -0.011(6) 0.004(6) -0.002(6) N12 0.041(5) 0.063(6) 0.058(7) -0.004(5) -0.012(5) -0.004(5) Ru1 0.0489(5) 0.0487(5) 0.0550(6) -0.0024(6) 0.0013(6) -0.0008(4) Ru2 0.0472(5) 0.0545(5) 0.0547(6) -0.0006(6) -0.0001(6) -0.0024(4) O1 0.25(3) 0.31(3) 0.46(7) 0.10(4) 0.07(5) 0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 N1 1.433(12) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 N3 1.436(11) . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 N4 1.439(12) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C19 N6 1.438(10) . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 N7 1.421(12) . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 N9 1.463(13) . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 N10 1.401(11) . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C43 N12 1.435(11) . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C50 C51 1.39(4) . ? C50 O1 1.43(4) . ? C51 C52 1.33(4) . ? C52 C53 1.48(5) . ? C53 O1 1.53(4) . ? N1 N2 1.309(14) . ? N1 Ru1 2.008(11) . ? N2 N3 1.314(13) . ? N3 Ru2 2.032(11) . ? N4 N5 1.310(13) . ? N4 Ru1 2.014(10) . ? N5 N6 1.338(13) . ? N6 Ru2 2.005(10) . ? N7 N8 1.347(15) . ? N7 Ru1 2.004(11) . ? N8 N9 1.277(14) . ? N9 Ru2 2.026(12) . ? N10 N11 1.321(14) . ? N10 Ru1 2.037(11) . ? N11 N12 1.312(13) . ? N12 Ru2 2.020(10) . ? Ru1 Ru2 2.4082(13) . ? 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 C1 C6 120.0 . . ? C2 C1 N1 124.3(8) . . ? C6 C1 N1 115.4(8) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 N3 121.9(7) . . ? C12 C7 N3 118.0(7) . . ? C7 C8 C9 120.0 . . ? C10 C9 C8 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 N4 122.9(8) . . ? C18 C13 N4 117.0(8) . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 N6 122.8(7) . . ? C24 C19 N6 117.1(7) . . ? C21 C20 C19 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 N7 121.6(10) . . ? C30 C25 N7 118.4(10) . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 N9 121.2(7) . . ? C36 C31 N9 118.7(7) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 N10 120.6(8) . . ? C42 C37 N10 119.0(8) . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C41 C40 C39 120.0 . . ? C40 C41 C42 120.0 . . ? C41 C42 C37 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 N12 121.6(7) . . ? C48 C43 N12 118.3(7) . . ? C43 C44 C45 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C47 120.0 . . ? C46 C47 C48 120.0 . . ? C47 C48 C43 120.0 . . ? C51 C50 O1 122(3) . . ? C52 C51 C50 93(3) . . ? C51 C52 C53 123(5) . . ? O1 C53 C52 95(3) . . ? N2 N1 C1 108.8(10) . . ? N2 N1 Ru1 124.8(8) . . ? C1 N1 Ru1 126.4(8) . . ? N1 N2 N3 115.4(10) . . ? N2 N3 C7 110.8(9) . . ? N2 N3 Ru2 125.1(7) . . ? C7 N3 Ru2 123.9(8) . . ? N5 N4 C13 110.2(9) . . ? N5 N4 Ru1 125.8(8) . . ? C13 N4 Ru1 123.8(7) . . ? N4 N5 N6 114.1(9) . . ? N5 N6 C19 109.1(9) . . ? N5 N6 Ru2 125.0(7) . . ? C19 N6 Ru2 125.6(7) . . ? N8 N7 C25 111.1(10) . . ? N8 N7 Ru1 124.8(8) . . ? C25 N7 Ru1 124.1(9) . . ? N9 N8 N7 113.7(11) . . ? N8 N9 C31 108.7(10) . . ? N8 N9 Ru2 127.1(9) . . ? C31 N9 Ru2 123.8(8) . . ? N11 N10 C37 110.6(10) . . ? N11 N10 Ru1 124.4(7) . . ? C37 N10 Ru1 125.0(8) . . ? N12 N11 N10 115.2(10) . . ? N11 N12 C43 111.0(10) . . ? N11 N12 Ru2 125.4(8) . . ? C43 N12 Ru2 123.2(7) . . ? N7 Ru1 N1 175.5(4) . . ? N7 Ru1 N4 90.4(5) . . ? N1 Ru1 N4 88.4(5) . . ? N7 Ru1 N10 90.6(5) . . ? N1 Ru1 N10 90.2(5) . . ? N4 Ru1 N10 174.2(4) . . ? N7 Ru1 Ru2 87.6(3) . . ? N1 Ru1 Ru2 88.0(3) . . ? N4 Ru1 Ru2 87.0(3) . . ? N10 Ru1 Ru2 87.3(3) . . ? N6 Ru2 N12 174.7(4) . . ? N6 Ru2 N9 89.7(4) . . ? N12 Ru2 N9 90.1(4) . . ? N6 Ru2 N3 90.0(4) . . ? N12 Ru2 N3 89.4(4) . . ? N9 Ru2 N3 172.7(4) . . ? N6 Ru2 Ru1 87.4(3) . . ? N12 Ru2 Ru1 87.3(3) . . ? N9 Ru2 Ru1 86.3(3) . . ? N3 Ru2 Ru1 86.4(3) . . ? C50 O1 C53 99(4) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.855 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.127 data_jru22 _database_code_depnum_ccdc_archive 'CCDC 814432' #TrackingRef '4376_web_deposit_cif_file_0_JosefinaPerles_1298468827.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 N12 Ru2' _chemical_formula_sum 'C48 H40 N12 Ru2' _chemical_formula_weight 987.06 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.7417(15) _cell_length_b 25.884(2) _cell_length_c 9.8779(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4791.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9355 _exptl_absorpt_correction_T_max 0.9542 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45021 _diffrn_reflns_av_R_equivalents 0.1351 _diffrn_reflns_av_sigmaI/netI 0.2077 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 29.17 _reflns_number_total 11992 _reflns_number_gt 4593 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Disordered molecules are present in the solid. The PLATON routine SQUEEZE has been used to remove these peaks as they could not be unequivocally identified. Total electron number in the voids suggests that triethylamine (used a a reagent) could be present ; _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^)+(0.1041P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00003(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.00(6) _refine_ls_number_reflns 11992 _refine_ls_number_parameters 466 _refine_ls_number_restraints 385 _refine_ls_R_factor_all 0.1845 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2550(4) 0.9660(2) 0.0101(7) 0.052(3) Uani 1 1 d GU . . C2 C 0.2613(4) 0.9293(3) 0.1122(6) 0.081(3) Uani 1 1 d GU . . H2 H 0.2851 0.9374 0.1920 0.097 Uiso 1 1 calc R . . C3 C 0.2318(5) 0.8804(3) 0.0950(9) 0.109(5) Uani 1 1 d GU . . H3 H 0.2360 0.8559 0.1633 0.130 Uiso 1 1 calc R . . C4 C 0.1962(5) 0.8683(2) -0.0243(10) 0.106(5) Uani 1 1 d GU . . H4 H 0.1766 0.8356 -0.0358 0.128 Uiso 1 1 calc R . . C5 C 0.1900(4) 0.9050(3) -0.1263(8) 0.098(4) Uani 1 1 d GU . . H5 H 0.1662 0.8968 -0.2061 0.118 Uiso 1 1 calc R . . C6 C 0.2194(4) 0.9538(3) -0.1091(6) 0.076(3) Uani 1 1 d GU . . H6 H 0.2153 0.9784 -0.1774 0.091 Uiso 1 1 calc R . . C7 C 0.4266(5) 1.0582(4) 0.2202(13) 0.108(5) Uani 1 1 d GU . . C8 C 0.4572(7) 1.0113(3) 0.2568(15) 0.176(8) Uani 1 1 d GU . . H8 H 0.4375 0.9805 0.2258 0.211 Uiso 1 1 calc R . . C9 C 0.5171(7) 1.0105(4) 0.3397(16) 0.186(8) Uani 1 1 d GU . . H9 H 0.5376 0.9791 0.3641 0.223 Uiso 1 1 calc R . . C10 C 0.5464(6) 1.0566(5) 0.3859(14) 0.170(8) Uani 1 1 d GU . . H10 H 0.5865 1.0560 0.4414 0.203 Uiso 1 1 calc R . . C11 C 0.5158(8) 1.1035(4) 0.3494(17) 0.212(9) Uani 1 1 d GU . . H11 H 0.5354 1.1343 0.3803 0.255 Uiso 1 1 calc R . . C12 C 0.4559(7) 1.1043(3) 0.2665(17) 0.212(9) Uani 1 1 d GU . . H12 H 0.4354 1.1356 0.2421 0.255 Uiso 1 1 calc R . . C13 C 0.2649(4) 1.0484(3) -0.3390(6) 0.065(3) Uani 1 1 d GU . . C14 C 0.3114(3) 1.0185(4) -0.4158(9) 0.110(5) Uani 1 1 d GU . . H14 H 0.3596 1.0172 -0.3938 0.132 Uiso 1 1 calc R . . C15 C 0.2857(4) 0.9905(4) -0.5256(9) 0.130(6) Uani 1 1 d GU . . H15 H 0.3168 0.9705 -0.5770 0.156 Uiso 1 1 calc R . . C16 C 0.2137(4) 0.9924(3) -0.5586(8) 0.098(4) Uani 1 1 d GU . . H16 H 0.1966 0.9737 -0.6321 0.118 Uiso 1 1 calc R . . C17 C 0.1673(3) 1.0223(3) -0.4818(8) 0.077(3) Uani 1 1 d GU . . H17 H 0.1191 1.0236 -0.5039 0.092 Uiso 1 1 calc R . . C18 C 0.1929(4) 1.0503(3) -0.3720(7) 0.068(3) Uani 1 1 d GU . . H18 H 0.1618 1.0703 -0.3206 0.082 Uiso 1 1 calc R . . C19 C 0.4587(4) 1.1256(5) -0.1530(11) 0.110(5) Uani 1 1 d GU . . C20 C 0.4827(6) 1.1398(6) -0.2808(10) 0.192(8) Uani 1 1 d GU . . H20 H 0.4514 1.1398 -0.3538 0.231 Uiso 1 1 calc R . . C21 C 0.5535(6) 1.1541(7) -0.2994(11) 0.217(9) Uani 1 1 d GU . . H21 H 0.5696 1.1637 -0.3849 0.261 Uiso 1 1 calc R . . C22 C 0.6003(4) 1.1542(6) -0.1902(15) 0.190(8) Uani 1 1 d GU . . H22 H 0.6477 1.1638 -0.2026 0.228 Uiso 1 1 calc R . . C23 C 0.5763(5) 1.1400(5) -0.0624(12) 0.176(7) Uani 1 1 d GU . . H23 H 0.6076 1.1400 0.0107 0.211 Uiso 1 1 calc R . . C24 C 0.5055(6) 1.1256(5) -0.0438(9) 0.145(6) Uani 1 1 d GU . . H24 H 0.4894 1.1161 0.0417 0.174 Uiso 1 1 calc R . . C25 C 0.1275(4) 1.1546(3) -0.1789(8) 0.063(3) Uani 1 1 d GU . . C26 C 0.1170(5) 1.1894(3) -0.2841(9) 0.118(5) Uani 1 1 d GU . . H26 H 0.1522 1.2134 -0.3052 0.141 Uiso 1 1 calc R . . C27 C 0.0539(5) 1.1883(4) -0.3579(9) 0.143(6) Uani 1 1 d GU . . H27 H 0.0468 1.2116 -0.4283 0.172 Uiso 1 1 calc R . . C28 C 0.0013(4) 1.1524(4) -0.3264(9) 0.109(5) Uani 1 1 d GU . . H28 H -0.0410 1.1517 -0.3758 0.131 Uiso 1 1 calc R . . C29 C 0.0118(4) 1.1176(4) -0.2212(10) 0.097(4) Uani 1 1 d GU . . H29 H -0.0234 1.0936 -0.2002 0.117 Uiso 1 1 calc R . . C30 C 0.0749(4) 1.1187(3) -0.1474(8) 0.079(3) Uani 1 1 d GU . . H30 H 0.0820 1.0954 -0.0770 0.095 Uiso 1 1 calc R . . C31 C 0.3186(5) 1.2438(3) -0.0363(12) 0.086(3) Uani 1 1 d GU . . C32 C 0.2771(4) 1.2882(3) -0.0443(14) 0.120(4) Uani 1 1 d GU . . H32 H 0.2283 1.2856 -0.0607 0.144 Uiso 1 1 calc R . . C33 C 0.3084(6) 1.3365(3) -0.0276(15) 0.152(6) Uani 1 1 d GU . . H33 H 0.2807 1.3662 -0.0329 0.183 Uiso 1 1 calc R . . C34 C 0.3813(7) 1.3403(3) -0.0030(16) 0.175(8) Uani 1 1 d GU . . H34 H 0.4022 1.3726 0.0081 0.210 Uiso 1 1 calc R . . C35 C 0.4227(5) 1.2959(5) 0.0049(19) 0.222(9) Uani 1 1 d GU . . H35 H 0.4715 1.2985 0.0213 0.266 Uiso 1 1 calc R . . C36 C 0.3914(5) 1.2477(4) -0.0118(16) 0.180(8) Uani 1 1 d GU . . H36 H 0.4192 1.2179 -0.0065 0.216 Uiso 1 1 calc R . . C37 C 0.1189(3) 1.0734(3) 0.1745(8) 0.065(3) Uani 1 1 d GU . . C38 C 0.0741(4) 1.0997(3) 0.2632(9) 0.094(4) Uani 1 1 d GU . . H38 H 0.0895 1.1300 0.3043 0.113 Uiso 1 1 calc R . . C39 C 0.0063(4) 1.0805(4) 0.2906(9) 0.109(5) Uani 1 1 d GU . . H39 H -0.0236 1.0981 0.3499 0.131 Uiso 1 1 calc R . . C40 C -0.0167(3) 1.0352(4) 0.2292(10) 0.114(5) Uani 1 1 d GU . . H40 H -0.0620 1.0224 0.2475 0.137 Uiso 1 1 calc R . . C41 C 0.0281(4) 1.0089(3) 0.1405(9) 0.089(4) Uani 1 1 d GU . . H41 H 0.0127 0.9786 0.0995 0.107 Uiso 1 1 calc R . . C42 C 0.0959(4) 1.0281(3) 0.1132(8) 0.082(3) Uani 1 1 d GU . . H42 H 0.1258 1.0105 0.0538 0.098 Uiso 1 1 calc R . . C43 C 0.3004(5) 1.1703(4) 0.3280(7) 0.078(3) Uani 1 1 d GU . . C44 C 0.2714(4) 1.1648(3) 0.4567(9) 0.098(4) Uani 1 1 d GU . . H44 H 0.2338 1.1420 0.4710 0.117 Uiso 1 1 calc R . . C45 C 0.2986(5) 1.1934(4) 0.5640(7) 0.094(4) Uani 1 1 d GU . . H45 H 0.2791 1.1898 0.6501 0.113 Uiso 1 1 calc R . . C46 C 0.3548(5) 1.2275(4) 0.5427(9) 0.119(5) Uani 1 1 d GU . . H46 H 0.3730 1.2466 0.6145 0.143 Uiso 1 1 calc R . . C47 C 0.3838(5) 1.2329(4) 0.4140(11) 0.221(9) Uani 1 1 d GU . . H47 H 0.4215 1.2557 0.3997 0.265 Uiso 1 1 calc R . . C48 C 0.3567(6) 1.2043(5) 0.3067(8) 0.201(9) Uani 1 1 d GU . . H48 H 0.3761 1.2080 0.2206 0.241 Uiso 1 1 calc R . . N1 N 0.2819(4) 1.0166(3) 0.0275(9) 0.057(2) Uani 1 1 d . . . N2 N 0.3416(5) 1.0179(4) 0.1051(9) 0.062(2) Uani 1 1 d . . . N3 N 0.3708(5) 1.0630(3) 0.1216(10) 0.061(2) Uani 1 1 d . . . N4 N 0.2879(5) 1.0759(4) -0.2169(10) 0.065(3) Uani 1 1 d . . . N5 N 0.3539(6) 1.0900(4) -0.2391(9) 0.071(3) Uani 1 1 d . . . N6 N 0.3848(5) 1.1147(3) -0.1309(9) 0.057(2) Uani 1 1 d . . . N7 N 0.1929(4) 1.1498(4) -0.1059(8) 0.055(2) Uani 1 1 d . . . N8 N 0.2265(5) 1.1934(4) -0.1017(9) 0.067(3) Uani 1 1 d . . . N9 N 0.2895(5) 1.1932(3) -0.0349(11) 0.067(2) Uani 1 1 d . . . N10 N 0.1863(5) 1.0921(3) 0.1397(9) 0.058(2) Uani 1 1 d . . . N11 N 0.2136(4) 1.1202(3) 0.2366(9) 0.053(2) Uani 1 1 d . . . N12 N 0.2770(5) 1.1402(3) 0.2144(9) 0.066(3) Uani 1 1 d . . . Ru1 Ru 0.23423(4) 1.08132(3) -0.04392(8) 0.0520(2) Uani 1 1 d . . . Ru2 Ru 0.33411(4) 1.12933(3) 0.04396(9) 0.0503(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.056(6) 0.037(5) 0.064(6) 0.000(4) -0.002(4) 0.005(4) C2 0.085(8) 0.062(7) 0.095(8) 0.021(6) -0.025(7) -0.009(6) C3 0.121(11) 0.070(7) 0.135(10) 0.034(8) -0.047(9) -0.018(7) C4 0.103(9) 0.065(7) 0.152(11) 0.010(7) -0.038(9) -0.042(7) C5 0.095(9) 0.090(8) 0.109(9) -0.001(6) -0.029(8) -0.042(8) C6 0.101(10) 0.055(6) 0.070(6) -0.002(5) -0.014(6) -0.021(6) C7 0.079(9) 0.057(7) 0.188(15) 0.014(8) -0.049(9) -0.011(7) C8 0.159(15) 0.135(9) 0.232(17) 0.037(13) -0.130(13) 0.008(11) C9 0.179(16) 0.167(11) 0.211(18) 0.068(14) -0.140(13) -0.032(12) C10 0.184(15) 0.129(12) 0.196(16) 0.047(12) -0.123(13) -0.010(11) C11 0.198(17) 0.155(11) 0.28(2) 0.038(16) -0.184(15) -0.029(13) C12 0.180(16) 0.140(9) 0.32(2) 0.023(15) -0.190(15) -0.035(12) C13 0.078(7) 0.074(8) 0.044(5) 0.008(5) -0.004(5) -0.002(6) C14 0.082(8) 0.115(11) 0.133(13) -0.067(9) -0.005(7) 0.006(7) C15 0.091(8) 0.160(13) 0.137(12) -0.087(10) -0.022(9) 0.015(9) C16 0.098(8) 0.119(10) 0.078(8) -0.034(7) -0.011(7) 0.003(8) C17 0.073(7) 0.079(8) 0.078(8) 0.000(6) -0.011(5) -0.010(6) C18 0.055(6) 0.086(8) 0.064(6) -0.010(6) -0.003(5) -0.011(6) C19 0.096(10) 0.155(13) 0.079(8) -0.007(9) 0.005(7) -0.055(10) C20 0.103(10) 0.38(2) 0.090(8) -0.017(13) 0.006(8) -0.126(14) C21 0.088(11) 0.38(2) 0.179(14) 0.046(19) 0.024(9) -0.098(16) C22 0.091(11) 0.30(2) 0.182(15) -0.012(18) 0.004(9) -0.067(14) C23 0.092(9) 0.27(2) 0.169(12) -0.062(15) 0.014(10) -0.046(12) C24 0.113(10) 0.210(16) 0.111(9) -0.015(12) -0.012(9) -0.054(11) C25 0.061(7) 0.064(7) 0.066(6) -0.003(5) -0.015(5) -0.003(5) C26 0.107(10) 0.135(12) 0.111(10) 0.057(8) -0.061(8) -0.031(9) C27 0.099(11) 0.226(17) 0.105(10) 0.052(10) -0.046(9) -0.014(10) C28 0.062(8) 0.170(14) 0.096(10) -0.027(8) -0.040(7) 0.016(7) C29 0.052(7) 0.149(12) 0.092(9) -0.018(7) -0.011(6) -0.010(8) C30 0.057(8) 0.095(9) 0.086(8) 0.014(7) -0.010(6) 0.002(6) C31 0.081(7) 0.071(7) 0.108(9) 0.023(8) -0.031(9) 0.003(6) C32 0.132(10) 0.062(7) 0.165(12) 0.001(10) -0.023(12) 0.005(6) C33 0.172(12) 0.063(7) 0.222(17) -0.010(11) 0.012(16) -0.028(8) C34 0.186(13) 0.070(8) 0.27(2) 0.035(12) -0.030(17) -0.054(9) C35 0.176(12) 0.101(9) 0.39(2) 0.045(17) -0.103(18) -0.059(8) C36 0.136(9) 0.081(8) 0.32(2) 0.048(13) -0.119(15) -0.021(8) C37 0.052(7) 0.078(8) 0.065(7) 0.013(5) 0.000(5) -0.012(5) C38 0.054(8) 0.119(10) 0.108(10) -0.014(8) 0.025(7) -0.010(7) C39 0.067(8) 0.163(13) 0.097(9) -0.028(8) 0.021(7) -0.034(8) C40 0.085(9) 0.149(12) 0.107(11) -0.014(8) 0.007(8) -0.033(8) C41 0.057(7) 0.099(9) 0.111(9) 0.003(7) -0.003(7) -0.025(6) C42 0.044(6) 0.094(8) 0.108(9) -0.007(6) -0.023(6) -0.003(6) C43 0.070(8) 0.099(9) 0.064(6) -0.018(7) 0.015(6) -0.017(7) C44 0.094(8) 0.138(11) 0.060(6) -0.024(9) 0.002(7) -0.035(7) C45 0.119(10) 0.120(11) 0.042(6) -0.018(6) -0.018(7) -0.012(7) C46 0.109(10) 0.122(11) 0.127(9) -0.100(10) 0.020(9) -0.015(7) C47 0.219(17) 0.30(2) 0.144(13) -0.129(14) 0.069(12) -0.162(14) C48 0.144(13) 0.34(2) 0.115(10) -0.111(13) 0.063(10) -0.166(13) N1 0.056(5) 0.056(5) 0.059(5) -0.004(4) 0.005(5) -0.007(4) N2 0.063(6) 0.068(7) 0.056(5) -0.006(5) 0.003(5) 0.014(5) N3 0.062(6) 0.040(5) 0.079(6) -0.004(5) -0.033(5) -0.007(5) N4 0.048(6) 0.080(7) 0.067(6) -0.028(5) 0.005(5) -0.015(5) N5 0.083(9) 0.077(7) 0.053(6) -0.010(5) -0.006(6) -0.004(6) N6 0.049(6) 0.065(6) 0.058(5) -0.003(5) 0.008(5) 0.002(5) N7 0.038(5) 0.055(6) 0.073(6) -0.013(4) -0.019(4) 0.003(5) N8 0.066(7) 0.062(6) 0.071(6) 0.000(5) 0.001(5) 0.010(6) N9 0.067(6) 0.055(5) 0.079(6) -0.017(6) 0.022(6) -0.004(5) N10 0.050(6) 0.054(6) 0.071(6) -0.008(5) 0.006(5) -0.009(4) N11 0.037(6) 0.058(6) 0.065(6) -0.014(5) 0.018(4) -0.016(4) N12 0.080(8) 0.057(6) 0.060(6) -0.018(4) 0.002(5) 0.003(5) Ru1 0.0474(4) 0.0547(5) 0.0537(4) 0.0000(5) 0.0000(6) -0.0019(4) Ru2 0.0488(5) 0.0482(4) 0.0539(4) -0.0026(5) 0.0016(5) -0.0004(4) _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 C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 N1 1.414(9) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 N3 1.434(10) . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 N4 1.465(10) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C19 N6 1.430(11) . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 N7 1.427(9) . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 N9 1.418(10) . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 N10 1.396(10) . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C43 N12 1.435(10) . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? N1 N2 1.357(11) . ? N1 Ru1 2.024(8) . ? N2 N3 1.300(11) . ? N3 Ru2 2.002(9) . ? N4 N5 1.308(12) . ? N4 Ru1 1.988(9) . ? N5 N6 1.373(12) . ? N6 Ru2 2.007(8) . ? N7 N8 1.293(12) . ? N7 Ru1 2.028(9) . ? N8 N9 1.353(12) . ? N9 Ru2 2.010(10) . ? N10 N11 1.306(11) . ? N10 Ru1 2.043(9) . ? N11 N12 1.314(11) . ? N12 Ru2 2.015(9) . ? Ru1 Ru2 2.4086(11) . ? 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 C1 C6 120.0 . . ? C2 C1 N1 121.1(6) . . ? C6 C1 N1 118.9(6) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 N3 123.5(7) . . ? C12 C7 N3 116.0(7) . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 N4 122.4(6) . . ? C18 C13 N4 117.5(6) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 N6 120.3(8) . . ? C24 C19 N6 119.5(8) . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 N7 123.8(7) . . ? C30 C25 N7 116.0(7) . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C29 C30 C25 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 N9 123.3(7) . . ? C36 C31 N9 116.2(7) . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 N10 122.2(6) . . ? C42 C37 N10 117.8(6) . . ? C39 C38 C37 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 N12 122.7(7) . . ? C48 C43 N12 117.2(7) . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? N2 N1 C1 112.5(8) . . ? N2 N1 Ru1 122.8(6) . . ? C1 N1 Ru1 124.6(6) . . ? N3 N2 N1 116.1(8) . . ? N2 N3 C7 108.4(8) . . ? N2 N3 Ru2 125.3(7) . . ? C7 N3 Ru2 125.7(6) . . ? N5 N4 C13 106.0(8) . . ? N5 N4 Ru1 127.1(7) . . ? C13 N4 Ru1 126.4(7) . . ? N4 N5 N6 113.5(9) . . ? N5 N6 C19 112.4(9) . . ? N5 N6 Ru2 123.9(7) . . ? C19 N6 Ru2 123.6(7) . . ? N8 N7 C25 111.0(9) . . ? N8 N7 Ru1 124.5(7) . . ? C25 N7 Ru1 123.8(6) . . ? N7 N8 N9 116.0(9) . . ? N8 N9 C31 109.1(9) . . ? N8 N9 Ru2 123.6(7) . . ? C31 N9 Ru2 127.2(8) . . ? N11 N10 C37 111.6(8) . . ? N11 N10 Ru1 123.6(6) . . ? C37 N10 Ru1 124.7(7) . . ? N10 N11 N12 116.9(8) . . ? N11 N12 C43 111.1(8) . . ? N11 N12 Ru2 124.3(7) . . ? C43 N12 Ru2 124.5(7) . . ? N4 Ru1 N1 91.0(4) . . ? N4 Ru1 N7 89.8(4) . . ? N1 Ru1 N7 174.9(3) . . ? N4 Ru1 N10 174.4(4) . . ? N1 Ru1 N10 89.9(3) . . ? N7 Ru1 N10 88.9(3) . . ? N4 Ru1 Ru2 87.3(3) . . ? N1 Ru1 Ru2 87.6(2) . . ? N7 Ru1 Ru2 87.4(2) . . ? N10 Ru1 Ru2 87.2(2) . . ? N3 Ru2 N6 90.3(4) . . ? N3 Ru2 N9 175.4(4) . . ? N6 Ru2 N9 91.0(4) . . ? N3 Ru2 N12 89.0(4) . . ? N6 Ru2 N12 175.4(4) . . ? N9 Ru2 N12 89.3(4) . . ? N3 Ru2 Ru1 87.9(2) . . ? N6 Ru2 Ru1 87.7(3) . . ? N9 Ru2 Ru1 87.8(3) . . ? N12 Ru2 Ru1 87.7(3) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.741 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.114 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.131 0.281 0.263 138 59 ' ' 2 0.369 0.781 -0.237 138 59 ' ' 3 0.631 0.219 0.263 138 59 ' ' 4 0.869 0.719 -0.237 138 59 ' ' _platon_squeeze_details ; ; data_Jru2dpf4 _database_code_depnum_ccdc_archive 'CCDC 814433' #TrackingRef '4376_web_deposit_cif_file_0_JosefinaPerles_1298468827.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 Cl N8 O5.25 Ru2' _chemical_formula_sum 'C52 H44 Cl N8 O5.25 Ru2' _chemical_formula_weight 1102.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2590 0.8360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 4/ncc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 15.028(2) _cell_length_b 15.028(2) _cell_length_c 21.962(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4960.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2236 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8027 _exptl_absorpt_correction_T_max 0.9381 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43783 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 29.05 _reflns_number_total 3249 _reflns_number_gt 1423 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Disordered solvent molecules of water (O1 O2 O3) are present in the solid. ; _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^)+(0.0527P)^2^+13.3051P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3249 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1307 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.004 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 O1 O 0.286(3) 0.674(3) 0.270(3) 0.24(3) Uani 0.53(7) 1 d P . . O2 O 0.194(2) 0.694(2) 0.2500 0.31(5) Uani 0.63(11) 2 d SP . . O3 O 0.2500 0.7500 0.308(4) 0.44(6) Uani 0.77(17) 2 d SP . . Ru1 Ru 0.2500 0.2500 0.26168(3) 0.0421(2) Uani 1 4 d S . . Ru2 Ru 0.2500 0.2500 0.15493(3) 0.0451(2) Uani 1 4 d S . . Cl1 Cl 0.2500 0.2500 0.37167(11) 0.0542(6) Uani 1 4 d S . . N1 N 0.1720(3) 0.1350(3) 0.2573(2) 0.0544(12) Uani 1 1 d . . . N2 N 0.2008(3) 0.1229(3) 0.15414(19) 0.0533(11) Uani 1 1 d . . . C1 C 0.1653(4) 0.0923(4) 0.2053(3) 0.0537(14) Uani 1 1 d . . . H1 H 0.1345 0.0387 0.2044 0.064 Uiso 1 1 calc R . . C2 C 0.1141(4) 0.1003(4) 0.3047(2) 0.0556(14) Uani 1 1 d . . . C3 C 0.0251(5) 0.1136(6) 0.3019(3) 0.086(2) Uani 1 1 d . . . H3 H 0.0011 0.1482 0.2708 0.103 Uiso 1 1 calc R . . C4 C -0.0307(6) 0.0755(6) 0.3455(4) 0.108(3) Uani 1 1 d . . . H4 H -0.0919 0.0840 0.3428 0.129 Uiso 1 1 calc R . . C5 C 0.0026(7) 0.0268(6) 0.3913(3) 0.097(3) Uani 1 1 d . . . H5 H -0.0350 0.0016 0.4202 0.116 Uiso 1 1 calc R . . C6 C 0.0921(7) 0.0147(5) 0.3950(3) 0.097(3) Uani 1 1 d . . . H6 H 0.1155 -0.0189 0.4267 0.117 Uiso 1 1 calc R . . C7 C 0.1487(6) 0.0515(5) 0.3525(3) 0.084(2) Uani 1 1 d . . . H7 H 0.2099 0.0435 0.3559 0.101 Uiso 1 1 calc R . . C8 C 0.2077(4) 0.0634(4) 0.1042(3) 0.0573(15) Uani 1 1 d . . . C9 C 0.1923(4) 0.0938(5) 0.0454(3) 0.0719(18) Uani 1 1 d . . . H9 H 0.1762 0.1528 0.0391 0.086 Uiso 1 1 calc R . . C10 C 0.2005(5) 0.0373(7) -0.0036(3) 0.090(2) Uani 1 1 d . . . H10 H 0.1912 0.0592 -0.0427 0.108 Uiso 1 1 calc R . . C11 C 0.2216(6) -0.0489(7) 0.0040(4) 0.100(3) Uani 1 1 d . . . H11 H 0.2257 -0.0866 -0.0295 0.119 Uiso 1 1 calc R . . C12 C 0.2371(5) -0.0808(5) 0.0616(4) 0.095(2) Uani 1 1 d . . . H12 H 0.2519 -0.1404 0.0671 0.114 Uiso 1 1 calc R . . C13 C 0.2309(5) -0.0247(5) 0.1117(3) 0.076(2) Uani 1 1 d . . . H13 H 0.2425 -0.0466 0.1505 0.091 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 O1 0.19(4) 0.24(4) 0.29(6) 0.05(3) -0.06(4) -0.04(2) O2 0.30(5) 0.30(5) 0.34(8) 0.11(4) -0.11(4) -0.14(5) O3 0.34(9) 0.71(17) 0.26(6) 0.000 0.000 0.09(9) Ru1 0.0459(3) 0.0459(3) 0.0344(4) 0.000 0.000 0.000 Ru2 0.0495(3) 0.0495(3) 0.0363(4) 0.000 0.000 0.000 Cl1 0.0635(10) 0.0635(10) 0.0357(12) 0.000 0.000 0.000 N1 0.062(3) 0.054(3) 0.046(3) 0.002(2) 0.000(2) -0.004(2) N2 0.064(3) 0.054(3) 0.041(2) -0.003(2) 0.001(2) -0.001(2) C1 0.058(3) 0.048(3) 0.055(3) -0.002(3) -0.006(3) -0.002(3) C2 0.069(4) 0.048(3) 0.050(3) 0.000(3) 0.001(3) -0.012(3) C3 0.066(5) 0.114(6) 0.078(5) 0.018(4) -0.003(4) -0.019(4) C4 0.082(6) 0.142(8) 0.100(6) 0.004(6) 0.016(5) -0.036(6) C5 0.139(9) 0.087(6) 0.065(4) -0.013(4) 0.032(5) -0.056(6) C6 0.132(8) 0.087(6) 0.073(5) 0.022(4) 0.008(5) -0.001(6) C7 0.102(6) 0.080(5) 0.069(5) 0.016(4) 0.008(4) 0.008(4) C8 0.051(3) 0.064(4) 0.057(4) -0.014(3) -0.002(3) -0.004(3) C9 0.079(5) 0.084(5) 0.053(4) -0.006(3) -0.006(3) 0.000(4) C10 0.089(6) 0.126(8) 0.056(4) -0.024(5) -0.005(4) -0.002(5) C11 0.107(7) 0.114(8) 0.078(5) -0.046(5) 0.009(5) -0.004(5) C12 0.101(6) 0.074(5) 0.111(6) -0.028(5) 0.011(5) 0.001(4) C13 0.084(5) 0.073(5) 0.071(4) -0.010(4) 0.000(4) 0.006(4) _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 O1 O1 1.22(9) 8_665 ? O1 O2 1.47(4) . ? O1 O3 1.51(5) . ? O2 O1 1.47(4) 7_455 ? O2 O3 1.74(5) . ? O2 O3 1.74(5) 7_455 ? O3 O1 1.51(5) 2_565 ? O3 O2 1.74(5) 2_565 ? Ru1 N1 2.091(5) 2 ? Ru1 N1 2.091(5) 4 ? Ru1 N1 2.091(5) . ? Ru1 N1 2.091(5) 3 ? Ru1 Ru2 2.3444(11) . ? Ru1 Cl1 2.416(2) . ? Ru2 N2 2.049(5) 2 ? Ru2 N2 2.049(5) 4 ? Ru2 N2 2.049(5) . ? Ru2 N2 2.049(5) 3 ? N1 C1 1.312(7) . ? N1 C2 1.453(7) . ? N2 C1 1.326(7) . ? N2 C8 1.419(7) . ? C2 C3 1.354(9) . ? C2 C7 1.382(8) . ? C3 C4 1.398(10) . ? C4 C5 1.340(11) . ? C5 C6 1.359(11) . ? C6 C7 1.379(10) . ? C8 C13 1.378(9) . ? C8 C9 1.388(8) . ? C9 C10 1.377(9) . ? C10 C11 1.344(11) . ? C11 C12 1.373(11) . ? C12 C13 1.389(9) . ? 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 O1 O2 99(5) 8_665 . ? O1 O1 O3 101(5) 8_665 . ? O2 O1 O3 71(4) . . ? O1 O2 O1 118(4) 7_455 . ? O1 O2 O3 82(4) 7_455 . ? O1 O2 O3 55(3) . . ? O1 O2 O3 55(3) 7_455 7_455 ? O1 O2 O3 82(4) . 7_455 ? O3 O2 O3 94(5) . 7_455 ? O1 O3 O1 113(5) 2_565 . ? O1 O3 O2 78(4) 2_565 . ? O1 O3 O2 53(2) . . ? O1 O3 O2 53(2) 2_565 2_565 ? O1 O3 O2 78(4) . 2_565 ? O2 O3 O2 86(5) . 2_565 ? N1 Ru1 N1 89.876(11) 2 4 ? N1 Ru1 N1 174.7(2) 2 . ? N1 Ru1 N1 89.876(12) 4 . ? N1 Ru1 N1 89.876(12) 2 3 ? N1 Ru1 N1 174.7(2) 4 3 ? N1 Ru1 N1 89.876(11) . 3 ? N1 Ru1 Ru2 87.34(12) 2 . ? N1 Ru1 Ru2 87.34(12) 4 . ? N1 Ru1 Ru2 87.34(12) . . ? N1 Ru1 Ru2 87.34(12) 3 . ? N1 Ru1 Cl1 92.66(12) 2 . ? N1 Ru1 Cl1 92.66(12) 4 . ? N1 Ru1 Cl1 92.66(12) . . ? N1 Ru1 Cl1 92.66(12) 3 . ? Ru2 Ru1 Cl1 180.0 . . ? N2 Ru2 N2 89.996(2) 2 4 ? N2 Ru2 N2 179.0(2) 2 . ? N2 Ru2 N2 89.996(2) 4 . ? N2 Ru2 N2 89.996(2) 2 3 ? N2 Ru2 N2 179.0(2) 4 3 ? N2 Ru2 N2 89.996(2) . 3 ? N2 Ru2 Ru1 90.49(12) 2 . ? N2 Ru2 Ru1 90.49(12) 4 . ? N2 Ru2 Ru1 90.49(12) . . ? N2 Ru2 Ru1 90.49(12) 3 . ? C1 N1 C2 113.7(5) . . ? C1 N1 Ru1 119.2(4) . . ? C2 N1 Ru1 126.8(3) . . ? C1 N2 C8 117.9(5) . . ? C1 N2 Ru2 117.4(4) . . ? C8 N2 Ru2 124.6(4) . . ? N1 C1 N2 122.5(5) . . ? C3 C2 C7 119.0(6) . . ? C3 C2 N1 120.3(6) . . ? C7 C2 N1 120.7(6) . . ? C2 C3 C4 120.1(7) . . ? C5 C4 C3 120.9(8) . . ? C4 C5 C6 119.2(8) . . ? C5 C6 C7 121.1(8) . . ? C6 C7 C2 119.7(8) . . ? C13 C8 C9 118.0(6) . . ? C13 C8 N2 122.0(6) . . ? C9 C8 N2 119.9(6) . . ? C10 C9 C8 120.6(7) . . ? C11 C10 C9 121.2(8) . . ? C10 C11 C12 119.4(7) . . ? C11 C12 C13 120.4(8) . . ? C8 C13 C12 120.3(7) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.759 _refine_diff_density_min -0.893 _refine_diff_density_rms 0.084 data_jss18 _database_code_depnum_ccdc_archive 'CCDC 814434' #TrackingRef '4376_web_deposit_cif_file_0_JosefinaPerles_1298468827.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H60 Cl N8 O8 Ru2' _chemical_formula_sum 'C60 H60 Cl N8 O8 Ru2' _chemical_formula_weight 1258.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 14.2592(8) _cell_length_b 14.2608(8) _cell_length_c 30.4171(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6185.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 'deep purple' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2580 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8572 _exptl_absorpt_correction_T_max 0.8913 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56611 _diffrn_reflns_av_R_equivalents 0.1297 _diffrn_reflns_av_sigmaI/netI 0.1025 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 29.24 _reflns_number_total 7940 _reflns_number_gt 2776 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1670P)^2^+23.5274P] 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 refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7940 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2048 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.3492 _refine_ls_wR_factor_gt 0.2314 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.004 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 C8 C 0.8099(11) 0.4261(13) 0.4759(5) 0.125(6) Uani 1 1 d . . . H8A H 0.7792 0.4363 0.5036 0.188 Uiso 1 1 calc R . . H8B H 0.7855 0.3702 0.4625 0.188 Uiso 1 1 calc R . . H8C H 0.7987 0.4787 0.4570 0.188 Uiso 1 1 calc R . . C14 C 1.3742(8) -0.0027(9) 0.1632(4) 0.071(3) Uani 1 1 d . . . H14 H 1.4119 0.0051 0.1385 0.085 Uiso 1 1 calc R . . C24 C 1.0752(13) -0.1901(11) 0.4760(5) 0.125(6) Uani 1 1 d . . . H24A H 1.0653 -0.2209 0.5037 0.188 Uiso 1 1 calc R . . H24B H 1.1314 -0.2138 0.4626 0.188 Uiso 1 1 calc R . . H24C H 1.0227 -0.2019 0.4570 0.188 Uiso 1 1 calc R . . C28 C 0.9221(9) 0.1821(9) 0.1663(4) 0.075(3) Uani 1 1 d . . . C29 C 0.9982(9) 0.1259(8) 0.1632(4) 0.073(3) Uani 1 1 d . . . H29 H 1.0060 0.0877 0.1387 0.087 Uiso 1 1 calc R . . C31 C 0.8515(13) 0.1233(11) 0.1006(5) 0.127(6) Uani 1 1 d . . . H31A H 0.8016 0.1375 0.0804 0.190 Uiso 1 1 calc R . . H31B H 0.8411 0.0626 0.1133 0.190 Uiso 1 1 calc R . . H31C H 0.9102 0.1233 0.0851 0.190 Uiso 1 1 calc R . . O5 O 1.0842(7) -0.0926(6) 0.4828(3) 0.091(3) Uani 1 1 d . . . O6 O 0.8538(7) 0.1899(7) 0.1333(4) 0.114(4) Uani 1 1 d . . . C1 C 1.1389(7) 0.4022(7) 0.3050(3) 0.057(3) Uani 1 1 d . . . H1 H 1.1008 0.4551 0.3054 0.068 Uiso 1 1 calc R . . C2 C 1.0852(7) 0.3689(7) 0.3760(3) 0.054(2) Uani 1 1 d . . . C3 C 0.9918(8) 0.3813(8) 0.3689(3) 0.067(3) Uani 1 1 d . . . H3 H 0.9689 0.3786 0.3403 0.080 Uiso 1 1 calc R . . C4 C 0.9286(8) 0.3981(8) 0.4037(4) 0.071(3) Uani 1 1 d . . . H4 H 0.8651 0.4070 0.3979 0.085 Uiso 1 1 calc R . . C5 C 0.9611(9) 0.4013(8) 0.4458(4) 0.069(3) Uani 1 1 d . . . C6 C 1.0561(9) 0.3874(8) 0.4537(4) 0.074(3) Uani 1 1 d . . . H6 H 1.0783 0.3872 0.4825 0.089 Uiso 1 1 calc R . . C7 C 1.1178(7) 0.3738(7) 0.4193(3) 0.061(3) Uani 1 1 d . . . H7 H 1.1817 0.3679 0.4250 0.073 Uiso 1 1 calc R . . C10 C 1.3197(7) 0.0512(7) 0.2335(3) 0.057(3) Uani 1 1 d . . . C11 C 1.2644(9) -0.0266(8) 0.2368(4) 0.077(3) Uani 1 1 d . . . H11 H 1.2273 -0.0352 0.2616 0.093 Uiso 1 1 calc R . . C12 C 1.2633(9) -0.0934(9) 0.2032(4) 0.084(4) Uani 1 1 d . . . H12 H 1.2260 -0.1466 0.2056 0.101 Uiso 1 1 calc R . . C13 C 1.3183(8) -0.0791(9) 0.1665(4) 0.076(3) Uani 1 1 d . . . C15 C 1.3754(7) 0.0644(8) 0.1964(3) 0.063(3) Uani 1 1 d . . . H15 H 1.4130 0.1175 0.1938 0.076 Uiso 1 1 calc R . . C16 C 1.3771(11) -0.1489(13) 0.1007(5) 0.125(6) Uani 1 1 d . . . H16A H 1.3626 -0.1980 0.0802 0.187 Uiso 1 1 calc R . . H16B H 1.4375 -0.1603 0.1135 0.187 Uiso 1 1 calc R . . H16C H 1.3779 -0.0897 0.0856 0.187 Uiso 1 1 calc R . . C17 C 1.0973(7) 0.1388(7) 0.3050(3) 0.056(3) Uani 1 1 d . . . H17 H 1.0442 0.1009 0.3056 0.068 Uiso 1 1 calc R . . C18 C 1.1308(7) 0.0845(7) 0.3759(3) 0.053(2) Uani 1 1 d . . . C19 C 1.1189(8) -0.0086(8) 0.3687(3) 0.069(3) Uani 1 1 d . . . H19 H 1.1224 -0.0316 0.3402 0.083 Uiso 1 1 calc R . . C20 C 1.1013(8) -0.0717(8) 0.4038(4) 0.071(3) Uani 1 1 d . . . H20 H 1.0920 -0.1352 0.3982 0.085 Uiso 1 1 calc R . . C21 C 1.0981(8) -0.0387(9) 0.4459(4) 0.068(3) Uani 1 1 d . . . C22 C 1.1131(8) 0.0555(9) 0.4538(4) 0.074(3) Uani 1 1 d . . . H22 H 1.1141 0.0776 0.4826 0.089 Uiso 1 1 calc R . . C23 C 1.1267(7) 0.1171(8) 0.4193(4) 0.063(3) Uani 1 1 d . . . H23 H 1.1333 0.1808 0.4250 0.076 Uiso 1 1 calc R . . C25 C 1.0517(7) 0.1806(7) 0.2335(3) 0.058(3) Uani 1 1 d . . . C26 C 0.9738(8) 0.2349(8) 0.2367(4) 0.074(3) Uani 1 1 d . . . H26 H 0.9642 0.2710 0.2617 0.089 Uiso 1 1 calc R . . C27 C 0.9083(9) 0.2371(9) 0.2029(4) 0.083(4) Uani 1 1 d . . . H27 H 0.8557 0.2753 0.2050 0.100 Uiso 1 1 calc R . . C30 C 1.0648(8) 0.1250(8) 0.1966(3) 0.066(3) Uani 1 1 d . . . H30 H 1.1178 0.0874 0.1942 0.079 Uiso 1 1 calc R . . N1 N 1.1490(5) 0.3522(5) 0.3419(2) 0.052(2) Uani 1 1 d . . . N2 N 1.3192(6) 0.1210(6) 0.2682(2) 0.054(2) Uani 1 1 d . . . N3 N 1.1477(5) 0.1493(6) 0.3418(3) 0.053(2) Uani 1 1 d . . . N4 N 1.1211(6) 0.1808(6) 0.2681(2) 0.053(2) Uani 1 1 d . . . O1 O 0.9073(6) 0.4158(6) 0.4828(3) 0.092(3) Uani 1 1 d . . . O2 O 1.3103(7) -0.1469(7) 0.1331(4) 0.113(3) Uani 1 1 d . . . Cl1 Cl 1.2500 0.2500 0.18697(10) 0.0585(8) Uani 1 2 d S . . Ru1 Ru 1.2500 0.2500 0.34184(3) 0.0429(3) Uani 1 2 d S . . Ru2 Ru 1.2500 0.2500 0.26529(3) 0.0422(3) Uani 1 2 d S . . 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 C8 0.104(13) 0.152(15) 0.119(12) 0.015(11) 0.044(10) 0.026(12) C14 0.066(7) 0.081(8) 0.067(7) -0.019(6) 0.003(5) 0.008(7) C24 0.159(15) 0.087(12) 0.129(13) 0.045(10) -0.010(12) -0.022(11) C28 0.073(8) 0.067(8) 0.085(8) 0.007(7) -0.022(7) -0.006(7) C29 0.092(8) 0.054(7) 0.072(7) -0.007(6) -0.015(6) -0.007(6) C31 0.167(16) 0.103(12) 0.110(12) -0.007(9) -0.068(11) -0.020(11) O5 0.116(7) 0.080(6) 0.078(6) 0.036(5) 0.011(5) 0.000(5) O6 0.114(7) 0.092(7) 0.135(9) -0.001(6) -0.070(7) 0.007(6) C1 0.057(6) 0.048(6) 0.066(7) 0.001(5) 0.003(5) 0.011(5) C2 0.064(7) 0.046(6) 0.052(6) -0.004(5) 0.005(5) 0.003(5) C3 0.066(7) 0.081(8) 0.054(6) -0.003(5) -0.003(5) 0.006(6) C4 0.051(6) 0.086(9) 0.076(8) 0.002(6) 0.007(5) -0.002(6) C5 0.073(8) 0.061(7) 0.073(8) 0.003(6) 0.016(6) 0.003(6) C6 0.077(8) 0.080(8) 0.066(7) -0.010(6) 0.002(6) -0.007(7) C7 0.062(6) 0.061(7) 0.058(7) -0.001(5) 0.004(5) 0.007(5) C10 0.054(6) 0.053(6) 0.065(7) -0.004(5) -0.005(5) 0.010(5) C11 0.100(10) 0.050(7) 0.082(8) -0.003(6) 0.012(6) -0.004(7) C12 0.082(9) 0.053(7) 0.117(11) -0.020(7) 0.013(8) -0.009(6) C13 0.067(7) 0.068(8) 0.093(9) -0.019(7) -0.004(7) 0.006(6) C15 0.055(6) 0.065(7) 0.069(7) -0.015(6) 0.004(5) -0.005(5) C16 0.108(12) 0.162(16) 0.104(12) -0.059(11) 0.008(9) 0.024(11) C17 0.051(6) 0.054(6) 0.065(7) 0.005(5) -0.003(5) -0.007(5) C18 0.056(6) 0.058(7) 0.045(5) 0.001(5) 0.004(4) -0.003(5) C19 0.094(8) 0.061(7) 0.052(6) -0.005(5) -0.002(5) -0.005(6) C20 0.086(8) 0.048(6) 0.078(8) 0.006(6) -0.004(6) 0.001(6) C21 0.065(7) 0.072(8) 0.068(7) 0.015(6) 0.001(5) 0.003(6) C22 0.087(8) 0.067(8) 0.067(7) -0.001(6) 0.011(6) 0.008(7) C23 0.066(7) 0.061(7) 0.063(7) 0.005(5) -0.001(5) -0.008(6) C25 0.060(6) 0.046(6) 0.066(7) 0.009(5) -0.002(5) -0.005(5) C26 0.056(6) 0.092(10) 0.074(7) -0.013(6) -0.005(5) 0.000(6) C27 0.061(7) 0.078(9) 0.111(11) -0.008(8) -0.013(6) 0.008(7) C30 0.072(7) 0.055(6) 0.071(7) -0.003(5) -0.018(6) 0.004(6) N1 0.059(5) 0.050(5) 0.047(5) 0.000(4) 0.006(4) 0.010(4) N2 0.058(5) 0.049(5) 0.055(5) -0.002(4) 0.000(4) 0.005(4) N3 0.053(5) 0.058(5) 0.049(5) 0.008(4) -0.003(4) -0.008(4) N4 0.055(5) 0.050(5) 0.054(5) 0.003(4) -0.003(4) -0.007(4) O1 0.090(6) 0.104(7) 0.081(6) -0.011(5) 0.033(5) 0.002(6) O2 0.098(7) 0.108(7) 0.133(9) -0.068(7) -0.002(6) -0.009(6) Cl1 0.069(2) 0.065(2) 0.0422(15) 0.000 0.000 0.000(2) Ru1 0.0452(6) 0.0418(6) 0.0418(6) 0.000 0.000 0.0000(6) Ru2 0.0452(6) 0.0419(6) 0.0394(5) 0.000 0.000 -0.0001(5) _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 C8 O1 1.413(16) . ? C14 C13 1.353(16) . ? C14 C15 1.391(14) . ? C24 O5 1.413(16) . ? C28 C29 1.352(16) . ? C28 C27 1.376(16) . ? C28 O6 1.404(13) . ? C29 C30 1.390(14) . ? C31 O6 1.376(16) . ? O5 C21 1.374(12) . ? C1 N2 1.312(11) 2_755 ? C1 N1 1.338(12) . ? C2 C3 1.361(14) . ? C2 C7 1.399(14) . ? C2 N1 1.400(12) . ? C3 C4 1.410(14) . ? C4 C5 1.364(15) . ? C5 O1 1.378(12) . ? C5 C6 1.389(16) . ? C6 C7 1.381(14) . ? C10 C11 1.365(15) . ? C10 C15 1.394(13) . ? C10 N2 1.450(12) . ? C11 C12 1.397(15) . ? C12 C13 1.381(16) . ? C13 O2 1.405(14) . ? C16 O2 1.373(16) . ? C17 N4 1.318(11) . ? C17 N3 1.338(12) . ? C18 C19 1.356(14) . ? C18 C23 1.402(14) . ? C18 N3 1.409(12) . ? C19 C20 1.420(14) . ? C20 C21 1.365(15) . ? C21 C22 1.381(16) . ? C22 C23 1.382(15) . ? C25 C26 1.357(14) . ? C25 C30 1.386(13) . ? C25 N4 1.445(12) . ? C26 C27 1.388(15) . ? N1 Ru1 2.049(7) . ? N2 C1 1.312(11) 2_755 ? N2 Ru2 2.089(8) . ? N3 Ru1 2.047(8) . ? N4 Ru2 2.087(8) . ? Cl1 Ru2 2.382(3) . ? Ru1 N3 2.047(8) 2_755 ? Ru1 N1 2.049(8) 2_755 ? Ru1 Ru2 2.3284(13) . ? Ru2 N4 2.087(8) 2_755 ? Ru2 N2 2.089(8) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 C14 C15 120.5(11) . . ? C29 C28 C27 120.6(11) . . ? C29 C28 O6 123.6(12) . . ? C27 C28 O6 115.8(12) . . ? C28 C29 C30 120.2(11) . . ? C21 O5 C24 116.3(11) . . ? C31 O6 C28 118.6(11) . . ? N2 C1 N1 122.2(9) 2_755 . ? C3 C2 C7 117.9(9) . . ? C3 C2 N1 122.8(9) . . ? C7 C2 N1 119.4(9) . . ? C2 C3 C4 122.0(10) . . ? C5 C4 C3 119.5(11) . . ? C4 C5 O1 125.7(12) . . ? C4 C5 C6 119.3(10) . . ? O1 C5 C6 115.0(11) . . ? C7 C6 C5 120.7(11) . . ? C6 C7 C2 120.6(10) . . ? C11 C10 C15 119.9(10) . . ? C11 C10 N2 120.1(9) . . ? C15 C10 N2 119.9(9) . . ? C10 C11 C12 120.4(11) . . ? C13 C12 C11 119.0(12) . . ? C14 C13 C12 120.8(11) . . ? C14 C13 O2 123.3(12) . . ? C12 C13 O2 115.8(12) . . ? C14 C15 C10 119.2(11) . . ? N4 C17 N3 121.5(9) . . ? C19 C18 C23 118.0(9) . . ? C19 C18 N3 123.1(9) . . ? C23 C18 N3 118.9(9) . . ? C18 C19 C20 121.5(10) . . ? C21 C20 C19 119.5(11) . . ? C20 C21 O5 125.4(12) . . ? C20 C21 C22 119.5(11) . . ? O5 C21 C22 115.1(11) . . ? C21 C22 C23 120.5(11) . . ? C22 C23 C18 120.7(11) . . ? C26 C25 C30 119.6(10) . . ? C26 C25 N4 120.5(10) . . ? C30 C25 N4 119.9(9) . . ? C25 C26 C27 120.7(11) . . ? C28 C27 C26 119.3(12) . . ? C25 C30 C29 119.6(11) . . ? C1 N1 C2 117.5(8) . . ? C1 N1 Ru1 117.0(6) . . ? C2 N1 Ru1 125.3(6) . . ? C1 N2 C10 116.4(8) 2_755 . ? C1 N2 Ru2 118.2(7) 2_755 . ? C10 N2 Ru2 125.2(6) . . ? C17 N3 C18 116.7(8) . . ? C17 N3 Ru1 117.5(6) . . ? C18 N3 Ru1 125.6(6) . . ? C17 N4 C25 116.3(8) . . ? C17 N4 Ru2 118.5(6) . . ? C25 N4 Ru2 125.0(6) . . ? C5 O1 C8 116.2(11) . . ? C16 O2 C13 118.4(11) . . ? N3 Ru1 N3 179.9(5) . 2_755 ? N3 Ru1 N1 90.1(3) . 2_755 ? N3 Ru1 N1 89.9(3) 2_755 2_755 ? N3 Ru1 N1 89.9(3) . . ? N3 Ru1 N1 90.1(3) 2_755 . ? N1 Ru1 N1 179.9(4) 2_755 . ? N3 Ru1 Ru2 90.0(2) . . ? N3 Ru1 Ru2 90.0(2) 2_755 . ? N1 Ru1 Ru2 90.0(2) 2_755 . ? N1 Ru1 Ru2 90.0(2) . . ? N4 Ru2 N4 175.3(4) 2_755 . ? N4 Ru2 N2 89.9(3) 2_755 2_755 ? N4 Ru2 N2 89.9(3) . 2_755 ? N4 Ru2 N2 89.9(3) 2_755 . ? N4 Ru2 N2 89.9(3) . . ? N2 Ru2 N2 175.2(4) 2_755 . ? N4 Ru2 Ru1 87.7(2) 2_755 . ? N4 Ru2 Ru1 87.7(2) . . ? N2 Ru2 Ru1 87.6(2) 2_755 . ? N2 Ru2 Ru1 87.6(2) . . ? N4 Ru2 Cl1 92.3(2) 2_755 . ? N4 Ru2 Cl1 92.3(2) . . ? N2 Ru2 Cl1 92.4(2) 2_755 . ? N2 Ru2 Cl1 92.4(2) . . ? Ru1 Ru2 Cl1 180.000(1) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.476 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.172