# Supplementary Material (ESI) for Green Chemistry # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Green Chemistry' _journal_coden_Cambridge 1048 _publ_contact_author_name 'Reyes Jimenez-Aparicio' _publ_contact_author_email REYESJA@QUIM.UCM.ES _publ_section_title ; First microwave synthesis of multiple metal-metal bond paddlewheel compounds ; loop_ _publ_author_name 'Reyes Jimenez-Aparicio' 'Santiago Herrero' 'Josefina Perles' 'Jose L Priego' 'Francisco A. Urbanos' # Attachment 'jru33.cif' data_jru33 _database_code_depnum_ccdc_archive 'CCDC 766373' #TrackingRef 'jru33.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H32 F8 N12 Ru2' _chemical_formula_sum 'C48 H32 F8 N12 Ru2' _chemical_formula_weight 1131.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 'P 21/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 9.6596(4) _cell_length_b 38.8963(17) _cell_length_c 12.5248(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.9890(10) _cell_angle_gamma 90.00 _cell_volume 4585.4(3) _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 purple _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7973 _exptl_absorpt_correction_T_max 0.8969 _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 43445 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 29.03 _reflns_number_total 11373 _reflns_number_gt 6961 _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^)+(0.0362P)^2^+7.9194P] 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 11373 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1869(5) 0.32972(11) 0.6873(3) 0.0404(10) Uani 1 1 d . . . C2 C 0.2783(5) 0.34535(14) 0.7732(4) 0.0536(12) Uani 1 1 d . . . H2 H 0.3431 0.3616 0.7603 0.064 Uiso 1 1 calc R . . C3 C 0.2731(7) 0.33662(17) 0.8801(4) 0.0751(18) Uani 1 1 d . . . H3 H 0.3338 0.3471 0.9394 0.090 Uiso 1 1 calc R . . C4 C 0.1790(8) 0.31296(18) 0.8959(4) 0.0754(19) Uani 1 1 d . . . C5 C 0.0868(7) 0.29668(16) 0.8122(5) 0.0776(18) Uani 1 1 d . . . H5 H 0.0224 0.2805 0.8263 0.093 Uiso 1 1 calc R . . C6 C 0.0925(6) 0.30511(13) 0.7060(4) 0.0612(14) Uani 1 1 d . . . H6 H 0.0327 0.2942 0.6473 0.073 Uiso 1 1 calc R . . C7 C 0.2869(5) 0.29391(10) 0.3700(3) 0.0362(9) Uani 1 1 d . . . C8 C 0.2467(5) 0.28927(12) 0.2579(3) 0.0504(12) Uani 1 1 d . . . H8 H 0.1736 0.3025 0.2165 0.060 Uiso 1 1 calc R . . C9 C 0.3152(6) 0.26492(13) 0.2067(4) 0.0558(13) Uani 1 1 d . . . H9 H 0.2897 0.2620 0.1311 0.067 Uiso 1 1 calc R . . C10 C 0.4189(5) 0.24563(12) 0.2682(4) 0.0524(12) Uani 1 1 d . . . C11 C 0.4580(5) 0.24870(13) 0.3797(4) 0.0556(13) Uani 1 1 d . . . H11 H 0.5278 0.2345 0.4204 0.067 Uiso 1 1 calc R . . C12 C 0.3925(5) 0.27319(12) 0.4309(4) 0.0466(11) Uani 1 1 d . . . H12 H 0.4193 0.2758 0.5065 0.056 Uiso 1 1 calc R . . C13 C 0.3789(4) 0.42474(10) 0.6304(3) 0.0353(9) Uani 1 1 d . . . C14 C 0.5165(5) 0.43697(13) 0.6452(4) 0.0520(12) Uani 1 1 d . . . H14 H 0.5669 0.4334 0.5911 0.062 Uiso 1 1 calc R . . C15 C 0.5799(6) 0.45443(15) 0.7393(4) 0.0649(15) Uani 1 1 d . . . H15 H 0.6725 0.4625 0.7489 0.078 Uiso 1 1 calc R . . C16 C 0.5046(6) 0.45974(14) 0.8185(4) 0.0603(14) Uani 1 1 d . . . C17 C 0.3699(6) 0.44785(14) 0.8076(4) 0.0586(14) Uani 1 1 d . . . H17 H 0.3209 0.4516 0.8626 0.070 Uiso 1 1 calc R . . C18 C 0.3061(5) 0.42998(12) 0.7126(4) 0.0479(11) Uani 1 1 d . . . H18 H 0.2142 0.4215 0.7044 0.057 Uiso 1 1 calc R . . C19 C 0.4186(4) 0.39041(12) 0.2927(3) 0.0405(10) Uani 1 1 d . . . C20 C 0.4679(5) 0.36116(14) 0.2516(4) 0.0542(13) Uani 1 1 d . . . H20 H 0.4526 0.3398 0.2800 0.065 Uiso 1 1 calc R . . C21 C 0.5405(6) 0.36354(17) 0.1678(4) 0.0676(15) Uani 1 1 d . . . H21 H 0.5734 0.3439 0.1389 0.081 Uiso 1 1 calc R . . C22 C 0.5621(6) 0.39524(18) 0.1294(4) 0.0681(16) Uani 1 1 d . . . C23 C 0.5158(6) 0.42471(16) 0.1682(4) 0.0711(17) Uani 1 1 d . . . H23 H 0.5326 0.4460 0.1395 0.085 Uiso 1 1 calc R . . C24 C 0.4428(6) 0.42234(13) 0.2520(4) 0.0573(13) Uani 1 1 d . . . H24 H 0.4105 0.4421 0.2804 0.069 Uiso 1 1 calc R . . C25 C -0.0786(5) 0.44977(11) 0.4733(3) 0.0390(10) Uani 1 1 d . . . C26 C -0.2141(5) 0.45742(14) 0.4151(4) 0.0566(13) Uani 1 1 d . . . H26 H -0.2497 0.4469 0.3478 0.068 Uiso 1 1 calc R . . C27 C -0.2973(6) 0.48062(15) 0.4560(5) 0.0686(16) Uani 1 1 d . . . H27 H -0.3878 0.4863 0.4164 0.082 Uiso 1 1 calc R . . C28 C -0.2435(6) 0.49497(13) 0.5556(5) 0.0575(14) Uani 1 1 d . . . C29 C -0.1124(6) 0.48781(12) 0.6157(4) 0.0540(13) Uani 1 1 d . . . H29 H -0.0790 0.4980 0.6838 0.065 Uiso 1 1 calc R . . C30 C -0.0286(5) 0.46483(11) 0.5734(4) 0.0450(11) Uani 1 1 d . . . H30 H 0.0623 0.4596 0.6134 0.054 Uiso 1 1 calc R . . C31 C 0.0395(5) 0.41907(11) 0.1596(3) 0.0373(10) Uani 1 1 d . . . C32 C 0.1156(5) 0.40102(12) 0.0964(3) 0.0493(12) Uani 1 1 d . . . H32 H 0.1728 0.3827 0.1271 0.059 Uiso 1 1 calc R . . C33 C 0.1074(6) 0.40997(15) -0.0125(4) 0.0604(14) Uani 1 1 d . . . H33 H 0.1582 0.3979 -0.0551 0.072 Uiso 1 1 calc R . . C34 C 0.0235(6) 0.43670(14) -0.0544(4) 0.0583(14) Uani 1 1 d . . . C35 C -0.0565(6) 0.45473(14) 0.0029(4) 0.0635(15) Uani 1 1 d . . . H35 H -0.1156 0.4725 -0.0300 0.076 Uiso 1 1 calc R . . C36 C -0.0475(6) 0.44590(13) 0.1122(4) 0.0552(13) Uani 1 1 d . . . H36 H -0.1001 0.4580 0.1535 0.066 Uiso 1 1 calc R . . C37 C -0.1708(5) 0.36130(11) 0.5619(3) 0.0384(10) Uani 1 1 d . . . C38 C -0.2983(5) 0.34399(13) 0.5468(4) 0.0546(13) Uani 1 1 d . . . H38 H -0.3352 0.3331 0.4804 0.066 Uiso 1 1 calc R . . C39 C -0.3717(6) 0.34270(14) 0.6298(4) 0.0613(14) Uani 1 1 d . . . H39 H -0.4579 0.3311 0.6195 0.074 Uiso 1 1 calc R . . C40 C -0.3161(5) 0.35858(14) 0.7262(4) 0.0549(13) Uani 1 1 d . . . C41 C -0.1921(5) 0.37652(14) 0.7440(4) 0.0603(14) Uani 1 1 d . . . H41 H -0.1566 0.3874 0.8107 0.072 Uiso 1 1 calc R . . C42 C -0.1202(5) 0.37825(12) 0.6601(4) 0.0500(12) Uani 1 1 d . . . H42 H -0.0368 0.3910 0.6699 0.060 Uiso 1 1 calc R . . C43 C -0.1136(5) 0.32045(12) 0.2352(3) 0.0416(10) Uani 1 1 d . . . C44 C -0.1064(6) 0.32877(15) 0.1305(4) 0.0604(14) Uani 1 1 d . . . H44 H -0.0765 0.3506 0.1152 0.072 Uiso 1 1 calc R . . C45 C -0.1439(6) 0.3047(2) 0.0471(4) 0.082(2) Uani 1 1 d . . . H45 H -0.1403 0.3103 -0.0244 0.098 Uiso 1 1 calc R . . C46 C -0.1857(7) 0.2730(2) 0.0710(6) 0.086(2) Uani 1 1 d . . . C47 C -0.2000(7) 0.26426(16) 0.1727(6) 0.084(2) Uani 1 1 d . . . H47 H -0.2345 0.2427 0.1857 0.101 Uiso 1 1 calc R . . C48 C -0.1624(6) 0.28792(14) 0.2568(5) 0.0651(15) Uani 1 1 d . . . H48 H -0.1697 0.2822 0.3274 0.078 Uiso 1 1 calc R . . N1 N 0.1882(4) 0.34027(9) 0.5776(2) 0.0353(8) Uani 1 1 d . . . N2 N 0.2278(4) 0.31460(9) 0.5230(3) 0.0399(8) Uani 1 1 d . . . N3 N 0.2211(4) 0.32105(8) 0.4189(3) 0.0363(8) Uani 1 1 d . . . N4 N 0.3070(4) 0.40642(8) 0.5337(3) 0.0347(8) Uani 1 1 d . . . N5 N 0.3860(4) 0.40547(9) 0.4607(3) 0.0370(8) Uani 1 1 d . . . N6 N 0.3331(4) 0.38720(9) 0.3729(3) 0.0368(8) Uani 1 1 d . . . N7 N 0.0097(4) 0.42643(8) 0.4297(3) 0.0360(8) Uani 1 1 d . . . N8 N -0.0058(4) 0.43200(9) 0.3244(3) 0.0383(8) Uani 1 1 d . . . N9 N 0.0543(4) 0.40903(9) 0.2721(3) 0.0354(8) Uani 1 1 d . . . N10 N -0.0842(4) 0.36240(9) 0.4831(3) 0.0362(8) Uani 1 1 d . . . N11 N -0.1359(4) 0.34406(9) 0.3958(3) 0.0399(8) Uani 1 1 d . . . N12 N -0.0574(4) 0.34365(9) 0.3225(3) 0.0389(8) Uani 1 1 d . . . F1 F 0.1723(5) 0.30458(13) 1.0005(3) 0.1272(17) Uani 1 1 d . . . F2 F 0.4875(3) 0.22194(8) 0.2192(2) 0.0762(9) Uani 1 1 d . . . F3 F 0.5664(4) 0.47738(10) 0.9105(3) 0.0953(12) Uani 1 1 d . . . F4 F 0.6316(4) 0.39806(12) 0.0462(3) 0.1108(14) Uani 1 1 d . . . F5 F -0.3250(4) 0.51790(9) 0.5969(3) 0.0886(11) Uani 1 1 d . . . F6 F 0.0162(4) 0.44599(9) -0.1615(2) 0.0874(11) Uani 1 1 d . . . F7 F -0.3862(4) 0.35720(10) 0.8088(3) 0.0923(12) Uani 1 1 d . . . F8 F -0.2161(4) 0.24886(13) -0.0097(4) 0.1321(18) Uani 1 1 d . . . Ru1 Ru 0.10997(4) 0.385660(9) 0.51406(2) 0.03282(9) Uani 1 1 d . . . Ru2 Ru 0.14044(4) 0.364341(9) 0.33923(2) 0.03377(9) 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 0.054(3) 0.040(2) 0.030(2) 0.0042(18) 0.015(2) 0.010(2) C2 0.060(3) 0.062(3) 0.037(3) 0.003(2) 0.007(2) 0.008(3) C3 0.094(5) 0.089(5) 0.037(3) 0.003(3) 0.004(3) 0.024(4) C4 0.106(5) 0.092(5) 0.036(3) 0.026(3) 0.033(3) 0.036(4) C5 0.100(5) 0.072(4) 0.074(4) 0.027(3) 0.047(4) 0.004(4) C6 0.086(4) 0.054(3) 0.047(3) 0.012(2) 0.022(3) -0.001(3) C7 0.046(3) 0.033(2) 0.031(2) -0.0041(17) 0.0125(19) 0.0036(19) C8 0.065(3) 0.052(3) 0.032(2) -0.001(2) 0.006(2) 0.017(2) C9 0.077(4) 0.059(3) 0.033(2) -0.005(2) 0.015(2) 0.019(3) C10 0.060(3) 0.047(3) 0.052(3) -0.014(2) 0.018(2) 0.010(2) C11 0.057(3) 0.056(3) 0.050(3) -0.008(2) 0.005(2) 0.021(3) C12 0.052(3) 0.052(3) 0.034(2) -0.002(2) 0.005(2) 0.009(2) C13 0.042(3) 0.035(2) 0.029(2) 0.0019(17) 0.0080(18) 0.0019(19) C14 0.053(3) 0.063(3) 0.042(3) -0.005(2) 0.016(2) -0.011(3) C15 0.056(3) 0.088(4) 0.049(3) -0.010(3) 0.010(3) -0.027(3) C16 0.070(4) 0.068(4) 0.039(3) -0.015(2) 0.005(3) -0.013(3) C17 0.066(4) 0.071(4) 0.041(3) -0.016(2) 0.018(3) 0.002(3) C18 0.045(3) 0.061(3) 0.039(2) -0.006(2) 0.014(2) 0.003(2) C19 0.033(2) 0.059(3) 0.031(2) -0.005(2) 0.0115(18) -0.004(2) C20 0.051(3) 0.060(3) 0.056(3) 0.003(2) 0.022(2) 0.008(3) C21 0.061(4) 0.090(4) 0.060(3) -0.011(3) 0.032(3) 0.009(3) C22 0.062(4) 0.105(5) 0.047(3) -0.012(3) 0.033(3) -0.016(3) C23 0.088(4) 0.078(4) 0.058(3) -0.002(3) 0.038(3) -0.024(3) C24 0.072(4) 0.054(3) 0.053(3) -0.009(2) 0.030(3) -0.013(3) C25 0.051(3) 0.033(2) 0.038(2) 0.0038(18) 0.021(2) 0.003(2) C26 0.049(3) 0.070(4) 0.051(3) -0.009(3) 0.010(2) 0.002(3) C27 0.050(3) 0.089(4) 0.069(4) 0.002(3) 0.019(3) 0.024(3) C28 0.069(4) 0.046(3) 0.068(4) 0.005(3) 0.040(3) 0.018(3) C29 0.086(4) 0.037(3) 0.047(3) -0.005(2) 0.031(3) 0.003(3) C30 0.056(3) 0.041(3) 0.040(2) -0.0002(19) 0.015(2) 0.004(2) C31 0.045(3) 0.037(2) 0.030(2) 0.0009(17) 0.0085(19) -0.0006(19) C32 0.061(3) 0.055(3) 0.032(2) 0.006(2) 0.009(2) 0.016(2) C33 0.072(4) 0.081(4) 0.032(2) -0.002(2) 0.021(2) 0.002(3) C34 0.076(4) 0.069(4) 0.030(2) 0.009(2) 0.010(2) -0.012(3) C35 0.080(4) 0.062(3) 0.043(3) 0.014(2) 0.003(3) 0.013(3) C36 0.071(4) 0.055(3) 0.040(3) 0.001(2) 0.013(2) 0.015(3) C37 0.044(3) 0.041(2) 0.033(2) 0.0042(18) 0.0157(19) 0.001(2) C38 0.055(3) 0.063(3) 0.047(3) -0.006(2) 0.014(2) -0.016(3) C39 0.059(3) 0.064(3) 0.068(3) -0.006(3) 0.029(3) -0.027(3) C40 0.054(3) 0.068(3) 0.051(3) -0.004(2) 0.029(2) -0.011(3) C41 0.056(3) 0.085(4) 0.045(3) -0.023(3) 0.022(2) -0.013(3) C42 0.041(3) 0.058(3) 0.056(3) -0.016(2) 0.023(2) -0.006(2) C43 0.037(2) 0.049(3) 0.038(2) -0.007(2) 0.0068(19) 0.003(2) C44 0.063(3) 0.078(4) 0.041(3) -0.009(3) 0.014(2) -0.012(3) C45 0.069(4) 0.135(6) 0.040(3) -0.034(4) 0.008(3) 0.003(4) C46 0.060(4) 0.105(6) 0.086(5) -0.061(4) 0.002(3) -0.001(4) C47 0.085(5) 0.061(4) 0.103(5) -0.036(4) 0.015(4) -0.016(3) C48 0.076(4) 0.056(3) 0.064(3) -0.013(3) 0.016(3) -0.013(3) N1 0.043(2) 0.040(2) 0.0241(16) 0.0004(14) 0.0102(15) 0.0039(16) N2 0.056(2) 0.037(2) 0.0290(18) 0.0043(15) 0.0141(17) 0.0056(17) N3 0.051(2) 0.0315(18) 0.0298(17) 0.0006(14) 0.0168(16) 0.0048(16) N4 0.040(2) 0.0373(19) 0.0280(17) 0.0042(14) 0.0108(15) 0.0020(16) N5 0.041(2) 0.043(2) 0.0295(18) 0.0007(15) 0.0123(16) -0.0002(16) N6 0.041(2) 0.042(2) 0.0304(17) 0.0008(15) 0.0144(15) 0.0029(17) N7 0.043(2) 0.0349(19) 0.0335(18) -0.0023(14) 0.0147(16) 0.0021(16) N8 0.050(2) 0.036(2) 0.0312(18) 0.0027(15) 0.0153(16) 0.0020(17) N9 0.042(2) 0.039(2) 0.0272(17) 0.0014(14) 0.0106(15) 0.0018(16) N10 0.038(2) 0.039(2) 0.0336(18) -0.0013(16) 0.0136(15) -0.0042(16) N11 0.043(2) 0.041(2) 0.0373(19) -0.0043(16) 0.0135(17) -0.0018(17) N12 0.048(2) 0.041(2) 0.0293(18) -0.0008(15) 0.0114(16) -0.0016(17) F1 0.161(4) 0.185(4) 0.048(2) 0.053(2) 0.051(2) 0.049(3) F2 0.090(2) 0.074(2) 0.069(2) -0.0216(17) 0.0247(17) 0.0320(18) F3 0.098(3) 0.126(3) 0.058(2) -0.043(2) 0.0083(18) -0.034(2) F4 0.120(3) 0.158(4) 0.080(2) -0.008(2) 0.076(2) -0.020(3) F5 0.108(3) 0.074(2) 0.102(3) -0.0026(19) 0.061(2) 0.036(2) F6 0.120(3) 0.111(3) 0.0313(15) 0.0218(16) 0.0166(17) -0.001(2) F7 0.093(3) 0.127(3) 0.075(2) -0.020(2) 0.058(2) -0.035(2) F8 0.099(3) 0.165(4) 0.122(3) -0.108(3) 0.003(2) -0.008(3) Ru1 0.0408(2) 0.03449(18) 0.02558(16) -0.00037(13) 0.01256(14) 0.00093(15) Ru2 0.0432(2) 0.03545(18) 0.02466(16) -0.00024(14) 0.01184(14) 0.00199(15) _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 1.372(6) . ? C1 C6 1.378(6) . ? C1 N1 1.437(5) . ? C2 C3 1.392(7) . ? C2 H2 0.9300 . ? C3 C4 1.339(9) . ? C3 H3 0.9300 . ? C4 F1 1.365(5) . ? C4 C5 1.369(9) . ? C5 C6 1.383(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.382(6) . ? C7 C12 1.386(6) . ? C7 N3 1.438(5) . ? C8 C9 1.392(6) . ? C8 H8 0.9300 . ? C9 C10 1.347(7) . ? C9 H9 0.9300 . ? C10 F2 1.360(5) . ? C10 C11 1.367(6) . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.384(6) . ? C13 C18 1.386(6) . ? C13 N4 1.442(5) . ? C14 C15 1.378(6) . ? C14 H14 0.9300 . ? C15 C16 1.371(7) . ? C15 H15 0.9300 . ? C16 C17 1.358(7) . ? C16 F3 1.359(5) . ? C17 C18 1.396(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.377(6) . ? C19 C24 1.382(6) . ? C19 N6 1.443(5) . ? C20 C21 1.390(6) . ? C20 H20 0.9300 . ? C21 C22 1.357(8) . ? C21 H21 0.9300 . ? C22 C23 1.359(8) . ? C22 F4 1.365(5) . ? C23 C24 1.393(6) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.370(6) . ? C25 C26 1.380(6) . ? C25 N7 1.434(5) . ? C26 C27 1.381(7) . ? C26 H26 0.9300 . ? C27 C28 1.358(7) . ? C27 H27 0.9300 . ? C28 C29 1.349(7) . ? C28 F5 1.365(5) . ? C29 C30 1.389(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.386(6) . ? C31 C36 1.387(6) . ? C31 N9 1.438(5) . ? C32 C33 1.393(6) . ? C32 H32 0.9300 . ? C33 C34 1.350(7) . ? C33 H33 0.9300 . ? C34 C35 1.361(7) . ? C34 F6 1.375(5) . ? C35 C36 1.396(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.379(6) . ? C37 C42 1.384(6) . ? C37 N10 1.431(5) . ? C38 C39 1.385(6) . ? C38 H38 0.9300 . ? C39 C40 1.355(7) . ? C39 H39 0.9300 . ? C40 F7 1.359(5) . ? C40 C41 1.360(7) . ? C41 C42 1.385(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.366(6) . ? C43 C48 1.398(7) . ? C43 N12 1.427(5) . ? C44 C45 1.390(7) . ? C44 H44 0.9300 . ? C45 C46 1.350(9) . ? C45 H45 0.9300 . ? C46 C47 1.355(9) . ? C46 F8 1.362(6) . ? C47 C48 1.385(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? N1 N2 1.314(4) . ? N1 Ru1 2.013(3) . ? N2 N3 1.316(4) . ? N3 Ru2 2.022(3) . ? N4 N5 1.317(4) . ? N4 Ru1 2.031(3) . ? N5 N6 1.313(4) . ? N6 Ru2 2.020(3) . ? N7 N8 1.312(4) . ? N7 Ru1 2.027(3) . ? N8 N9 1.317(4) . ? N9 Ru2 2.026(3) . ? N10 N11 1.307(4) . ? N10 Ru1 2.039(3) . ? N11 N12 1.316(4) . ? N12 Ru2 2.040(4) . ? Ru1 Ru2 2.4205(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.5(4) . . ? C2 C1 N1 118.8(4) . . ? C6 C1 N1 120.6(4) . . ? C1 C2 C3 119.4(5) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 118.8(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 F1 119.1(7) . . ? C3 C4 C5 123.4(5) . . ? F1 C4 C5 117.5(6) . . ? C4 C5 C6 117.9(6) . . ? C4 C5 H5 121.1 . . ? C6 C5 H5 121.1 . . ? C1 C6 C5 120.0(5) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C12 119.1(4) . . ? C8 C7 N3 118.6(4) . . ? C12 C7 N3 122.3(4) . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.0(4) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 F2 119.6(4) . . ? C9 C10 C11 122.4(4) . . ? F2 C10 C11 118.0(4) . . ? C10 C11 C12 119.0(5) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C7 120.3(4) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 118.8(4) . . ? C14 C13 N4 123.3(4) . . ? C18 C13 N4 117.8(4) . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 119.1(5) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 F3 119.1(5) . . ? C17 C16 C15 121.9(5) . . ? F3 C16 C15 119.1(5) . . ? C16 C17 C18 119.0(4) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C13 C18 C17 120.4(5) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C24 120.3(4) . . ? C20 C19 N6 119.2(4) . . ? C24 C19 N6 120.3(4) . . ? C19 C20 C21 120.1(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 118.2(5) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C21 C22 C23 123.4(5) . . ? C21 C22 F4 119.0(5) . . ? C23 C22 F4 117.6(6) . . ? C22 C23 C24 118.5(5) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C19 C24 C23 119.5(5) . . ? C19 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C30 C25 C26 119.3(4) . . ? C30 C25 N7 120.1(4) . . ? C26 C25 N7 120.7(4) . . ? C25 C26 C27 120.4(5) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 118.4(5) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C29 C28 C27 123.0(5) . . ? C29 C28 F5 118.2(5) . . ? C27 C28 F5 118.8(5) . . ? C28 C29 C30 118.3(5) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C25 C30 C29 120.6(5) . . ? C25 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C36 119.0(4) . . ? C32 C31 N9 118.2(4) . . ? C36 C31 N9 122.7(4) . . ? C31 C32 C33 120.8(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 118.1(5) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C33 C34 C35 123.6(4) . . ? C33 C34 F6 118.5(5) . . ? C35 C34 F6 117.9(5) . . ? C34 C35 C36 118.2(5) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C31 C36 C35 120.2(5) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C42 118.7(4) . . ? C38 C37 N10 124.2(4) . . ? C42 C37 N10 117.0(4) . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 119.0(5) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 F7 119.6(4) . . ? C39 C40 C41 122.6(4) . . ? F7 C40 C41 117.8(4) . . ? C40 C41 C42 118.3(4) . . ? C40 C41 H41 120.9 . . ? C42 C41 H41 120.9 . . ? C37 C42 C41 120.9(4) . . ? C37 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 C48 119.5(5) . . ? C44 C43 N12 119.5(4) . . ? C48 C43 N12 120.7(4) . . ? C43 C44 C45 120.0(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 119.2(6) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 122.4(6) . . ? C45 C46 F8 119.3(7) . . ? C47 C46 F8 118.2(7) . . ? C46 C47 C48 118.9(6) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C47 C48 C43 119.8(6) . . ? C47 C48 H48 120.1 . . ? C43 C48 H48 120.1 . . ? N2 N1 C1 110.3(3) . . ? N2 N1 Ru1 126.0(2) . . ? C1 N1 Ru1 123.0(3) . . ? N1 N2 N3 114.5(3) . . ? N2 N3 C7 110.7(3) . . ? N2 N3 Ru2 125.1(3) . . ? C7 N3 Ru2 124.0(2) . . ? N5 N4 C13 110.6(3) . . ? N5 N4 Ru1 125.3(3) . . ? C13 N4 Ru1 124.0(2) . . ? N6 N5 N4 114.8(3) . . ? N5 N6 C19 111.1(3) . . ? N5 N6 Ru2 125.5(2) . . ? C19 N6 Ru2 122.5(3) . . ? N8 N7 C25 109.6(3) . . ? N8 N7 Ru1 125.9(3) . . ? C25 N7 Ru1 123.5(3) . . ? N7 N8 N9 115.1(3) . . ? N8 N9 C31 110.2(3) . . ? N8 N9 Ru2 124.2(2) . . ? C31 N9 Ru2 125.5(3) . . ? N11 N10 C37 112.8(3) . . ? N11 N10 Ru1 124.3(2) . . ? C37 N10 Ru1 122.5(3) . . ? N10 N11 N12 114.7(3) . . ? N11 N12 C43 111.3(3) . . ? N11 N12 Ru2 126.6(3) . . ? C43 N12 Ru2 120.9(3) . . ? N1 Ru1 N7 170.13(13) . . ? N1 Ru1 N4 92.44(13) . . ? N7 Ru1 N4 94.43(13) . . ? N1 Ru1 N10 86.19(14) . . ? N7 Ru1 N10 86.36(14) . . ? N4 Ru1 N10 174.96(13) . . ? N1 Ru1 Ru2 86.89(9) . . ? N7 Ru1 Ru2 86.42(9) . . ? N4 Ru1 Ru2 86.83(9) . . ? N10 Ru1 Ru2 88.25(9) . . ? N6 Ru2 N3 91.65(14) . . ? N6 Ru2 N9 88.97(14) . . ? N3 Ru2 N9 174.78(12) . . ? N6 Ru2 N12 173.16(13) . . ? N3 Ru2 N12 88.31(14) . . ? N9 Ru2 N12 90.46(14) . . ? N6 Ru2 Ru1 87.37(9) . . ? N3 Ru2 Ru1 87.18(9) . . ? N9 Ru2 Ru1 87.67(9) . . ? N12 Ru2 Ru1 85.80(9) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.838 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.096