# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nicholas Fletcher' _publ_contact_author_email n.fletcher@qub.ac.uk loop_ _publ_author_name N.Baker N.Fletcher P.Horton M.Hursthouse data_2006src1519sq _database_code_depnum_ccdc_archive 'CCDC 859683' #TrackingRef '- RuL3PF6.cif' #There was some highly disordered solvent molecules in the #asymmetric unit that was removed from the calculations using #the SQUEEZE program. _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. N. Fletcher ; _chemical_name_common 'Dr. N. Fletcher' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H36 F12 N10 O3 P2 Ru' _chemical_formula_weight 1083.79 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.497(2) _cell_length_b 14.048(2) _cell_length_c 16.370(3) _cell_angle_alpha 65.572(9) _cell_angle_beta 89.168(7) _cell_angle_gamma 62.936(8) _cell_volume 2458.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2947 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Blade _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9193 _exptl_absorpt_correction_T_max 0.9766 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 21398 reflections reduced R(int) from 0.1762 to 0.0778 Ratio of minimum to maximum apparent transmission: 0.610346 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30256 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.1238 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10255 _reflns_number_gt 5393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. Both geometrical (SAME) and thermal (SIMU) parameters were restrained for the PF6 anions. ; _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^)+(0.1224P)^2^+14.3051P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10255 _refine_ls_number_parameters 668 _refine_ls_number_restraints 354 _refine_ls_R_factor_all 0.2123 _refine_ls_R_factor_gt 0.1316 _refine_ls_wR_factor_ref 0.3252 _refine_ls_wR_factor_gt 0.2851 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _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 0.0091(11) 0.3208(11) 1.0301(10) 0.093(4) Uani 1 1 d . . . H1A H -0.0063 0.3676 1.0648 0.112 Uiso 1 1 calc R . . H1B H -0.0459 0.2910 1.0381 0.112 Uiso 1 1 calc R . . C2 C -0.0102(12) 0.4026(10) 0.9302(8) 0.088(4) Uani 1 1 d . . . H2A H -0.0871 0.4740 0.9100 0.106 Uiso 1 1 calc R . . H2B H 0.0463 0.4306 0.9213 0.106 Uiso 1 1 calc R . . C3 C -0.0739(9) 0.3935(9) 0.7958(7) 0.064(3) Uani 1 1 d . . . C4 C -0.0486(8) 0.3145(10) 0.7496(7) 0.065(3) Uani 1 1 d . . . C5 C 0.0593(9) 0.2322(9) 0.7508(7) 0.066(3) Uani 1 1 d . . . H5 H 0.1218 0.2306 0.7784 0.079 Uiso 1 1 calc R . . C6 C -0.1366(9) 0.3195(11) 0.7035(8) 0.083(4) Uani 1 1 d . . . H6 H -0.2129 0.3773 0.6970 0.100 Uiso 1 1 calc R . . C7 C -0.1151(9) 0.2416(12) 0.6669(7) 0.078(3) Uani 1 1 d . . . H7 H -0.1764 0.2455 0.6353 0.093 Uiso 1 1 calc R . . C8 C -0.0044(9) 0.1579(11) 0.6763(7) 0.068(3) Uani 1 1 d . . . C9 C 0.0287(9) 0.0580(11) 0.6527(7) 0.068(3) Uani 1 1 d . . . C10 C -0.0454(11) 0.0338(14) 0.6206(8) 0.083(4) Uani 1 1 d . . . H10 H -0.1248 0.0884 0.6065 0.099 Uiso 1 1 calc R . . C11 C -0.0105(13) -0.0640(14) 0.6081(9) 0.091(4) Uani 1 1 d . . . H11 H -0.0636 -0.0803 0.5874 0.109 Uiso 1 1 calc R . . C12 C 0.1070(12) -0.1415(12) 0.6265(8) 0.082(3) Uani 1 1 d . . . H12 H 0.1354 -0.2114 0.6177 0.099 Uiso 1 1 calc R . . C13 C 0.1802(10) -0.1149(11) 0.6573(7) 0.071(3) Uani 1 1 d . . . H13 H 0.2600 -0.1669 0.6696 0.086 Uiso 1 1 calc R . . C14 C 0.1997(11) 0.2536(11) 1.0975(9) 0.082(3) Uani 1 1 d . . . H14A H 0.1857 0.2559 1.1564 0.099 Uiso 1 1 calc R . . H14B H 0.1781 0.3362 1.0508 0.099 Uiso 1 1 calc R . . C15 C 0.3257(10) 0.1723(11) 1.1090(9) 0.079(3) Uani 1 1 d . . . H15A H 0.3703 0.1963 1.1358 0.095 Uiso 1 1 calc R . . H15B H 0.3470 0.0883 1.1519 0.095 Uiso 1 1 calc R . . C16 C 0.3618(9) 0.0991(11) 0.9946(7) 0.064(3) Uani 1 1 d . . . C17 C 0.3643(8) 0.1306(10) 0.8958(8) 0.067(3) Uani 1 1 d . . . C18 C 0.3445(8) 0.0621(10) 0.8664(7) 0.060(3) Uani 1 1 d . . . H18 H 0.3460 -0.0087 0.9110 0.072 Uiso 1 1 calc R . . C19 C 0.3740(12) 0.2246(12) 0.8295(10) 0.089(4) Uani 1 1 d . . . H19 H 0.3926 0.2720 0.8471 0.107 Uiso 1 1 calc R . . C20 C 0.3571(12) 0.2508(12) 0.7382(9) 0.088(4) Uani 1 1 d . . . H20 H 0.3667 0.3140 0.6937 0.106 Uiso 1 1 calc R . . C21 C 0.3263(9) 0.1850(10) 0.7116(8) 0.068(3) Uani 1 1 d . . . C22 C 0.2927(10) 0.2135(11) 0.6151(8) 0.072(3) Uani 1 1 d . . . C23 C 0.2967(10) 0.3030(10) 0.5398(8) 0.083(4) Uani 1 1 d . . . H23 H 0.3226 0.3521 0.5472 0.100 Uiso 1 1 calc R . . C24 C 0.2633(11) 0.3205(12) 0.4551(9) 0.093(4) Uani 1 1 d . . . H24 H 0.2647 0.3829 0.4023 0.112 Uiso 1 1 calc R . . C25 C 0.2268(11) 0.2464(13) 0.4452(8) 0.088(4) Uani 1 1 d . . . H25 H 0.2043 0.2563 0.3863 0.106 Uiso 1 1 calc R . . C26 C 0.2248(9) 0.1596(11) 0.5232(8) 0.080(3) Uani 1 1 d . . . H26 H 0.2018 0.1074 0.5179 0.096 Uiso 1 1 calc R . . C27 C 0.1306(11) 0.1148(11) 1.1520(8) 0.076(3) Uani 1 1 d . . . H27A H 0.0872 0.1458 1.1930 0.091 Uiso 1 1 calc R . . H27B H 0.2107 0.0574 1.1859 0.091 Uiso 1 1 calc R . . C28 C 0.0819(12) 0.0497(11) 1.1280(8) 0.079(3) Uani 1 1 d . . . H28A H 0.0759 -0.0090 1.1850 0.094 Uiso 1 1 calc R . . H28B H 0.0043 0.1083 1.0893 0.094 Uiso 1 1 calc R . . C29 C 0.1387(10) -0.0951(9) 1.0646(7) 0.064(3) Uani 1 1 d . . . C30 C 0.2140(8) -0.1415(9) 1.0071(6) 0.056(2) Uani 1 1 d . . . C31 C 0.1889(9) -0.0694(9) 0.9154(6) 0.056(2) Uani 1 1 d . . . H31 H 0.1202 0.0056 0.8907 0.068 Uiso 1 1 calc R . . C32 C 0.3076(9) -0.2551(10) 1.0428(7) 0.068(3) Uani 1 1 d . . . H32 H 0.3242 -0.3098 1.1059 0.081 Uiso 1 1 calc R . . C33 C 0.3766(9) -0.2883(9) 0.9859(8) 0.065(3) Uani 1 1 d . . . H33 H 0.4411 -0.3665 1.0096 0.078 Uiso 1 1 calc R . . C34 C 0.3516(9) -0.2066(9) 0.8929(7) 0.058(2) Uani 1 1 d . . . C35 C 0.4265(8) -0.2246(9) 0.8292(7) 0.058(2) Uani 1 1 d . . . C36 C 0.5256(9) -0.3300(10) 0.8493(8) 0.071(3) Uani 1 1 d . . . H36 H 0.5480 -0.3974 0.9077 0.085 Uiso 1 1 calc R . . C37 C 0.5919(10) -0.3385(11) 0.7860(9) 0.073(3) Uani 1 1 d . . . H37 H 0.6594 -0.4116 0.7991 0.087 Uiso 1 1 calc R . . C38 C 0.5584(10) -0.2390(12) 0.7033(9) 0.081(3) Uani 1 1 d . . . H38 H 0.6025 -0.2417 0.6577 0.097 Uiso 1 1 calc R . . C39 C 0.4617(9) -0.1365(11) 0.6871(8) 0.071(3) Uani 1 1 d . . . H39 H 0.4398 -0.0688 0.6290 0.086 Uiso 1 1 calc R . . N1 N 0.1265(8) 0.2159(8) 1.0697(6) 0.069(2) Uani 1 1 d . . . N2 N -0.0001(8) 0.3413(8) 0.8737(7) 0.079(3) Uani 1 1 d . . . H2 H 0.0567 0.2678 0.8922 0.094 Uiso 1 1 calc R . . N3 N 0.3534(8) 0.1796(9) 1.0206(6) 0.073(2) Uani 1 1 d . . . H3 H 0.3647 0.2388 0.9839 0.088 Uiso 1 1 calc R . . N4 N 0.1538(8) -0.0141(8) 1.0781(6) 0.068(2) Uani 1 1 d . . . H4 H 0.2077 0.0016 1.0567 0.082 Uiso 1 1 calc R . . N5 N 0.0839(6) 0.1546(7) 0.7166(5) 0.056(2) Uani 1 1 d . . . N6 N 0.1417(7) -0.0163(8) 0.6707(5) 0.062(2) Uani 1 1 d . . . N7 N 0.3227(6) 0.0904(7) 0.7760(5) 0.056(2) Uani 1 1 d . . . N8 N 0.2539(7) 0.1455(8) 0.6066(6) 0.067(2) Uani 1 1 d . . . N9 N 0.2550(7) -0.0966(7) 0.8559(6) 0.060(2) Uani 1 1 d . . . N10 N 0.3939(7) -0.1238(7) 0.7478(6) 0.060(2) Uani 1 1 d . . . O1 O -0.1532(7) 0.4924(7) 0.7630(5) 0.089(3) Uani 1 1 d . . . O2 O 0.3625(7) 0.0045(7) 1.0454(5) 0.075(2) Uani 1 1 d . . . O3 O 0.0666(7) -0.1236(6) 1.0927(5) 0.0682(19) Uani 1 1 d . . . Ru1 Ru 0.24368(7) 0.02277(8) 0.72817(5) 0.0554(3) Uani 1 1 d . . . F1 F 0.5640(6) 0.0536(7) 0.6710(5) 0.100(2) Uani 1 1 d DU . . F2 F 0.5405(6) 0.2006(7) 0.5338(6) 0.131(3) Uani 1 1 d DU . . F3 F 0.5743(7) 0.0245(8) 0.5453(5) 0.111(2) Uani 1 1 d DU . . F4 F 0.7315(6) -0.0683(7) 0.6531(5) 0.105(2) Uani 1 1 d DU . . F5 F 0.6972(6) 0.1076(7) 0.6431(5) 0.105(2) Uani 1 1 d DU . . F6 F 0.7084(6) 0.0783(8) 0.5168(5) 0.110(2) Uani 1 1 d DU . . P1 P 0.6354(3) 0.0666(4) 0.5938(2) 0.0898(11) Uani 1 1 d DU . . F11 F 0.1916(12) 0.6727(10) 0.8405(12) 0.162(6) Uani 0.774(10) 1 d PDU A 1 F12 F 0.2562(10) 0.5172(9) 0.9805(6) 0.122(4) Uani 0.774(10) 1 d PDU A 1 F13 F 0.1821(10) 0.5032(13) 0.8705(10) 0.147(4) Uani 0.774(10) 1 d PDU A 1 F14 F 0.2998(12) 0.5465(14) 0.7854(8) 0.170(6) Uani 0.774(10) 1 d PDU A 1 F15 F 0.3782(9) 0.5548(10) 0.9003(10) 0.122(4) Uani 0.774(10) 1 d PDU A 1 F16 F 0.3693(9) 0.3927(8) 0.9287(8) 0.115(3) Uani 0.774(10) 1 d PDU A 1 P11 P 0.2778(6) 0.5333(6) 0.8826(4) 0.1012(19) Uani 0.774(10) 1 d PDU A 1 F111 F 0.185(3) 0.657(3) 0.841(3) 0.142(10) Uani 0.226(10) 1 d PDU A 2 F112 F 0.350(3) 0.526(3) 0.9447(19) 0.115(8) Uani 0.226(10) 1 d PDU A 2 F113 F 0.236(3) 0.461(3) 0.913(2) 0.128(8) Uani 0.226(10) 1 d PDU A 2 F114 F 0.239(3) 0.545(4) 0.767(2) 0.137(11) Uani 0.226(10) 1 d PDU A 2 F115 F 0.351(3) 0.609(3) 0.798(2) 0.128(9) Uani 0.226(10) 1 d PDU A 2 F116 F 0.403(3) 0.415(2) 0.870(3) 0.126(9) Uani 0.226(10) 1 d PDU A 2 P111 P 0.295(2) 0.535(2) 0.8567(15) 0.123(5) Uani 0.226(10) 1 d PDU A 2 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 0.089(9) 0.078(8) 0.114(11) -0.056(8) 0.025(8) -0.031(7) C2 0.092(9) 0.056(7) 0.084(8) -0.029(6) 0.006(7) -0.014(6) C3 0.056(6) 0.054(6) 0.056(6) -0.021(5) 0.016(5) -0.010(5) C4 0.043(6) 0.083(7) 0.048(5) -0.023(5) 0.018(4) -0.022(5) C5 0.051(6) 0.065(6) 0.067(6) -0.019(5) 0.025(5) -0.028(5) C6 0.043(6) 0.087(8) 0.072(7) -0.032(7) 0.009(5) 0.001(6) C7 0.040(6) 0.123(10) 0.066(7) -0.047(7) 0.016(5) -0.034(6) C8 0.044(6) 0.099(8) 0.051(6) -0.033(6) 0.018(5) -0.030(6) C9 0.058(7) 0.092(8) 0.051(6) -0.037(6) 0.023(5) -0.031(6) C10 0.079(8) 0.122(11) 0.075(8) -0.051(8) 0.032(7) -0.065(8) C11 0.100(11) 0.115(11) 0.073(8) -0.041(8) 0.026(7) -0.067(10) C12 0.091(10) 0.091(9) 0.061(7) -0.032(6) 0.014(6) -0.044(8) C13 0.075(7) 0.088(8) 0.044(5) -0.030(5) 0.027(5) -0.036(7) C14 0.107(10) 0.076(8) 0.091(8) -0.055(7) 0.037(7) -0.052(8) C15 0.077(8) 0.087(8) 0.100(9) -0.061(7) 0.019(7) -0.045(7) C16 0.063(7) 0.092(8) 0.062(6) -0.048(6) 0.020(5) -0.047(6) C17 0.045(6) 0.077(7) 0.084(8) -0.045(6) 0.017(5) -0.026(5) C18 0.051(6) 0.072(7) 0.058(6) -0.034(5) 0.017(5) -0.028(5) C19 0.116(11) 0.103(10) 0.100(10) -0.063(8) 0.045(8) -0.078(9) C20 0.118(11) 0.098(9) 0.084(9) -0.044(7) 0.044(8) -0.078(9) C21 0.066(7) 0.069(7) 0.084(8) -0.044(6) 0.038(6) -0.037(6) C22 0.067(7) 0.084(8) 0.065(7) -0.043(6) 0.032(6) -0.029(6) C23 0.074(8) 0.068(7) 0.075(8) -0.028(6) 0.041(6) -0.015(6) C24 0.081(9) 0.076(8) 0.067(8) -0.024(7) 0.032(6) -0.004(7) C25 0.075(8) 0.095(10) 0.062(7) -0.037(7) 0.020(6) -0.017(7) C26 0.061(7) 0.093(9) 0.058(7) -0.025(6) 0.027(5) -0.026(6) C27 0.112(10) 0.090(8) 0.068(7) -0.052(6) 0.044(7) -0.067(8) C28 0.118(10) 0.097(9) 0.062(7) -0.051(6) 0.048(7) -0.071(8) C29 0.082(8) 0.056(6) 0.049(5) -0.024(5) 0.021(5) -0.031(6) C30 0.059(6) 0.062(6) 0.047(5) -0.025(5) 0.019(4) -0.029(5) C31 0.059(6) 0.057(6) 0.059(6) -0.034(5) 0.019(5) -0.027(5) C32 0.070(7) 0.067(7) 0.058(6) -0.025(5) 0.024(5) -0.031(6) C33 0.054(6) 0.047(6) 0.082(7) -0.029(5) 0.016(5) -0.017(5) C34 0.061(6) 0.051(6) 0.071(6) -0.034(5) 0.023(5) -0.030(5) C35 0.051(6) 0.054(6) 0.071(6) -0.038(5) 0.013(5) -0.018(5) C36 0.050(6) 0.064(7) 0.087(8) -0.045(6) 0.010(5) -0.010(5) C37 0.062(7) 0.076(8) 0.101(9) -0.067(8) 0.022(6) -0.025(6) C38 0.058(7) 0.092(9) 0.102(10) -0.066(8) 0.039(7) -0.026(7) C39 0.066(7) 0.090(8) 0.068(7) -0.045(6) 0.014(5) -0.039(7) N1 0.078(6) 0.065(5) 0.083(6) -0.050(5) 0.028(5) -0.035(5) N2 0.080(6) 0.055(5) 0.083(7) -0.036(5) 0.017(5) -0.015(5) N3 0.078(6) 0.085(6) 0.083(6) -0.054(6) 0.028(5) -0.047(5) N4 0.084(6) 0.072(6) 0.069(5) -0.044(5) 0.040(5) -0.043(5) N5 0.036(4) 0.062(5) 0.049(4) -0.024(4) 0.019(3) -0.010(4) N6 0.056(5) 0.077(6) 0.051(5) -0.031(4) 0.019(4) -0.031(5) N7 0.045(4) 0.062(5) 0.061(5) -0.031(4) 0.022(4) -0.025(4) N8 0.047(5) 0.073(6) 0.055(5) -0.021(4) 0.015(4) -0.017(4) N9 0.052(5) 0.070(5) 0.061(5) -0.039(4) 0.009(4) -0.026(4) N10 0.051(5) 0.063(5) 0.080(6) -0.051(5) 0.035(4) -0.021(4) O1 0.073(5) 0.063(5) 0.074(5) -0.022(4) 0.017(4) 0.001(4) O2 0.080(5) 0.075(5) 0.074(5) -0.036(4) 0.017(4) -0.040(4) O3 0.082(5) 0.071(5) 0.061(4) -0.036(4) 0.032(4) -0.041(4) Ru1 0.0470(5) 0.0659(5) 0.0512(5) -0.0294(4) 0.0204(3) -0.0240(4) F1 0.083(5) 0.146(6) 0.088(5) -0.060(4) 0.039(4) -0.064(5) F2 0.082(5) 0.132(7) 0.127(7) -0.027(5) 0.023(5) -0.041(5) F3 0.107(5) 0.173(7) 0.083(5) -0.064(5) 0.032(4) -0.087(5) F4 0.083(5) 0.123(6) 0.087(5) -0.048(4) 0.019(4) -0.034(4) F5 0.093(5) 0.138(6) 0.123(6) -0.083(5) 0.043(4) -0.065(5) F6 0.087(5) 0.146(6) 0.098(5) -0.056(5) 0.039(4) -0.060(5) P1 0.069(2) 0.129(3) 0.076(2) -0.052(2) 0.0273(16) -0.049(2) F11 0.123(8) 0.099(7) 0.145(9) 0.008(7) 0.013(7) -0.021(7) F12 0.127(7) 0.110(7) 0.095(6) -0.045(5) 0.032(6) -0.034(6) F13 0.119(8) 0.176(9) 0.163(10) -0.074(8) 0.017(7) -0.088(7) F14 0.121(9) 0.188(9) 0.131(8) -0.056(7) 0.042(7) -0.040(8) F15 0.115(7) 0.099(6) 0.160(8) -0.053(6) 0.015(6) -0.065(5) F16 0.129(7) 0.091(5) 0.149(8) -0.066(6) 0.040(6) -0.064(5) P11 0.111(4) 0.101(3) 0.099(4) -0.041(3) 0.019(3) -0.061(3) F111 0.120(11) 0.108(11) 0.126(11) -0.018(11) 0.021(11) -0.034(11) F112 0.124(10) 0.098(10) 0.115(10) -0.049(9) 0.017(10) -0.049(10) F113 0.124(10) 0.123(9) 0.128(10) -0.051(9) 0.019(9) -0.059(9) F114 0.121(15) 0.159(13) 0.127(14) -0.073(12) 0.013(13) -0.060(13) F115 0.121(12) 0.122(11) 0.145(12) -0.058(11) 0.030(11) -0.066(10) F116 0.145(14) 0.094(12) 0.146(15) -0.066(12) 0.020(13) -0.055(12) P111 0.122(6) 0.114(6) 0.124(7) -0.047(6) 0.017(6) -0.057(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 C1 N1 1.489(15) . ? C1 C2 1.499(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.471(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O1 1.188(11) . ? C3 N2 1.326(13) . ? C3 C4 1.503(15) . ? C4 C6 1.375(16) . ? C4 C5 1.382(14) . ? C5 N5 1.335(13) . ? C5 H5 0.9500 . ? C6 C7 1.375(17) . ? C6 H6 0.9500 . ? C7 C8 1.377(15) . ? C7 H7 0.9500 . ? C8 N5 1.342(13) . ? C8 C9 1.481(16) . ? C9 N6 1.346(13) . ? C9 C10 1.366(16) . ? C10 C11 1.338(17) . ? C10 H10 0.9500 . ? C11 C12 1.400(18) . ? C11 H11 0.9500 . ? C12 C13 1.371(16) . ? C12 H12 0.9500 . ? C13 N6 1.353(14) . ? C13 H13 0.9500 . ? C14 N1 1.467(14) . ? C14 C15 1.515(16) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N3 1.463(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O2 1.238(13) . ? C16 N3 1.324(13) . ? C16 C17 1.494(15) . ? C17 C18 1.359(14) . ? C17 C19 1.381(16) . ? C18 N7 1.362(12) . ? C18 H18 0.9500 . ? C19 C20 1.378(17) . ? C19 H19 0.9500 . ? C20 C21 1.380(16) . ? C20 H20 0.9500 . ? C21 N7 1.334(13) . ? C21 C22 1.482(16) . ? C22 N8 1.331(15) . ? C22 C23 1.372(15) . ? C23 C24 1.350(18) . ? C23 H23 0.9500 . ? C24 C25 1.400(19) . ? C24 H24 0.9500 . ? C25 C26 1.364(16) . ? C25 H25 0.9500 . ? C26 N8 1.334(14) . ? C26 H26 0.9500 . ? C27 N1 1.478(13) . ? C27 C28 1.508(15) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N4 1.484(13) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 O3 1.229(12) . ? C29 N4 1.343(13) . ? C29 C30 1.490(14) . ? C30 C31 1.357(12) . ? C30 C32 1.378(14) . ? C31 N9 1.364(12) . ? C31 H31 0.9500 . ? C32 C33 1.375(14) . ? C32 H32 0.9500 . ? C33 C34 1.402(14) . ? C33 H33 0.9500 . ? C34 N9 1.367(12) . ? C34 C35 1.459(13) . ? C35 N10 1.365(12) . ? C35 C36 1.377(13) . ? C36 C37 1.366(15) . ? C36 H36 0.9500 . ? C37 C38 1.368(16) . ? C37 H37 0.9500 . ? C38 C39 1.353(15) . ? C38 H38 0.9500 . ? C39 N10 1.351(13) . ? C39 H39 0.9500 . ? N2 H2 0.8800 . ? N3 H3 0.8800 . ? N4 H4 0.8800 . ? N5 Ru1 2.050(7) . ? N6 Ru1 2.057(9) . ? N7 Ru1 2.053(8) . ? N8 Ru1 2.079(9) . ? N9 Ru1 2.021(8) . ? N10 Ru1 2.032(7) . ? F1 P1 1.578(6) . ? F2 P1 1.570(8) . ? F3 P1 1.584(8) . ? F4 P1 1.579(7) . ? F5 P1 1.588(7) . ? F6 P1 1.590(7) . ? F11 P11 1.581(10) . ? F12 P11 1.567(9) . ? F13 P11 1.568(10) . ? F14 P11 1.564(11) . ? F15 P11 1.571(9) . ? F16 P11 1.603(9) . ? F111 P111 1.591(14) . ? F112 P111 1.568(14) . ? F113 P111 1.573(15) . ? F114 P111 1.584(14) . ? F115 P111 1.577(14) . ? F116 P111 1.575(14) . ? 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 N1 C1 C2 113.8(11) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 111.4(10) . . ? N2 C2 H2A 109.4 . . ? C1 C2 H2A 109.4 . . ? N2 C2 H2B 109.4 . . ? C1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? O1 C3 N2 125.4(11) . . ? O1 C3 C4 121.2(10) . . ? N2 C3 C4 113.4(9) . . ? C6 C4 C5 115.2(11) . . ? C6 C4 C3 119.9(9) . . ? C5 C4 C3 124.9(10) . . ? N5 C5 C4 125.9(11) . . ? N5 C5 H5 117.0 . . ? C4 C5 H5 117.0 . . ? C4 C6 C7 120.6(10) . . ? C4 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 119.7(11) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? N5 C8 C7 121.3(11) . . ? N5 C8 C9 113.8(9) . . ? C7 C8 C9 124.6(11) . . ? N6 C9 C10 119.9(11) . . ? N6 C9 C8 114.8(10) . . ? C10 C9 C8 125.2(11) . . ? C11 C10 C9 122.5(13) . . ? C11 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C10 C11 C12 117.8(13) . . ? C10 C11 H11 121.1 . . ? C12 C11 H11 121.1 . . ? C13 C12 C11 118.9(13) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N6 C13 C12 121.6(11) . . ? N6 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? N1 C14 C15 113.8(9) . . ? N1 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N1 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N3 C15 C14 110.8(10) . . ? N3 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? O2 C16 N3 124.2(10) . . ? O2 C16 C17 119.4(10) . . ? N3 C16 C17 116.3(11) . . ? C18 C17 C19 116.3(11) . . ? C18 C17 C16 114.3(10) . . ? C19 C17 C16 129.1(11) . . ? C17 C18 N7 122.9(10) . . ? C17 C18 H18 118.6 . . ? N7 C18 H18 118.6 . . ? C20 C19 C17 121.0(12) . . ? C20 C19 H19 119.5 . . ? C17 C19 H19 119.5 . . ? C19 C20 C21 119.9(11) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? N7 C21 C20 119.0(11) . . ? N7 C21 C22 116.2(10) . . ? C20 C21 C22 124.8(11) . . ? N8 C22 C23 121.6(11) . . ? N8 C22 C21 113.7(10) . . ? C23 C22 C21 124.7(12) . . ? C24 C23 C22 119.2(14) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 119.8(13) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 117.7(12) . . ? C26 C25 H25 121.2 . . ? C24 C25 H25 121.2 . . ? N8 C26 C25 122.3(14) . . ? N8 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? N1 C27 C28 112.2(9) . . ? N1 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? N1 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? N4 C28 C27 111.6(10) . . ? N4 C28 H28A 109.3 . . ? C27 C28 H28A 109.3 . . ? N4 C28 H28B 109.3 . . ? C27 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? O3 C29 N4 123.7(9) . . ? O3 C29 C30 123.3(10) . . ? N4 C29 C30 112.9(10) . . ? C31 C30 C32 118.4(9) . . ? C31 C30 C29 118.7(9) . . ? C32 C30 C29 122.9(9) . . ? C30 C31 N9 124.8(9) . . ? C30 C31 H31 117.6 . . ? N9 C31 H31 117.6 . . ? C33 C32 C30 119.2(10) . . ? C33 C32 H32 120.4 . . ? C30 C32 H32 120.4 . . ? C32 C33 C34 119.9(9) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? N9 C34 C33 121.0(9) . . ? N9 C34 C35 113.9(9) . . ? C33 C34 C35 124.9(9) . . ? N10 C35 C36 121.6(10) . . ? N10 C35 C34 113.9(8) . . ? C36 C35 C34 124.5(10) . . ? C37 C36 C35 120.7(11) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 118.2(10) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C39 C38 C37 119.2(11) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? N10 C39 C38 124.6(11) . . ? N10 C39 H39 117.7 . . ? C38 C39 H39 117.7 . . ? C14 N1 C27 107.8(9) . . ? C14 N1 C1 108.2(9) . . ? C27 N1 C1 112.0(10) . . ? C3 N2 C2 122.1(9) . . ? C3 N2 H2 119.0 . . ? C2 N2 H2 119.0 . . ? C16 N3 C15 121.5(10) . . ? C16 N3 H3 119.3 . . ? C15 N3 H3 119.3 . . ? C29 N4 C28 121.7(9) . . ? C29 N4 H4 119.1 . . ? C28 N4 H4 119.1 . . ? C5 N5 C8 117.0(8) . . ? C5 N5 Ru1 125.9(7) . . ? C8 N5 Ru1 117.0(7) . . ? C9 N6 C13 119.2(10) . . ? C9 N6 Ru1 116.1(8) . . ? C13 N6 Ru1 124.4(8) . . ? C21 N7 C18 120.5(9) . . ? C21 N7 Ru1 115.0(7) . . ? C18 N7 Ru1 122.7(7) . . ? C22 N8 C26 119.3(10) . . ? C22 N8 Ru1 115.9(7) . . ? C26 N8 Ru1 124.8(9) . . ? C31 N9 C34 116.3(8) . . ? C31 N9 Ru1 125.4(7) . . ? C34 N9 Ru1 116.6(6) . . ? C39 N10 C35 115.7(9) . . ? C39 N10 Ru1 127.7(8) . . ? C35 N10 Ru1 116.4(6) . . ? N9 Ru1 N10 78.7(3) . . ? N9 Ru1 N5 95.4(3) . . ? N10 Ru1 N5 172.2(3) . . ? N9 Ru1 N7 93.1(3) . . ? N10 Ru1 N7 92.4(3) . . ? N5 Ru1 N7 93.1(3) . . ? N9 Ru1 N6 91.5(3) . . ? N10 Ru1 N6 96.7(3) . . ? N5 Ru1 N6 78.1(4) . . ? N7 Ru1 N6 170.4(3) . . ? N9 Ru1 N8 170.7(4) . . ? N10 Ru1 N8 97.9(3) . . ? N5 Ru1 N8 88.7(3) . . ? N7 Ru1 N8 78.2(4) . . ? N6 Ru1 N8 97.5(4) . . ? F2 P1 F1 90.5(5) . . ? F2 P1 F4 179.3(5) . . ? F1 P1 F4 90.2(4) . . ? F2 P1 F3 89.8(5) . . ? F1 P1 F3 90.6(4) . . ? F4 P1 F3 90.0(5) . . ? F2 P1 F5 90.7(5) . . ? F1 P1 F5 89.3(4) . . ? F4 P1 F5 89.5(4) . . ? F3 P1 F5 179.5(6) . . ? F2 P1 F6 90.1(5) . . ? F1 P1 F6 179.4(6) . . ? F4 P1 F6 89.2(4) . . ? F3 P1 F6 89.5(4) . . ? F5 P1 F6 90.6(4) . . ? F14 P11 F12 178.7(9) . . ? F14 P11 F13 90.5(9) . . ? F12 P11 F13 88.8(8) . . ? F14 P11 F15 91.3(9) . . ? F12 P11 F15 89.4(8) . . ? F13 P11 F15 176.1(8) . . ? F14 P11 F11 90.9(8) . . ? F12 P11 F11 90.2(8) . . ? F13 P11 F11 93.2(8) . . ? F15 P11 F11 90.1(7) . . ? F14 P11 F16 90.8(7) . . ? F12 P11 F16 88.2(6) . . ? F13 P11 F16 89.4(7) . . ? F15 P11 F16 87.1(6) . . ? F11 P11 F16 176.9(8) . . ? F112 P111 F113 92.6(14) . . ? F112 P111 F116 90.4(14) . . ? F113 P111 F116 90.6(14) . . ? F112 P111 F115 88.9(15) . . ? F113 P111 F115 178.4(17) . . ? F116 P111 F115 90.0(14) . . ? F112 P111 F114 179.0(17) . . ? F113 P111 F114 88.4(16) . . ? F116 P111 F114 90.0(14) . . ? F115 P111 F114 90.2(14) . . ? F112 P111 F111 90.4(14) . . ? F113 P111 F111 90.5(14) . . ? F116 P111 F111 178.7(17) . . ? F115 P111 F111 88.9(14) . . ? F114 P111 F111 89.3(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 F16 0.88 2.00 2.850(14) 161.9 . N3 H3 F113 0.88 2.50 3.14(4) 130.4 . N4 H4 O2 0.88 2.11 2.967(12) 163.4 . _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.939 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.120 # 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 -0.254 0.500 0.500 485 100 ' ' _platon_squeeze_details ; It was not possible to determine the solvent type present the was removed using SQUEEZE and as such it could not be included in formula. ; #===END # Attachment '- RuL4Br.cif' data_2006src1520 _database_code_depnum_ccdc_archive 'CCDC 859684' #TrackingRef '- RuL4Br.cif' #There was some highly disordered solvent molecules (an estimate #was perhaps seven molecules of acetonitrile) in the asymmetric #unit that was removed from the calculations using the #SQUEEZE program. _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. N. Fletcher ; _chemical_name_common 'Dr. N. Fletcher' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Br2 N12 O9 Ru' _chemical_formula_weight 1197.87 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9778(8) _cell_length_b 15.1648(11) _cell_length_c 18.1787(14) _cell_angle_alpha 101.915(3) _cell_angle_beta 98.313(4) _cell_angle_gamma 92.738(4) _cell_volume 3452.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7056 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 1.434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8031 _exptl_absorpt_correction_T_max 0.9189 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 39207 reflections reduced R(int) from 0.1269 to 0.0608 Ratio of minimum to maximum apparent transmission: 0.687852 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47358 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15327 _reflns_number_gt 10333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. The hydrogen atoms of the water molecules and amide hydrogen atoms were geometrically restrained (DFIX (and DANG for water hydrogen atoms)). ; _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^)+(0.0885P)^2^+27.9227P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15327 _refine_ls_number_parameters 685 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.2493 _refine_ls_wR_factor_gt 0.2304 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.45812(4) 0.26550(4) 0.26164(3) 0.02725(16) Uani 1 1 d . . . Br2 Br 0.11628(8) 0.37460(7) 0.62297(5) 0.0555(3) Uani 1 1 d . . . Br1 Br 0.33182(6) 0.77235(5) 0.16774(5) 0.0402(2) Uani 1 1 d . . . C1 C -0.0635(6) 0.2532(5) 0.1157(4) 0.0327(16) Uani 1 1 d . . . C2 C -0.0983(5) 0.2355(5) 0.1789(4) 0.0324(16) Uani 1 1 d . . . H2 H -0.1205 0.1752 0.1799 0.039 Uiso 1 1 calc R . . C3 C -0.1017(5) 0.3061(5) 0.2430(4) 0.0320(16) Uani 1 1 d . . . C4 C -0.0681(6) 0.3939(5) 0.2408(4) 0.0328(16) Uani 1 1 d . . . H4 H -0.0703 0.4421 0.2832 0.039 Uiso 1 1 calc R . . C5 C -0.0313(6) 0.4110(5) 0.1767(4) 0.0317(16) Uani 1 1 d . . . C6 C -0.0267(5) 0.3406(5) 0.1140(4) 0.0294(15) Uani 1 1 d . . . H6 H 0.0012 0.3522 0.0711 0.035 Uiso 1 1 calc R . . C11 C -0.0640(6) 0.1743(5) 0.0500(4) 0.0327(16) Uani 1 1 d . . . C12 C -0.0737(6) 0.1253(5) -0.0872(4) 0.0344(16) Uani 1 1 d . . . H12A H -0.1235 0.1390 -0.1292 0.041 Uiso 1 1 calc R . . H12B H -0.0968 0.0653 -0.0791 0.041 Uiso 1 1 calc R . . C13 C 0.0361(6) 0.1213(6) -0.1104(4) 0.0393(18) Uani 1 1 d . . . H13A H 0.0331 0.0759 -0.1586 0.047 Uiso 1 1 calc R . . H13B H 0.0593 0.1809 -0.1192 0.047 Uiso 1 1 calc R . . C14 C 0.1777(6) 0.1587(5) -0.0008(4) 0.0354(17) Uani 1 1 d . . . C15 C 0.2468(5) 0.1251(5) 0.0590(4) 0.0324(16) Uani 1 1 d . . . C16 C 0.2961(5) 0.1908(5) 0.1221(4) 0.0297(15) Uani 1 1 d . . . H16 H 0.2811 0.2520 0.1249 0.036 Uiso 1 1 calc R . . C17 C 0.2673(6) 0.0363(5) 0.0564(4) 0.0358(17) Uani 1 1 d . . . H17 H 0.2342 -0.0100 0.0150 0.043 Uiso 1 1 calc R . . C18 C 0.3367(6) 0.0149(5) 0.1148(4) 0.0365(18) Uani 1 1 d . . . H18 H 0.3521 -0.0460 0.1133 0.044 Uiso 1 1 calc R . . C19 C 0.3828(6) 0.0828(5) 0.1746(4) 0.0328(16) Uani 1 1 d . . . C20 C 0.4596(6) 0.0694(5) 0.2384(5) 0.0346(16) Uani 1 1 d . . . C21 C 0.4859(7) -0.0167(5) 0.2493(5) 0.0426(19) Uani 1 1 d . . . H21 H 0.4535 -0.0700 0.2149 0.051 Uiso 1 1 calc R . . C22 C 0.5592(6) -0.0220(5) 0.3104(5) 0.0384(18) Uani 1 1 d . . . H22 H 0.5768 -0.0793 0.3196 0.046 Uiso 1 1 calc R . . C23 C 0.6067(7) 0.0559(6) 0.3582(5) 0.0411(18) Uani 1 1 d . . . H23 H 0.6572 0.0527 0.4008 0.049 Uiso 1 1 calc R . . C24 C 0.5816(6) 0.1376(6) 0.3444(5) 0.0385(18) Uani 1 1 d . . . H24 H 0.6167 0.1908 0.3774 0.046 Uiso 1 1 calc R . . C31 C -0.1393(6) 0.2785(5) 0.3091(4) 0.0338(16) Uani 1 1 d . . . C32 C -0.1133(6) 0.2909(5) 0.4458(4) 0.0367(17) Uani 1 1 d . . . H32A H -0.1889 0.2743 0.4419 0.044 Uiso 1 1 calc R . . H32B H -0.0917 0.3394 0.4919 0.044 Uiso 1 1 calc R . . C33 C -0.0523(5) 0.2087(6) 0.4525(5) 0.0358(17) Uani 1 1 d . . . H33A H -0.0638 0.1882 0.4992 0.043 Uiso 1 1 calc R . . H33B H -0.0775 0.1587 0.4082 0.043 Uiso 1 1 calc R . . C34 C 0.1071(6) 0.2105(5) 0.3960(4) 0.0318(16) Uani 1 1 d . . . C35 C 0.2188(6) 0.2470(5) 0.4072(4) 0.0337(16) Uani 1 1 d . . . C36 C 0.2719(5) 0.2368(5) 0.3438(4) 0.0305(15) Uani 1 1 d . . . H36 H 0.2372 0.2038 0.2957 0.037 Uiso 1 1 calc R . . C37 C 0.2747(6) 0.2942(6) 0.4777(4) 0.0399(18) Uani 1 1 d . . . H37 H 0.2425 0.3016 0.5221 0.048 Uiso 1 1 calc R . . C38 C 0.3731(6) 0.3289(5) 0.4824(4) 0.0363(17) Uani 1 1 d . . . H38 H 0.4098 0.3609 0.5303 0.044 Uiso 1 1 calc R . . C39 C 0.4217(5) 0.3189(5) 0.4188(4) 0.0307(15) Uani 1 1 d . . . C40 C 0.5251(6) 0.3609(5) 0.4195(4) 0.0337(16) Uani 1 1 d . . . C41 C 0.5893(6) 0.4107(6) 0.4845(5) 0.0399(18) Uani 1 1 d . . . H41 H 0.5673 0.4164 0.5328 0.048 Uiso 1 1 calc R . . C42 C 0.6851(6) 0.4519(5) 0.4791(5) 0.0408(19) Uani 1 1 d . . . H42 H 0.7294 0.4857 0.5230 0.049 Uiso 1 1 calc R . . C43 C 0.7133(6) 0.4423(5) 0.4091(5) 0.0387(18) Uani 1 1 d . . . H43 H 0.7769 0.4720 0.4036 0.046 Uiso 1 1 calc R . . C44 C 0.6508(5) 0.3902(5) 0.3461(5) 0.0370(17) Uani 1 1 d . . . H44 H 0.6736 0.3829 0.2980 0.044 Uiso 1 1 calc R . . C51 C 0.0076(5) 0.5048(5) 0.1703(4) 0.0299(15) Uani 1 1 d . . . C52 C 0.0249(6) 0.6674(5) 0.2295(4) 0.0346(16) Uani 1 1 d . . . H52A H -0.0292 0.7084 0.2443 0.041 Uiso 1 1 calc R . . H52B H 0.0421 0.6772 0.1803 0.041 Uiso 1 1 calc R . . C53 C 0.1231(6) 0.6911(5) 0.2901(4) 0.0346(17) Uani 1 1 d . . . H53A H 0.1437 0.7567 0.2997 0.041 Uiso 1 1 calc R . . H53B H 0.1080 0.6768 0.3384 0.041 Uiso 1 1 calc R . . C54 C 0.2304(6) 0.5606(5) 0.2797(5) 0.0383(18) Uani 1 1 d . . . C55 C 0.3074(6) 0.5083(5) 0.2362(4) 0.0322(16) Uani 1 1 d . . . C56 C 0.3363(5) 0.4311(5) 0.2601(4) 0.0305(15) Uani 1 1 d . . . H56 H 0.3067 0.4147 0.3007 0.037 Uiso 1 1 calc R . . C57 C 0.3502(6) 0.5313(5) 0.1773(4) 0.0346(16) Uani 1 1 d . . . H57 H 0.3293 0.5831 0.1591 0.042 Uiso 1 1 calc R . . C58 C 0.4232(6) 0.4799(5) 0.1441(4) 0.0349(16) Uani 1 1 d . . . H58 H 0.4545 0.4966 0.1043 0.042 Uiso 1 1 calc R . . C59 C 0.4494(5) 0.4032(5) 0.1707(4) 0.0278(15) Uani 1 1 d . . . C60 C 0.5264(5) 0.3416(5) 0.1393(4) 0.0303(15) Uani 1 1 d . . . C61 C 0.5730(6) 0.3524(6) 0.0777(5) 0.0401(18) Uani 1 1 d . . . H61 H 0.5600 0.4017 0.0537 0.048 Uiso 1 1 calc R . . C62 C 0.6397(7) 0.2879(6) 0.0523(5) 0.0434(19) Uani 1 1 d . . . H62 H 0.6725 0.2924 0.0097 0.052 Uiso 1 1 calc R . . C63 C 0.6583(6) 0.2197(6) 0.0873(4) 0.0397(18) Uani 1 1 d . . . H63 H 0.7036 0.1757 0.0691 0.048 Uiso 1 1 calc R . . C64 C 0.6116(6) 0.2128(5) 0.1500(4) 0.0339(16) Uani 1 1 d . . . H64 H 0.6266 0.1648 0.1751 0.041 Uiso 1 1 calc R . . N1 N -0.0755(5) 0.1926(4) -0.0187(4) 0.0318(13) Uani 1 1 d D . . H1 H -0.073(6) 0.2514(13) -0.016(5) 0.038 Uiso 1 1 d D . . N2 N 0.1111(5) 0.0973(5) -0.0511(4) 0.0364(14) Uani 1 1 d D . . H2A H 0.107(7) 0.0392(16) -0.051(5) 0.044 Uiso 1 1 d D . . N3 N 0.3630(4) 0.1710(4) 0.1782(3) 0.0260(12) Uani 1 1 d . . . N4 N 0.5079(4) 0.1464(4) 0.2851(3) 0.0303(13) Uani 1 1 d . . . N31 N -0.0943(5) 0.3234(4) 0.3795(4) 0.0331(14) Uani 1 1 d D . . H31 H -0.066(6) 0.377(2) 0.379(5) 0.040 Uiso 1 1 d D . . N32 N 0.0576(5) 0.2311(4) 0.4556(4) 0.0361(14) Uani 1 1 d D . . H32 H 0.076(6) 0.274(4) 0.497(3) 0.043 Uiso 1 1 d D . . N33 N 0.3711(5) 0.2729(4) 0.3500(4) 0.0316(13) Uani 1 1 d . . . N34 N 0.5574(5) 0.3486(4) 0.3507(4) 0.0327(14) Uani 1 1 d . . . N51 N -0.0163(5) 0.5749(4) 0.2199(4) 0.0327(14) Uani 1 1 d D . . H51 H -0.055(5) 0.570(6) 0.255(3) 0.039 Uiso 1 1 d D . . N52 N 0.2096(5) 0.6396(4) 0.2646(4) 0.0356(14) Uani 1 1 d D . . H52 H 0.243(6) 0.671(5) 0.238(4) 0.043 Uiso 1 1 d D . . N53 N 0.4063(4) 0.3774(4) 0.2270(3) 0.0303(13) Uani 1 1 d . . . N54 N 0.5444(4) 0.2739(4) 0.1763(3) 0.0306(13) Uani 1 1 d . . . O1 O -0.0581(4) 0.0962(4) 0.0629(3) 0.0413(13) Uani 1 1 d . . . O2 O 0.1833(4) 0.2398(4) -0.0022(3) 0.0447(14) Uani 1 1 d . . . O31 O -0.2096(4) 0.2169(4) 0.2992(3) 0.0393(13) Uani 1 1 d . . . O32 O 0.0669(4) 0.1614(4) 0.3335(3) 0.0440(14) Uani 1 1 d . . . O51 O 0.0600(4) 0.5129(3) 0.1207(3) 0.0367(12) Uani 1 1 d . . . O52 O 0.1867(4) 0.5253(4) 0.3244(3) 0.0433(13) Uani 1 1 d . . . O91 O 0.1399(5) 0.6427(4) 0.0536(3) 0.0411(13) Uani 1 1 d D . . H91A H 0.194(5) 0.674(6) 0.081(4) 0.062 Uiso 1 1 d D . . H91B H 0.113(6) 0.610(5) 0.078(4) 0.062 Uiso 1 1 d D . . O92 O 0.0579(5) 0.4771(4) 0.4228(4) 0.0516(16) Uani 1 1 d D . . H92A H 0.018(6) 0.520(5) 0.426(7) 0.077 Uiso 1 1 d D . . H92B H 0.111(5) 0.493(6) 0.405(6) 0.077 Uiso 1 1 d D . . O93 O 0.1054(5) 0.0893(5) 0.1877(4) 0.0512(15) Uani 1 1 d D . . H93A H 0.080(7) 0.109(7) 0.229(3) 0.077 Uiso 1 1 d D . . H93B H 0.051(5) 0.072(7) 0.154(4) 0.077 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0240(3) 0.0284(3) 0.0265(3) 0.0008(2) 0.0027(2) -0.0005(2) Br2 0.0530(5) 0.0634(6) 0.0432(5) -0.0099(4) 0.0203(4) -0.0096(4) Br1 0.0419(4) 0.0345(4) 0.0411(5) 0.0034(3) 0.0065(3) -0.0056(3) C1 0.034(4) 0.029(4) 0.029(4) -0.006(3) 0.004(3) 0.004(3) C2 0.026(3) 0.036(4) 0.032(4) 0.000(3) 0.006(3) 0.003(3) C3 0.024(3) 0.031(4) 0.035(4) -0.002(3) -0.005(3) 0.004(3) C4 0.030(4) 0.032(4) 0.032(4) -0.002(3) 0.005(3) 0.002(3) C5 0.033(4) 0.029(4) 0.030(4) 0.001(3) 0.007(3) -0.002(3) C6 0.027(3) 0.030(4) 0.028(4) 0.005(3) -0.003(3) -0.008(3) C11 0.032(4) 0.027(4) 0.033(4) -0.003(3) 0.002(3) -0.007(3) C12 0.033(4) 0.038(4) 0.027(4) 0.001(3) 0.002(3) -0.007(3) C13 0.043(4) 0.041(4) 0.029(4) -0.002(3) 0.004(3) 0.003(3) C14 0.042(4) 0.030(4) 0.029(4) -0.004(3) 0.004(3) 0.004(3) C15 0.026(3) 0.037(4) 0.034(4) 0.007(3) 0.006(3) -0.002(3) C16 0.029(4) 0.025(3) 0.034(4) 0.000(3) 0.008(3) 0.002(3) C17 0.034(4) 0.041(4) 0.028(4) -0.001(3) 0.003(3) -0.003(3) C18 0.027(4) 0.035(4) 0.039(4) -0.011(3) 0.004(3) 0.000(3) C19 0.028(4) 0.030(4) 0.041(4) 0.007(3) 0.009(3) -0.002(3) C20 0.027(4) 0.041(4) 0.040(4) 0.016(3) 0.009(3) 0.002(3) C21 0.048(5) 0.030(4) 0.047(5) 0.001(4) 0.013(4) 0.001(3) C22 0.044(4) 0.034(4) 0.037(4) 0.011(3) 0.002(3) 0.004(3) C23 0.044(5) 0.043(5) 0.036(4) 0.012(4) 0.001(4) 0.003(4) C24 0.033(4) 0.049(5) 0.036(4) 0.009(4) 0.011(3) 0.004(3) C31 0.030(4) 0.038(4) 0.031(4) 0.002(3) 0.006(3) 0.001(3) C32 0.030(4) 0.045(4) 0.033(4) 0.004(3) 0.008(3) -0.003(3) C33 0.023(3) 0.050(5) 0.038(4) 0.016(4) 0.012(3) 0.000(3) C34 0.034(4) 0.036(4) 0.025(4) 0.001(3) 0.007(3) 0.006(3) C35 0.033(4) 0.033(4) 0.029(4) -0.001(3) -0.006(3) 0.004(3) C36 0.031(4) 0.030(4) 0.026(4) 0.002(3) 0.000(3) 0.001(3) C37 0.042(4) 0.049(5) 0.026(4) -0.001(3) 0.008(3) 0.001(4) C38 0.033(4) 0.043(4) 0.027(4) 0.002(3) -0.005(3) -0.006(3) C39 0.028(3) 0.033(4) 0.026(4) -0.006(3) 0.004(3) 0.003(3) C40 0.031(4) 0.034(4) 0.033(4) 0.000(3) 0.004(3) 0.002(3) C41 0.031(4) 0.044(5) 0.038(4) -0.001(4) 0.000(3) -0.001(3) C42 0.026(4) 0.039(4) 0.043(5) -0.013(4) -0.009(3) -0.003(3) C43 0.023(4) 0.037(4) 0.048(5) -0.002(4) -0.003(3) -0.003(3) C44 0.022(3) 0.044(4) 0.044(5) 0.005(4) 0.011(3) 0.001(3) C51 0.023(3) 0.032(4) 0.030(4) -0.002(3) 0.001(3) 0.006(3) C52 0.036(4) 0.031(4) 0.035(4) 0.002(3) 0.005(3) 0.004(3) C53 0.031(4) 0.035(4) 0.036(4) 0.000(3) 0.013(3) 0.003(3) C54 0.034(4) 0.033(4) 0.041(5) 0.000(3) -0.006(3) 0.003(3) C55 0.030(4) 0.033(4) 0.030(4) 0.006(3) -0.003(3) -0.001(3) C56 0.022(3) 0.032(4) 0.034(4) 0.003(3) 0.001(3) -0.002(3) C57 0.044(4) 0.035(4) 0.026(4) 0.008(3) 0.007(3) 0.002(3) C58 0.040(4) 0.039(4) 0.025(4) 0.003(3) 0.009(3) 0.006(3) C59 0.020(3) 0.031(4) 0.026(4) -0.002(3) -0.001(3) -0.004(3) C60 0.030(4) 0.031(4) 0.025(4) -0.002(3) 0.001(3) -0.002(3) C61 0.041(4) 0.042(4) 0.036(4) 0.001(3) 0.012(3) 0.003(3) C62 0.043(5) 0.050(5) 0.036(5) 0.004(4) 0.011(4) 0.002(4) C63 0.037(4) 0.047(5) 0.030(4) -0.003(4) 0.010(3) -0.001(3) C64 0.041(4) 0.022(3) 0.035(4) 0.001(3) 0.003(3) 0.001(3) N1 0.035(3) 0.025(3) 0.031(3) 0.000(3) 0.003(3) 0.003(3) N2 0.038(3) 0.040(4) 0.027(3) 0.001(3) 0.001(3) -0.006(3) N3 0.020(3) 0.036(3) 0.019(3) 0.002(2) 0.002(2) -0.003(2) N4 0.027(3) 0.033(3) 0.030(3) 0.009(3) 0.002(2) -0.004(2) N31 0.033(3) 0.033(3) 0.027(3) -0.005(3) 0.005(3) -0.009(3) N32 0.035(3) 0.039(4) 0.030(3) 0.002(3) 0.002(3) -0.008(3) N33 0.027(3) 0.032(3) 0.034(3) 0.000(3) 0.009(3) 0.000(2) N34 0.031(3) 0.029(3) 0.035(4) 0.007(3) -0.003(3) 0.004(2) N51 0.033(3) 0.029(3) 0.034(4) 0.000(3) 0.009(3) 0.000(3) N52 0.030(3) 0.037(4) 0.040(4) 0.008(3) 0.007(3) 0.007(3) N53 0.028(3) 0.033(3) 0.025(3) 0.001(2) -0.001(2) -0.003(2) N54 0.020(3) 0.035(3) 0.033(3) -0.003(3) 0.007(2) -0.002(2) O1 0.047(3) 0.039(3) 0.033(3) -0.001(2) 0.003(2) 0.002(2) O2 0.045(3) 0.039(3) 0.043(3) 0.011(3) -0.017(3) -0.010(2) O31 0.035(3) 0.044(3) 0.034(3) 0.003(2) 0.004(2) -0.010(2) O32 0.036(3) 0.046(3) 0.044(3) -0.007(3) 0.013(3) -0.008(2) O51 0.039(3) 0.028(3) 0.041(3) 0.000(2) 0.010(2) -0.006(2) O52 0.044(3) 0.046(3) 0.047(3) 0.016(3) 0.018(3) 0.008(3) O91 0.052(3) 0.037(3) 0.032(3) 0.006(2) 0.009(3) -0.012(3) O92 0.045(4) 0.063(4) 0.040(3) 0.001(3) 0.005(3) -0.017(3) O93 0.051(4) 0.064(4) 0.035(3) -0.002(3) 0.010(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N53 2.038(6) . ? Ru1 N4 2.052(6) . ? Ru1 N54 2.060(6) . ? Ru1 N34 2.066(6) . ? Ru1 N3 2.067(5) . ? Ru1 N33 2.080(6) . ? C1 C2 1.364(11) . ? C1 C6 1.395(10) . ? C1 C11 1.504(10) . ? C2 C3 1.419(10) . ? C2 H2 0.9500 . ? C3 C4 1.391(10) . ? C3 C31 1.488(11) . ? C4 C5 1.389(10) . ? C4 H4 0.9500 . ? C5 C6 1.402(10) . ? C5 C51 1.519(10) . ? C6 H6 0.9500 . ? C11 O1 1.258(9) . ? C11 N1 1.325(10) . ? C12 N1 1.442(9) . ? C12 C13 1.544(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N2 1.462(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 O2 1.234(9) . ? C14 N2 1.339(10) . ? C14 C15 1.496(11) . ? C15 C17 1.378(11) . ? C15 C16 1.403(10) . ? C16 N3 1.335(9) . ? C16 H16 0.9500 . ? C17 C18 1.392(11) . ? C17 H17 0.9500 . ? C18 C19 1.376(10) . ? C18 H18 0.9500 . ? C19 N3 1.363(9) . ? C19 C20 1.472(11) . ? C20 N4 1.359(10) . ? C20 C21 1.410(11) . ? C21 C22 1.373(12) . ? C21 H21 0.9500 . ? C22 C23 1.372(11) . ? C22 H22 0.9500 . ? C23 C24 1.360(11) . ? C23 H23 0.9500 . ? C24 N4 1.367(10) . ? C24 H24 0.9500 . ? C31 O31 1.241(9) . ? C31 N31 1.352(9) . ? C32 N31 1.441(10) . ? C32 C33 1.525(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 N32 1.440(9) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 O32 1.249(9) . ? C34 N32 1.328(9) . ? C34 C35 1.498(10) . ? C35 C37 1.408(10) . ? C35 C36 1.411(11) . ? C36 N33 1.356(9) . ? C36 H36 0.9500 . ? C37 C38 1.342(11) . ? C37 H37 0.9500 . ? C38 C39 1.381(10) . ? C38 H38 0.9500 . ? C39 N33 1.356(9) . ? C39 C40 1.456(10) . ? C40 N34 1.357(10) . ? C40 C41 1.394(10) . ? C41 C42 1.390(11) . ? C41 H41 0.9500 . ? C42 C43 1.354(12) . ? C42 H42 0.9500 . ? C43 C44 1.375(11) . ? C43 H43 0.9500 . ? C44 N34 1.360(9) . ? C44 H44 0.9500 . ? C51 O51 1.227(9) . ? C51 N51 1.325(9) . ? C52 N51 1.444(9) . ? C52 C53 1.535(11) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 N52 1.473(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O52 1.246(10) . ? C54 N52 1.316(10) . ? C54 C55 1.516(11) . ? C55 C57 1.373(10) . ? C55 C56 1.381(10) . ? C56 N53 1.371(9) . ? C56 H56 0.9500 . ? C57 C58 1.383(10) . ? C57 H57 0.9500 . ? C58 C59 1.387(10) . ? C58 H58 0.9500 . ? C59 N53 1.351(9) . ? C59 C60 1.494(10) . ? C60 N54 1.351(10) . ? C60 C61 1.382(11) . ? C61 C62 1.388(11) . ? C61 H61 0.9500 . ? C62 C63 1.335(12) . ? C62 H62 0.9500 . ? C63 C64 1.386(11) . ? C63 H63 0.9500 . ? C64 N54 1.364(9) . ? C64 H64 0.9500 . ? N1 H1 0.883(10) . ? N2 H2A 0.882(10) . ? N31 H31 0.878(10) . ? N32 H32 0.880(10) . ? N51 H51 0.880(10) . ? N52 H52 0.878(10) . ? O91 H91A 0.85(3) . ? O91 H91B 0.83(3) . ? O92 H92A 0.85(3) . ? O92 H92B 0.85(3) . ? O93 H93A 0.87(3) . ? O93 H93B 0.86(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N53 Ru1 N4 174.2(2) . . ? N53 Ru1 N54 78.1(2) . . ? N4 Ru1 N54 98.0(2) . . ? N53 Ru1 N34 89.2(2) . . ? N4 Ru1 N34 95.7(2) . . ? N54 Ru1 N34 98.0(2) . . ? N53 Ru1 N3 96.9(2) . . ? N4 Ru1 N3 78.3(2) . . ? N54 Ru1 N3 84.3(2) . . ? N34 Ru1 N3 173.8(2) . . ? N53 Ru1 N33 96.2(2) . . ? N4 Ru1 N33 87.8(2) . . ? N54 Ru1 N33 173.5(2) . . ? N34 Ru1 N33 78.5(2) . . ? N3 Ru1 N33 99.7(2) . . ? C2 C1 C6 120.6(7) . . ? C2 C1 C11 117.0(7) . . ? C6 C1 C11 122.3(7) . . ? C1 C2 C3 120.7(7) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 119.0(7) . . ? C4 C3 C31 125.1(7) . . ? C2 C3 C31 115.9(7) . . ? C5 C4 C3 119.9(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.8(7) . . ? C4 C5 C51 123.0(6) . . ? C6 C5 C51 116.2(6) . . ? C1 C6 C5 118.9(7) . . ? C1 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? O1 C11 N1 124.4(7) . . ? O1 C11 C1 119.1(7) . . ? N1 C11 C1 116.4(7) . . ? N1 C12 C13 112.3(6) . . ? N1 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C12 110.7(6) . . ? N2 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? O2 C14 N2 122.9(7) . . ? O2 C14 C15 120.2(7) . . ? N2 C14 C15 117.0(7) . . ? C17 C15 C16 118.1(7) . . ? C17 C15 C14 125.5(7) . . ? C16 C15 C14 116.4(7) . . ? N3 C16 C15 122.9(7) . . ? N3 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C15 C17 C18 119.5(7) . . ? C15 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 119.3(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N3 C19 C18 121.8(7) . . ? N3 C19 C20 113.6(6) . . ? C18 C19 C20 124.5(7) . . ? N4 C20 C21 121.6(7) . . ? N4 C20 C19 115.1(7) . . ? C21 C20 C19 123.2(7) . . ? C22 C21 C20 118.7(8) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C23 C22 C21 119.6(8) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 119.9(8) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 N4 122.7(8) . . ? C23 C24 H24 118.7 . . ? N4 C24 H24 118.7 . . ? O31 C31 N31 121.9(7) . . ? O31 C31 C3 120.7(7) . . ? N31 C31 C3 117.3(6) . . ? N31 C32 C33 110.2(6) . . ? N31 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? N31 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? N32 C33 C32 110.2(6) . . ? N32 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? N32 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? O32 C34 N32 124.0(7) . . ? O32 C34 C35 119.5(6) . . ? N32 C34 C35 116.5(6) . . ? C37 C35 C36 117.0(7) . . ? C37 C35 C34 123.8(7) . . ? C36 C35 C34 119.1(6) . . ? N33 C36 C35 121.6(6) . . ? N33 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C38 C37 C35 120.3(7) . . ? C38 C37 H37 119.9 . . ? C35 C37 H37 119.9 . . ? C37 C38 C39 120.9(7) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? N33 C39 C38 120.6(6) . . ? N33 C39 C40 116.1(6) . . ? C38 C39 C40 123.2(6) . . ? N34 C40 C41 120.4(7) . . ? N34 C40 C39 114.9(6) . . ? C41 C40 C39 124.6(7) . . ? C42 C41 C40 120.4(8) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 118.0(7) . . ? C43 C42 H42 121.0 . . ? C41 C42 H42 121.0 . . ? C42 C43 C44 120.7(7) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? N34 C44 C43 121.9(7) . . ? N34 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? O51 C51 N51 122.8(7) . . ? O51 C51 C5 119.5(6) . . ? N51 C51 C5 117.7(6) . . ? N51 C52 C53 112.1(6) . . ? N51 C52 H52A 109.2 . . ? C53 C52 H52A 109.2 . . ? N51 C52 H52B 109.2 . . ? C53 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? N52 C53 C52 110.3(6) . . ? N52 C53 H53A 109.6 . . ? C52 C53 H53A 109.6 . . ? N52 C53 H53B 109.6 . . ? C52 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? O52 C54 N52 123.7(7) . . ? O52 C54 C55 119.1(7) . . ? N52 C54 C55 117.1(7) . . ? C57 C55 C56 118.6(7) . . ? C57 C55 C54 126.3(7) . . ? C56 C55 C54 115.1(7) . . ? N53 C56 C55 122.0(7) . . ? N53 C56 H56 119.0 . . ? C55 C56 H56 119.0 . . ? C55 C57 C58 120.9(7) . . ? C55 C57 H57 119.6 . . ? C58 C57 H57 119.6 . . ? C57 C58 C59 117.8(7) . . ? C57 C58 H58 121.1 . . ? C59 C58 H58 121.1 . . ? N53 C59 C58 122.7(6) . . ? N53 C59 C60 114.1(6) . . ? C58 C59 C60 123.2(6) . . ? N54 C60 C61 123.6(7) . . ? N54 C60 C59 113.4(6) . . ? C61 C60 C59 123.0(7) . . ? C60 C61 C62 117.0(8) . . ? C60 C61 H61 121.5 . . ? C62 C61 H61 121.5 . . ? C63 C62 C61 120.7(8) . . ? C63 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C62 C63 C64 120.2(8) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? N54 C64 C63 121.1(7) . . ? N54 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C11 N1 C12 123.2(6) . . ? C11 N1 H1 111(6) . . ? C12 N1 H1 125(6) . . ? C14 N2 C13 122.7(7) . . ? C14 N2 H2A 124(6) . . ? C13 N2 H2A 113(6) . . ? C16 N3 C19 118.4(6) . . ? C16 N3 Ru1 124.6(5) . . ? C19 N3 Ru1 116.2(5) . . ? C20 N4 C24 117.5(7) . . ? C20 N4 Ru1 116.2(5) . . ? C24 N4 Ru1 126.3(5) . . ? C31 N31 C32 120.5(6) . . ? C31 N31 H31 112(6) . . ? C32 N31 H31 127(6) . . ? C34 N32 C33 123.6(7) . . ? C34 N32 H32 127(6) . . ? C33 N32 H32 106(6) . . ? C36 N33 C39 119.5(6) . . ? C36 N33 Ru1 126.0(5) . . ? C39 N33 Ru1 114.5(5) . . ? C40 N34 C44 118.3(6) . . ? C40 N34 Ru1 115.6(5) . . ? C44 N34 Ru1 126.1(5) . . ? C51 N51 C52 125.6(6) . . ? C51 N51 H51 124(6) . . ? C52 N51 H51 110(6) . . ? C54 N52 C53 124.2(7) . . ? C54 N52 H52 128(6) . . ? C53 N52 H52 108(6) . . ? C59 N53 C56 118.0(6) . . ? C59 N53 Ru1 117.3(5) . . ? C56 N53 Ru1 124.6(5) . . ? C60 N54 C64 117.3(6) . . ? C60 N54 Ru1 117.0(5) . . ? C64 N54 Ru1 125.5(5) . . ? H91A O91 H91B 110(5) . . ? H92A O92 H92B 108(5) . . ? H93A O93 H93B 103(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O91 0.883(10) 2.05(5) 2.835(9) 148(7) 2_565 N2 H2A O1 0.882(10) 2.08(3) 2.938(9) 166(8) 2 N31 H31 O92 0.878(10) 2.11(5) 2.882(8) 147(8) . N32 H32 Br2 0.880(10) 2.45(2) 3.318(6) 169(8) . N51 H51 Br2 0.880(10) 2.46(4) 3.270(6) 153(7) 2_566 N52 H52 Br1 0.878(10) 2.535(14) 3.410(7) 175(8) . O91 H91A Br1 0.85(3) 2.43(3) 3.275(6) 173(9) . O91 H91B O51 0.83(3) 1.94(3) 2.758(7) 168(10) . O92 H92A Br2 0.85(3) 2.61(6) 3.402(7) 157(11) 2_566 O92 H92B O52 0.85(3) 2.00(6) 2.796(8) 155(11) . O93 H93A O32 0.87(3) 1.93(4) 2.777(8) 163(9) . O93 H93B O1 0.86(3) 2.12(6) 2.895(9) 150(11) . _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.424 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.151 # 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 -0.020 0.000 0.470 1215 330 ' ' 2 0.150 0.306 0.219 7 2 ' ' 3 0.850 0.694 0.781 7 3 ' ' _platon_squeeze_details ; Only those water molecules around the complex forming strong hydrogen bonds could be located. It was not possible to determine the rest of the solvent, which could be a random mixture of acetonitrile and water, and was removed using SQUEEZE and as such it could not be included in formula. ;