#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:52:10 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270127 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708641.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7708641 loop_ _publ_author_name 'Biancalana, Lorenzo' 'Zanda, Emanuele' 'Hadiji, Mouna' 'Zacchini, Stefano' 'Pratesi, Alessandro' 'Pampaloni, Guido' 'Dyson, Paul J.' 'Marchetti, Fabio' _publ_section_title ; Role of the (pseudo)halido ligand in ruthenium(II) p-cymene \a-amino acid complexes in speciation, protein reactivity and cytotoxicity. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d1dt03274g _journal_year 2021 _chemical_formula_sum 'C20 H28 N12 Ru2' _chemical_formula_weight 638.68 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-08-23 deposited with the CCDC. 2021-10-22 downloaded from the CCDC. ; _cell_angle_alpha 83.3520(10) _cell_angle_beta 85.0850(10) _cell_angle_gamma 77.2420(10) _cell_formula_units_Z 1 _cell_length_a 8.0847(4) _cell_length_b 8.2571(5) _cell_length_c 9.7821(5) _cell_measurement_reflns_used 9937 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 34.845 _cell_measurement_theta_min 2.588 _cell_volume 631.39(6) _computing_cell_refinement 'APEX3 (Bruker AXS, 2015)' _computing_data_collection 'APEX3 (Bruker AXS, 2015)' _computing_data_reduction 'SAINT (Bruker AXS, 2015)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1996)' _computing_publication_material 'XCIF 2014/2 (Bruker AXS, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'PHOTON100 area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 9239 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.999 _diffrn_reflns_theta_min 2.100 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.229 _exptl_absorpt_correction_T_max 0.7469 _exptl_absorpt_correction_T_min 0.6414 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Data were corrected for Lorentz polarization and absorption effects (empirical absorption correction SADABS). R(int) = 0.1081 (selected reflections only, before parameter refinement) R(int) = 0.0339 (selected reflections only, after parameter refinement) ; _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 1.680 _exptl_crystal_description prism _exptl_crystal_F_000 320 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.325 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 3024 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.0183 _refine_ls_R_factor_gt 0.0177 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+0.5034P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0457 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2959 _reflns_number_total 3024 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03274g2.cif _cod_data_source_block RuN3 _cod_database_code 7708641 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.774 _shelx_estimated_absorpt_t_max 0.847 _shelx_res_file ; p-1.res created by SHELXL-2014/7 TITL p-1_a.res in P-1 CELL 0.71073 8.0847 8.2571 9.7821 83.352 85.085 77.242 ZERR 1.000 0.0004 0.0005 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N Ru UNIT 20 28 12 2 omit -4 1 2 OMIT -3 56 L.S. 10 ACTA BOND $H conf FMAP 2 PLAN 20 size 0.22 0.16 0.14 TEMP -173 WGHT 0.017500 0.503400 FVAR 0.28045 C1 1 0.142634 0.810444 0.532537 11.00000 0.01784 0.01418 = 0.01552 0.00060 0.00069 0.00668 C2 1 0.055274 0.745262 0.439163 11.00000 0.00954 0.02044 = 0.01869 0.00305 0.00128 0.00250 AFIX 13 H2 2 -0.032378 0.680318 0.476232 11.00000 -1.20000 AFIX 0 C3 1 0.116918 0.739570 0.298522 11.00000 0.01063 0.01910 = 0.01645 0.00187 -0.00254 -0.00042 AFIX 13 H3 2 0.070903 0.669533 0.240667 11.00000 -1.20000 AFIX 0 C4 1 0.263525 0.798852 0.246932 11.00000 0.01272 0.01373 = 0.01329 0.00287 -0.00127 -0.00004 C5 1 0.348502 0.866625 0.342740 11.00000 0.01570 0.00986 = 0.01848 0.00239 -0.00169 -0.00143 AFIX 13 H5 2 0.465012 0.886210 0.315109 11.00000 -1.20000 AFIX 0 C6 1 0.288429 0.875110 0.482053 11.00000 0.02216 0.00929 = 0.01838 -0.00149 -0.00469 0.00179 AFIX 13 H6 2 0.363623 0.899700 0.549475 11.00000 -1.20000 AFIX 0 C7 1 0.087259 0.802897 0.683249 11.00000 0.03143 0.02280 = 0.01569 -0.00044 0.00444 0.00877 AFIX 137 H7A 2 0.187038 0.785157 0.737798 11.00000 -1.50000 H7B 2 0.028740 0.710509 0.707527 11.00000 -1.50000 H7C 2 0.009868 0.908102 0.702760 11.00000 -1.50000 AFIX 0 C8 1 0.332388 0.792440 0.097963 11.00000 0.01568 0.01928 = 0.01313 0.00306 0.00042 -0.00115 AFIX 13 H8 2 0.459079 0.771912 0.097037 11.00000 -1.20000 AFIX 0 C9 1 0.287382 0.652465 0.028928 11.00000 0.04172 0.02457 = 0.01471 -0.00173 0.00246 -0.00920 AFIX 137 H9A 2 0.320078 0.546507 0.086354 11.00000 -1.50000 H9B 2 0.348455 0.644428 -0.061827 11.00000 -1.50000 H9C 2 0.164734 0.676647 0.017963 11.00000 -1.50000 AFIX 0 C10 1 0.269861 0.963978 0.018954 11.00000 0.02379 0.02070 = 0.01692 0.00510 -0.00093 -0.00191 AFIX 137 H10A 2 0.145694 0.987522 0.018132 11.00000 -1.50000 H10B 2 0.319588 0.963953 -0.076000 11.00000 -1.50000 H10C 2 0.304381 1.049973 0.064289 11.00000 -1.50000 AFIX 0 N1 3 0.276250 0.383963 0.399328 11.00000 0.01772 0.01872 = 0.02412 -0.00387 0.00412 -0.00948 N2 3 0.364309 0.298085 0.319862 11.00000 0.02140 0.01204 = 0.01795 0.00170 -0.00298 -0.00899 N3 3 0.445254 0.209403 0.244008 11.00000 0.03908 0.01973 = 0.02824 -0.01013 0.01024 -0.01128 N4 3 0.582058 0.506993 0.379125 11.00000 0.01037 0.01298 = 0.01356 0.00201 0.00126 -0.00126 N5 3 0.673729 0.579574 0.300328 11.00000 0.01073 0.01758 = 0.01430 0.00309 -0.00125 -0.00097 N6 3 0.759503 0.642639 0.223249 11.00000 0.01598 0.03976 = 0.02699 0.01507 -0.00033 -0.00955 RU1 4 0.322928 0.618471 0.427929 11.00000 0.00806 0.00960 = 0.01034 0.00045 0.00059 -0.00136 HKLF 4 REM p-1_a.res in P-1 REM R1 = 0.0177 for 2959 Fo > 4sig(Fo) and 0.0183 for all 3024 data REM 157 parameters refined using 0 restraints END WGHT 0.0175 0.5033 REM Highest difference peak 0.325, deepest hole -0.707, 1-sigma level 0.083 Q1 1 0.1117 0.8067 0.6056 11.00000 0.05 0.33 Q2 1 0.4127 0.9145 0.2977 11.00000 0.05 0.30 Q3 1 0.2994 0.8447 0.2968 11.00000 0.05 0.29 Q4 1 0.0784 0.7594 0.3627 11.00000 0.05 0.28 Q5 1 0.2923 0.8774 0.0619 11.00000 0.05 0.27 Q6 1 0.2132 0.8441 0.5057 11.00000 0.05 0.26 Q7 1 0.3868 0.9025 -0.1301 11.00000 0.05 0.26 Q8 1 0.2840 0.7365 0.0627 11.00000 0.05 0.25 Q9 1 0.4212 1.1042 -0.0974 11.00000 0.05 0.23 Q10 1 0.0538 0.7247 0.2365 11.00000 0.05 0.22 Q11 1 0.2976 0.3198 0.0455 11.00000 0.05 0.22 Q12 1 0.3761 0.2545 0.1438 11.00000 0.05 0.20 Q13 1 0.3770 0.2225 0.3149 11.00000 0.05 0.20 Q14 1 0.4453 0.9570 0.3462 11.00000 0.05 0.20 Q15 1 -0.1574 0.7400 0.6752 11.00000 0.05 0.19 Q16 1 0.3337 0.1951 0.2139 11.00000 0.05 0.19 Q17 1 0.1699 0.8054 0.2666 11.00000 0.05 0.19 Q18 1 0.2014 0.4137 0.0107 11.00000 0.05 0.19 Q19 1 0.0560 1.1287 -0.0024 11.00000 0.05 0.19 Q20 1 0.1810 1.3273 0.0375 11.00000 0.05 0.19 ; _shelx_res_checksum 61867 _shelx_hkl_file ; -1 0 0 284.21 7.79 1 0 0 273.20 7.70 2 0 0 585.74 13.42 -3 0 0 831.43 23.21 3 0 0 834.26 23.19 -4 0 0 28.43 0.76 -4 0 0 28.13 0.87 4 0 0 28.36 0.72 4 0 0 27.13 0.70 4 0 0 28.14 0.86 -5 0 0 277.50 6.52 -5 0 0 297.43 6.69 5 0 0 279.95 6.44 5 0 0 277.14 6.68 5 0 0 267.95 6.46 -6 0 0 96.58 2.29 6 0 0 87.25 2.17 6 0 0 92.54 2.20 6 0 0 91.95 2.48 -7 0 0 1.43 0.28 -7 0 0 1.51 0.24 7 0 0 1.79 0.33 -8 0 0 70.15 1.86 -8 0 0 67.56 2.04 8 0 0 70.89 2.13 -9 0 0 55.48 1.78 -9 0 0 55.59 1.59 9 0 0 54.77 1.87 -10 0 0 0.88 0.29 -10 0 0 1.30 0.40 10 0 0 0.63 0.40 -11 0 0 45.97 1.69 -11 0 0 44.95 1.48 11 0 0 47.01 1.86 -12 0 0 25.81 1.30 -12 0 0 26.40 1.28 12 0 0 26.36 1.45 -12 1 0 4.86 0.85 11 -1 0 56.94 2.14 -11 1 0 56.95 1.97 10 -1 0 42.37 1.68 -10 1 0 39.80 1.51 -10 1 0 40.42 1.28 9 -1 0 6.33 0.67 -9 1 0 7.75 0.62 -9 1 0 7.31 0.46 8 -1 0 87.91 2.58 -8 1 0 89.72 2.29 -8 1 0 89.30 2.53 7 -1 0 50.53 1.26 7 -1 0 48.67 1.58 -7 1 0 49.85 1.36 -7 1 0 49.71 1.57 6 -1 0 4.73 0.22 6 -1 0 4.57 0.39 -6 1 0 4.29 0.24 -6 1 0 4.03 0.44 5 -1 0 185.45 4.36 5 -1 0 187.20 4.61 -5 1 0 191.17 4.61 -5 1 0 185.15 4.40 4 -1 0 173.76 4.14 4 -1 0 180.18 4.32 4 -1 0 177.05 4.13 -4 1 0 180.78 4.33 3 -1 0 214.98 4.94 3 -1 0 208.38 4.79 3 -1 0 206.25 4.81 3 -1 0 202.13 4.85 2 -1 0 134.93 3.34 2 -1 0 143.75 3.28 2 -1 0 138.72 3.28 -2 1 0 143.73 3.37 -2 1 0 143.53 3.28 -2 1 0 141.68 3.28 1 -1 0 163.26 3.71 1 -1 0 159.53 3.67 -1 1 0 153.28 3.70 0 -1 0 316.08 8.51 0 1 0 330.30 8.53 -1 -1 0 985.58 23.85 1 1 0 1000.00 23.82 -2 -1 0 62.92 1.46 -2 -1 0 62.85 1.45 -2 -1 0 58.52 1.45 2 1 0 56.39 1.47 2 1 0 63.13 1.45 2 1 0 60.46 1.50 -3 -1 0 222.23 5.01 -3 -1 0 215.55 4.94 3 1 0 212.68 4.95 3 1 0 205.27 5.04 -4 -1 0 435.03 9.61 -4 -1 0 395.49 9.45 4 1 0 408.76 9.63 4 1 0 411.70 9.48 -5 -1 0 2.88 0.27 -5 -1 0 3.17 0.19 -5 -1 0 3.01 0.13 5 1 0 2.58 0.24 5 1 0 2.93 0.16 -6 -1 0 181.75 4.35 -6 -1 0 177.34 4.07 -6 -1 0 160.89 4.28 6 1 0 180.41 4.42 6 1 0 181.04 4.13 -7 -1 0 65.08 1.95 -7 -1 0 72.08 1.83 7 1 0 69.85 2.03 -8 -1 0 18.49 0.83 -8 -1 0 19.60 0.72 8 1 0 19.13 0.88 -9 -1 0 89.59 2.61 -9 -1 0 96.74 2.49 9 1 0 94.84 2.77 -10 -1 0 17.00 0.89 10 1 0 17.70 1.04 -11 -1 0 21.85 1.10 11 1 0 22.94 1.28 -12 -1 0 48.85 1.76 12 1 0 48.94 2.02 11 -2 0 3.71 0.71 -11 2 0 4.63 0.74 10 -2 0 81.57 2.64 -10 2 0 81.47 2.52 9 -2 0 30.38 1.37 -9 2 0 25.48 0.89 -9 2 0 26.07 1.24 8 -2 0 34.42 1.32 -8 2 0 35.72 1.28 -8 2 0 28.66 0.96 7 -2 0 147.38 4.00 7 -2 0 165.69 3.74 -7 2 0 152.20 3.98 -7 2 0 150.31 3.71 6 -2 0 8.00 0.52 6 -2 0 8.06 0.31 -6 2 0 7.78 0.31 -6 2 0 7.82 0.52 5 -2 0 43.92 1.35 5 -2 0 44.79 1.11 -5 2 0 40.94 1.34 -5 2 0 43.62 1.12 4 -2 0 137.31 3.50 4 -2 0 137.65 3.31 -4 2 0 148.44 3.53 3 -2 0 7.54 0.35 3 -2 0 8.04 0.27 -3 2 0 7.85 0.37 -3 2 0 7.70 0.28 2 -2 0 172.02 4.05 2 -2 0 175.12 4.16 -2 2 0 175.56 4.04 -2 2 0 176.59 4.17 -2 2 0 176.44 4.11 1 -2 0 23.18 0.55 1 -2 0 22.46 0.64 -1 2 0 22.92 0.64 -1 2 0 22.63 0.55 -1 2 0 23.61 0.65 0 -2 0 144.79 3.17 0 -2 0 134.07 3.13 0 -2 0 137.89 3.22 0 2 0 125.71 3.17 0 2 0 137.15 3.12 -1 -2 0 66.72 1.68 -1 -2 0 69.74 1.60 -1 -2 0 69.63 1.62 1 2 0 69.79 1.62 1 2 0 67.85 1.60 -2 -2 0 52.06 1.25 -2 -2 0 52.44 1.21 -2 -2 0 52.27 1.21 -2 -2 0 47.21 1.28 2 2 0 51.63 1.28 -3 -2 0 1.85 0.13 -3 -2 0 1.53 0.13 3 2 0 1.69 0.10 3 2 0 1.52 0.12 3 2 0 1.58 0.15 -4 -2 0 65.03 1.63 -4 -2 0 67.16 1.66 4 2 0 64.91 1.74 4 2 0 64.70 1.62 -5 -2 0 112.82 2.76 -5 -2 0 111.08 2.70 5 2 0 107.75 2.83 5 2 0 110.73 2.66 -6 -2 0 28.06 0.91 -6 -2 0 28.08 0.86 6 2 0 27.74 0.77 6 2 0 26.81 0.99 -7 -2 0 114.87 2.81 -7 -2 0 108.11 3.02 7 2 0 111.51 2.67 7 2 0 110.37 3.00 -8 -2 0 9.36 0.48 -8 -2 0 9.24 0.59 8 2 0 8.97 0.60 -9 -2 0 43.38 1.44 9 2 0 44.68 1.60 -10 -2 0 41.94 1.45 10 2 0 40.52 1.62 -11 -2 0 0.66 0.43 11 2 0 -0.07 0.46 12 2 0 42.74 1.87 11 -3 0 5.31 0.94 -11 3 0 5.05 0.80 10 -3 0 13.78 1.06 -10 3 0 13.97 0.92 9 -3 0 42.64 1.66 -9 3 0 40.96 1.55 8 -3 0 0.15 0.33 -8 3 0 0.23 0.16 -8 3 0 0.27 0.28 7 -3 0 84.33 2.47 -7 3 0 83.02 2.16 -7 3 0 82.57 2.40 6 -3 0 74.03 1.83 6 -3 0 72.11 2.13 -6 3 0 71.84 2.10 -6 3 0 73.57 1.81 5 -3 0 1.82 0.17 5 -3 0 1.80 0.30 -5 3 0 1.31 0.27 -5 3 0 1.70 0.14 -4 3 0 39.01 1.57 -4 3 0 40.90 1.09 3 -3 0 176.17 4.16 3 -3 0 183.30 4.35 -3 3 0 171.64 4.13 -3 3 0 182.30 4.25 -3 3 0 179.74 4.34 2 -3 0 26.31 0.71 -2 3 0 28.10 0.82 -2 3 0 26.69 0.79 -2 3 0 28.52 0.67 1 -3 0 106.59 2.64 1 -3 0 104.65 2.51 -1 3 0 107.40 2.51 -1 3 0 108.98 2.65 -1 3 0 115.74 2.63 0 -3 0 69.77 1.66 0 3 0 71.06 1.79 0 3 0 71.50 1.66 -1 -3 0 40.46 0.97 -1 -3 0 39.96 0.97 1 3 0 38.94 0.96 1 3 0 39.25 1.07 1 3 0 38.82 0.99 -2 -3 0 833.77 21.77 2 3 0 815.25 21.71 -3 -3 0 93.74 2.24 -3 -3 0 91.44 2.18 -3 -3 0 92.66 2.18 3 3 0 92.93 2.29 3 3 0 93.02 2.35 -4 -3 0 96.64 2.34 -4 -3 0 97.30 2.32 4 3 0 93.28 2.37 4 3 0 96.71 2.48 -5 -3 0 208.90 5.00 -5 -3 0 211.07 5.00 5 3 0 211.03 5.16 5 3 0 212.82 4.99 -6 -3 0 14.62 0.56 -6 -3 0 14.53 0.56 6 3 0 15.54 0.51 6 3 0 14.20 0.67 -7 -3 0 60.27 1.69 -7 -3 0 62.86 1.68 7 3 0 61.02 1.86 7 3 0 59.66 1.57 -8 -3 0 54.84 1.63 -8 -3 0 54.04 1.56 8 3 0 53.77 1.77 -9 -3 0 0.26 0.26 -9 -3 0 0.06 0.22 9 3 0 0.72 0.32 -10 -3 0 33.64 1.23 -10 -3 0 32.41 1.19 10 3 0 32.54 1.44 -11 -3 0 22.80 0.99 11 3 0 21.71 1.28 -12 -3 0 0.75 0.41 12 3 0 2.71 0.64 10 -4 0 0.39 0.57 -10 4 0 0.58 0.41 9 -4 0 29.96 1.44 -9 4 0 30.10 1.30 8 -4 0 28.29 1.31 -8 4 0 28.98 1.24 7 -4 0 1.13 0.37 -7 4 0 1.24 0.34 6 -4 0 114.70 2.78 6 -4 0 112.33 3.12 -6 4 0 112.43 2.70 -6 4 0 112.31 3.04 5 -4 0 47.04 1.52 -5 4 0 47.74 1.29 -5 4 0 46.06 1.17 -5 4 0 46.73 1.47 4 -4 0 9.05 0.52 -4 4 0 8.55 0.38 -4 4 0 8.82 0.51 3 -4 0 238.86 5.78 -3 4 0 267.82 6.03 -3 4 0 242.33 5.76 -3 4 0 255.03 5.96 2 -4 0 236.99 5.70 -2 4 0 237.58 5.67 -2 4 0 238.15 5.47 -2 4 0 242.30 5.67 1 -4 0 152.14 3.77 -1 4 0 158.66 3.74 -1 4 0 160.08 3.61 -1 4 0 155.89 3.80 0 -4 0 227.41 5.28 0 -4 0 220.54 5.38 0 4 0 233.94 5.27 0 4 0 234.25 5.46 -1 -4 0 22.89 0.60 1 4 0 21.71 0.59 1 4 0 22.02 0.71 -2 -4 0 300.96 6.87 -2 -4 0 300.57 6.92 2 4 0 292.75 6.87 2 4 0 301.89 7.04 2 4 0 299.23 7.07 -3 -4 0 328.73 7.48 -3 -4 0 320.42 7.57 3 4 0 323.83 7.72 3 4 0 332.77 7.67 -4 -4 0 11.41 0.35 -4 -4 0 12.07 0.37 -4 -4 0 12.08 0.43 4 4 0 12.24 0.52 4 4 0 11.74 0.46 -5 -4 0 242.65 5.57 -5 -4 0 251.11 5.52 5 4 0 205.20 5.57 5 4 0 241.33 5.75 -6 -4 0 204.41 4.79 -6 -4 0 197.78 4.82 6 4 0 200.84 4.82 6 4 0 199.12 5.02 -7 -4 0 0.28 0.15 -7 -4 0 0.03 0.15 7 4 0 0.35 0.14 7 4 0 0.04 0.21 -8 -4 0 88.53 2.41 -8 -4 0 90.17 2.38 8 4 0 89.34 2.64 8 4 0 94.39 2.38 -9 -4 0 59.57 1.77 -9 -4 0 63.42 1.81 9 4 0 61.98 2.06 -10 -4 0 2.65 0.46 10 4 0 3.35 0.58 -11 -4 0 47.99 1.60 11 4 0 48.32 1.93 -12 -4 0 15.15 0.90 12 4 0 15.88 1.22 10 -5 0 13.06 1.14 -10 5 0 10.11 0.92 9 -5 0 5.62 0.88 -9 5 0 6.12 0.75 8 -5 0 62.48 2.17 -8 5 0 60.52 2.00 7 -5 0 39.89 1.57 -7 5 0 38.26 1.43 6 -5 0 23.14 0.84 6 -5 0 26.37 1.13 -6 5 0 26.02 1.04 5 -5 0 238.19 6.02 -5 5 0 234.98 5.79 -5 5 0 250.52 5.96 4 -5 0 24.85 0.99 -4 5 0 24.77 0.62 -4 5 0 24.43 0.97 -4 5 0 26.52 0.93 3 -5 0 71.21 2.01 -3 5 0 72.04 1.95 -3 5 0 70.91 1.94 2 -5 0 334.16 8.12 -2 5 0 347.34 8.07 -2 5 0 348.07 8.12 1 -5 0 10.52 0.45 1 -5 0 10.00 0.27 -1 5 0 9.10 0.43 -1 5 0 8.54 0.37 -1 5 0 8.77 0.26 0 -5 0 236.76 5.72 0 -5 0 238.01 5.57 0 5 0 249.11 5.81 -1 -5 0 135.19 3.14 -1 -5 0 130.79 3.24 1 5 0 131.91 3.14 1 5 0 134.38 3.33 2 5 0 0.22 0.10 -3 -5 0 122.54 2.99 -3 -5 0 124.86 2.89 3 5 0 122.81 3.12 3 5 0 126.36 3.17 -4 -5 0 52.97 1.30 -4 -5 0 55.21 1.33 -4 -5 0 54.68 1.44 4 5 0 54.99 1.53 4 5 0 55.31 1.61 -5 -5 0 16.40 0.60 -5 -5 0 16.84 0.50 5 5 0 15.72 0.71 5 5 0 15.34 0.60 -6 -5 0 140.24 3.21 -6 -5 0 133.31 3.30 6 5 0 124.35 3.31 6 5 0 132.63 3.50 -7 -5 0 49.60 1.31 -7 -5 0 46.48 1.39 7 5 0 48.14 1.60 7 5 0 47.23 1.38 -8 -5 0 20.14 0.78 8 5 0 18.51 0.68 8 5 0 18.14 0.93 -9 -5 0 102.33 2.73 9 5 0 99.44 2.99 -10 -5 0 21.35 0.93 10 5 0 21.08 1.17 -11 -5 0 15.39 0.85 11 5 0 15.88 1.14 -12 -5 0 41.94 1.54 12 5 0 43.31 1.88 9 -6 0 1.99 0.60 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7 0 114.36 2.98 -8 -7 0 75.39 2.12 8 7 0 72.95 2.12 8 7 0 74.92 2.42 -9 -7 0 1.38 0.33 9 7 0 1.71 0.47 -10 -7 0 50.59 1.68 10 7 0 51.74 1.99 -11 -7 0 19.86 1.01 11 7 0 21.30 1.34 7 -8 0 3.67 0.68 -7 8 0 3.21 0.56 6 -8 0 37.15 1.64 -6 8 0 35.42 1.41 5 -8 0 22.82 1.19 -5 8 0 22.92 0.99 -5 8 0 22.20 1.11 4 -8 0 6.10 1.09 -4 8 0 3.86 0.53 3 -8 0 76.11 2.32 -3 8 0 75.66 2.24 -3 8 0 76.80 2.17 2 -8 0 15.67 0.82 -2 8 0 15.04 0.67 -2 8 0 15.67 0.79 1 -8 0 35.96 1.24 -1 8 0 34.31 1.24 -1 8 0 33.95 1.08 0 -8 0 102.37 2.76 0 8 0 105.86 2.62 0 8 0 100.45 2.83 -1 -8 0 6.59 0.29 -1 -8 0 5.97 0.45 1 8 0 6.76 0.49 1 8 0 7.21 0.32 -2 -8 0 56.87 1.46 -2 -8 0 54.95 1.62 2 8 0 52.45 1.70 2 8 0 54.60 1.42 -3 -8 0 102.47 2.59 -3 -8 0 103.09 2.71 3 8 0 102.00 2.83 -4 -8 0 0.39 0.19 -4 -8 0 0.65 0.21 -5 -8 0 48.33 1.40 5 8 0 46.04 1.62 5 8 0 48.02 1.56 -6 -8 0 24.41 0.90 6 8 0 24.22 1.08 6 8 0 23.42 1.01 -7 -8 0 5.09 0.49 7 8 0 5.77 0.59 7 8 0 5.27 0.64 -8 -8 0 62.18 1.87 8 8 0 61.26 1.93 8 8 0 63.44 2.16 -9 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1.13 1 6 14 9.87 1.08 -2 -6 -14 15.48 1.24 2 6 14 15.15 1.14 -3 -6 -14 2.03 0.84 -3 -6 -14 0.89 0.67 -3 -7 -14 1.65 0.76 -1 2 -15 35.66 2.55 -2 2 -15 7.85 1.40 0 1 -15 2.55 0.82 -1 1 -15 15.15 1.41 -2 1 -15 25.83 1.71 1 0 -15 27.85 2.36 -1 0 15 24.28 1.17 0 0 -15 34.68 1.79 0 0 15 36.58 1.43 -1 0 -15 1.59 0.71 1 0 15 1.52 0.48 -2 0 -15 28.33 1.68 2 0 15 28.64 1.73 -3 0 -15 21.61 1.30 1 -1 -15 0.82 0.93 -1 1 15 1.57 0.44 0 -1 -15 45.19 2.05 0 1 15 49.86 1.71 -1 -1 -15 25.50 1.59 -1 -1 -15 25.10 1.47 1 1 15 25.94 1.22 -2 -1 -15 6.63 0.95 -2 -1 -15 5.37 0.72 2 1 15 6.92 0.80 -3 -1 -15 40.29 1.70 -2 2 15 18.30 1.13 1 -2 -15 4.35 1.48 0 -2 -15 3.13 0.74 0 -2 -15 3.79 0.59 -1 -2 -15 26.32 1.27 -1 -2 -15 22.08 1.47 1 2 15 24.48 1.17 -2 -2 -15 1.36 0.71 -2 -2 -15 -0.28 0.46 2 2 15 0.92 0.47 -3 -2 -15 9.57 1.38 -3 -2 -15 8.97 0.96 3 2 15 9.48 0.90 -1 3 15 12.10 1.12 0 -3 -15 1.11 0.72 -1 -3 -15 12.32 1.30 -1 -3 -15 12.01 0.96 -2 -3 -15 11.48 1.22 -2 -3 -15 10.65 0.96 2 3 15 11.29 0.94 -3 -3 -15 5.86 1.07 -3 -3 -15 8.04 1.13 3 3 15 4.87 0.85 -1 -4 -15 1.52 0.77 -2 -4 -15 38.59 1.89 -3 -4 -15 7.71 1.20 -2 -5 -15 3.21 1.47 -3 -5 -15 43.26 2.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 16670 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1426(2) 0.8104(2) 0.53254(18) 0.0177(3) Uani 1 1 d . . . . . C2 C 0.0553(2) 0.7453(2) 0.43916(18) 0.0176(3) Uani 1 1 d . . . . . H2 H -0.0324 0.6803 0.4762 0.021 Uiso 1 1 calc R U . . . C3 C 0.1169(2) 0.7396(2) 0.29852(18) 0.0160(3) Uani 1 1 d . . . . . H3 H 0.0709 0.6695 0.2407 0.019 Uiso 1 1 calc R U . . . C4 C 0.2635(2) 0.7989(2) 0.24693(17) 0.0140(3) Uani 1 1 d . . . . . C5 C 0.3485(2) 0.8666(2) 0.34274(18) 0.0152(3) Uani 1 1 d . . . . . H5 H 0.4650 0.8862 0.3151 0.018 Uiso 1 1 calc R U . . . C6 C 0.2884(2) 0.8751(2) 0.48205(18) 0.0172(3) Uani 1 1 d . . . . . H6 H 0.3636 0.8997 0.5495 0.021 Uiso 1 1 calc R U . . . C7 C 0.0873(3) 0.8029(3) 0.68325(19) 0.0260(4) Uani 1 1 d . . . . . H7A H 0.1870 0.7852 0.7378 0.039 Uiso 1 1 calc R U . . . H7B H 0.0287 0.7105 0.7075 0.039 Uiso 1 1 calc R U . . . H7C H 0.0099 0.9081 0.7028 0.039 Uiso 1 1 calc R U . . . C8 C 0.3324(2) 0.7924(2) 0.09796(17) 0.0169(3) Uani 1 1 d . . . . . H8 H 0.4591 0.7719 0.0970 0.020 Uiso 1 1 calc R U . . . C9 C 0.2874(3) 0.6525(3) 0.0289(2) 0.0269(4) Uani 1 1 d . . . . . H9A H 0.3201 0.5465 0.0864 0.040 Uiso 1 1 calc R U . . . H9B H 0.3485 0.6444 -0.0618 0.040 Uiso 1 1 calc R U . . . H9C H 0.1647 0.6766 0.0180 0.040 Uiso 1 1 calc R U . . . C10 C 0.2699(2) 0.9640(2) 0.01895(19) 0.0215(4) Uani 1 1 d . . . . . H10A H 0.1457 0.9875 0.0181 0.032 Uiso 1 1 calc R U . . . H10B H 0.3196 0.9640 -0.0760 0.032 Uiso 1 1 calc R U . . . H10C H 0.3044 1.0500 0.0643 0.032 Uiso 1 1 calc R U . . . N1 N 0.2763(2) 0.38396(19) 0.39933(17) 0.0195(3) Uani 1 1 d . . . . . N2 N 0.36431(19) 0.29808(18) 0.31986(15) 0.0164(3) Uani 1 1 d . . . . . N3 N 0.4453(2) 0.2094(2) 0.24401(19) 0.0283(4) Uani 1 1 d . . . . . N4 N 0.58206(17) 0.50699(17) 0.37913(15) 0.0129(3) Uani 1 1 d . . . . . N5 N 0.67373(18) 0.57957(18) 0.30033(15) 0.0149(3) Uani 1 1 d . . . . . N6 N 0.7595(2) 0.6426(2) 0.22325(18) 0.0286(4) Uani 1 1 d . . . . . Ru1 Ru 0.32293(2) 0.61847(2) 0.42793(2) 0.00960(5) 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 0.0178(8) 0.0142(8) 0.0155(8) 0.0006(6) 0.0007(6) 0.0067(6) C2 0.0095(7) 0.0204(8) 0.0187(8) 0.0030(7) 0.0013(6) 0.0025(6) C3 0.0106(7) 0.0191(8) 0.0165(8) 0.0019(6) -0.0025(6) -0.0004(6) C4 0.0127(7) 0.0137(7) 0.0133(7) 0.0029(6) -0.0013(6) 0.0000(6) C5 0.0157(8) 0.0099(7) 0.0185(8) 0.0024(6) -0.0017(6) -0.0014(6) C6 0.0222(8) 0.0093(7) 0.0184(8) -0.0015(6) -0.0047(7) 0.0018(6) C7 0.0314(10) 0.0228(9) 0.0157(8) -0.0004(7) 0.0044(7) 0.0088(8) C8 0.0157(8) 0.0193(8) 0.0131(8) 0.0031(6) 0.0004(6) -0.0012(6) C9 0.0417(12) 0.0246(10) 0.0147(8) -0.0017(7) 0.0025(8) -0.0092(9) C10 0.0238(9) 0.0207(9) 0.0169(8) 0.0051(7) -0.0009(7) -0.0019(7) N1 0.0177(7) 0.0187(7) 0.0241(8) -0.0039(6) 0.0041(6) -0.0095(6) N2 0.0214(7) 0.0120(6) 0.0179(7) 0.0017(5) -0.0030(6) -0.0090(6) N3 0.0391(10) 0.0197(8) 0.0282(9) -0.0101(7) 0.0102(8) -0.0113(7) N4 0.0104(6) 0.0130(6) 0.0136(6) 0.0020(5) 0.0013(5) -0.0013(5) N5 0.0107(6) 0.0176(7) 0.0143(7) 0.0031(5) -0.0013(5) -0.0010(5) N6 0.0160(7) 0.0398(10) 0.0270(9) 0.0151(7) -0.0003(6) -0.0095(7) Ru1 0.00806(7) 0.00960(7) 0.01034(7) 0.00045(4) 0.00059(4) -0.00136(4) 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' 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 118.95(16) . . ? C2 C1 C7 120.23(17) . . ? C6 C1 C7 120.75(17) . . ? C2 C1 Ru1 70.99(10) . . ? C6 C1 Ru1 71.34(10) . . ? C7 C1 Ru1 126.75(12) . . ? C1 C2 C3 120.05(16) . . ? C1 C2 Ru1 71.13(9) . . ? C3 C2 Ru1 70.32(9) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? Ru1 C2 H2 119.2 . . ? C4 C3 C2 122.01(16) . . ? C4 C3 Ru1 71.93(9) . . ? C2 C3 Ru1 71.49(9) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? Ru1 C3 H3 118.3 . . ? C3 C4 C5 117.01(15) . . ? C3 C4 C8 122.90(15) . . ? C5 C4 C8 120.10(15) . . ? C3 C4 Ru1 70.28(9) . . ? C5 C4 Ru1 69.85(9) . . ? C8 C4 Ru1 130.46(12) . . ? C6 C5 C4 121.86(16) . . ? C6 C5 Ru1 72.23(10) . . ? C4 C5 Ru1 71.66(9) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? Ru1 C5 H5 118.5 . . ? C5 C6 C1 120.06(16) . . ? C5 C6 Ru1 70.04(9) . . ? C1 C6 Ru1 70.67(10) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? Ru1 C6 H6 119.1 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 C9 113.31(15) . . ? C4 C8 C10 108.57(14) . . ? C9 C8 C10 111.78(15) . . ? C4 C8 H8 107.6 . . ? C9 C8 H8 107.6 . . ? C10 C8 H8 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 N1 Ru1 120.67(12) . . ? N3 N2 N1 176.90(18) . . ? N5 N4 Ru1 121.88(11) . . ? N5 N4 Ru1 119.03(11) . 2_666 ? Ru1 N4 Ru1 104.97(6) . 2_666 ? N6 N5 N4 177.27(19) . . ? N1 Ru1 N4 84.78(6) . . ? N1 Ru1 N4 83.98(6) . 2_666 ? N4 Ru1 N4 75.03(6) . 2_666 ? N1 Ru1 C5 149.39(7) . . ? N4 Ru1 C5 94.12(6) . . ? N4 Ru1 C5 125.35(6) 2_666 . ? N1 Ru1 C3 89.91(7) . . ? N4 Ru1 C3 131.81(6) . . ? N4 Ru1 C3 151.89(6) 2_666 . ? C5 Ru1 C3 68.14(7) . . ? N1 Ru1 C2 95.15(7) . . ? N4 Ru1 C2 169.96(6) . . ? N4 Ru1 C2 114.97(6) 2_666 . ? C5 Ru1 C2 80.81(7) . . ? C3 Ru1 C2 38.19(6) . . ? N1 Ru1 C1 124.26(7) . . ? N4 Ru1 C1 147.35(6) . . ? N4 Ru1 C1 92.10(6) 2_666 . ? C5 Ru1 C1 68.74(7) . . ? C3 Ru1 C1 68.87(7) . . ? C2 Ru1 C1 37.89(7) . . ? N1 Ru1 C4 111.73(6) . . ? N4 Ru1 C4 101.57(6) . . ? N4 Ru1 C4 163.78(6) 2_666 . ? C5 Ru1 C4 38.49(6) . . ? C3 Ru1 C4 37.79(6) . . ? C2 Ru1 C4 69.09(6) . . ? C1 Ru1 C4 82.42(6) . . ? N1 Ru1 C6 162.10(7) . . ? N4 Ru1 C6 112.85(6) . . ? N4 Ru1 C6 97.24(6) 2_666 . ? C5 Ru1 C6 37.73(7) . . ? C3 Ru1 C6 80.61(7) . . ? C2 Ru1 C6 68.05(7) . . ? C1 Ru1 C6 37.99(7) . . ? C4 Ru1 C6 69.14(6) . . ? 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 1.420(3) . ? C1 C6 1.427(3) . ? C1 C7 1.502(2) . ? C1 Ru1 2.1872(17) . ? C2 C3 1.425(2) . ? C2 Ru1 2.1854(16) . ? C2 H2 1.0000 . ? C3 C4 1.413(2) . ? C3 Ru1 2.1700(16) . ? C3 H3 1.0000 . ? C4 C5 1.437(2) . ? C4 C8 1.517(2) . ? C4 Ru1 2.1916(16) . ? C5 C6 1.411(2) . ? C5 Ru1 2.1675(16) . ? C5 H5 1.0000 . ? C6 Ru1 2.1959(17) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.527(3) . ? C8 C10 1.535(2) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N1 N2 1.193(2) . ? N1 Ru1 2.1063(15) . ? N2 N3 1.160(2) . ? N4 N5 1.222(2) . ? N4 Ru1 2.1314(14) . ? N4 Ru1 2.1610(14) 2_666 ? N5 N6 1.140(2) . ? Ru1 N4 2.1610(14) 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 2.2(2) . . . . ? C7 C1 C2 C3 -174.60(16) . . . . ? Ru1 C1 C2 C3 -52.48(14) . . . . ? C6 C1 C2 Ru1 54.73(14) . . . . ? C7 C1 C2 Ru1 -122.12(16) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? Ru1 C2 C3 C4 -53.48(15) . . . . ? C1 C2 C3 Ru1 52.85(14) . . . . ? C2 C3 C4 C5 -0.3(2) . . . . ? Ru1 C3 C4 C5 -53.59(13) . . . . ? C2 C3 C4 C8 179.38(16) . . . . ? Ru1 C3 C4 C8 126.09(16) . . . . ? C2 C3 C4 Ru1 53.29(15) . . . . ? C3 C4 C5 C6 -0.4(2) . . . . ? C8 C4 C5 C6 179.89(15) . . . . ? Ru1 C4 C5 C6 -54.22(14) . . . . ? C3 C4 C5 Ru1 53.80(13) . . . . ? C8 C4 C5 Ru1 -125.89(15) . . . . ? C4 C5 C6 C1 2.1(2) . . . . ? Ru1 C5 C6 C1 -51.90(14) . . . . ? C4 C5 C6 Ru1 53.97(14) . . . . ? C2 C1 C6 C5 -2.9(2) . . . . ? C7 C1 C6 C5 173.88(16) . . . . ? Ru1 C1 C6 C5 51.61(14) . . . . ? C2 C1 C6 Ru1 -54.56(14) . . . . ? C7 C1 C6 Ru1 122.27(16) . . . . ? C3 C4 C8 C9 -26.8(2) . . . . ? C5 C4 C8 C9 152.90(16) . . . . ? Ru1 C4 C8 C9 64.6(2) . . . . ? C3 C4 C8 C10 98.06(19) . . . . ? C5 C4 C8 C10 -82.27(19) . . . . ? Ru1 C4 C8 C10 -170.60(13) . . . . ?