# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Apr 2 17:04:38 2003' _audit_creation_method 'PLATON option' _audit_update_record ; ? ; _journal_coden_Cambridge 440 loop_ _publ_author_name 'Anna C.G. Hotze' 'Huub Kooijman' 'Anthony L. Spek' 'Jaap G. Haasnoot' 'Jan Reedijk' _publ_contact_author_name 'Prof Jan Reedijk' _publ_contact_author_address ; Leiden Institute of Chemistry Leiden University P.O. Box 9502 Leiden 2300 RA NETHERLANDS ; _publ_contact_author_email REEDIJK@CHEM.LEIDENUNIV.NL _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Synthesis and characterization of ruthenium(II) complexes with the new ligand 2-phenylazopyridine-5-sulfonic acid (Hsazpy): in search for new anticancer agents ; #=============================================================================== # 4. TEXT _publ_section_references ; Flack, H.D. (1983). Acta Cryst. A39, 876-881. Nonius (1998). Collect Software, Nonius B.V., Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C.W. Carter & R.M. Sweet, pp. 307-326. London: Academic Press. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G"ottingen, Germany, 1997. Sheldrick, G.M. SHELXS86. Program for Crystal Structure solution. University of Gottingen, Germany, 1986. Spek, A.L. (2002). PLATON, A multi-purpose crystallographic tool, Utrecht University, The Netherlands. Internet: http://www.cryst.chem.uu.nl/platon/ Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_acknowledgements ; This work was supported in part (ALS) by the Council for the Chemical Sciences of the Netherlands Organization for Scientific Research (CW-NWO). ; #=============================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 228185' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Cl2 N6 O6 Ru S2, 2(C8 H20 N), 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C38 H60 Cl2 N8 O8 Ru S2' _chemical_formula_iupac ? _chemical_formula_weight 993.05 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 9.3614(12) _cell_length_b 9.8737(12) _cell_length_c 24.449(4) _cell_angle_alpha 90 _cell_angle_beta 90.81(3) _cell_angle_gamma 90 _cell_volume 2259.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 1108 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _cell_special_details ; Quoted _cell_measurement_* data items refer to the initial cell determination. The cell parameters as reported in _cell_* are based on the complete data set. ; _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.615 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD area detector' _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_detector_area_resol_mean 18.4 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 20733 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.26 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_reduction_process ; ? ; _reflns_number_total 8023 _reflns_number_gt 7131 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'Denzo (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2002)' _computing_publication_material 'PLATON (Spek, 2002)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs 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 measured crystal turned out to be a pseudo-merohedral twin. The twin operation is a 2-fold rotation axis parallel to a. The crystal was also an inversion twin, leading to a total of 4 components, related by symmetry operations 1, 2, m and \=1 with respect to the a-axis. Since \b is close to 90 deg a refinement model (SHELXL-97-2) of complete overlap of the twin components lead to satisfactory results. The ratio in which the four components 1, 2, m and \=1 were present refined to 0.28(4):0.15(3):0.42(5):0.15(4). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(F~o~^2^)+(0.0010P)^2^+14.0P] where P=(F~o~^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct ' _atom_sites_solution_secondary 'difmap ' _atom_sites_solution_hydrogens 'geom ' # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # (mixed) SHELXL _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'none ' _refine_ls_abs_structure_details ; The crystal is both a racemic AND a pseudo-merohedral twin (2-rotation around a), see _refine_special_details. The Flack parameter is indirectly incorporated in the 4-component twin model. The value reported in _refine_ls_abs_structure_Flack is therefore meaningless. ; _refine_ls_abs_structure_Flack 0.0 # Permitted for _chemical_absolute_configuration: # Absolute configuration details # rm = Det. by chiral ref. mol. with known abs.conf # ad = Det. by anomalous dispersion # rmad = Det. by 'rm' and 'ad' # syn = Det. with reference to synthesis # unk = Unknown/Arbitrary _chemical_absolute_configuration ad _refine_ls_number_reflns 8023 _refine_ls_number_parameters 535 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.357 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.108 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ru1 Ru Uani 0.56598(7) 0.36118(7) 0.24899(4) 1.000 0.0237(2) . . Cl1 Cl Uani 0.7831(2) 0.4923(2) 0.24834(13) 1.000 0.0329(7) . . Cl2 Cl Uani 0.6986(3) 0.1556(2) 0.23924(10) 1.000 0.0349(8) . . S1 S Uani 0.7078(3) 0.1657(2) 0.46849(10) 1.000 0.0286(7) . . S2 S Uani 0.7370(3) 0.4418(3) 0.02354(11) 1.000 0.0310(8) . . O1 O Uani 0.6183(9) 0.0469(7) 0.4629(3) 1.000 0.045(3) . . O2 O Uani 0.8498(8) 0.1471(8) 0.4490(3) 1.000 0.042(3) . . O3 O Uani 0.7029(8) 0.2238(7) 0.5221(3) 1.000 0.039(3) . . O4 O Uani 0.7907(9) 0.3290(7) -0.0068(3) 1.000 0.043(3) . . O5 O Uani 0.6436(10) 0.5281(9) -0.0090(4) 1.000 0.053(3) . . O6 O Uani 0.8455(9) 0.5166(8) 0.0550(3) 1.000 0.044(3) . . N1 N Uani 0.5739(9) 0.3621(10) 0.3321(3) 1.000 0.024(2) . . N7 N Uani 0.4470(10) 0.5649(8) 0.3183(3) 1.000 0.029(3) . . N8 N Uani 0.4611(8) 0.5324(7) 0.2677(3) 1.000 0.024(3) . . N21 N Uani 0.5484(9) 0.3532(10) 0.1651(3) 1.000 0.020(2) . . N27 N Uani 0.3520(10) 0.2174(9) 0.1883(4) 1.000 0.031(3) . . N28 N Uani 0.3889(8) 0.2549(7) 0.2369(3) 1.000 0.023(2) . . C2 C Uani 0.5015(12) 0.4707(10) 0.3548(4) 1.000 0.028(3) . . C3 C Uani 0.4877(12) 0.4893(10) 0.4102(5) 1.000 0.033(3) . . C4 C Uani 0.5495(13) 0.3963(10) 0.4456(5) 1.000 0.036(4) . . C5 C Uani 0.6278(11) 0.2884(10) 0.4237(4) 1.000 0.029(3) . . C6 C Uani 0.6362(12) 0.2751(10) 0.3682(4) 1.000 0.028(3) . . C9 C Uani 0.4110(10) 0.6347(8) 0.2312(4) 1.000 0.026(3) . . C10 C Uani 0.3237(12) 0.6002(10) 0.1861(5) 1.000 0.033(4) . . C11 C Uani 0.2716(12) 0.7021(11) 0.1534(5) 1.000 0.042(4) . . C12 C Uani 0.3051(13) 0.8371(11) 0.1639(5) 1.000 0.041(4) . . C13 C Uani 0.3940(11) 0.8687(13) 0.2078(4) 1.000 0.043(3) . . C14 C Uani 0.4442(12) 0.7688(8) 0.2435(5) 1.000 0.035(3) . . C22 C Uani 0.4438(12) 0.2651(9) 0.1484(4) 1.000 0.028(3) . . C23 C Uani 0.4271(12) 0.2250(9) 0.0951(4) 1.000 0.030(3) . . C24 C Uani 0.5183(12) 0.2779(11) 0.0569(5) 1.000 0.034(4) . . C25 C Uani 0.6226(10) 0.3716(12) 0.0728(4) 1.000 0.027(3) . . C26 C Uani 0.6334(11) 0.4085(10) 0.1279(4) 1.000 0.026(3) . . C29 C Uani 0.2892(12) 0.2202(9) 0.2778(4) 1.000 0.031(3) . . C30 C Uani 0.3326(12) 0.1449(11) 0.3225(4) 1.000 0.033(3) . . C31 C Uani 0.2329(15) 0.1144(11) 0.3616(5) 1.000 0.046(4) . . C32 C Uani 0.0935(13) 0.1590(12) 0.3566(5) 1.000 0.045(4) . . C33 C Uani 0.0503(13) 0.2298(12) 0.3117(5) 1.000 0.048(4) . . C34 C Uani 0.1475(11) 0.2633(11) 0.2710(5) 1.000 0.043(4) . . N60 N Uani 0.9151(9) 0.7075(7) 0.3928(3) 1.000 0.029(3) . . C61 C Uani 0.7932(12) 0.7543(10) 0.3549(4) 1.000 0.032(3) . . C62 C Uani 0.7954(14) 0.9033(10) 0.3397(5) 1.000 0.039(4) . . C63 C Uani 1.0590(12) 0.7493(10) 0.3707(4) 1.000 0.035(3) . . C64 C Uani 1.0911(14) 0.6985(13) 0.3154(5) 1.000 0.055(5) . . C65 C Uani 0.9011(14) 0.7701(10) 0.4488(4) 1.000 0.041(4) . . C66 C Uani 0.7766(13) 0.7267(12) 0.4817(5) 1.000 0.047(4) . . C67 C Uani 0.9042(12) 0.5527(9) 0.3950(5) 1.000 0.035(4) . . C68 C Uani 1.0172(14) 0.4847(11) 0.4320(5) 1.000 0.048(4) . . N70 N Uani 0.8242(10) 0.9339(9) 0.0820(4) 1.000 0.040(3) . . C71 C Uani 0.8508(12) 0.8975(10) 0.0228(5) 1.000 0.042(4) . . C72 C Uani 0.7823(15) 0.9874(11) -0.0201(5) 1.000 0.048(4) . . C73 C Uani 0.8648(13) 1.0829(10) 0.0933(5) 1.000 0.038(3) . . C74 C Uani 1.0184(13) 1.1162(12) 0.0840(6) 1.000 0.054(5) . . C75 C Uani 0.9155(15) 0.8406(13) 0.1170(5) 1.000 0.055(5) . . C76 C Uani 0.9054(18) 0.8548(18) 0.1780(5) 1.000 0.073(5) . . C77 C Uani 0.6693(14) 0.9217(13) 0.0938(6) 1.000 0.048(4) . . C78 C Uani 0.6097(15) 0.7765(13) 0.0929(6) 1.000 0.056(5) . . O40 O Uani 0.4720(10) 0.8595(13) 0.3940(4) 1.000 0.075(3) . . O50 O Uani 0.0212(9) 0.4510(11) 0.1483(4) 1.000 0.066(4) . . H3 H Uiso 0.43670 0.56490 0.42390 1.000 0.0390 calc R H4 H Uiso 0.53900 0.40520 0.48400 1.000 0.0430 calc R H6 H Uiso 0.68860 0.20080 0.35410 1.000 0.0330 calc R H10 H Uiso 0.30130 0.50820 0.17850 1.000 0.0400 calc R H11 H Uiso 0.21160 0.68020 0.12300 1.000 0.0500 calc R H12 H Uiso 0.26720 0.90680 0.14120 1.000 0.0500 calc R H13 H Uiso 0.42140 0.96030 0.21360 1.000 0.0520 calc R H14 H Uiso 0.49920 0.79150 0.27520 1.000 0.0430 calc R H23 H Uiso 0.35460 0.16230 0.08470 1.000 0.0370 calc R H24 H Uiso 0.51030 0.25070 0.01970 1.000 0.0410 calc R H26 H Uiso 0.70220 0.47410 0.13900 1.000 0.0320 calc R H30 H Uiso 0.42870 0.11480 0.32620 1.000 0.0390 calc R H31 H Uiso 0.26060 0.06200 0.39260 1.000 0.0550 calc R H32 H Uiso 0.02750 0.13990 0.38470 1.000 0.0530 calc R H33 H Uiso -0.04680 0.25680 0.30800 1.000 0.0570 calc R H34 H Uiso 0.11840 0.31370 0.23960 1.000 0.0510 calc R H61A H Uiso 0.79620 0.70020 0.32090 1.000 0.0380 calc R H61B H Uiso 0.70130 0.73440 0.37280 1.000 0.0380 calc R H62A H Uiso 0.71410 0.92360 0.31530 1.000 0.0580 calc R H62B H Uiso 0.88470 0.92420 0.32100 1.000 0.0580 calc R H62C H Uiso 0.78890 0.95840 0.37290 1.000 0.0580 calc R H63A H Uiso 1.06370 0.84940 0.37000 1.000 0.0420 calc R H63B H Uiso 1.13450 0.71700 0.39620 1.000 0.0420 calc R H64A H Uiso 1.18450 0.73250 0.30420 1.000 0.0820 calc R H64B H Uiso 1.01740 0.72990 0.28950 1.000 0.0820 calc R H64C H Uiso 1.09260 0.59920 0.31590 1.000 0.0820 calc R H65A H Uiso 0.98920 0.74960 0.47010 1.000 0.0480 calc R H65B H Uiso 0.89620 0.86970 0.44430 1.000 0.0480 calc R H66A H Uiso 0.77820 0.77440 0.51680 1.000 0.0700 calc R H66B H Uiso 0.78170 0.62890 0.48810 1.000 0.0700 calc R H66C H Uiso 0.68790 0.74830 0.46180 1.000 0.0700 calc R H67A H Uiso 0.91350 0.51660 0.35740 1.000 0.0420 calc R H67B H Uiso 0.80820 0.52770 0.40810 1.000 0.0420 calc R H68A H Uiso 1.00130 0.38660 0.43230 1.000 0.0720 calc R H68B H Uiso 1.00960 0.52010 0.46930 1.000 0.0720 calc R H68C H Uiso 1.11270 0.50390 0.41800 1.000 0.0720 calc R H71A H Uiso 0.95530 0.89770 0.01710 1.000 0.0510 calc R H71B H Uiso 0.81670 0.80370 0.01670 1.000 0.0510 calc R H72A H Uiso 0.81220 0.95800 -0.05650 1.000 0.0720 calc R H72B H Uiso 0.81220 1.08130 -0.01410 1.000 0.0720 calc R H72C H Uiso 0.67810 0.98100 -0.01770 1.000 0.0720 calc R H73A H Uiso 0.80500 1.14180 0.06960 1.000 0.0460 calc R H73B H Uiso 0.84190 1.10440 0.13180 1.000 0.0460 calc R H74A H Uiso 1.03380 1.21330 0.08990 1.000 0.0820 calc R H74B H Uiso 1.04340 1.09260 0.04640 1.000 0.0820 calc R H74C H Uiso 1.07860 1.06450 0.10970 1.000 0.0820 calc R H75A H Uiso 0.89050 0.74610 0.10740 1.000 0.0670 calc R H75B H Uiso 1.01650 0.85460 0.10700 1.000 0.0670 calc R H76A H Uiso 0.97260 0.79210 0.19580 1.000 0.1090 calc R H76B H Uiso 0.80790 0.83370 0.18930 1.000 0.1090 calc R H76C H Uiso 0.92910 0.94790 0.18860 1.000 0.1090 calc R H77A H Uiso 0.61520 0.97640 0.06660 1.000 0.0570 calc R H77B H Uiso 0.65190 0.96140 0.13030 1.000 0.0570 calc R H78A H Uiso 0.50640 0.77900 0.09880 1.000 0.0840 calc R H78B H Uiso 0.65590 0.72330 0.12200 1.000 0.0840 calc R H78C H Uiso 0.62880 0.73480 0.05740 1.000 0.0840 calc R H40A H Uiso 0.51450 0.91350 0.41390 1.000 0.1130 . R H40B H Uiso 0.42350 0.82140 0.41710 1.000 0.1130 . R H50A H Uiso -0.02850 0.46940 0.12150 1.000 0.1000 . R H50B H Uiso -0.03670 0.46090 0.17290 1.000 0.1000 . R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0258(3) 0.0118(3) 0.0334(3) -0.0001(4) 0.0012(5) 0.0009(4) Cl1 0.0313(12) 0.0251(11) 0.0422(13) -0.0047(13) 0.0020(15) -0.0061(9) Cl2 0.0404(14) 0.0228(11) 0.0414(16) 0.0000(11) 0.0022(12) 0.0083(10) S1 0.0309(13) 0.0213(11) 0.0337(13) 0.0034(11) 0.0018(12) -0.0013(10) S2 0.0362(15) 0.0239(13) 0.0331(14) 0.0050(11) 0.0041(12) 0.0020(11) O1 0.057(5) 0.025(4) 0.054(5) 0.006(4) -0.006(4) -0.013(4) O2 0.032(4) 0.044(5) 0.051(5) 0.017(4) 0.003(4) 0.010(4) O3 0.036(4) 0.032(4) 0.048(5) 0.001(3) 0.002(4) 0.011(3) O4 0.056(5) 0.030(4) 0.045(4) -0.001(3) 0.022(4) -0.005(4) O5 0.060(6) 0.046(5) 0.052(5) 0.036(4) 0.006(5) 0.011(4) O6 0.040(5) 0.043(5) 0.050(5) -0.006(4) 0.002(4) -0.014(4) N1 0.030(4) 0.017(4) 0.024(4) 0.000(5) 0.006(3) -0.013(5) N7 0.034(5) 0.024(4) 0.029(5) 0.001(3) 0.000(4) 0.000(4) N8 0.021(4) 0.020(4) 0.032(5) -0.001(3) 0.000(3) -0.006(3) N21 0.030(4) 0.014(4) 0.017(4) -0.002(4) -0.003(3) 0.006(5) N27 0.039(5) 0.023(4) 0.032(5) -0.003(4) 0.005(4) 0.006(4) N28 0.031(4) 0.010(3) 0.028(5) 0.002(3) 0.005(3) 0.004(3) C2 0.034(6) 0.018(5) 0.031(6) -0.004(4) 0.004(5) 0.002(4) C3 0.037(6) 0.017(5) 0.045(7) -0.003(5) 0.005(5) 0.004(5) C4 0.041(7) 0.037(8) 0.029(5) -0.001(4) 0.003(5) -0.007(5) C5 0.019(5) 0.029(6) 0.039(6) -0.003(5) -0.005(5) -0.001(4) C6 0.031(5) 0.015(5) 0.037(6) 0.005(4) -0.003(5) 0.000(4) C9 0.025(5) 0.012(4) 0.042(6) 0.002(4) 0.000(4) 0.004(4) C10 0.036(7) 0.015(5) 0.049(7) -0.001(5) -0.002(5) 0.001(4) C11 0.038(7) 0.036(7) 0.051(7) 0.003(5) -0.008(6) 0.008(5) C12 0.051(7) 0.024(7) 0.049(6) 0.016(5) -0.002(6) 0.014(5) C13 0.057(7) 0.020(5) 0.053(6) 0.017(6) 0.007(5) 0.004(7) C14 0.045(6) 0.017(4) 0.044(6) -0.007(5) -0.011(7) -0.003(4) C22 0.032(6) 0.014(4) 0.039(6) 0.002(4) 0.002(5) 0.000(4) C23 0.034(6) 0.013(4) 0.044(6) -0.004(4) 0.006(5) -0.003(5) C24 0.042(7) 0.029(6) 0.030(6) -0.004(5) -0.006(5) 0.013(5) C25 0.028(5) 0.019(5) 0.033(5) -0.004(5) -0.001(4) 0.008(5) C26 0.022(5) 0.020(5) 0.037(6) 0.004(4) 0.001(4) 0.001(4) C29 0.036(6) 0.017(4) 0.040(6) -0.010(4) 0.006(5) -0.012(4) C30 0.035(6) 0.030(6) 0.034(6) -0.001(5) 0.008(5) -0.004(5) C31 0.065(9) 0.031(6) 0.042(7) -0.001(5) 0.005(6) -0.015(6) C32 0.043(7) 0.041(6) 0.050(7) -0.004(6) 0.009(6) -0.017(6) C33 0.026(6) 0.056(7) 0.062(8) -0.011(6) 0.011(6) -0.006(6) C34 0.025(6) 0.034(5) 0.070(8) 0.007(5) 0.009(5) -0.004(5) N60 0.030(5) 0.015(4) 0.041(5) 0.000(3) -0.004(4) -0.002(4) C61 0.044(6) 0.020(5) 0.031(6) 0.002(4) 0.000(5) 0.001(5) C62 0.056(7) 0.023(6) 0.038(6) 0.004(4) -0.006(6) 0.004(5) C63 0.024(5) 0.028(5) 0.054(7) 0.001(5) -0.008(5) 0.000(5) C64 0.045(8) 0.056(8) 0.063(8) 0.008(7) 0.011(7) 0.003(6) C65 0.064(8) 0.022(5) 0.036(6) -0.006(5) -0.002(6) 0.001(5) C66 0.047(7) 0.041(7) 0.053(8) -0.004(6) 0.001(6) 0.002(6) C67 0.040(7) 0.016(5) 0.049(7) -0.007(4) -0.007(5) 0.003(4) C68 0.055(8) 0.025(6) 0.063(8) 0.001(6) -0.018(7) 0.005(5) N70 0.038(5) 0.020(4) 0.061(6) -0.003(5) 0.006(5) 0.005(4) C71 0.040(7) 0.029(7) 0.058(7) -0.012(5) 0.009(6) -0.002(4) C72 0.064(9) 0.035(6) 0.045(7) 0.005(6) -0.005(7) -0.004(6) C73 0.055(7) 0.022(5) 0.038(6) -0.004(5) -0.001(6) -0.001(5) C74 0.049(8) 0.034(7) 0.080(10) -0.006(7) -0.003(7) 0.000(6) C75 0.063(8) 0.032(8) 0.071(8) 0.009(6) -0.001(7) 0.013(7) C76 0.115(12) 0.048(7) 0.055(7) 0.016(9) -0.016(8) -0.004(12) C77 0.046(8) 0.037(6) 0.060(8) -0.013(6) 0.015(7) -0.001(6) C78 0.059(10) 0.042(7) 0.067(9) -0.010(7) 0.018(8) -0.012(7) O40 0.081(7) 0.063(5) 0.081(6) -0.013(8) 0.002(5) -0.012(8) O50 0.034(5) 0.087(7) 0.078(7) 0.011(6) 0.003(5) 0.009(5) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 Cl1 2.410(2) . . yes Ru1 Cl2 2.393(2) . . yes Ru1 N1 2.032(7) . . yes Ru1 N8 2.011(7) . . yes Ru1 N21 2.057(7) . . yes Ru1 N28 1.981(7) . . yes S1 O1 1.447(8) . . yes S1 O2 1.430(8) . . yes S1 O3 1.432(8) . . yes S1 C5 1.790(10) . . yes S2 O4 1.433(8) . . yes S2 O5 1.450(10) . . yes S2 O6 1.465(9) . . yes S2 C25 1.765(10) . . yes O40 H40A 0.8209 . . no O40 H40B 0.8209 . . no O50 H50A 0.8186 . . no O50 H50B 0.8212 . . no N1 C2 1.388(14) . . yes N1 C6 1.357(13) . . yes N7 N8 1.287(10) . . yes N7 C2 1.382(13) . . yes N8 C9 1.423(11) . . yes N21 C26 1.334(13) . . yes N21 C22 1.368(14) . . yes N27 N28 1.287(12) . . yes N27 C22 1.391(14) . . yes N28 C29 1.419(13) . . yes N60 C63 1.516(14) . . yes N60 C61 1.531(13) . . yes N60 C67 1.533(11) . . yes N60 C65 1.510(12) . . yes N70 C77 1.487(16) . . yes N70 C75 1.514(16) . . yes N70 C71 1.515(15) . . yes N70 C73 1.543(14) . . yes C2 C3 1.375(16) . . no C3 C4 1.383(16) . . no C4 C5 1.404(15) . . no C5 C6 1.367(14) . . no C9 C10 1.405(15) . . no C9 C14 1.392(12) . . no C10 C11 1.371(16) . . no C11 C12 1.392(15) . . no C12 C13 1.384(16) . . no C13 C14 1.394(15) . . no C22 C23 1.369(14) . . no C23 C24 1.377(16) . . no C24 C25 1.396(15) . . no C25 C26 1.398(14) . . no C29 C34 1.401(15) . . no C29 C30 1.378(14) . . no C30 C31 1.379(17) . . no C31 C32 1.381(18) . . no C32 C33 1.358(17) . . no C33 C34 1.398(17) . . no C3 H3 0.9497 . . no C4 H4 0.9494 . . no C6 H6 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9502 . . no C12 H12 0.9497 . . no C13 H13 0.9502 . . no C14 H14 0.9512 . . no C23 H23 0.9506 . . no C24 H24 0.9503 . . no C26 H26 0.9503 . . no C30 H30 0.9505 . . no C31 H31 0.9507 . . no C32 H32 0.9494 . . no C33 H33 0.9504 . . no C34 H34 0.9515 . . no C61 C62 1.518(14) . . no C63 C64 1.477(16) . . no C65 C66 1.488(17) . . no C67 C68 1.537(17) . . no C61 H61B 0.9904 . . no C61 H61A 0.9888 . . no C62 H62C 0.9798 . . no C62 H62A 0.9811 . . no C62 H62B 0.9804 . . no C63 H63B 0.9887 . . no C63 H63A 0.9895 . . no C64 H64C 0.9806 . . no C64 H64B 0.9802 . . no C64 H64A 0.9793 . . no C65 H65A 0.9901 . . no C65 H65B 0.9905 . . no C66 H66B 0.9793 . . no C66 H66C 0.9799 . . no C66 H66A 0.9788 . . no C67 H67B 0.9896 . . no C67 H67A 0.9909 . . no C68 H68B 0.9802 . . no C68 H68C 0.9803 . . no C68 H68A 0.9800 . . no C71 C72 1.510(17) . . no C73 C74 1.496(17) . . no C75 C76 1.502(17) . . no C77 C78 1.538(18) . . no C71 H71A 0.9901 . . no C71 H71B 0.9902 . . no C72 H72B 0.9789 . . no C72 H72C 0.9801 . . no C72 H72A 0.9806 . . no C73 H73A 0.9890 . . no C73 H73B 0.9913 . . no C74 H74C 0.9813 . . no C74 H74A 0.9799 . . no C74 H74B 0.9799 . . no C75 H75B 0.9896 . . no C75 H75A 0.9894 . . no C76 H76A 0.9801 . . no C76 H76B 0.9798 . . no C76 H76C 0.9797 . . no C77 H77A 0.9904 . . no C77 H77B 0.9903 . . no C78 H78B 0.9800 . . no C78 H78C 0.9794 . . no C78 H78A 0.9801 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ru1 Cl2 90.93(9) . . . yes Cl1 Ru1 N1 89.2(3) . . . yes Cl1 Ru1 N8 88.0(2) . . . yes Cl1 Ru1 N21 94.0(3) . . . yes Cl1 Ru1 N28 171.0(2) . . . yes Cl2 Ru1 N1 95.3(3) . . . yes Cl2 Ru1 N8 172.5(2) . . . yes Cl2 Ru1 N21 84.4(3) . . . yes Cl2 Ru1 N28 88.3(2) . . . yes N1 Ru1 N8 77.3(3) . . . yes N1 Ru1 N21 176.8(3) . . . yes N1 Ru1 N28 99.8(3) . . . yes N8 Ru1 N21 103.1(3) . . . yes N8 Ru1 N28 94.0(3) . . . yes N21 Ru1 N28 77.0(3) . . . yes O1 S1 O2 113.8(5) . . . yes O1 S1 O3 112.7(4) . . . yes O1 S1 C5 104.7(5) . . . yes O2 S1 O3 113.5(5) . . . yes O2 S1 C5 105.4(5) . . . yes O3 S1 C5 105.7(4) . . . yes O4 S2 O5 112.7(5) . . . yes O4 S2 O6 114.7(5) . . . yes O4 S2 C25 105.6(5) . . . yes O5 S2 O6 113.6(5) . . . yes O5 S2 C25 103.8(5) . . . yes O6 S2 C25 105.2(5) . . . yes H40A O40 H40B 99.09 . . . no H50A O50 H50B 100.73 . . . no C2 N1 C6 115.9(8) . . . yes Ru1 N1 C2 113.1(6) . . . yes Ru1 N1 C6 131.0(7) . . . yes N8 N7 C2 114.3(8) . . . yes Ru1 N8 N7 119.0(6) . . . yes Ru1 N8 C9 127.7(6) . . . yes N7 N8 C9 112.9(7) . . . yes Ru1 N21 C22 111.6(6) . . . yes C22 N21 C26 119.2(8) . . . yes Ru1 N21 C26 128.6(7) . . . yes N28 N27 C22 112.9(8) . . . yes Ru1 N28 N27 120.2(6) . . . yes Ru1 N28 C29 125.5(6) . . . yes N27 N28 C29 114.2(8) . . . yes C63 N60 C67 110.1(7) . . . yes C61 N60 C63 111.1(7) . . . yes C61 N60 C65 110.6(8) . . . yes C61 N60 C67 105.8(7) . . . yes C63 N60 C65 107.5(8) . . . yes C65 N60 C67 111.7(7) . . . yes C75 N70 C77 112.7(9) . . . yes C71 N70 C75 107.3(8) . . . yes C71 N70 C77 109.9(9) . . . yes C71 N70 C73 110.7(8) . . . yes C73 N70 C77 106.3(9) . . . yes C73 N70 C75 110.1(9) . . . yes N7 C2 C3 120.5(9) . . . yes N1 C2 C3 123.4(9) . . . yes N1 C2 N7 116.1(8) . . . yes C2 C3 C4 118.9(10) . . . no C3 C4 C5 118.8(11) . . . no C4 C5 C6 119.3(10) . . . no S1 C5 C4 119.8(8) . . . yes S1 C5 C6 120.9(8) . . . yes N1 C6 C5 123.7(9) . . . yes C10 C9 C14 121.7(9) . . . no N8 C9 C10 120.2(8) . . . yes N8 C9 C14 118.0(9) . . . yes C9 C10 C11 118.6(9) . . . no C10 C11 C12 121.2(11) . . . no C11 C12 C13 119.3(11) . . . no C12 C13 C14 121.3(11) . . . no C9 C14 C13 117.7(10) . . . no N27 C22 C23 120.4(9) . . . yes N21 C22 C23 122.7(9) . . . yes N21 C22 N27 116.9(9) . . . yes C22 C23 C24 118.2(10) . . . no C23 C24 C25 120.0(10) . . . no S2 C25 C24 119.9(8) . . . yes S2 C25 C26 121.3(8) . . . yes C24 C25 C26 118.8(10) . . . no N21 C26 C25 121.0(9) . . . yes N28 C29 C34 118.3(9) . . . yes C30 C29 C34 121.7(10) . . . no N28 C29 C30 120.0(10) . . . yes C29 C30 C31 118.2(11) . . . no C30 C31 C32 121.1(11) . . . no C31 C32 C33 120.4(11) . . . no C32 C33 C34 120.5(11) . . . no C29 C34 C33 117.9(10) . . . no C2 C3 H3 120.48 . . . no C4 C3 H3 120.60 . . . no C3 C4 H4 120.61 . . . no C5 C4 H4 120.62 . . . no C5 C6 H6 118.15 . . . no N1 C6 H6 118.17 . . . no C11 C10 H10 120.80 . . . no C9 C10 H10 120.64 . . . no C10 C11 H11 119.39 . . . no C12 C11 H11 119.42 . . . no C13 C12 H12 120.35 . . . no C11 C12 H12 120.31 . . . no C12 C13 H13 119.23 . . . no C14 C13 H13 119.48 . . . no C9 C14 H14 121.12 . . . no C13 C14 H14 121.14 . . . no C24 C23 H23 120.85 . . . no C22 C23 H23 120.97 . . . no C25 C24 H24 119.94 . . . no C23 C24 H24 120.04 . . . no C25 C26 H26 119.50 . . . no N21 C26 H26 119.52 . . . no C29 C30 H30 120.80 . . . no C31 C30 H30 120.98 . . . no C32 C31 H31 119.40 . . . no C30 C31 H31 119.47 . . . no C33 C32 H32 119.85 . . . no C31 C32 H32 119.76 . . . no C32 C33 H33 119.65 . . . no C34 C33 H33 119.82 . . . no C33 C34 H34 121.09 . . . no C29 C34 H34 120.96 . . . no N60 C61 C62 115.4(9) . . . yes N60 C63 C64 115.3(9) . . . yes N60 C65 C66 116.8(9) . . . yes N60 C67 C68 114.3(9) . . . yes N60 C61 H61A 108.42 . . . no N60 C61 H61B 108.50 . . . no C62 C61 H61A 108.49 . . . no C62 C61 H61B 108.39 . . . no H61A C61 H61B 107.43 . . . no H62A C62 H62B 109.43 . . . no C61 C62 H62C 109.52 . . . no C61 C62 H62A 109.50 . . . no H62A C62 H62C 109.49 . . . no H62B C62 H62C 109.44 . . . no C61 C62 H62B 109.44 . . . no N60 C63 H63B 108.57 . . . no C64 C63 H63A 108.28 . . . no N60 C63 H63A 108.55 . . . no C64 C63 H63B 108.35 . . . no H63A C63 H63B 107.55 . . . no H64A C64 H64B 109.51 . . . no C63 C64 H64A 109.49 . . . no C63 C64 H64B 109.48 . . . no C63 C64 H64C 109.34 . . . no H64A C64 H64C 109.48 . . . no H64B C64 H64C 109.52 . . . no N60 C65 H65B 108.07 . . . no C66 C65 H65A 108.04 . . . no C66 C65 H65B 108.09 . . . no H65A C65 H65B 107.36 . . . no N60 C65 H65A 108.12 . . . no C65 C66 H66A 109.44 . . . no C65 C66 H66B 109.48 . . . no C65 C66 H66C 109.48 . . . no H66A C66 H66B 109.53 . . . no H66A C66 H66C 109.45 . . . no H66B C66 H66C 109.45 . . . no N60 C67 H67A 108.62 . . . no N60 C67 H67B 108.74 . . . no C68 C67 H67A 108.67 . . . no H67A C67 H67B 107.61 . . . no C68 C67 H67B 108.74 . . . no H68B C68 H68C 109.54 . . . no C67 C68 H68C 109.49 . . . no H68A C68 H68B 109.42 . . . no C67 C68 H68B 109.48 . . . no C67 C68 H68A 109.44 . . . no H68A C68 H68C 109.46 . . . no N70 C71 C72 116.8(9) . . . yes N70 C73 C74 114.7(9) . . . yes N70 C75 C76 117.5(11) . . . yes N70 C77 C78 115.3(10) . . . yes N70 C71 H71B 107.98 . . . no C72 C71 H71A 108.17 . . . no H71A C71 H71B 107.32 . . . no C72 C71 H71B 108.20 . . . no N70 C71 H71A 108.06 . . . no C71 C72 H72A 109.42 . . . no H72A C72 H72B 109.37 . . . no H72A C72 H72C 109.41 . . . no H72B C72 H72C 109.56 . . . no C71 C72 H72C 109.50 . . . no C71 C72 H72B 109.57 . . . no N70 C73 H73B 108.55 . . . no N70 C73 H73A 108.64 . . . no H73A C73 H73B 107.59 . . . no C74 C73 H73B 108.58 . . . no C74 C73 H73A 108.61 . . . no C73 C74 H74B 109.47 . . . no C73 C74 H74C 109.45 . . . no H74A C74 H74C 109.44 . . . no H74B C74 H74C 109.53 . . . no H74A C74 H74B 109.52 . . . no C73 C74 H74A 109.42 . . . no C76 C75 H75A 107.79 . . . no C76 C75 H75B 107.82 . . . no H75A C75 H75B 107.26 . . . no N70 C75 H75B 108.01 . . . no N70 C75 H75A 108.06 . . . no C75 C76 H76B 109.39 . . . no C75 C76 H76A 109.44 . . . no H76A C76 H76C 109.49 . . . no H76B C76 H76C 109.47 . . . no C75 C76 H76C 109.45 . . . no H76A C76 H76B 109.58 . . . no N70 C77 H77A 108.44 . . . no C78 C77 H77B 108.51 . . . no N70 C77 H77B 108.42 . . . no C78 C77 H77A 108.46 . . . no H77A C77 H77B 107.47 . . . no C77 C78 H78B 109.44 . . . no C77 C78 H78C 109.49 . . . no H78A C78 H78C 109.51 . . . no H78B C78 H78C 109.50 . . . no H78A C78 H78B 109.44 . . . no C77 C78 H78A 109.44 . . . no 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 Cl1 Ru1 N1 C2 90.6(7) . . . . no Cl1 Ru1 N1 C6 -89.9(9) . . . . no Cl2 Ru1 N1 C2 -178.5(7) . . . . no Cl2 Ru1 N1 C6 0.9(10) . . . . no N8 Ru1 N1 C2 2.5(7) . . . . no N8 Ru1 N1 C6 -178.0(10) . . . . no N28 Ru1 N1 C2 -89.4(7) . . . . no N28 Ru1 N1 C6 90.1(10) . . . . no Cl1 Ru1 N8 N7 -89.2(7) . . . . no Cl1 Ru1 N8 C9 83.2(7) . . . . no N1 Ru1 N8 N7 0.4(7) . . . . no N1 Ru1 N8 C9 172.8(8) . . . . no N21 Ru1 N8 N7 177.2(7) . . . . no N21 Ru1 N8 C9 -10.4(8) . . . . no N28 Ru1 N8 N7 99.6(7) . . . . no N28 Ru1 N8 C9 -88.0(7) . . . . no Cl1 Ru1 N21 C22 170.4(7) . . . . no Cl1 Ru1 N21 C26 -1.3(9) . . . . no Cl2 Ru1 N21 C22 79.9(7) . . . . no Cl2 Ru1 N21 C26 -91.8(9) . . . . no N8 Ru1 N21 C22 -100.8(7) . . . . no N8 Ru1 N21 C26 87.5(9) . . . . no N28 Ru1 N21 C22 -9.7(7) . . . . no N28 Ru1 N21 C26 178.6(10) . . . . no Cl2 Ru1 N28 N27 -77.4(7) . . . . no Cl2 Ru1 N28 C29 106.4(7) . . . . no N1 Ru1 N28 N27 -172.5(7) . . . . no N1 Ru1 N28 C29 11.4(8) . . . . no N8 Ru1 N28 N27 109.8(7) . . . . no N8 Ru1 N28 C29 -66.4(7) . . . . no N21 Ru1 N28 N27 7.2(7) . . . . no N21 Ru1 N28 C29 -168.9(8) . . . . no O1 S1 C5 C4 105.2(9) . . . . no O1 S1 C5 C6 -71.7(10) . . . . no O2 S1 C5 C4 -134.4(9) . . . . no O2 S1 C5 C6 48.7(10) . . . . no O3 S1 C5 C4 -14.0(10) . . . . no O3 S1 C5 C6 169.1(9) . . . . no O4 S2 C25 C24 -49.3(10) . . . . no O4 S2 C25 C26 131.1(9) . . . . no O5 S2 C25 C24 69.4(10) . . . . no O5 S2 C25 C26 -110.2(9) . . . . no O6 S2 C25 C24 -171.0(9) . . . . no O6 S2 C25 C26 9.4(10) . . . . no Ru1 N1 C2 N7 -5.1(12) . . . . no Ru1 N1 C2 C3 177.4(9) . . . . no C6 N1 C2 N7 175.4(9) . . . . no C6 N1 C2 C3 -2.1(15) . . . . no Ru1 N1 C6 C5 -178.0(8) . . . . no C2 N1 C6 C5 1.5(15) . . . . no C2 N7 N8 Ru1 -3.3(11) . . . . no C2 N7 N8 C9 -176.8(8) . . . . no N8 N7 C2 N1 5.5(13) . . . . no N8 N7 C2 C3 -176.9(10) . . . . no Ru1 N8 C9 C10 53.2(12) . . . . no Ru1 N8 C9 C14 -130.5(8) . . . . no N7 N8 C9 C10 -134.0(10) . . . . no N7 N8 C9 C14 42.3(12) . . . . no Ru1 N21 C22 N27 11.7(11) . . . . no Ru1 N21 C22 C23 -168.9(8) . . . . no C26 N21 C22 N27 -175.8(9) . . . . no C26 N21 C22 C23 3.7(15) . . . . no Ru1 N21 C26 C25 167.3(8) . . . . no C22 N21 C26 C25 -3.9(15) . . . . no C22 N27 N28 Ru1 -3.0(11) . . . . no C22 N27 N28 C29 173.6(8) . . . . no N28 N27 C22 N21 -6.2(13) . . . . no N28 N27 C22 C23 174.4(9) . . . . no Ru1 N28 C29 C30 -59.4(11) . . . . no Ru1 N28 C29 C34 121.1(9) . . . . no N27 N28 C29 C30 124.2(10) . . . . no N27 N28 C29 C34 -55.2(11) . . . . no C65 N60 C67 C68 -58.8(12) . . . . no C67 N60 C63 C64 58.9(11) . . . . no C63 N60 C61 C62 -51.8(11) . . . . no C65 N60 C61 C62 67.5(11) . . . . no C61 N60 C65 C66 66.9(11) . . . . no C61 N60 C63 C64 -58.1(11) . . . . no C65 N60 C63 C64 -179.2(9) . . . . no C67 N60 C65 C66 -50.7(12) . . . . no C67 N60 C61 C62 -171.4(9) . . . . no C63 N60 C65 C66 -171.6(9) . . . . no C63 N60 C67 C68 60.6(11) . . . . no C61 N60 C67 C68 -179.2(9) . . . . no C71 N70 C75 C76 -178.7(11) . . . . no C77 N70 C73 C74 179.7(11) . . . . no C75 N70 C71 C72 -173.8(10) . . . . no C77 N70 C71 C72 63.4(12) . . . . no C71 N70 C73 C74 -61.0(13) . . . . no C73 N70 C75 C76 60.8(14) . . . . no C73 N70 C71 C72 -53.7(12) . . . . no C71 N70 C77 C78 68.2(13) . . . . no C73 N70 C77 C78 -171.9(11) . . . . no C75 N70 C77 C78 -51.3(15) . . . . no C77 N70 C75 C76 -57.6(15) . . . . no C75 N70 C73 C74 57.4(13) . . . . no N1 C2 C3 C4 0.5(17) . . . . no N7 C2 C3 C4 -176.9(10) . . . . no C2 C3 C4 C5 1.9(16) . . . . no C3 C4 C5 C6 -2.5(16) . . . . no C3 C4 C5 S1 -179.5(8) . . . . no S1 C5 C6 N1 177.8(8) . . . . no C4 C5 C6 N1 0.8(16) . . . . no N8 C9 C14 C13 -179.6(9) . . . . no C10 C9 C14 C13 -3.3(16) . . . . no C14 C9 C10 C11 0.6(16) . . . . no N8 C9 C10 C11 176.8(10) . . . . no C9 C10 C11 C12 0.7(17) . . . . no C10 C11 C12 C13 0.8(18) . . . . no C11 C12 C13 C14 -3.6(17) . . . . no C12 C13 C14 C9 4.8(16) . . . . no N27 C22 C23 C24 178.3(9) . . . . no N21 C22 C23 C24 -1.2(15) . . . . no C22 C23 C24 C25 -1.1(16) . . . . no C23 C24 C25 C26 0.9(16) . . . . no C23 C24 C25 S2 -178.7(8) . . . . no S2 C25 C26 N21 -178.7(8) . . . . no C24 C25 C26 N21 1.6(16) . . . . no C30 C29 C34 C33 1.2(16) . . . . no N28 C29 C30 C31 179.4(9) . . . . no C34 C29 C30 C31 -1.2(15) . . . . no N28 C29 C34 C33 -179.4(9) . . . . no C29 C30 C31 C32 -0.6(17) . . . . no C30 C31 C32 C33 2.6(18) . . . . no C31 C32 C33 C34 -2.6(18) . . . . no C32 C33 C34 C29 0.8(17) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ru1 H10 3.3311 . . no Ru1 H30 3.3469 . . no Cl1 O50 3.357(10) . 1_655 no Cl2 C62 3.605(11) . 1_545 no Cl1 H26 2.7740 . . no Cl1 H61A 2.7147 . . no Cl1 H67A 2.9267 . . no Cl1 H50B 2.5361 . 1_655 no Cl2 H6 2.8463 . . no Cl2 H33 3.0646 . 1_655 no Cl2 H62A 2.9528 . 1_545 no Cl2 H73B 3.0091 . 1_545 no S1 H3 3.1374 . 2_646 no S2 H78C 3.1787 . . no S2 H71A 3.0911 . 2_745 no S2 H74B 3.0768 . 2_745 no O1 O40 2.841(13) . 1_545 no O1 C4 3.128(14) . 2_646 no O1 C3 3.320(14) . 2_646 no O2 C32 3.235(14) . 1_655 no O3 C3 3.372(13) . 2_646 no O3 O40 2.963(13) . 2_646 no O4 C72 3.389(13) . 1_545 no O5 C23 2.934(13) . 2_655 no O5 C24 3.115(14) . 2_655 no O6 O50 2.867(12) . 1_655 no O40 C61 3.334(15) . . no O40 C62 3.351(16) . . no O40 O1 2.841(13) . 1_565 no O40 O3 2.963(13) . 2_656 no O50 O6 2.867(12) . 1_455 no O50 C11 3.413(15) . . no O50 Cl1 3.357(10) . 1_455 no O50 C10 3.312(14) . . no O1 H3 2.8278 . 2_646 no O1 H62C 2.8732 . 1_545 no O1 H40A 2.0202 . 1_545 no O1 H4 2.4219 . 2_646 no O2 H32 2.3060 . 1_655 no O2 H62C 2.6885 . 1_545 no O2 H68A 2.7904 . . no O2 H65B 2.7758 . 1_545 no O2 H68B 2.6871 . 2_746 no O2 H65A 2.6690 . 2_746 no O2 H6 2.8005 . . no O3 H63B 2.4951 . 2_746 no O3 H3 2.4416 . 2_646 no O3 H4 2.5277 . . no O3 H40B 2.1420 . 2_646 no O3 H65A 2.8972 . 2_746 no O4 H71A 2.4889 . 2_745 no O4 H73A 2.6299 . 1_545 no O4 H72B 2.4607 . 1_545 no O4 H24 2.8206 . . no O5 H23 2.2765 . 2_655 no O5 H77A 2.8314 . 2_645 no O5 H78C 2.6127 . . no O5 H24 2.6390 . 2_655 no O6 H75A 2.6341 . . no O6 H71A 2.8383 . 2_745 no O6 H74B 2.8042 . 2_745 no O6 H26 2.5043 . . no O6 H50A 2.0488 . 1_655 no O40 H61B 2.5365 . . no O40 H66C 2.8184 . . no O40 H31 2.8131 . 1_565 no O50 H10 2.7722 . . no O50 H34 2.7552 . . no O50 H74A 2.7506 . 1_445 no O50 H72A 2.7520 . 2_645 no N1 C30 3.121(14) . . no N21 C10 3.266(14) . . no N1 H30 2.7973 . . no N7 H14 2.5238 . . no N21 H10 2.7968 . . no N27 H10 2.9195 . . no N27 H34 2.7087 . . no N27 H13 2.6903 . 1_545 no C3 O3 3.372(13) . 2_656 no C3 O1 3.320(14) . 2_656 no C4 O1 3.128(14) . 2_656 no C6 C30 3.300(15) . . no C10 O50 3.312(14) . . no C10 N21 3.266(14) . . no C11 C78 3.589(18) . . no C11 O50 3.413(15) . . no C12 C78 3.412(19) . . no C13 C78 3.600(18) . . no C23 O5 2.934(13) . 2_645 no C24 O5 3.115(14) . 2_645 no C24 C72 3.597(17) . 2_645 no C30 C6 3.300(15) . . no C30 N1 3.121(14) . . no C32 O2 3.235(14) . 1_455 no C61 O40 3.334(15) . . no C62 C64 3.486(18) . . no C62 O40 3.351(16) . . no C62 Cl2 3.605(11) . 1_565 no C64 C62 3.486(18) . . no C66 C68 3.512(17) . . no C68 C66 3.512(17) . . no C72 C74 3.581(19) . . no C72 C24 3.597(17) . 2_655 no C72 O4 3.389(13) . 1_565 no C74 C72 3.581(19) . . no C76 C78 3.53(2) . . no C78 C11 3.589(18) . . no C78 C12 3.412(19) . . no C78 C13 3.600(18) . . no C78 C76 3.53(2) . . no C3 H67B 3.0253 . . no C4 H67B 2.9072 . . no C5 H67B 2.9323 . . no C6 H30 2.6975 . . no C9 H64A 2.9531 . 1_455 no C11 H78A 2.6968 . . no C11 H75B 3.0299 . 1_455 no C12 H78A 2.5492 . . no C12 H75B 3.0262 . 1_455 no C13 H78A 3.0121 . . no C14 H64A 2.8885 . 1_455 no C22 H10 2.8479 . . no C24 H73A 3.0136 . 1_545 no C24 H72C 2.8758 . 2_645 no C25 H73A 2.8414 . 1_545 no C31 H63A 3.0670 . 1_445 no C32 H68A 3.0440 . 1_455 no C32 H63A 3.0875 . 1_445 no C61 H64B 2.6673 . . no C61 H66C 2.8069 . . no C62 H65B 2.7336 . . no C62 H63A 2.6623 . . no C62 H64B 2.9713 . . no C63 H68C 2.7285 . . no C63 H62B 2.6580 . . no C64 H67A 2.6632 . . no C64 H62B 2.9539 . . no C64 H61A 2.7659 . . no C65 H62C 2.8193 . . no C65 H68B 2.7132 . . no C66 H68B 3.0049 . . no C66 H67B 2.6835 . . no C66 H61B 2.7456 . . no C67 H64C 2.6754 . . no C67 H66B 2.6713 . . no C68 H65A 2.7901 . . no C68 H66B 2.9756 . . no C68 H63B 2.6944 . . no C68 H66A 3.0789 . 2_746 no C71 H78C 2.7686 . . no C71 H74B 2.6954 . . no C72 H74B 3.0959 . . no C72 H73A 2.6769 . . no C72 H77A 2.6544 . . no C73 H76C 2.7438 . . no C73 H72B 2.6648 . . no C74 H71A 2.7661 . . no C74 H75B 2.6436 . . no C74 H72B 3.0768 . . no C75 H78B 2.6964 . . no C75 H74C 2.6941 . . no C76 H73B 2.7720 . . no C76 H77B 2.8322 . . no C76 H78B 2.9875 . . no C77 H72C 2.7906 . . no C77 H76B 2.7936 . . no C78 H75A 2.6645 . . no C78 H76B 3.0320 . . no C78 H71B 2.7203 . . no C78 H24 2.9695 . 2_655 no H3 O1 2.8278 . 2_656 no H3 H40B 2.5409 . . no H3 O3 2.4416 . 2_656 no H3 S1 3.1374 . 2_656 no H4 H40B 2.5750 . 2_646 no H4 H40A 2.5542 . 2_646 no H4 O1 2.4219 . 2_656 no H4 O3 2.5277 . . no H6 Cl2 2.8463 . . no H6 O2 2.8005 . . no H10 Ru1 3.3311 . . no H10 C22 2.8479 . . no H10 N21 2.7968 . . no H10 N27 2.9195 . . no H10 O50 2.7722 . . no H11 H75B 2.5365 . 1_455 no H12 H75B 2.5332 . 1_455 no H12 H74C 2.4691 . 1_455 no H13 N27 2.6903 . 1_565 no H14 H62A 2.5795 . . no H14 N7 2.5238 . . no H23 O5 2.2765 . 2_645 no H24 O4 2.8206 . . no H24 H78C 2.2813 . 2_645 no H24 O5 2.6390 . 2_645 no H24 C78 2.9695 . 2_645 no H26 H78B 2.5317 . . no H26 O6 2.5043 . . no H26 H50B 2.5731 . 1_655 no H26 Cl1 2.7740 . . no H26 H50A 2.5635 . 1_655 no H30 C6 2.6975 . . no H30 Ru1 3.3469 . . no H30 N1 2.7973 . . no H31 O40 2.8131 . 1_545 no H32 O2 2.3060 . 1_455 no H33 Cl2 3.0646 . 1_455 no H34 N27 2.7087 . . no H34 O50 2.7552 . . no H40A H4 2.5542 . 2_656 no H40A O1 2.0202 . 1_565 no H40A H66C 2.5716 . . no H40B O3 2.1420 . 2_656 no H40B H4 2.5750 . 2_656 no H40B H3 2.5409 . . no H50A O6 2.0488 . 1_455 no H50A H26 2.5635 . 1_455 no H50A H72A 2.5941 . 2_645 no H50B Cl1 2.5361 . 1_455 no H50B H26 2.5731 . 1_455 no H61A H64B 2.2379 . . no H61A Cl1 2.7147 . . no H61A C64 2.7659 . . no H61A H67A 2.2936 . . no H61B H66C 2.1857 . . no H61B H67B 2.4263 . . no H61B C66 2.7456 . . no H61B O40 2.5365 . . no H62A Cl2 2.9528 . 1_565 no H62A H14 2.5795 . . no H62B C63 2.6580 . . no H62B H63A 2.1753 . . no H62B H64B 2.4174 . . no H62B C64 2.9539 . . no H62C O1 2.8732 . 1_565 no H62C H65B 2.1849 . . no H62C O2 2.6885 . 1_565 no H62C C65 2.8193 . . no H63A C31 3.0670 . 1_665 no H63A H65B 2.4247 . . no H63A C32 3.0875 . 1_665 no H63A C62 2.6623 . . no H63A H62B 2.1753 . . no H63B H68C 2.1808 . . no H63B O3 2.4951 . 2_756 no H63B H65A 2.2995 . . no H63B C68 2.6944 . . no H64A C9 2.9531 . 1_655 no H64A C14 2.8885 . 1_655 no H64B H62B 2.4174 . . no H64B C62 2.9713 . . no H64B H76A 2.4029 . . no H64B H61A 2.2379 . . no H64B C61 2.6673 . . no H64C C67 2.6754 . . no H64C H67A 2.1340 . . no H65A O2 2.6690 . 2_756 no H65A O3 2.8972 . 2_756 no H65A H68B 2.2742 . . no H65A C68 2.7901 . . no H65A H63B 2.2995 . . no H65B H62C 2.1849 . . no H65B O2 2.7758 . 1_565 no H65B C62 2.7336 . . no H65B H63A 2.4247 . . no H66A C68 3.0789 . 2_756 no H66B H68B 2.4382 . . no H66B C67 2.6713 . . no H66B H67B 2.2134 . . no H66B C68 2.9756 . . no H66C O40 2.8184 . . no H66C H40A 2.5716 . . no H66C H61B 2.1857 . . no H66C C61 2.8069 . . no H67A H61A 2.2936 . . no H67A C64 2.6632 . . no H67A H64C 2.1340 . . no H67A Cl1 2.9267 . . no H67B H61B 2.4263 . . no H67B H66B 2.2134 . . no H67B C3 3.0253 . . no H67B C66 2.6835 . . no H67B C5 2.9323 . . no H67B C4 2.9072 . . no H68A O2 2.7904 . . no H68A C32 3.0440 . 1_655 no H68B H66B 2.4382 . . no H68B O2 2.6871 . 2_756 no H68B H65A 2.2742 . . no H68B C65 2.7132 . . no H68B C66 3.0049 . . no H68C H63B 2.1808 . . no H68C C63 2.7285 . . no H71A H75B 2.3032 . . no H71A C74 2.7661 . . no H71A H74B 2.2091 . . no H71A O6 2.8383 . 2_755 no H71A S2 3.0911 . 2_755 no H71A O4 2.4889 . 2_755 no H71B H78C 2.1440 . . no H71B H75A 2.3822 . . no H71B C78 2.7203 . . no H72A H50A 2.5941 . 2_655 no H72A O50 2.7520 . 2_655 no H72B O4 2.4607 . 1_565 no H72B C74 3.0768 . . no H72B H73A 2.1338 . . no H72B C73 2.6648 . . no H72C C77 2.7906 . . no H72C C24 2.8758 . 2_655 no H72C H77A 2.1520 . . no H73A O4 2.6299 . 1_565 no H73A C72 2.6769 . . no H73A H72B 2.1338 . . no H73A H77A 2.4137 . . no H73A C24 3.0136 . 1_565 no H73A C25 2.8414 . 1_565 no H73B H76C 2.2250 . . no H73B Cl2 3.0091 . 1_565 no H73B C76 2.7720 . . no H73B H77B 2.2708 . . no H74A O50 2.7506 . 1_665 no H74B C71 2.6954 . . no H74B C72 3.0959 . . no H74B S2 3.0768 . 2_755 no H74B O6 2.8042 . 2_755 no H74B H71A 2.2091 . . no H74C H75B 2.1532 . . no H74C H12 2.4691 . 1_655 no H74C C75 2.6941 . . no H75A H78B 2.2413 . . no H75A H71B 2.3822 . . no H75A C78 2.6645 . . no H75A O6 2.6341 . . no H75B C12 3.0262 . 1_655 no H75B C74 2.6436 . . no H75B C11 3.0299 . 1_655 no H75B H71A 2.3032 . . no H75B H74C 2.1532 . . no H75B H11 2.5365 . 1_655 no H75B H12 2.5332 . 1_655 no H76A H64B 2.4029 . . no H76B C78 3.0320 . . no H76B C77 2.7936 . . no H76B H78B 2.4195 . . no H76B H77B 2.3966 . . no H76C C73 2.7438 . . no H76C H73B 2.2250 . . no H77A C72 2.6544 . . no H77A H72C 2.1520 . . no H77A H73A 2.4137 . . no H77A O5 2.8314 . 2_655 no H77B H76B 2.3966 . . no H77B C76 2.8322 . . no H77B H73B 2.2708 . . no H78A C11 2.6968 . . no H78A C12 2.5492 . . no H78A C13 3.0121 . . no H78B C75 2.6964 . . no H78B H76B 2.4195 . . no H78B H75A 2.2413 . . no H78B C76 2.9875 . . no H78B H26 2.5317 . . no H78C O5 2.6127 . . no H78C C71 2.7686 . . no H78C H71B 2.1440 . . no H78C H24 2.2813 . 2_655 no H78C S2 3.1787 . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O40 H40A O1 0.8200 2.0200 2.841(13) 180.00 1_565 yes O40 H40B O3 0.8200 2.1400 2.963(13) 179.00 2_656 yes O50 H50A O6 0.8200 2.0500 2.867(12) 179.00 1_455 yes O50 H50B Cl1 0.8200 2.5400 3.357(10) 180.00 1_455 yes C3 H3 O3 0.9500 2.4400 3.372(13) 166.00 2_656 yes C4 H4 O3 0.9500 2.5300 2.896(14) 103.00 . yes C4 H4 O1 0.9500 2.4200 3.128(14) 131.00 2_656 yes C23 H23 O5 0.9500 2.2800 2.934(13) 126.00 2_645 yes C26 H26 Cl1 0.9500 2.7700 3.347(10) 120.00 . yes C26 H26 O6 0.9500 2.5000 2.891(13) 104.00 . yes C32 H32 O2 0.9500 2.3100 3.235(14) 166.00 1_455 yes C61 H61A Cl1 0.9900 2.7100 3.672(10) 163.00 . yes C61 H61B O40 0.9900 2.5400 3.334(15) 137.00 . yes C63 H63B O3 0.9900 2.5000 3.426(13) 157.00 2_756 yes C71 H71A O4 0.9900 2.4900 3.451(14) 164.00 2_755 yes C72 H72B O4 0.9800 2.4600 3.389(13) 158.00 1_565 yes #===END