# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1474 data_Severin _audit_creation_date 2-11-98 _audit_creation_method SHELXL _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author ; Kay Severin Institut f\"ur Anorganische Chemie Universit\"at M\"unchen Butenandtstr. 5 - 13 81377 M\"unchen Bundesrepublik Deutschland ; _publ_contact_author_email 'kse@cup.uni-muenchen.de' _publ_contact_author_fax '049 89 2180-7866' _publ_contact_author_phone '049 89 2180-7768' _publ_requested_journal 'Inorg. Chem.' _publ_requested_coeditor_name ? _publ_contact_letter ; ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; A Facile Method for the Synthesis of Heterobimetallic Chloro-bridged Complexes containing (R3P)2MCl (M = Pt, Pd) Fragments. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Polborn, Kurt' ; Institut f\"ur Organische Chemie Universit\"at M\"unchen Butenandtr. 5 - 13 81377 M\"unchen Bundesrepublik Deutschland ; 'Severin, Kay' ; Institut f\"ur Anorganische Chemie Universit\"at M\"unchen Butenandtstr. 5 - 13 81377 M\"unchen Bundesrepublik Deutschland ; # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. Enraf-Nonius, CAD4 Operations Manual, Delft, 1977. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, Enraf - Nonius, Delft, The Netherlands. SHELXS-86, G. M. Sheldrick, University of G\"ottigen, Germany, 1986. SHELXL-93, G. M. Sheldrick, University of G\"ottigen, Germany, 1993. International Tables for X-Ray Crystallography, Vol. IV, The Kynoch Press, Birmingham, England, 1974 Zsolnai, L. (1994). ZORTEP. University of Heidelberg. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H37 N2 O4 P S 0.5 C H4 O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32.50 H39 N2 O4.50 P Ru S' _chemical_formula_weight 693.76 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' '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' _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 10.387(2) _cell_length_b 11.762(5) _cell_length_c 14.362(2) _cell_angle_alpha 88.05(3) _cell_angle_beta 81.10(2) _cell_angle_gamma 73.33(3) _cell_volume 1660.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 16 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max .47 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method ? _exptl_crystal_F_000 718 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6402 _exptl_absorpt_correction_T_max 0.9990 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device Nonius_CAD4 _diffrn_measurement_method \o-2\T-scan _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 7200 _diffrn_standards_decay_% -1.3 _diffrn_reflns_number 5439 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 23.98 _reflns_number_total 5196 _reflns_number_observed 4742 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4(Nonius,_1977) _computing_cell_refinement CAD4(Nonius,_1977) _computing_data_reduction process_MOLEN(Fair,_1990) _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ZORTEP(Zsolnai,_1994) _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+2.4412P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5196 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_obs 0.0471 _refine_ls_wR_factor_all 0.1380 _refine_ls_wR_factor_obs 0.1233 _refine_ls_goodness_of_fit_all 1.136 _refine_ls_goodness_of_fit_obs 1.067 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 1.067 _refine_ls_shift/esd_max 0.107 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.47520(3) 0.52136(3) 0.22635(2) 0.03083(15) Uani 1 d . . S1 S 0.65153(13) 0.62837(10) 0.35863(8) 0.0436(3) Uani 1 d . . P1 P 0.71172(11) 0.28853(9) 0.11495(7) 0.0322(3) Uani 1 d . . O1 O 0.5346(4) 0.6384(3) 0.4310(2) 0.0523(8) Uani 1 d . . O2 O 0.7169(5) 0.7223(3) 0.3573(3) 0.0664(11) Uani 1 d . . O3 O 0.6582(3) 0.3763(2) 0.1967(2) 0.0350(6) Uani 1 d . . O4 O 0.6655(3) 0.3293(3) 0.0224(2) 0.0415(7) Uani 1 d . . N1 N 0.6105(4) 0.6136(3) 0.2586(3) 0.0383(8) Uani 1 d . . N2 N 0.5466(4) 0.5787(3) 0.0905(2) 0.0334(7) Uani 1 d . . H2A H 0.5931(4) 0.5147(3) 0.0544(2) 0.040 Uiso 1 calc R . H2B H 0.4747(4) 0.6183(3) 0.0630(2) 0.040 Uiso 1 calc R . C1 C 0.6715(4) 0.1506(4) 0.1490(3) 0.0373(9) Uani 1 d . . C2 C 0.5804(5) 0.1129(4) 0.1053(4) 0.0473(11) Uani 1 d . . H2 H 0.5440(5) 0.1550(4) 0.0549(4) 0.057 Uiso 1 calc R . C3 C 0.5435(6) 0.0118(5) 0.1373(4) 0.0577(13) Uani 1 d . . H3 H 0.4816(6) -0.0129(5) 0.1086(4) 0.069 Uiso 1 calc R . C4 C 0.5980(5) -0.0513(4) 0.2108(4) 0.0571(13) Uani 1 d . . H4 H 0.5715(5) -0.1177(4) 0.2329(4) 0.069 Uiso 1 calc R . C5 C 0.6916(5) -0.0168(4) 0.2518(4) 0.0541(12) Uani 1 d . . H5 H 0.7302(5) -0.0611(4) 0.3006(4) 0.065 Uiso 1 calc R . C6 C 0.7293(5) 0.0837(4) 0.2213(4) 0.0461(11) Uani 1 d . . H6 H 0.7933(5) 0.1063(4) 0.2492(4) 0.055 Uiso 1 calc R . C7 C 0.8963(4) 0.2452(4) 0.1017(3) 0.0378(9) Uani 1 d . . C8 C 0.9715(6) 0.1766(6) 0.0250(4) 0.0645(15) Uani 1 d . . H8 H 0.9272(6) 0.1550(6) -0.0200(4) 0.077 Uiso 1 calc R . C9 C 1.1131(6) 0.1393(7) 0.0144(5) 0.081(2) Uani 1 d . . H9 H 1.1634(6) 0.0947(7) -0.0382(5) 0.097 Uiso 1 calc R . C10 C 1.1764(6) 0.1687(6) 0.0816(6) 0.078(2) Uani 1 d . . H10 H 1.2708(6) 0.1432(6) 0.0750(6) 0.094 Uiso 1 calc R . C11 C 1.1049(6) 0.2349(6) 0.1586(5) 0.074(2) Uani 1 d . . H11 H 1.1504(6) 0.2537(6) 0.2042(5) 0.089 Uiso 1 calc R . C12 C 0.9630(5) 0.2745(5) 0.1690(4) 0.0568(13) Uani 1 d . . H12 H 0.9138(5) 0.3205(5) 0.2212(4) 0.068 Uiso 1 calc R . C13 C 0.7767(5) 0.4956(4) 0.3834(3) 0.0459(11) Uani 1 d . . C14 C 0.7385(5) 0.3930(4) 0.4034(3) 0.0488(11) Uani 1 d . . H14 H 0.6493(5) 0.3929(4) 0.4022(3) 0.059 Uiso 1 calc R . C15 C 0.8335(7) 0.2906(6) 0.4252(4) 0.068(2) Uani 1 d . . H15 H 0.8074(7) 0.2216(6) 0.4377(4) 0.082 Uiso 1 calc R . C16 C 0.9672(7) 0.2883(7) 0.4289(5) 0.082(2) Uani 1 d . . C17 C 1.0016(7) 0.3919(8) 0.4086(6) 0.091(2) Uani 1 d . . H17 H 1.0905(7) 0.3924(8) 0.4103(6) 0.109 Uiso 1 calc R . C18 C 0.9090(6) 0.4951(6) 0.3856(4) 0.070(2) Uani 1 d . . H18 H 0.9357(6) 0.5636(6) 0.3718(4) 0.084 Uiso 1 calc R . C19 C 1.0703(11) 0.1815(13) 0.4532(8) 0.147(5) Uani 0.64(4) d P 1 H19 H 1.1342(11) 0.2014(13) 0.4832(8) 0.177 Uiso 0.64(4) calc PR 1 C20 C 1.0914(29) 0.0931(20) 0.4466(21) 0.187(15) Uani 0.64(4) d P 1 H20A H 1.0354(29) 0.0608(20) 0.4177(21) 0.224 Uiso 0.64(4) calc PR 1 H20B H 1.1668(29) 0.0434(20) 0.4693(21) 0.224 Uiso 0.64(4) calc PR 1 C19A C 1.0703(11) 0.1815(13) 0.4532(8) 0.147(5) Uani 0.36(4) d P 2 H19A H 1.0567(11) 0.1195(13) 0.4212(8) 0.177 Uiso 0.36(4) calc PR 2 C20A C 1.1533(26) 0.1411(25) 0.4900(19) 0.095(11) Uani 0.36(4) d P 2 H20C H 1.1848(26) 0.1873(25) 0.5272(19) 0.114 Uiso 0.36(4) calc PR 2 H20D H 1.1942(26) 0.0597(25) 0.4848(19) 0.114 Uiso 0.36(4) calc PR 2 C21 C 0.7124(5) 0.6199(4) 0.1770(3) 0.0447(10) Uani 1 d . . H21A H 0.7792(5) 0.5432(4) 0.1646(3) 0.054 Uiso 1 calc R . H21B H 0.7588(5) 0.6777(4) 0.1885(3) 0.054 Uiso 1 calc R . C22 C 0.6357(5) 0.6567(4) 0.0950(3) 0.0480(11) Uani 1 d . . H22A H 0.5811(5) 0.7388(4) 0.1029(3) 0.058 Uiso 1 calc R . H22B H 0.6992(5) 0.6496(4) 0.0369(3) 0.058 Uiso 1 calc R . C23 C 0.2669(4) 0.6381(4) 0.2440(3) 0.0457(11) Uani 1 d . . C24 C 0.2796(4) 0.5380(5) 0.1861(3) 0.0472(11) Uani 1 d . . H24 H 0.2541(4) 0.5501(5) 0.1265(3) 0.057 Uiso 1 calc R . C25 C 0.3295(5) 0.4227(5) 0.2170(3) 0.0489(12) Uani 1 d . . H25 H 0.3369(5) 0.3594(5) 0.1775(3) 0.059 Uiso 1 calc R . C26 C 0.3694(5) 0.3992(4) 0.3076(3) 0.0457(11) Uani 1 d . . C27 C 0.3597(5) 0.4972(4) 0.3648(3) 0.0452(11) Uani 1 d . . H27 H 0.3858(5) 0.4846(4) 0.4243(3) 0.054 Uiso 1 calc R . C28 C 0.3102(4) 0.6160(4) 0.3324(3) 0.0420(10) Uani 1 d . . H28 H 0.3068(4) 0.6794(4) 0.3705(3) 0.050 Uiso 1 calc R . C29 C 0.2071(5) 0.7636(5) 0.2093(4) 0.0630(15) Uani 1 d . . H29 H 0.2284(5) 0.7632(5) 0.1404(4) 0.076 Uiso 1 calc R . C30 C 0.2621(9) 0.8544(6) 0.2477(7) 0.104(3) Uani 1 d . . H30A H 0.2308(47) 0.8644(37) 0.3142(10) 0.125 Uiso 1 calc R . H30B H 0.2310(49) 0.9287(15) 0.2168(29) 0.125 Uiso 1 calc R . H30C H 0.3597(9) 0.8280(25) 0.2367(36) 0.125 Uiso 1 calc R . C31 C 0.0519(6) 0.7971(7) 0.2366(6) 0.100(3) Uani 1 d . . H31A H 0.0117(8) 0.8729(23) 0.2106(33) 0.120 Uiso 1 calc R . H31B H 0.0289(7) 0.8011(47) 0.3040(6) 0.120 Uiso 1 calc R . H31C H 0.0179(9) 0.7381(26) 0.2124(33) 0.120 Uiso 1 calc R . C32 C 0.4267(6) 0.2754(5) 0.3405(4) 0.066(2) Uani 1 d . . H32A H 0.3828(29) 0.2668(11) 0.4032(11) 0.079 Uiso 1 calc R . H32B H 0.5226(10) 0.2601(12) 0.3406(26) 0.079 Uiso 1 calc R . H32C H 0.4115(35) 0.2200(5) 0.2989(16) 0.079 Uiso 1 calc R . O5 O 0.6184(14) 0.1211(12) 0.5089(12) 0.128(5) Uani 0.50 d P -1 H5A H 0.5673(36) 0.1879(29) 0.5215(159) 0.154 Uiso 0.50 calc PR -1 C33 C 0.5449(24) 0.0410(19) 0.5193(15) 0.137(8) Uani 0.50 d P -1 H33A H 0.5890(24) -0.0251(19) 0.4772(15) 0.164 Uiso 0.50 calc PR -1 H33B H 0.4552(24) 0.0782(19) 0.5048(15) 0.164 Uiso 0.50 calc PR -1 H33C H 0.5386(24) 0.0136(19) 0.5831(15) 0.164 Uiso 0.50 calc PR -1 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 0.0344(2) 0.0328(2) 0.0277(2) 0.00321(14) -0.00351(14) -0.01430(15) S1 0.0604(7) 0.0382(6) 0.0397(6) 0.0014(5) -0.0176(5) -0.0208(5) P1 0.0344(6) 0.0302(5) 0.0329(5) 0.0029(4) -0.0064(4) -0.0101(4) O1 0.059(2) 0.059(2) 0.037(2) -0.0060(15) -0.0082(15) -0.012(2) O2 0.104(3) 0.054(2) 0.062(2) 0.007(2) -0.036(2) -0.045(2) O3 0.040(2) 0.0358(15) 0.0293(14) 0.0032(12) -0.0052(12) -0.0107(12) O4 0.047(2) 0.041(2) 0.036(2) 0.0041(13) -0.0101(13) -0.0094(13) N1 0.048(2) 0.037(2) 0.036(2) 0.0046(15) -0.009(2) -0.021(2) N2 0.043(2) 0.030(2) 0.031(2) 0.0054(14) -0.0099(15) -0.0133(15) C1 0.037(2) 0.034(2) 0.041(2) 0.000(2) -0.004(2) -0.012(2) C2 0.053(3) 0.040(2) 0.055(3) 0.003(2) -0.018(2) -0.018(2) C3 0.061(3) 0.046(3) 0.077(4) -0.002(3) -0.019(3) -0.029(2) C4 0.057(3) 0.040(3) 0.077(4) 0.006(2) -0.005(3) -0.023(2) C5 0.058(3) 0.044(3) 0.059(3) 0.014(2) -0.013(2) -0.013(2) C6 0.046(3) 0.042(2) 0.054(3) 0.009(2) -0.014(2) -0.016(2) C7 0.029(2) 0.035(2) 0.046(2) 0.009(2) 0.000(2) -0.008(2) C8 0.046(3) 0.078(4) 0.061(3) -0.013(3) 0.001(2) -0.007(3) C9 0.047(3) 0.092(5) 0.083(5) -0.010(4) 0.010(3) 0.003(3) C10 0.036(3) 0.083(4) 0.112(6) 0.028(4) -0.003(3) -0.019(3) C11 0.042(3) 0.100(5) 0.086(4) -0.002(4) -0.014(3) -0.026(3) C12 0.051(3) 0.068(3) 0.059(3) 0.001(3) -0.010(2) -0.028(3) C13 0.052(3) 0.056(3) 0.037(2) 0.005(2) -0.013(2) -0.023(2) C14 0.049(3) 0.051(3) 0.043(3) 0.006(2) -0.006(2) -0.011(2) C15 0.077(4) 0.064(3) 0.048(3) 0.010(3) 0.004(3) -0.002(3) C16 0.072(4) 0.090(5) 0.059(4) 0.016(3) -0.003(3) 0.011(4) C17 0.046(3) 0.127(7) 0.094(5) 0.016(5) -0.026(3) -0.010(4) C18 0.057(3) 0.094(5) 0.071(4) 0.014(3) -0.018(3) -0.038(3) C19 0.107(7) 0.148(11) 0.120(8) 0.041(7) -0.010(6) 0.061(7) C20 0.177(23) 0.082(13) 0.265(31) 0.011(16) -0.082(21) 0.045(14) C19A 0.107(7) 0.148(11) 0.120(8) 0.041(7) -0.010(6) 0.061(7) C20A 0.090(17) 0.088(17) 0.109(19) 0.011(13) -0.052(13) -0.010(13) C21 0.052(3) 0.046(3) 0.045(3) 0.006(2) -0.009(2) -0.026(2) C22 0.065(3) 0.049(3) 0.039(2) 0.011(2) -0.010(2) -0.030(2) C23 0.030(2) 0.058(3) 0.041(2) 0.007(2) 0.003(2) -0.005(2) C24 0.033(2) 0.071(3) 0.042(3) 0.005(2) -0.004(2) -0.023(2) C25 0.046(3) 0.063(3) 0.048(3) -0.008(2) 0.002(2) -0.036(2) C26 0.044(3) 0.049(3) 0.045(3) 0.005(2) 0.008(2) -0.023(2) C27 0.045(3) 0.053(3) 0.033(2) 0.006(2) 0.003(2) -0.011(2) C28 0.041(2) 0.046(2) 0.037(2) -0.003(2) 0.001(2) -0.011(2) C29 0.046(3) 0.070(4) 0.057(3) 0.013(3) 0.001(2) 0.002(3) C30 0.117(6) 0.049(4) 0.140(8) 0.018(4) -0.030(6) -0.010(4) C31 0.049(4) 0.103(6) 0.119(6) 0.025(5) -0.001(4) 0.015(4) C32 0.073(4) 0.050(3) 0.070(4) 0.014(3) 0.016(3) -0.024(3) O5 0.119(10) 0.087(8) 0.151(12) 0.010(8) -0.010(9) 0.006(7) C33 0.151(21) 0.126(19) 0.109(16) 0.021(13) 0.023(14) -0.025(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.115(4) . ? Ru1 N2 2.135(3) . ? Ru1 C24 2.151(5) . ? Ru1 O3 2.155(3) . ? Ru1 C28 2.170(4) . ? Ru1 C25 2.176(4) . ? Ru1 C23 2.187(4) . ? Ru1 C27 2.211(4) . ? Ru1 C26 2.242(4) . ? S1 O1 1.451(4) . ? S1 O2 1.451(4) . ? S1 N1 1.590(4) . ? S1 C13 1.787(5) . ? P1 O4 1.499(3) . ? P1 O3 1.518(3) . ? P1 C7 1.818(4) . ? P1 C1 1.822(4) . ? N1 C21 1.467(6) . ? N2 C22 1.488(6) . ? C1 C6 1.387(6) . ? C1 C2 1.388(6) . ? C2 C3 1.392(7) . ? C3 C4 1.370(8) . ? C4 C5 1.370(8) . ? C5 C6 1.386(7) . ? C7 C12 1.379(7) . ? C7 C8 1.380(7) . ? C8 C9 1.394(8) . ? C9 C10 1.355(10) . ? C10 C11 1.361(10) . ? C11 C12 1.398(8) . ? C13 C18 1.378(7) . ? C13 C14 1.383(7) . ? C14 C15 1.382(7) . ? C15 C16 1.391(10) . ? C16 C17 1.375(11) . ? C16 C19A 1.470(10) . ? C16 C19 1.470(10) . ? C17 C18 1.382(10) . ? C19 C20 1.00(3) . ? C19A C20A 1.07(2) . ? C21 C22 1.505(7) . ? C23 C28 1.404(7) . ? C23 C24 1.428(7) . ? C23 C29 1.527(7) . ? C24 C25 1.390(7) . ? C25 C26 1.419(7) . ? C26 C27 1.410(7) . ? C26 C32 1.497(7) . ? C27 C28 1.431(7) . ? C29 C30 1.502(10) . ? C29 C31 1.536(8) . ? O5 C33 1.36(2) . ? 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 Ru1 N2 77.97(13) . . ? N1 Ru1 C24 145.6(2) . . ? N2 Ru1 C24 91.0(2) . . ? N1 Ru1 O3 83.38(13) . . ? N2 Ru1 O3 82.81(12) . . ? C24 Ru1 O3 128.0(2) . . ? N1 Ru1 C28 93.7(2) . . ? N2 Ru1 C28 129.3(2) . . ? C24 Ru1 C28 68.2(2) . . ? O3 Ru1 C28 146.59(14) . . ? N1 Ru1 C25 171.0(2) . . ? N2 Ru1 C25 111.0(2) . . ? C24 Ru1 C25 37.5(2) . . ? O3 Ru1 C25 97.9(2) . . ? C28 Ru1 C25 80.3(2) . . ? N1 Ru1 C23 110.5(2) . . ? N2 Ru1 C23 98.6(2) . . ? C24 Ru1 C23 38.4(2) . . ? O3 Ru1 C23 166.0(2) . . ? C28 Ru1 C23 37.6(2) . . ? C25 Ru1 C23 68.5(2) . . ? N1 Ru1 C27 104.2(2) . . ? N2 Ru1 C27 166.8(2) . . ? C24 Ru1 C27 79.9(2) . . ? O3 Ru1 C27 110.36(14) . . ? C28 Ru1 C27 38.1(2) . . ? C25 Ru1 C27 67.0(2) . . ? C23 Ru1 C27 68.3(2) . . ? N1 Ru1 C26 133.9(2) . . ? N2 Ru1 C26 146.4(2) . . ? C24 Ru1 C26 67.8(2) . . ? O3 Ru1 C26 90.13(15) . . ? C28 Ru1 C26 68.1(2) . . ? C25 Ru1 C26 37.4(2) . . ? C23 Ru1 C26 81.0(2) . . ? C27 Ru1 C26 36.9(2) . . ? O1 S1 O2 116.0(2) . . ? O1 S1 N1 109.3(2) . . ? O2 S1 N1 111.0(2) . . ? O1 S1 C13 106.0(2) . . ? O2 S1 C13 105.5(2) . . ? N1 S1 C13 108.6(2) . . ? O4 P1 O3 116.5(2) . . ? O4 P1 C7 110.1(2) . . ? O3 P1 C7 107.5(2) . . ? O4 P1 C1 109.9(2) . . ? O3 P1 C1 109.0(2) . . ? C7 P1 C1 102.9(2) . . ? P1 O3 Ru1 131.9(2) . . ? C21 N1 S1 115.4(3) . . ? C21 N1 Ru1 112.0(3) . . ? S1 N1 Ru1 127.7(2) . . ? C22 N2 Ru1 112.6(3) . . ? C6 C1 C2 119.3(4) . . ? C6 C1 P1 119.8(3) . . ? C2 C1 P1 120.9(3) . . ? C1 C2 C3 119.8(5) . . ? C4 C3 C2 120.3(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 120.6(5) . . ? C5 C6 C1 119.9(5) . . ? C12 C7 C8 119.1(4) . . ? C12 C7 P1 121.3(4) . . ? C8 C7 P1 119.5(4) . . ? C7 C8 C9 120.8(6) . . ? C10 C9 C8 119.1(6) . . ? C9 C10 C11 121.5(6) . . ? C10 C11 C12 119.8(6) . . ? C7 C12 C11 119.7(5) . . ? C18 C13 C14 119.8(5) . . ? C18 C13 S1 121.0(4) . . ? C14 C13 S1 119.2(4) . . ? C15 C14 C13 119.8(5) . . ? C14 C15 C16 121.5(6) . . ? C17 C16 C15 117.2(6) . . ? C17 C16 C19A 119.9(9) . . ? C15 C16 C19A 123.0(10) . . ? C17 C16 C19 119.9(9) . . ? C15 C16 C19 123.0(10) . . ? C16 C17 C18 122.5(6) . . ? C13 C18 C17 119.3(6) . . ? C20 C19 C16 138.0(27) . . ? C20A C19A C16 149.7(26) . . ? N1 C21 C22 106.2(4) . . ? N2 C22 C21 108.8(4) . . ? C28 C23 C24 117.5(4) . . ? C28 C23 C29 122.3(5) . . ? C24 C23 C29 120.1(4) . . ? C28 C23 Ru1 70.5(2) . . ? C24 C23 Ru1 69.4(3) . . ? C29 C23 Ru1 131.6(3) . . ? C25 C24 C23 121.4(4) . . ? C25 C24 Ru1 72.3(3) . . ? C23 C24 Ru1 72.1(3) . . ? C24 C25 C26 121.6(5) . . ? C24 C25 Ru1 70.3(3) . . ? C26 C25 Ru1 73.8(3) . . ? C27 C26 C25 117.7(4) . . ? C27 C26 C32 120.3(5) . . ? C25 C26 C32 121.9(5) . . ? C27 C26 Ru1 70.4(3) . . ? C25 C26 Ru1 68.8(2) . . ? C32 C26 Ru1 129.8(3) . . ? C26 C27 C28 120.8(4) . . ? C26 C27 Ru1 72.7(3) . . ? C28 C27 Ru1 69.4(2) . . ? C23 C28 C27 121.0(4) . . ? C23 C28 Ru1 71.9(2) . . ? C27 C28 Ru1 72.5(2) . . ? C30 C29 C23 113.4(5) . . ? C30 C29 C31 110.2(6) . . ? C23 C29 C31 108.2(5) . . ? 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 O4 P1 O3 Ru1 26.7(3) . . . . ? C7 P1 O3 Ru1 150.8(2) . . . . ? C1 P1 O3 Ru1 -98.3(2) . . . . ? N1 Ru1 O3 P1 -133.9(2) . . . . ? N2 Ru1 O3 P1 -55.3(2) . . . . ? C24 Ru1 O3 P1 30.3(3) . . . . ? C28 Ru1 O3 P1 139.3(3) . . . . ? C25 Ru1 O3 P1 55.1(3) . . . . ? C23 Ru1 O3 P1 41.6(7) . . . . ? C27 Ru1 O3 P1 123.4(2) . . . . ? C26 Ru1 O3 P1 91.8(3) . . . . ? O1 S1 N1 C21 171.4(3) . . . . ? O2 S1 N1 C21 42.2(4) . . . . ? C13 S1 N1 C21 -73.4(4) . . . . ? O1 S1 N1 Ru1 -35.5(3) . . . . ? O2 S1 N1 Ru1 -164.7(3) . . . . ? C13 S1 N1 Ru1 79.7(3) . . . . ? N2 Ru1 N1 C21 -23.3(3) . . . . ? C24 Ru1 N1 C21 -97.0(4) . . . . ? O3 Ru1 N1 C21 60.7(3) . . . . ? C28 Ru1 N1 C21 -152.7(3) . . . . ? C25 Ru1 N1 C21 159.5(10) . . . . ? C23 Ru1 N1 C21 -118.1(3) . . . . ? C27 Ru1 N1 C21 170.1(3) . . . . ? C26 Ru1 N1 C21 144.5(3) . . . . ? N2 Ru1 N1 S1 -177.1(3) . . . . ? C24 Ru1 N1 S1 109.1(3) . . . . ? O3 Ru1 N1 S1 -93.1(3) . . . . ? C28 Ru1 N1 S1 53.5(3) . . . . ? C25 Ru1 N1 S1 5.7(12) . . . . ? C23 Ru1 N1 S1 88.0(3) . . . . ? C27 Ru1 N1 S1 16.3(3) . . . . ? C26 Ru1 N1 S1 -9.3(4) . . . . ? N1 Ru1 N2 C22 -5.3(3) . . . . ? C24 Ru1 N2 C22 141.8(3) . . . . ? O3 Ru1 N2 C22 -90.0(3) . . . . ? C28 Ru1 N2 C22 79.6(3) . . . . ? C25 Ru1 N2 C22 174.3(3) . . . . ? C23 Ru1 N2 C22 104.0(3) . . . . ? C27 Ru1 N2 C22 95.5(7) . . . . ? C26 Ru1 N2 C22 -169.3(3) . . . . ? O4 P1 C1 C6 166.6(4) . . . . ? O3 P1 C1 C6 -64.6(4) . . . . ? C7 P1 C1 C6 49.3(4) . . . . ? O4 P1 C1 C2 -15.3(4) . . . . ? O3 P1 C1 C2 113.5(4) . . . . ? C7 P1 C1 C2 -132.6(4) . . . . ? C6 C1 C2 C3 2.9(7) . . . . ? P1 C1 C2 C3 -175.2(4) . . . . ? C1 C2 C3 C4 -0.8(8) . . . . ? C2 C3 C4 C5 -1.5(9) . . . . ? C3 C4 C5 C6 1.7(8) . . . . ? C4 C5 C6 C1 0.4(8) . . . . ? C2 C1 C6 C5 -2.7(7) . . . . ? P1 C1 C6 C5 175.4(4) . . . . ? O4 P1 C7 C12 138.9(4) . . . . ? O3 P1 C7 C12 10.9(4) . . . . ? C1 P1 C7 C12 -104.0(4) . . . . ? O4 P1 C7 C8 -44.3(5) . . . . ? O3 P1 C7 C8 -172.3(4) . . . . ? C1 P1 C7 C8 72.8(4) . . . . ? C12 C7 C8 C9 -1.3(9) . . . . ? P1 C7 C8 C9 -178.2(5) . . . . ? C7 C8 C9 C10 1.6(11) . . . . ? C8 C9 C10 C11 -0.7(11) . . . . ? C9 C10 C11 C12 -0.4(11) . . . . ? C8 C7 C12 C11 0.2(8) . . . . ? P1 C7 C12 C11 177.0(5) . . . . ? C10 C11 C12 C7 0.7(10) . . . . ? O1 S1 C13 C18 -131.4(4) . . . . ? O2 S1 C13 C18 -7.7(5) . . . . ? N1 S1 C13 C18 111.3(5) . . . . ? O1 S1 C13 C14 46.7(4) . . . . ? O2 S1 C13 C14 170.3(4) . . . . ? N1 S1 C13 C14 -70.7(4) . . . . ? C18 C13 C14 C15 -0.2(8) . . . . ? S1 C13 C14 C15 -178.3(4) . . . . ? C13 C14 C15 C16 0.9(8) . . . . ? C14 C15 C16 C17 -1.0(10) . . . . ? C14 C15 C16 C19A 179.1(8) . . . . ? C14 C15 C16 C19 179.1(8) . . . . ? C15 C16 C17 C18 0.3(11) . . . . ? C19A C16 C17 C18 -179.8(8) . . . . ? C19 C16 C17 C18 -179.8(8) . . . . ? C14 C13 C18 C17 -0.5(9) . . . . ? S1 C13 C18 C17 177.5(5) . . . . ? C16 C17 C18 C13 0.4(11) . . . . ? C17 C16 C19 C20 -149.4(28) . . . . ? C15 C16 C19 C20 30.6(31) . . . . ? C19A C16 C19 C20 0.0(1000) . . . . ? C17 C16 C19A C20A 42.2(38) . . . . ? C15 C16 C19A C20A -137.8(36) . . . . ? C19 C16 C19A C20A 0.0(1000) . . . . ? S1 N1 C21 C22 -156.2(3) . . . . ? Ru1 N1 C21 C22 46.6(4) . . . . ? Ru1 N2 C22 C21 31.8(5) . . . . ? N1 C21 C22 N2 -50.1(5) . . . . ? N1 Ru1 C23 C28 -68.1(3) . . . . ? N2 Ru1 C23 C28 -148.4(3) . . . . ? C24 Ru1 C23 C28 131.0(4) . . . . ? O3 Ru1 C23 C28 116.6(6) . . . . ? C28 Ru1 C23 C28 0.0 . . . . ? C25 Ru1 C23 C28 102.3(3) . . . . ? C27 Ru1 C23 C28 29.5(3) . . . . ? C26 Ru1 C23 C28 65.5(3) . . . . ? N1 Ru1 C23 C24 160.9(3) . . . . ? N2 Ru1 C23 C24 80.6(3) . . . . ? C24 Ru1 C23 C24 0.0 . . . . ? O3 Ru1 C23 C24 -14.4(7) . . . . ? C28 Ru1 C23 C24 -131.0(4) . . . . ? C25 Ru1 C23 C24 -28.7(3) . . . . ? C27 Ru1 C23 C24 -101.5(3) . . . . ? C26 Ru1 C23 C24 -65.5(3) . . . . ? N1 Ru1 C23 C29 48.3(5) . . . . ? N2 Ru1 C23 C29 -32.0(5) . . . . ? C24 Ru1 C23 C29 -112.6(6) . . . . ? O3 Ru1 C23 C29 -127.0(6) . . . . ? C28 Ru1 C23 C29 116.4(6) . . . . ? C25 Ru1 C23 C29 -141.3(5) . . . . ? C27 Ru1 C23 C29 145.9(6) . . . . ? C26 Ru1 C23 C29 -178.0(5) . . . . ? C28 C23 C24 C25 1.8(6) . . . . ? C29 C23 C24 C25 -177.9(4) . . . . ? Ru1 C23 C24 C25 55.2(4) . . . . ? C28 C23 C24 Ru1 -53.4(4) . . . . ? C29 C23 C24 Ru1 127.0(4) . . . . ? Ru1 C23 C24 Ru1 0.0 . . . . ? N1 Ru1 C24 C25 -165.5(3) . . . . ? N2 Ru1 C24 C25 124.6(3) . . . . ? O3 Ru1 C24 C25 43.0(3) . . . . ? C28 Ru1 C24 C25 -102.9(3) . . . . ? C25 Ru1 C24 C25 0.0 . . . . ? C23 Ru1 C24 C25 -132.6(4) . . . . ? C27 Ru1 C24 C25 -65.1(3) . . . . ? C26 Ru1 C24 C25 -28.6(3) . . . . ? N1 Ru1 C24 C23 -32.8(4) . . . . ? N2 Ru1 C24 C23 -102.7(3) . . . . ? O3 Ru1 C24 C23 175.6(2) . . . . ? C28 Ru1 C24 C23 29.7(3) . . . . ? C25 Ru1 C24 C23 132.6(4) . . . . ? C23 Ru1 C24 C23 0.0 . . . . ? C27 Ru1 C24 C23 67.6(3) . . . . ? C26 Ru1 C24 C23 104.0(3) . . . . ? C23 C24 C25 C26 0.3(7) . . . . ? Ru1 C24 C25 C26 55.4(4) . . . . ? C23 C24 C25 Ru1 -55.1(4) . . . . ? Ru1 C24 C25 Ru1 0.0 . . . . ? N1 Ru1 C25 C24 115.3(10) . . . . ? N2 Ru1 C25 C24 -61.8(3) . . . . ? C24 Ru1 C25 C24 0.0 . . . . ? O3 Ru1 C25 C24 -147.1(3) . . . . ? C28 Ru1 C25 C24 66.7(3) . . . . ? C23 Ru1 C25 C24 29.4(3) . . . . ? C27 Ru1 C25 C24 104.1(3) . . . . ? C26 Ru1 C25 C24 133.1(4) . . . . ? N1 Ru1 C25 C26 -17.8(12) . . . . ? N2 Ru1 C25 C26 165.1(3) . . . . ? C24 Ru1 C25 C26 -133.1(4) . . . . ? O3 Ru1 C25 C26 79.8(3) . . . . ? C28 Ru1 C25 C26 -66.4(3) . . . . ? C23 Ru1 C25 C26 -103.7(3) . . . . ? C27 Ru1 C25 C26 -29.0(3) . . . . ? C26 Ru1 C25 C26 0.0 . . . . ? C24 C25 C26 C27 -1.4(7) . . . . ? Ru1 C25 C26 C27 52.4(4) . . . . ? C24 C25 C26 C32 -178.3(4) . . . . ? Ru1 C25 C26 C32 -124.6(4) . . . . ? C24 C25 C26 Ru1 -53.8(4) . . . . ? Ru1 C25 C26 Ru1 0.0 . . . . ? N1 Ru1 C26 C27 44.3(4) . . . . ? N2 Ru1 C26 C27 -157.7(3) . . . . ? C24 Ru1 C26 C27 -103.2(3) . . . . ? O3 Ru1 C26 C27 125.2(3) . . . . ? C28 Ru1 C26 C27 -28.8(3) . . . . ? C25 Ru1 C26 C27 -131.9(4) . . . . ? C23 Ru1 C26 C27 -65.6(3) . . . . ? C27 Ru1 C26 C27 0.0 . . . . ? N1 Ru1 C26 C25 176.2(3) . . . . ? N2 Ru1 C26 C25 -25.8(4) . . . . ? C24 Ru1 C26 C25 28.7(3) . . . . ? O3 Ru1 C26 C25 -102.9(3) . . . . ? C28 Ru1 C26 C25 103.1(3) . . . . ? C25 Ru1 C26 C25 0.0 . . . . ? C23 Ru1 C26 C25 66.3(3) . . . . ? C27 Ru1 C26 C25 131.9(4) . . . . ? N1 Ru1 C26 C32 -69.3(6) . . . . ? N2 Ru1 C26 C32 88.8(6) . . . . ? C24 Ru1 C26 C32 143.2(5) . . . . ? O3 Ru1 C26 C32 11.6(5) . . . . ? C28 Ru1 C26 C32 -142.4(5) . . . . ? C25 Ru1 C26 C32 114.5(6) . . . . ? C23 Ru1 C26 C32 -179.2(5) . . . . ? C27 Ru1 C26 C32 -113.6(6) . . . . ? C25 C26 C27 C28 0.5(7) . . . . ? C32 C26 C27 C28 177.5(4) . . . . ? Ru1 C26 C27 C28 52.1(4) . . . . ? C25 C26 C27 Ru1 -51.6(4) . . . . ? C32 C26 C27 Ru1 125.4(4) . . . . ? Ru1 C26 C27 Ru1 0.0 . . . . ? N1 Ru1 C27 C26 -148.7(3) . . . . ? N2 Ru1 C27 C26 113.5(7) . . . . ? C24 Ru1 C27 C26 66.3(3) . . . . ? O3 Ru1 C27 C26 -60.6(3) . . . . ? C28 Ru1 C27 C26 133.6(4) . . . . ? C25 Ru1 C27 C26 29.5(3) . . . . ? C23 Ru1 C27 C26 104.5(3) . . . . ? C26 Ru1 C27 C26 0.0 . . . . ? N1 Ru1 C27 C28 77.7(3) . . . . ? N2 Ru1 C27 C28 -20.0(8) . . . . ? C24 Ru1 C27 C28 -67.3(3) . . . . ? O3 Ru1 C27 C28 165.8(2) . . . . ? C28 Ru1 C27 C28 0.000(1) . . . . ? C25 Ru1 C27 C28 -104.1(3) . . . . ? C23 Ru1 C27 C28 -29.1(3) . . . . ? C26 Ru1 C27 C28 -133.6(4) . . . . ? C24 C23 C28 C27 -2.7(6) . . . . ? C29 C23 C28 C27 177.0(4) . . . . ? Ru1 C23 C28 C27 -55.5(4) . . . . ? C24 C23 C28 Ru1 52.8(4) . . . . ? C29 C23 C28 Ru1 -127.5(4) . . . . ? Ru1 C23 C28 Ru1 0.0 . . . . ? C26 C27 C28 C23 1.6(7) . . . . ? Ru1 C27 C28 C23 55.2(4) . . . . ? C26 C27 C28 Ru1 -53.6(4) . . . . ? Ru1 C27 C28 Ru1 0.0 . . . . ? N1 Ru1 C28 C23 119.5(3) . . . . ? N2 Ru1 C28 C23 42.0(4) . . . . ? C24 Ru1 C28 C23 -30.3(3) . . . . ? O3 Ru1 C28 C23 -156.9(3) . . . . ? C25 Ru1 C28 C23 -67.3(3) . . . . ? C23 Ru1 C28 C23 0.0 . . . . ? C27 Ru1 C28 C23 -132.2(4) . . . . ? C26 Ru1 C28 C23 -104.2(3) . . . . ? N1 Ru1 C28 C27 -108.3(3) . . . . ? N2 Ru1 C28 C27 174.2(2) . . . . ? C24 Ru1 C28 C27 101.9(3) . . . . ? O3 Ru1 C28 C27 -24.7(4) . . . . ? C25 Ru1 C28 C27 64.9(3) . . . . ? C23 Ru1 C28 C27 132.2(4) . . . . ? C27 Ru1 C28 C27 0.000(1) . . . . ? C26 Ru1 C28 C27 28.0(3) . . . . ? C28 C23 C29 C30 30.0(7) . . . . ? C24 C23 C29 C30 -150.3(6) . . . . ? Ru1 C23 C29 C30 -61.9(7) . . . . ? C28 C23 C29 C31 -92.5(7) . . . . ? C24 C23 C29 C31 87.2(6) . . . . ? Ru1 C23 C29 C31 175.6(5) . . . . ? _refine_diff_density_max 0.587 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.124 #===END