# Copyright The Royal Society of Chemistry, 1998 data_ruthzet1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common RuTHZET1 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H24 Cl2 N3 P Ru S3' _chemical_formula_weight 689.61 _chemical_melting_point unknown _chemical_compound_source 'by us' 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' 'P' 'P' 0.1023 0.0942 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Least-squares, 28 randomly selected refls' _symmetry_space_group_name_H-M 'P(-1), no. 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.355(3) _cell_length_b 11.152(3) _cell_length_c 14.225(4) _cell_angle_alpha 88.55(2) _cell_angle_beta 76.89(2) _cell_angle_gamma 80.32(2) _cell_volume 1424.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 5 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'prism, from ethylacetate' _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method ? _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type psi _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.94 _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 'Siemens P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 4266 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 23.50 _reflns_number_total 3988 _reflns_number_observed 3114 _reflns_observed_criterion >2sigma(I) _computing_data_collection XSCAN/Siemens _computing_cell_refinement XSCAN/Siemens _computing_data_reduction XSCAN/Siemens _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XPMA, ZORTEP (L.Zsolnai, 1994)' _computing_publication_material 'CIFTAB-SHELX93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 17 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^)+(0.1081P)^2^+0.3160P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding on the heavy atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3971 _refine_ls_number_parameters 362 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_obs 0.0556 _refine_ls_wR_factor_all 0.1640 _refine_ls_wR_factor_obs 0.1403 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.102 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.13200(5) 0.24223(4) 0.20735(3) 0.0305(2) Uani 1 d . . Cl1 Cl 0.1002(2) 0.46079(14) 0.21678(12) 0.0432(4) Uani 1 d . . Cl2 Cl 0.1946(2) 0.02261(14) 0.19125(11) 0.0407(4) Uani 1 d . . P P -0.1047(2) 0.24931(14) 0.30060(11) 0.0341(4) Uani 1 d . . S1 S -0.0334(6) 0.1862(5) -0.0634(4) 0.0557(14) Uani 0.671(10) d PD 1 S1B S 0.0203(14) 0.2960(10) -0.0901(6) 0.060(3) Uani 0.329(10) d PD 2 S2 S 0.3709(3) 0.2787(3) 0.4507(2) 0.0906(8) Uani 1 d D . S3 S 0.5787(2) 0.3200(2) 0.0108(2) 0.0662(6) Uani 1 d . . N1 N 0.0573(5) 0.2449(4) 0.0800(3) 0.0333(11) Uani 1 d . . N2 N 0.2327(6) 0.2315(5) 0.3262(4) 0.0395(13) Uani 1 d . . N3 N 0.3472(5) 0.2470(5) 0.1091(4) 0.0360(12) Uani 1 d . . C21 C -0.0069(7) 0.1590(6) 0.0495(4) 0.042(2) Uani 1 d D . H21 H -0.0337(7) 0.0926(6) 0.0860(4) 0.050 Uiso 1 calc R 1 C41 C 0.0479(23) 0.3133(17) -0.0756(13) 0.052(6) Uiso 0.671(10) d PD 1 C41B C -0.0385(46) 0.1667(28) -0.0396(18) 0.040(12) Uiso 0.329(10) d PD 2 C51 C 0.0811(8) 0.3297(6) 0.0104(4) 0.045(2) Uani 1 d D . H51 H 0.1197(8) 0.3981(6) 0.0217(4) 0.053 Uiso 1 calc R 1 C22 C 0.3006(8) 0.3154(7) 0.3527(5) 0.053(2) Uani 1 d D . H22 H 0.3088(8) 0.3882(7) 0.3202(5) 0.063 Uiso 1 calc R . C42 C 0.3169(8) 0.1437(5) 0.4621(4) 0.044(2) Uani 1 d D . H42 H 0.3338(8) 0.0853(5) 0.5079(4) 0.053 Uiso 1 calc R . C52 C 0.2397(8) 0.1351(7) 0.3881(5) 0.054(2) Uani 1 d D . H52 H 0.1961(8) 0.0676(7) 0.3817(5) 0.064 Uiso 1 calc R . C23 C 0.4250(8) 0.3318(7) 0.1027(5) 0.052(2) Uani 1 d . . H23 H 0.3989(8) 0.3968(7) 0.1463(5) 0.063 Uiso 1 calc R . C43 C 0.5372(8) 0.1911(6) -0.0282(5) 0.052(2) Uani 1 d . . H43 H 0.5921(8) 0.1446(6) -0.0817(5) 0.063 Uiso 1 calc R . C53 C 0.4069(8) 0.1660(6) 0.0330(5) 0.047(2) Uani 1 d . . H53 H 0.3634(8) 0.0996(6) 0.0233(5) 0.056 Uiso 1 calc R . C1A C -0.2409(7) 0.3855(6) 0.2840(5) 0.0377(14) Uani 1 d . . C2A C -0.2461(8) 0.4289(6) 0.1928(5) 0.049(2) Uani 1 d . . H2A H -0.1773(8) 0.3911(6) 0.1398(5) 0.059 Uiso 1 calc R . C3A C -0.3495(8) 0.5260(7) 0.1779(6) 0.053(2) Uani 1 d . . H3A H -0.3516(8) 0.5512(7) 0.1153(6) 0.064 Uiso 1 calc R . C4A C -0.4493(9) 0.5858(7) 0.2542(6) 0.056(2) Uani 1 d . . H4A H -0.5184(9) 0.6524(7) 0.2442(6) 0.067 Uiso 1 calc R . C5A C -0.4459(9) 0.5456(8) 0.3468(6) 0.070(2) Uani 1 d . . H5A H -0.5146(9) 0.5843(8) 0.3994(6) 0.084 Uiso 1 calc R . C6A C -0.3418(8) 0.4490(7) 0.3612(5) 0.056(2) Uani 1 d . . H6A H -0.3383(8) 0.4253(7) 0.4240(5) 0.067 Uiso 1 calc R . C1B C -0.2017(7) 0.1240(6) 0.2835(4) 0.0358(14) Uani 1 d . . C2B C -0.1437(8) 0.0067(6) 0.3048(5) 0.043(2) Uani 1 d . . H2B H -0.0585(8) -0.0066(6) 0.3295(5) 0.052 Uiso 1 calc R . C3B C -0.2092(9) -0.0909(7) 0.2902(6) 0.059(2) Uani 1 d . . H3B H -0.1691(9) -0.1689(7) 0.3057(6) 0.071 Uiso 1 calc R . C4B C -0.3356(9) -0.0723(7) 0.2521(6) 0.060(2) Uani 1 d . . H4B H -0.3797(9) -0.1379(7) 0.2414(6) 0.072 Uiso 1 calc R . C5B C -0.3952(9) 0.0442(8) 0.2305(6) 0.062(2) Uani 1 d . . H5B H -0.4796(9) 0.0573(8) 0.2049(6) 0.075 Uiso 1 calc R . C6B C -0.3294(8) 0.1413(7) 0.2468(5) 0.048(2) Uani 1 d . . H6B H -0.3711(8) 0.2196(7) 0.2331(5) 0.058 Uiso 1 calc R . C1C C -0.1280(7) 0.2544(6) 0.4324(4) 0.0380(15) Uani 1 d . . C2C C -0.0588(8) 0.3358(7) 0.4713(5) 0.052(2) Uani 1 d . . H2C H -0.0026(8) 0.3850(7) 0.4299(5) 0.062 Uiso 1 calc R . C3C C -0.0709(9) 0.3458(8) 0.5687(5) 0.062(2) Uani 1 d . . H3C H -0.0243(9) 0.4015(8) 0.5929(5) 0.074 Uiso 1 calc R . C4C C -0.1542(10) 0.2715(8) 0.6312(5) 0.063(2) Uani 1 d . . H4C H -0.1611(10) 0.2758(8) 0.6974(5) 0.076 Uiso 1 calc R . C5C C -0.2247(10) 0.1934(7) 0.5956(5) 0.062(2) Uani 1 d . . H5C H -0.2823(10) 0.1457(7) 0.6376(5) 0.075 Uiso 1 calc R . C6C C -0.2124(8) 0.1831(6) 0.4970(5) 0.050(2) Uani 1 d . . H6C H -0.2610(8) 0.1281(6) 0.4738(5) 0.060 Uiso 1 calc 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 Ru 0.0364(3) 0.0282(3) 0.0260(3) -0.0038(2) -0.0061(2) -0.0034(2) Cl1 0.0524(10) 0.0302(8) 0.0460(9) -0.0054(7) -0.0104(7) -0.0043(7) Cl2 0.0482(9) 0.0315(8) 0.0395(9) -0.0051(6) -0.0069(7) -0.0017(7) P 0.0396(9) 0.0336(9) 0.0268(8) -0.0022(7) -0.0043(7) -0.0043(7) S1 0.064(3) 0.071(3) 0.035(2) -0.010(2) -0.017(2) -0.011(2) S1B 0.080(6) 0.062(6) 0.038(4) 0.001(3) -0.021(4) 0.001(4) S2 0.102(2) 0.116(2) 0.069(2) -0.0059(14) -0.0434(14) -0.026(2) S3 0.0484(11) 0.0712(14) 0.0716(14) 0.0016(11) 0.0045(10) -0.0141(10) N1 0.035(3) 0.033(3) 0.028(3) -0.006(2) -0.001(2) -0.001(2) N2 0.046(3) 0.038(3) 0.033(3) -0.004(2) -0.009(2) -0.004(3) N3 0.033(3) 0.033(3) 0.041(3) 0.001(2) -0.005(2) -0.007(2) C21 0.044(4) 0.047(4) 0.034(4) -0.003(3) -0.010(3) -0.006(3) C51 0.056(4) 0.042(4) 0.031(3) 0.000(3) -0.007(3) -0.001(3) C22 0.054(4) 0.062(5) 0.045(4) -0.006(4) -0.014(3) -0.015(4) C42 0.066(4) 0.048(4) 0.019(3) 0.006(3) -0.016(3) -0.002(3) C52 0.066(5) 0.049(4) 0.043(4) -0.003(3) -0.013(4) 0.000(4) C23 0.047(4) 0.055(5) 0.050(4) -0.008(3) 0.000(3) -0.008(4) C43 0.051(4) 0.046(4) 0.048(4) -0.008(3) 0.003(3) 0.008(3) C53 0.049(4) 0.039(4) 0.048(4) -0.006(3) -0.004(3) -0.001(3) C1A 0.036(3) 0.034(3) 0.043(4) -0.004(3) -0.009(3) -0.005(3) C2A 0.046(4) 0.049(4) 0.042(4) 0.000(3) 0.001(3) 0.005(3) C3A 0.045(4) 0.058(5) 0.055(4) 0.013(4) -0.013(3) -0.004(4) C4A 0.058(5) 0.042(4) 0.066(5) -0.004(4) -0.024(4) 0.010(3) C5A 0.066(5) 0.062(5) 0.066(5) -0.021(4) -0.013(4) 0.033(4) C6A 0.062(5) 0.059(5) 0.039(4) -0.010(3) -0.008(3) 0.011(4) C1B 0.039(3) 0.041(4) 0.023(3) -0.005(3) -0.001(3) -0.005(3) C2B 0.045(4) 0.045(4) 0.038(4) -0.007(3) -0.003(3) -0.009(3) C3B 0.069(5) 0.039(4) 0.058(5) -0.005(3) 0.003(4) -0.001(4) C4B 0.068(5) 0.054(5) 0.062(5) -0.006(4) -0.009(4) -0.024(4) C5B 0.057(5) 0.069(6) 0.067(5) -0.002(4) -0.022(4) -0.016(4) C6B 0.053(4) 0.047(4) 0.047(4) 0.003(3) -0.016(3) -0.008(3) C1C 0.043(4) 0.035(3) 0.029(3) -0.003(3) -0.002(3) 0.007(3) C2C 0.061(5) 0.051(4) 0.040(4) -0.010(3) -0.002(3) -0.006(4) C3C 0.071(5) 0.063(5) 0.049(5) -0.028(4) -0.019(4) 0.005(4) C4C 0.080(6) 0.065(5) 0.031(4) -0.008(4) -0.008(4) 0.019(5) C5C 0.089(6) 0.047(4) 0.036(4) 0.004(3) 0.007(4) 0.003(4) C6C 0.066(5) 0.044(4) 0.034(4) -0.001(3) -0.004(3) -0.003(4) _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 Ru N1 2.082(5) . ? Ru N2 2.106(5) . ? Ru N3 2.183(5) . ? Ru P 2.299(2) . ? Ru Cl1 2.409(2) . ? Ru Cl2 2.425(2) . ? P C1C 1.839(6) . ? P C1B 1.838(6) . ? P C1A 1.858(6) . ? S1 C21 1.693(7) . ? S1 C41 1.705(15) . ? S1B C41B 1.71(2) . ? S1B C51 1.725(11) . ? S2 C42 1.659(6) . ? S2 C22 1.685(6) . ? S3 C43 1.689(8) . ? S3 C23 1.699(7) . ? N1 C21 1.341(8) . ? N1 C51 1.359(8) . ? N2 C22 1.322(9) . ? N2 C52 1.375(9) . ? N3 C23 1.276(9) . ? N3 C53 1.381(8) . ? C21 C41B 1.36(2) . ? C41 C51 1.352(15) . ? C42 C52 1.418(7) . ? C43 C53 1.394(10) . ? C1A C2A 1.383(9) . ? C1A C6A 1.394(9) . ? C2A C3A 1.372(10) . ? C3A C4A 1.365(10) . ? C4A C5A 1.387(11) . ? C5A C6A 1.370(11) . ? C1B C2B 1.384(10) . ? C1B C6B 1.391(9) . ? C2B C3B 1.377(10) . ? C3B C4B 1.392(11) . ? C4B C5B 1.381(12) . ? C5B C6B 1.381(10) . ? C1C C2C 1.391(10) . ? C1C C6C 1.394(9) . ? C2C C3C 1.370(10) . ? C3C C4C 1.397(12) . ? C4C C5C 1.348(12) . ? C5C C6C 1.386(10) . ? 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 Ru N2 173.2(2) . . ? N1 Ru N3 83.4(2) . . ? N2 Ru N3 90.3(2) . . ? N1 Ru P 92.13(14) . . ? N2 Ru P 94.30(15) . . ? N3 Ru P 174.46(14) . . ? N1 Ru Cl1 93.00(14) . . ? N2 Ru Cl1 89.26(15) . . ? N3 Ru Cl1 87.42(14) . . ? P Ru Cl1 89.56(6) . . ? N1 Ru Cl2 88.49(14) . . ? N2 Ru Cl2 88.56(15) . . ? N3 Ru Cl2 86.32(14) . . ? P Ru Cl2 96.85(6) . . ? Cl1 Ru Cl2 173.37(6) . . ? C1C P C1B 102.6(3) . . ? C1C P C1A 100.2(3) . . ? C1B P C1A 102.2(3) . . ? C1C P Ru 117.4(2) . . ? C1B P Ru 116.5(2) . . ? C1A P Ru 115.4(2) . . ? C21 S1 C41 93.4(6) . . ? C41B S1B C51 92.5(9) . . ? C42 S2 C22 93.9(3) . . ? C43 S3 C23 90.0(4) . . ? C21 N1 C51 109.7(5) . . ? C21 N1 Ru 126.1(4) . . ? C51 N1 Ru 123.9(4) . . ? C22 N2 C52 109.1(6) . . ? C22 N2 Ru 125.6(5) . . ? C52 N2 Ru 125.3(4) . . ? C23 N3 C53 109.4(6) . . ? C23 N3 Ru 126.7(5) . . ? C53 N3 Ru 123.1(4) . . ? N1 C21 C41B 120.1(11) . . ? N1 C21 S1 111.8(5) . . ? C51 C41 S1 105.6(11) . . ? C21 C41B S1B 106.2(15) . . ? C41 C51 N1 119.2(9) . . ? N1 C51 S1B 111.5(6) . . ? N2 C22 S2 114.0(6) . . ? C52 C42 S2 106.4(5) . . ? N2 C52 C42 116.7(6) . . ? N3 C23 S3 116.8(5) . . ? C53 C43 S3 108.7(5) . . ? N3 C53 C43 115.0(6) . . ? C2A C1A C6A 116.6(6) . . ? C2A C1A P 120.7(5) . . ? C6A C1A P 122.7(5) . . ? C3A C2A C1A 122.1(6) . . ? C4A C3A C2A 120.5(7) . . ? C3A C4A C5A 118.9(7) . . ? C6A C5A C4A 120.3(7) . . ? C5A C6A C1A 121.5(7) . . ? C2B C1B C6B 118.1(6) . . ? C2B C1B P 119.2(5) . . ? C6B C1B P 122.7(5) . . ? C3B C2B C1B 121.5(7) . . ? C2B C3B C4B 119.7(7) . . ? C5B C4B C3B 119.6(7) . . ? C6B C5B C4B 119.9(7) . . ? C5B C6B C1B 121.2(7) . . ? C2C C1C C6C 117.1(6) . . ? C2C C1C P 118.3(5) . . ? C6C C1C P 124.6(5) . . ? C3C C2C C1C 122.1(7) . . ? C2C C3C C4C 119.2(8) . . ? C5C C4C C3C 119.9(7) . . ? C4C C5C C6C 120.9(8) . . ? C5C C6C C1C 120.8(7) . . ? _refine_diff_density_max '0.987 at 0.989 Angstrom from Ru' _refine_diff_density_min -0.758 _refine_diff_density_rms 0.116