# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1647 data_2.PF6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Cl F6 N4 O2 P Ru S' _chemical_formula_weight 718.05 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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.594(3) _cell_length_b 17.951(4) _cell_length_c 14.171(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.445(10) _cell_angle_gamma 90.00 _cell_volume 3148.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 15.0 _exptl_crystal_description parallelopiped _exptl_crystal_colour red _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type n/a _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method 'omega2 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.67 _diffrn_reflns_number 15404 _diffrn_reflns_av_R_equivalents 0.0118 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7247 _reflns_number_gt 6120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+5.0665P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7247 _refine_ls_number_parameters 353 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.170 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.233867(19) 0.129726(14) 0.640679(19) 0.03594(11) Uani 1 d . . . Cl1 Cl 0.21286(8) 0.26083(5) 0.66655(8) 0.0528(2) Uani 1 d . . . S1 S 0.11439(7) 0.09305(5) 0.70510(7) 0.0452(2) Uani 1 d . . . P1 P 0.29043(10) 0.18676(8) 0.10123(10) 0.0679(3) Uani 0.50 d P A 1 F11 F 0.3348(14) 0.1303(9) 0.2027(13) 0.1089(7) Uiso 0.264(3) d P A 1 F12 F 0.4115(13) 0.1903(9) 0.1284(13) 0.1089(7) Uiso 0.264(3) d P A 1 F13 F 0.1615(13) 0.1675(10) 0.0267(13) 0.1089(7) Uiso 0.264(3) d P A 1 F14 F 0.2708(14) 0.2187(9) -0.0052(12) 0.1089(7) Uiso 0.264(3) d P A 1 F15 F 0.2617(15) 0.2467(10) 0.1619(14) 0.1089(7) Uiso 0.264(3) d P A 1 F16 F 0.2813(14) 0.0998(11) 0.0564(15) 0.1089(7) Uiso 0.264(3) d P A 1 P1 P 0.29043(10) 0.18676(8) 0.10123(10) 0.0679(3) Uani 0.50 d P A 2 F21 F 0.3969(5) 0.1823(3) 0.2047(5) 0.1089(7) Uiso 0.736(3) d P A 2 F22 F 0.3645(5) 0.2333(3) 0.0543(5) 0.1089(7) Uiso 0.736(3) d P A 2 F23 F 0.3181(5) 0.1158(4) 0.0562(5) 0.1089(7) Uiso 0.736(3) d P A 2 F24 F 0.1932(5) 0.2081(3) -0.0017(5) 0.1089(7) Uiso 0.736(3) d P A 2 F25 F 0.2169(4) 0.1560(4) 0.1502(4) 0.1089(7) Uiso 0.736(3) d P A 2 F26 F 0.2771(5) 0.2699(4) 0.1435(5) 0.1089(7) Uiso 0.736(3) d P A 2 O1 O 0.0205(2) 0.0490(2) 0.6360(2) 0.0698(9) Uani 1 d . . . C1 C 0.1754(4) 0.0373(3) 0.8185(3) 0.0690(13) Uani 1 d . . . H12A H 0.2305 0.0656 0.8718 0.083 Uiso 1 calc R . . H12B H 0.2072 -0.0061 0.8027 0.083 Uiso 1 calc R . . H12C H 0.1216 0.0223 0.8420 0.083 Uiso 1 calc R . . C2 C 0.0629(5) 0.1669(3) 0.7560(5) 0.0857(16) Uani 1 d . . . H21A H 0.1215 0.1908 0.8117 0.103 Uiso 1 calc R . . H21B H 0.0129 0.1470 0.7816 0.103 Uiso 1 calc R . . H21C H 0.0265 0.2025 0.7023 0.103 Uiso 1 calc R . . ND1 N 0.3631(2) 0.11264(18) 0.7821(2) 0.0439(6) Uani 1 d . . . CD2 C 0.4049(3) 0.1630(2) 0.8579(3) 0.0520(9) Uani 1 d . . . HD2 H 0.3684 0.2077 0.8528 0.062 Uiso 1 calc R . . CD3 C 0.5009(4) 0.1506(3) 0.9439(3) 0.0676(12) Uani 1 d . . . HD3 H 0.5288 0.1868 0.9951 0.081 Uiso 1 calc R . . CD4 C 0.5538(4) 0.0848(3) 0.9524(4) 0.0772(15) Uani 1 d . . . HD4 H 0.6188 0.0758 1.0092 0.093 Uiso 1 calc R . . CD5 C 0.5103(4) 0.0316(3) 0.8763(4) 0.0683(12) Uani 1 d . . . HD5 H 0.5454 -0.0137 0.8817 0.082 Uiso 1 calc R . . CD6 C 0.4139(3) 0.0459(2) 0.7917(3) 0.0490(8) Uani 1 d . . . CC2 C 0.3592(3) -0.0063(2) 0.7061(3) 0.0503(8) Uani 1 d . . . CC3 C 0.3918(4) -0.0794(3) 0.7051(4) 0.0721(13) Uani 1 d . . . HC3 H 0.4525 -0.0977 0.7601 0.087 Uiso 1 calc R . . CC4 C 0.3332(5) -0.1247(3) 0.6219(5) 0.0786(15) Uani 1 d . . . HC4 H 0.3544 -0.1737 0.6200 0.094 Uiso 1 calc R . . CC5 C 0.2436(4) -0.0966(3) 0.5422(4) 0.0696(13) Uani 1 d . . . HC5 H 0.2037 -0.1263 0.4855 0.084 Uiso 1 calc R . . CC6 C 0.2130(3) -0.0237(2) 0.5468(3) 0.0532(9) Uani 1 d . . . HC6 H 0.1515 -0.0051 0.4929 0.064 Uiso 1 calc R . . NC1 N 0.2698(2) 0.02099(16) 0.6269(2) 0.0420(6) Uani 1 d . . . NA1 N 0.1246(2) 0.14421(16) 0.4869(2) 0.0413(6) Uani 1 d . . . CA6 C 0.0171(3) 0.1328(2) 0.4469(3) 0.0511(9) Uani 1 d . . . HA6 H -0.0137 0.1164 0.4908 0.061 Uiso 1 calc R . . CA5 C -0.0490(3) 0.1441(2) 0.3441(3) 0.0588(11) Uani 1 d . . . HA5 H -0.1231 0.1363 0.3196 0.071 Uiso 1 calc R . . CA4 C -0.0049(4) 0.1670(3) 0.2786(3) 0.0701(13) Uani 1 d . . . HA4 H -0.0482 0.1746 0.2086 0.084 Uiso 1 calc R . . CA3 C 0.1037(4) 0.1788(3) 0.3170(3) 0.0719(13) Uani 1 d . . . HA3 H 0.1352 0.1938 0.2730 0.086 Uiso 1 calc R . . CA2 C 0.1675(3) 0.1683(2) 0.4222(3) 0.0503(8) Uani 1 d . . . CB2 C 0.2858(3) 0.1805(3) 0.4695(3) 0.0548(9) Uani 1 d . . . CB3 C 0.3428(4) 0.2082(4) 0.4159(4) 0.0823(16) Uani 1 d . . . HB3 H 0.3071 0.2209 0.3463 0.099 Uiso 1 calc R . . CB4 C 0.4532(4) 0.2168(4) 0.4668(5) 0.0870(17) Uani 1 d . . . HB4 H 0.4925 0.2357 0.4319 0.104 Uiso 1 calc R . . CB5 C 0.5037(4) 0.1977(3) 0.5676(4) 0.0721(13) Uani 1 d . . . HB5 H 0.5782 0.2028 0.6027 0.086 Uiso 1 calc R . . CB6 C 0.4433(3) 0.1704(3) 0.6182(3) 0.0569(10) Uani 1 d . . . HB6 H 0.4786 0.1570 0.6876 0.068 Uiso 1 calc R . . NB1 N 0.3351(2) 0.16254(17) 0.5706(2) 0.0442(6) Uani 1 d . . . C61A C 0.897(4) 0.035(3) 0.938(2) 0.20(2) Uiso 0.25 d PD B 1 C61B C 0.825(3) 0.073(2) 0.923(2) 0.145(14) Uiso 0.25 d PD B 1 C62 C 0.8506(19) 0.0658(16) 0.831(2) 0.227(13) Uiso 0.50 d PD B 1 O63 O 0.7895(17) 0.0220(14) 0.7454(17) 0.318(13) Uiso 0.50 d PD B 1 C64 C 0.6790(16) 0.0413(11) 0.7093(16) 0.153(7) Uiso 0.50 d PD B 1 C65A C 0.678(2) 0.1115(13) 0.785(2) 0.091(7) Uiso 0.25 d PD B 1 C65B C 0.608(2) -0.0053(18) 0.616(2) 0.126(11) Uiso 0.25 d PD B 1 O600 O 0.7445(17) 0.0769(12) 0.8033(16) 0.208(7) Uiso 0.50 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02955(15) 0.03635(16) 0.03414(15) -0.00035(9) 0.00539(10) -0.00119(9) Cl1 0.0464(5) 0.0413(4) 0.0541(5) -0.0045(4) 0.0040(4) 0.0026(4) S1 0.0376(4) 0.0532(5) 0.0410(4) -0.0009(4) 0.0125(3) -0.0038(4) P1 0.0599(7) 0.0900(9) 0.0541(6) 0.0093(6) 0.0239(5) 0.0238(6) P1 0.0599(7) 0.0900(9) 0.0541(6) 0.0093(6) 0.0239(5) 0.0238(6) O1 0.0543(17) 0.091(2) 0.0560(17) -0.0029(16) 0.0141(14) -0.0314(16) C1 0.062(3) 0.090(3) 0.055(2) 0.022(2) 0.023(2) -0.002(2) C2 0.093(4) 0.077(3) 0.114(5) -0.009(3) 0.069(4) 0.010(3) ND1 0.0342(14) 0.0502(16) 0.0386(14) 0.0042(12) 0.0064(11) 0.0002(12) CD2 0.0440(19) 0.060(2) 0.0407(18) -0.0005(17) 0.0057(15) -0.0045(17) CD3 0.051(2) 0.091(3) 0.041(2) -0.001(2) -0.0006(18) -0.013(2) CD4 0.045(2) 0.110(4) 0.050(2) 0.019(3) -0.0063(19) 0.007(3) CD5 0.050(2) 0.077(3) 0.063(3) 0.022(2) 0.008(2) 0.018(2) CD6 0.0377(17) 0.054(2) 0.050(2) 0.0110(16) 0.0126(15) 0.0059(15) CC2 0.0443(19) 0.0449(19) 0.061(2) 0.0094(17) 0.0207(17) 0.0076(15) CC3 0.066(3) 0.054(2) 0.091(4) 0.012(2) 0.027(3) 0.018(2) CC4 0.087(4) 0.044(2) 0.113(4) -0.002(3) 0.049(3) 0.012(2) CC5 0.075(3) 0.047(2) 0.094(4) -0.018(2) 0.042(3) -0.008(2) CC6 0.051(2) 0.046(2) 0.062(2) -0.0076(17) 0.0229(18) -0.0059(16) NC1 0.0391(14) 0.0365(14) 0.0492(16) 0.0000(12) 0.0172(12) -0.0022(11) NA1 0.0370(14) 0.0401(14) 0.0364(14) -0.0007(11) 0.0049(11) -0.0002(11) CA6 0.0400(18) 0.053(2) 0.047(2) 0.0044(16) 0.0045(15) -0.0062(15) CA5 0.045(2) 0.056(2) 0.052(2) 0.0051(18) -0.0035(17) -0.0023(17) CA4 0.063(3) 0.084(3) 0.041(2) 0.007(2) -0.0009(19) 0.003(2) CA3 0.064(3) 0.103(4) 0.041(2) 0.010(2) 0.0134(19) 0.001(3) CA2 0.0463(19) 0.059(2) 0.0397(18) -0.0001(16) 0.0115(15) -0.0019(17) CB2 0.051(2) 0.067(3) 0.047(2) -0.0015(18) 0.0212(17) -0.0025(19) CB3 0.065(3) 0.128(5) 0.060(3) 0.014(3) 0.032(2) -0.006(3) CB4 0.069(3) 0.127(5) 0.081(4) 0.004(3) 0.047(3) -0.017(3) CB5 0.047(2) 0.092(4) 0.082(3) -0.002(3) 0.031(2) -0.011(2) CB6 0.0388(18) 0.066(3) 0.060(2) 0.001(2) 0.0144(17) -0.0057(17) NB1 0.0364(14) 0.0453(16) 0.0467(16) -0.0001(13) 0.0131(12) -0.0039(12) _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 NC1 2.041(3) . ? Ru1 ND1 2.069(3) . ? Ru1 NA1 2.084(3) . ? Ru1 NB1 2.088(3) . ? Ru1 S1 2.2653(10) . ? Ru1 Cl1 2.4168(11) . ? S1 O1 1.476(3) . ? S1 C1 1.780(4) . ? S1 C2 1.785(5) . ? P1 F15 1.525(19) . ? P1 F12 1.529(16) . ? P1 F14 1.530(16) . ? P1 F11 1.655(16) . ? P1 F16 1.671(19) . ? P1 F13 1.666(16) . ? P1 F25 1.537(6) . ? P1 F23 1.539(7) . ? P1 F24 1.557(6) . ? P1 F21 1.580(6) . ? P1 F26 1.646(7) . ? P1 F22 1.646(6) . ? ND1 CD2 1.338(5) . ? ND1 CD6 1.361(5) . ? CD2 CD3 1.386(5) . ? CD3 CD4 1.364(8) . ? CD4 CD5 1.377(8) . ? CD5 CD6 1.386(5) . ? CD6 CC2 1.469(6) . ? CC2 NC1 1.359(5) . ? CC2 CC3 1.386(6) . ? CC3 CC4 1.382(8) . ? CC4 CC5 1.369(8) . ? CC5 CC6 1.382(6) . ? CC6 NC1 1.343(5) . ? NA1 CA6 1.346(5) . ? NA1 CA2 1.345(5) . ? CA6 CA5 1.374(5) . ? CA5 CA4 1.361(7) . ? CA4 CA3 1.361(7) . ? CA3 CA2 1.394(5) . ? CA2 CB2 1.481(5) . ? CB2 NB1 1.346(5) . ? CB2 CB3 1.382(6) . ? CB3 CB4 1.378(7) . ? CB4 CB5 1.348(8) . ? CB5 CB6 1.385(6) . ? CB6 NB1 1.347(5) . ? C61A C62 1.481(19) . ? C61B C62 1.484(18) . ? C62 O63 1.399(17) . ? C62 C64 2.300(17) . ? O63 C64 1.416(16) . ? C64 C65B 1.527(17) . ? C64 C65A 1.657(17) . ? 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 NC1 Ru1 ND1 79.06(12) . . ? NC1 Ru1 NA1 96.57(12) . . ? ND1 Ru1 NA1 169.47(12) . . ? NC1 Ru1 NB1 89.61(12) . . ? ND1 Ru1 NB1 92.29(12) . . ? NA1 Ru1 NB1 78.03(12) . . ? NC1 Ru1 S1 90.04(9) . . ? ND1 Ru1 S1 91.69(9) . . ? NA1 Ru1 S1 97.92(9) . . ? NB1 Ru1 S1 175.86(8) . . ? NC1 Ru1 Cl1 173.59(8) . . ? ND1 Ru1 Cl1 95.95(9) . . ? NA1 Ru1 Cl1 87.66(8) . . ? NB1 Ru1 Cl1 86.56(9) . . ? S1 Ru1 Cl1 94.15(4) . . ? O1 S1 C1 104.5(2) . . ? O1 S1 C2 106.8(3) . . ? C1 S1 C2 99.6(3) . . ? O1 S1 Ru1 117.12(14) . . ? C1 S1 Ru1 112.51(16) . . ? C2 S1 Ru1 114.5(2) . . ? F15 P1 F12 109.2(9) . . ? F15 P1 F14 108.1(9) . . ? F12 P1 F14 87.9(9) . . ? F15 P1 F11 91.6(9) . . ? F12 P1 F11 80.7(8) . . ? F14 P1 F11 159.7(8) . . ? F15 P1 F16 151.3(9) . . ? F12 P1 F16 92.1(8) . . ? F14 P1 F16 91.2(9) . . ? F11 P1 F16 72.6(9) . . ? F15 P1 F13 93.2(9) . . ? F12 P1 F13 155.4(8) . . ? F14 P1 F13 75.2(8) . . ? F11 P1 F13 109.5(9) . . ? F16 P1 F13 70.9(8) . . ? F25 P1 F23 101.9(3) . . ? F25 P1 F24 93.0(3) . . ? F23 P1 F24 94.2(3) . . ? F25 P1 F21 94.6(3) . . ? F23 P1 F21 93.2(3) . . ? F24 P1 F21 168.1(3) . . ? F25 P1 F26 88.3(3) . . ? F23 P1 F26 169.7(3) . . ? F24 P1 F26 86.5(3) . . ? F21 P1 F26 84.6(3) . . ? F25 P1 F22 170.5(3) . . ? F23 P1 F22 87.6(3) . . ? F24 P1 F22 85.5(3) . . ? F21 P1 F22 85.5(3) . . ? F26 P1 F22 82.2(3) . . ? CD2 ND1 CD6 119.0(3) . . ? CD2 ND1 Ru1 125.9(3) . . ? CD6 ND1 Ru1 114.8(2) . . ? ND1 CD2 CD3 122.0(4) . . ? CD4 CD3 CD2 119.2(5) . . ? CD3 CD4 CD5 119.5(4) . . ? CD4 CD5 CD6 119.6(4) . . ? ND1 CD6 CD5 120.6(4) . . ? ND1 CD6 CC2 114.6(3) . . ? CD5 CD6 CC2 124.8(4) . . ? NC1 CC2 CC3 120.9(4) . . ? NC1 CC2 CD6 115.2(3) . . ? CC3 CC2 CD6 123.9(4) . . ? CC4 CC3 CC2 119.5(5) . . ? CC5 CC4 CC3 119.2(4) . . ? CC4 CC5 CC6 119.5(5) . . ? NC1 CC6 CC5 121.7(4) . . ? CC6 NC1 CC2 119.2(3) . . ? CC6 NC1 Ru1 125.2(3) . . ? CC2 NC1 Ru1 115.7(2) . . ? CA6 NA1 CA2 117.6(3) . . ? CA6 NA1 Ru1 127.0(3) . . ? CA2 NA1 Ru1 115.4(2) . . ? NA1 CA6 CA5 123.0(4) . . ? CA4 CA5 CA6 119.2(4) . . ? CA3 CA4 CA5 119.1(4) . . ? CA4 CA3 CA2 119.9(5) . . ? NA1 CA2 CA3 121.3(4) . . ? NA1 CA2 CB2 115.8(3) . . ? CA3 CA2 CB2 122.9(4) . . ? NB1 CB2 CB3 121.7(4) . . ? NB1 CB2 CA2 114.5(3) . . ? CB3 CB2 CA2 123.8(4) . . ? CB4 CB3 CB2 119.3(5) . . ? CB5 CB4 CB3 119.5(5) . . ? CB4 CB5 CB6 119.2(4) . . ? NB1 CB6 CB5 122.4(4) . . ? CB2 NB1 CB6 117.9(3) . . ? CB2 NB1 Ru1 116.0(2) . . ? CB6 NB1 Ru1 126.1(3) . . ? C61A C62 O63 122(2) . . ? C61B C62 O63 123(2) . . ? C64 O63 C62 109.6(15) . . ? O63 C64 C65B 112.1(15) . . ? O63 C64 C65A 104.0(12) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.196 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.094 _publ_section_references ; TeXsan, Molecular Structure Corporation (1995). Single Crystal Structure Analysis Software, Version 1.7 MSC, 3200 Research Forest Drive, The Woodlands, TX77381, USA Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #===END data_2.I _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 Cl I N4 O3 Ru S' _chemical_formula_weight 689.95 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' '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' 'S' 'S' 0.1246 0.1234 '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' 'I' 'I' -0.4742 1.8119 '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 8.1710(17) _cell_length_b 10.372(3) _cell_length_c 16.133(3) _cell_angle_alpha 79.83(2) _cell_angle_beta 76.820(18) _cell_angle_gamma 72.490(15) _cell_volume 1261.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 15.0 _exptl_crystal_description parallelopiped _exptl_crystal_colour red _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 2.066 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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_type 'Rigaku AFC7R' _diffrn_measurement_method 'omega2 scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.06 _diffrn_reflns_number 12650 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.80 _reflns_number_total 5871 _reflns_number_gt 5153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+1.3100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5871 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.39370(3) 0.32518(2) 0.287475(15) 0.02611(9) Uani 1 d . . . S1 S 0.21333(11) 0.49232(8) 0.21524(5) 0.03393(18) Uani 1 d . . . O1 O 0.1495(4) 0.6281(3) 0.2464(2) 0.0536(7) Uani 1 d . . . C1 C 0.3016(7) 0.5244(5) 0.1062(3) 0.0623(12) Uani 1 d . . . H1A H 0.3329 0.4423 0.0797 0.075 Uiso 1 calc R . . H1B H 0.4036 0.5552 0.1008 0.075 Uiso 1 calc R . . H1C H 0.2165 0.5932 0.0786 0.075 Uiso 1 calc R . . C2 C 0.0253(6) 0.4472(5) 0.2062(4) 0.0653(14) Uani 1 d . . . H2A H -0.0376 0.4256 0.2625 0.078 Uiso 1 calc R . . H2B H 0.0605 0.3695 0.1752 0.078 Uiso 1 calc R . . H2C H -0.0486 0.5222 0.1762 0.078 Uiso 1 calc R . . Cl1 Cl 0.17303(12) 0.36398(10) 0.41437(6) 0.0447(2) Uani 1 d . . . NA1 N 0.5137(4) 0.4489(3) 0.32668(18) 0.0318(5) Uani 1 d . . . CA6 C 0.5014(5) 0.5808(4) 0.3009(3) 0.0409(8) Uani 1 d . . . HA6 H 0.4373 0.6245 0.2582 0.049 Uiso 1 calc R . . CA5 C 0.5800(6) 0.6549(4) 0.3350(3) 0.0555(11) Uani 1 d . . . HA5 H 0.5702 0.7461 0.3148 0.067 Uiso 1 calc R . . CA4 C 0.6715(7) 0.5929(5) 0.3982(4) 0.0620(12) Uani 1 d . . . HA4 H 0.7230 0.6416 0.4228 0.074 Uiso 1 calc R . . CA3 C 0.6871(6) 0.4569(4) 0.4255(3) 0.0483(9) Uani 1 d . . . HA3 H 0.7488 0.4130 0.4691 0.058 Uiso 1 calc R . . CA2 C 0.6103(4) 0.3862(4) 0.3877(2) 0.0348(7) Uani 1 d . . . CB2 C 0.6337(4) 0.2389(3) 0.4079(2) 0.0336(6) Uani 1 d . . . CB3 C 0.7354(5) 0.1569(4) 0.4657(3) 0.0473(9) Uani 1 d . . . HB3 H 0.7836 0.1955 0.4988 0.057 Uiso 1 calc R . . CB4 C 0.7642(6) 0.0181(5) 0.4736(3) 0.0552(10) Uani 1 d . . . HB4 H 0.8319 -0.0380 0.5120 0.066 Uiso 1 calc R . . CB5 C 0.6927(6) -0.0369(4) 0.4245(3) 0.0555(11) Uani 1 d . . . HB5 H 0.7136 -0.1308 0.4280 0.067 Uiso 1 calc R . . CB6 C 0.5899(5) 0.0482(4) 0.3700(3) 0.0449(8) Uani 1 d . . . HB6 H 0.5399 0.0107 0.3373 0.054 Uiso 1 calc R . . NB1 N 0.5585(3) 0.1839(3) 0.36231(18) 0.0321(5) Uani 1 d . . . ND1 N 0.3067(4) 0.1774(3) 0.25311(18) 0.0326(5) Uani 1 d . . . CD6 C 0.1667(5) 0.1335(4) 0.2942(3) 0.0434(8) Uani 1 d . . . HD6 H 0.0979 0.1743 0.3420 0.052 Uiso 1 calc R . . CD5 C 0.1206(7) 0.0313(5) 0.2689(4) 0.0632(12) Uani 1 d . . . HD5 H 0.0225 0.0042 0.2987 0.076 Uiso 1 calc R . . CD4 C 0.2222(8) -0.0292(5) 0.1991(4) 0.0690(14) Uani 1 d . . . HD4 H 0.1940 -0.0984 0.1805 0.083 Uiso 1 calc R . . CD3 C 0.3672(6) 0.0129(4) 0.1562(3) 0.0537(10) Uani 1 d . . . HD3 H 0.4376 -0.0276 0.1086 0.064 Uiso 1 calc R . . CD2 C 0.4068(4) 0.1165(3) 0.1851(2) 0.0345(7) Uani 1 d . . . CC2 C 0.5604(4) 0.1673(3) 0.1457(2) 0.0331(6) Uani 1 d . . . CC3 C 0.6834(6) 0.1142(4) 0.0769(3) 0.0470(9) Uani 1 d . . . HC3 H 0.6720 0.0430 0.0528 0.056 Uiso 1 calc R . . CC4 C 0.8237(5) 0.1686(4) 0.0447(3) 0.0510(10) Uani 1 d . . . HC4 H 0.9074 0.1345 -0.0015 0.061 Uiso 1 calc R . . CC5 C 0.8384(5) 0.2735(5) 0.0815(3) 0.0500(9) Uani 1 d . . . HC5 H 0.9321 0.3109 0.0606 0.060 Uiso 1 calc R . . CC6 C 0.7124(5) 0.3223(4) 0.1497(2) 0.0416(8) Uani 1 d . . . HC6 H 0.7216 0.3940 0.1743 0.050 Uiso 1 calc R . . NC1 N 0.5763(3) 0.2693(3) 0.18200(17) 0.0311(5) Uani 1 d . . . I2 I 0.71025(4) 0.71220(3) 0.057705(18) 0.05167(11) Uani 1 d . . . O100 O -0.1536(7) 0.8540(5) 0.2151(4) 0.1047(17) Uani 1 d . . . O200 O -0.0758(5) 0.2761(4) 0.5910(2) 0.0646(8) Uani 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 Ru1 0.02648(14) 0.03086(14) 0.02437(14) -0.00124(9) -0.00778(9) -0.01166(9) S1 0.0368(4) 0.0363(4) 0.0327(4) -0.0019(3) -0.0166(3) -0.0095(3) O1 0.0621(17) 0.0427(14) 0.0585(18) -0.0142(13) -0.0320(15) 0.0021(12) C1 0.084(3) 0.062(3) 0.038(2) 0.0086(19) -0.023(2) -0.015(2) C2 0.050(2) 0.063(3) 0.096(4) 0.006(3) -0.045(3) -0.019(2) Cl1 0.0399(4) 0.0614(5) 0.0317(4) -0.0073(4) -0.0016(3) -0.0151(4) NA1 0.0327(13) 0.0340(13) 0.0340(14) -0.0041(10) -0.0111(10) -0.0132(10) CA6 0.0469(19) 0.0393(17) 0.0435(19) 0.0006(14) -0.0186(15) -0.0176(15) CA5 0.063(3) 0.0404(19) 0.076(3) -0.0032(19) -0.026(2) -0.0252(18) CA4 0.071(3) 0.058(2) 0.079(3) -0.012(2) -0.037(3) -0.030(2) CA3 0.055(2) 0.052(2) 0.051(2) -0.0060(17) -0.0301(19) -0.0176(18) CA2 0.0310(15) 0.0423(17) 0.0348(16) -0.0053(13) -0.0107(12) -0.0118(13) CB2 0.0300(14) 0.0414(16) 0.0308(15) -0.0025(13) -0.0094(12) -0.0102(12) CB3 0.047(2) 0.055(2) 0.043(2) 0.0030(17) -0.0236(17) -0.0130(17) CB4 0.053(2) 0.055(2) 0.054(2) 0.0121(19) -0.0261(19) -0.0068(18) CB5 0.062(3) 0.0348(18) 0.069(3) 0.0080(18) -0.028(2) -0.0084(17) CB6 0.050(2) 0.0368(17) 0.051(2) -0.0005(15) -0.0191(17) -0.0117(15) NB1 0.0315(13) 0.0351(13) 0.0302(13) 0.0014(10) -0.0093(10) -0.0102(10) ND1 0.0339(13) 0.0357(13) 0.0325(13) -0.0012(11) -0.0091(11) -0.0149(11) CD6 0.0393(17) 0.053(2) 0.044(2) -0.0022(16) -0.0041(15) -0.0254(16) CD5 0.063(3) 0.070(3) 0.073(3) -0.008(2) -0.005(2) -0.048(2) CD4 0.083(3) 0.067(3) 0.079(4) -0.022(3) -0.008(3) -0.050(3) CD3 0.065(3) 0.049(2) 0.058(3) -0.0188(19) -0.010(2) -0.026(2) CD2 0.0370(16) 0.0325(15) 0.0370(17) -0.0028(13) -0.0102(13) -0.0123(13) CC2 0.0331(15) 0.0349(15) 0.0317(15) -0.0013(12) -0.0075(12) -0.0100(12) CC3 0.055(2) 0.0439(19) 0.041(2) -0.0109(16) -0.0026(17) -0.0125(17) CC4 0.044(2) 0.059(2) 0.039(2) -0.0057(17) 0.0067(16) -0.0095(17) CC5 0.0380(18) 0.068(3) 0.045(2) -0.0019(18) 0.0006(15) -0.0240(18) CC6 0.0359(17) 0.055(2) 0.0385(18) -0.0039(15) -0.0029(14) -0.0237(15) NC1 0.0301(12) 0.0372(13) 0.0281(13) -0.0010(10) -0.0058(10) -0.0137(10) I2 0.04979(17) 0.05245(18) 0.05079(18) -0.00544(12) -0.00638(12) -0.01351(12) O100 0.113(4) 0.067(2) 0.146(5) -0.013(3) -0.068(4) -0.010(2) O200 0.069(2) 0.071(2) 0.057(2) -0.0144(16) -0.0096(16) -0.0210(17) _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 NC1 2.032(3) . ? Ru1 ND1 2.073(3) . ? Ru1 NA1 2.082(3) . ? Ru1 NB1 2.085(3) . ? Ru1 S1 2.2512(10) . ? Ru1 Cl1 2.4032(11) . ? S1 O1 1.482(3) . ? S1 C1 1.756(5) . ? S1 C2 1.777(4) . ? NA1 CA6 1.338(4) . ? NA1 CA2 1.354(4) . ? CA6 CA5 1.383(5) . ? CA5 CA4 1.356(7) . ? CA4 CA3 1.378(6) . ? CA3 CA2 1.384(5) . ? CA2 CB2 1.467(5) . ? CB2 NB1 1.345(4) . ? CB2 CB3 1.390(5) . ? CB3 CB4 1.375(6) . ? CB4 CB5 1.365(7) . ? CB5 CB6 1.369(5) . ? CB6 NB1 1.340(5) . ? ND1 CD2 1.341(5) . ? ND1 CD6 1.347(4) . ? CD6 CD5 1.377(6) . ? CD5 CD4 1.364(8) . ? CD4 CD3 1.380(7) . ? CD3 CD2 1.389(5) . ? CD2 CC2 1.474(5) . ? CC2 CC3 1.385(5) . ? CC2 NC1 1.348(4) . ? CC3 CC4 1.384(6) . ? CC4 CC5 1.374(7) . ? CC5 CC6 1.376(6) . ? CC6 NC1 1.347(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 NC1 Ru1 ND1 78.90(11) . . ? NC1 Ru1 NA1 97.70(11) . . ? ND1 Ru1 NA1 171.12(11) . . ? NC1 Ru1 NB1 88.43(11) . . ? ND1 Ru1 NB1 93.15(11) . . ? NA1 Ru1 NB1 78.49(11) . . ? NC1 Ru1 S1 95.16(8) . . ? ND1 Ru1 S1 91.64(8) . . ? NA1 Ru1 S1 96.85(8) . . ? NB1 Ru1 S1 174.50(8) . . ? NC1 Ru1 Cl1 173.04(8) . . ? ND1 Ru1 Cl1 94.86(8) . . ? NA1 Ru1 Cl1 88.03(9) . . ? NB1 Ru1 Cl1 88.86(8) . . ? S1 Ru1 Cl1 88.04(4) . . ? O1 S1 C1 104.5(2) . . ? O1 S1 C2 106.4(2) . . ? C1 S1 C2 99.9(3) . . ? O1 S1 Ru1 117.93(12) . . ? C1 S1 Ru1 113.63(17) . . ? C2 S1 Ru1 112.60(16) . . ? CA6 NA1 CA2 117.8(3) . . ? CA6 NA1 Ru1 127.9(2) . . ? CA2 NA1 Ru1 114.3(2) . . ? NA1 CA6 CA5 122.8(3) . . ? CA4 CA5 CA6 119.2(4) . . ? CA5 CA4 CA3 119.2(4) . . ? CA4 CA3 CA2 119.4(4) . . ? NA1 CA2 CA3 121.5(3) . . ? NA1 CA2 CB2 115.8(3) . . ? CA3 CA2 CB2 122.7(3) . . ? NB1 CB2 CB3 120.5(3) . . ? NB1 CB2 CA2 115.6(3) . . ? CB3 CB2 CA2 123.8(3) . . ? CB4 CB3 CB2 119.3(4) . . ? CB5 CB4 CB3 119.6(4) . . ? CB6 CB5 CB4 119.0(4) . . ? NB1 CB6 CB5 122.3(4) . . ? CB6 NB1 CB2 119.2(3) . . ? CB6 NB1 Ru1 126.2(2) . . ? CB2 NB1 Ru1 114.6(2) . . ? CD2 ND1 CD6 117.9(3) . . ? CD2 ND1 Ru1 115.3(2) . . ? CD6 ND1 Ru1 126.7(3) . . ? ND1 CD6 CD5 123.3(4) . . ? CD4 CD5 CD6 118.4(4) . . ? CD3 CD4 CD5 119.5(4) . . ? CD4 CD3 CD2 119.2(4) . . ? ND1 CD2 CD3 121.6(3) . . ? ND1 CD2 CC2 114.4(3) . . ? CD3 CD2 CC2 123.9(4) . . ? CC3 CC2 CD2 123.4(3) . . ? CC3 CC2 NC1 121.2(3) . . ? CD2 CC2 NC1 115.5(3) . . ? CC2 CC3 CC4 119.0(4) . . ? CC5 CC4 CC3 119.6(4) . . ? CC4 CC5 CC6 119.0(4) . . ? NC1 CC6 CC5 121.9(4) . . ? CC6 NC1 CC2 119.4(3) . . ? CC6 NC1 Ru1 124.8(2) . . ? CC2 NC1 Ru1 115.8(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.80 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.407 _refine_diff_density_min -1.779 _refine_diff_density_rms 0.136 #===END