Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Sylviane Sabo-Etienne' 'Isabelle Atheaux' 'Jean-Claude Barthelat' 'Bruno Chaudret' 'Bruno Donnadieu' 'Mary Grellier' 'Khansaa Hussein' 'Ridha Ben Said' _publ_contact_author_name 'Dr Sylviane Sabo-Etienne' _publ_contact_author_address ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; _publ_contact_author_email sabo@lcc-toulouse.fr _publ_requested_journal 'Dalton Transactions.' _publ_section_title ; Redistribution at silicon by ruthenium complexes. Bonding Mode of the Bridging Silanes in Ru2H4(m-h2:h2:h2:h2-SiH4)(PCy3)4 and Ru2H2(m-h2:h2-H2Si(OMe)2)3(PCy3)2. ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. DIFABS - N. Walker and D. Stuart, Acta Crystallogr., Sect A 1983, 39, 158-166. Farrugia, L. J., ORTEP3 for Windows, J. Appl. Crystallogr. 1997, 30, 565. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. ; #**************************************************************************** data_(2) _database_code_CSD 208492 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H132 P4 Ru2 Si' _chemical_formula_weight 1351.89 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y, -z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 15.831(2) _cell_length_b 19.063(2) _cell_length_c 24.035(3) _cell_angle_alpha 90.058(15) _cell_angle_beta 90.030(17) _cell_angle_gamma 90.098(16) _cell_volume 7253.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 24.1 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type none _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 80 mm. 313 frames (2 min per frame) were obtained with 0 < \f < 200.2\% and with the crystals rotated through 1.3\% in \f. Coverage of the unique set was over 98.7% complete to at least 20.82\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 160(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 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 29110 _diffrn_reflns_av_R_equivalents 0.4025 _diffrn_reflns_av_sigmaI/netI 0.2991 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 20.82 _reflns_number_total 3755 _reflns_number_gt 1324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _computing_corr_abs DIFABS _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3755 _refine_ls_number_parameters 357 _refine_ls_number_restraints 288 _refine_ls_R_factor_all 0.2334 _refine_ls_R_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.2128 _refine_ls_wR_factor_gt 0.1595 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.838 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.58513(9) 0.12012(9) 0.67755(6) 0.0509(5) Uani 1 1 d . . . Si1 Si 0.5000 0.1163(5) 0.7500 0.0467(17) Uani 1 2 d S . . P1 P 0.5001(3) 0.1759(3) 0.61377(18) 0.0483(13) Uani 1 1 d . . . P2 P 0.7098(3) 0.0590(3) 0.69259(19) 0.0577(15) Uani 1 1 d . . . C111 C 0.4247(13) 0.2487(10) 0.6356(7) 0.054(5) Uani 1 1 d U . . H111 H 0.3790 0.2250 0.6574 0.065 Uiso 1 1 calc R . . C112 C 0.4704(15) 0.2993(13) 0.6781(11) 0.102(7) Uani 1 1 d U . . H11A H 0.5003 0.2717 0.7069 0.123 Uiso 1 1 calc R . . H11B H 0.5122 0.3290 0.6584 0.123 Uiso 1 1 calc R . . C113 C 0.4017(19) 0.3452(13) 0.7050(10) 0.119(9) Uani 1 1 d U . . H11C H 0.4275 0.3777 0.7323 0.143 Uiso 1 1 calc R . . H11D H 0.3603 0.3153 0.7248 0.143 Uiso 1 1 calc R . . C114 C 0.3560(14) 0.3879(14) 0.6582(7) 0.085(7) Uani 1 1 d U . . H11E H 0.3123 0.4183 0.6750 0.102 Uiso 1 1 calc R . . H11F H 0.3975 0.4184 0.6390 0.102 Uiso 1 1 calc R . . C115 C 0.3154(13) 0.3388(11) 0.6164(8) 0.068(6) Uani 1 1 d U . . H11G H 0.2901 0.3663 0.5857 0.082 Uiso 1 1 calc R . . H11H H 0.2697 0.3118 0.6347 0.082 Uiso 1 1 calc R . . C116 C 0.3818(11) 0.2882(11) 0.5930(7) 0.053(5) Uani 1 1 d U . . H11I H 0.3539 0.2551 0.5670 0.064 Uiso 1 1 calc R . . H11J H 0.4240 0.3154 0.5715 0.064 Uiso 1 1 calc R . . C121 C 0.4266(13) 0.1175(12) 0.5789(6) 0.063(5) Uani 1 1 d U . . H121 H 0.3917 0.1486 0.5546 0.076 Uiso 1 1 calc R . . C122 C 0.3629(15) 0.0811(14) 0.6175(8) 0.086(7) Uani 1 1 d U . . H12A H 0.3932 0.0443 0.6387 0.104 Uiso 1 1 calc R . . H12B H 0.3422 0.1160 0.6447 0.104 Uiso 1 1 calc R . . C123 C 0.287(2) 0.0474(18) 0.5894(12) 0.129(10) Uani 1 1 d U . . H12C H 0.2527 0.0215 0.6171 0.155 Uiso 1 1 calc R . . H12D H 0.2508 0.0840 0.5724 0.155 Uiso 1 1 calc R . . C124 C 0.317(2) -0.0010(19) 0.5462(14) 0.137(11) Uani 1 1 d U . . H12E H 0.2691 -0.0219 0.5259 0.165 Uiso 1 1 calc R . . H12F H 0.3504 -0.0394 0.5634 0.165 Uiso 1 1 calc R . . C125 C 0.374(2) 0.041(2) 0.5057(13) 0.158(12) Uani 1 1 d U . . H12G H 0.3448 0.0846 0.4933 0.190 Uiso 1 1 calc R . . H12H H 0.3885 0.0130 0.4726 0.190 Uiso 1 1 calc R . . C126 C 0.458(2) 0.0606(18) 0.5413(11) 0.131(9) Uani 1 1 d U . . H12I H 0.4782 0.0197 0.5627 0.157 Uiso 1 1 calc R . . H12J H 0.5039 0.0777 0.5169 0.157 Uiso 1 1 calc R . . C131 C 0.5605(12) 0.2135(14) 0.5534(8) 0.074(7) Uani 1 1 d U . . H131 H 0.6019 0.1753 0.5453 0.089 Uiso 1 1 calc R . . C132 C 0.5251(19) 0.226(2) 0.4996(10) 0.138(10) Uani 1 1 d U . . H13A H 0.4974 0.2728 0.4988 0.166 Uiso 1 1 calc R . . H13B H 0.4824 0.1901 0.4905 0.166 Uiso 1 1 calc R . . C133 C 0.602(2) 0.224(2) 0.4544(11) 0.155(11) Uani 1 1 d U . . H13C H 0.6308 0.1778 0.4554 0.187 Uiso 1 1 calc R . . H13D H 0.5805 0.2319 0.4163 0.187 Uiso 1 1 calc R . . C134 C 0.666(2) 0.284(2) 0.4712(14) 0.185(14) Uani 1 1 d U . . H13E H 0.7218 0.2714 0.4561 0.222 Uiso 1 1 calc R . . H13F H 0.6474 0.3273 0.4524 0.222 Uiso 1 1 calc R . . C135 C 0.674(2) 0.297(2) 0.5227(12) 0.180(13) Uani 1 1 d U . . H13G H 0.6750 0.3489 0.5258 0.216 Uiso 1 1 calc R . . H13H H 0.7317 0.2811 0.5327 0.216 Uiso 1 1 calc R . . C136 C 0.6162(15) 0.2714(16) 0.5699(9) 0.096(8) Uani 1 1 d U . . H13I H 0.6516 0.2560 0.6015 0.116 Uiso 1 1 calc R . . H13J H 0.5811 0.3111 0.5828 0.116 Uiso 1 1 calc R . . C211 C 0.7770(12) 0.0851(12) 0.7543(8) 0.057(5) Uani 1 1 d U . . H211 H 0.7464 0.0684 0.7882 0.068 Uiso 1 1 calc R . . C212 C 0.8661(13) 0.0524(13) 0.7566(7) 0.074(6) Uani 1 1 d U . . H21A H 0.8621 0.0011 0.7509 0.088 Uiso 1 1 calc R . . H21B H 0.9017 0.0723 0.7267 0.088 Uiso 1 1 calc R . . C213 C 0.9063(15) 0.0679(12) 0.8138(8) 0.084(7) Uani 1 1 d U . . H21C H 0.9623 0.0451 0.8168 0.100 Uiso 1 1 calc R . . H21D H 0.8697 0.0504 0.8442 0.100 Uiso 1 1 calc R . . C214 C 0.9153(15) 0.1487(12) 0.8171(9) 0.084(6) Uani 1 1 d U . . H21E H 0.9506 0.1655 0.7858 0.101 Uiso 1 1 calc R . . H21F H 0.9437 0.1618 0.8523 0.101 Uiso 1 1 calc R . . C215 C 0.8268(13) 0.1837(12) 0.8143(8) 0.072(6) Uani 1 1 d U . . H21G H 0.7916 0.1665 0.8455 0.086 Uiso 1 1 calc R . . H21H H 0.8331 0.2351 0.8183 0.086 Uiso 1 1 calc R . . C216 C 0.7832(13) 0.1672(12) 0.7595(8) 0.067(6) Uani 1 1 d U . . H21I H 0.8161 0.1867 0.7280 0.081 Uiso 1 1 calc R . . H21J H 0.7260 0.1882 0.7588 0.081 Uiso 1 1 calc R . . C221 C 0.6984(12) -0.0367(10) 0.7020(7) 0.053(5) Uani 1 1 d U . . H221 H 0.7565 -0.0565 0.7063 0.063 Uiso 1 1 calc R . . C222 C 0.6480(13) -0.0558(12) 0.7557(8) 0.071(6) Uani 1 1 d U . . H22A H 0.6777 -0.0372 0.7888 0.086 Uiso 1 1 calc R . . H22B H 0.5911 -0.0343 0.7542 0.086 Uiso 1 1 calc R . . C223 C 0.6397(13) -0.1352(13) 0.7602(9) 0.082(7) Uani 1 1 d U . . H22C H 0.6962 -0.1561 0.7659 0.099 Uiso 1 1 calc R . . H22D H 0.6043 -0.1472 0.7928 0.099 Uiso 1 1 calc R . . C224 C 0.6019(14) -0.1641(13) 0.7105(9) 0.082(6) Uani 1 1 d U . . H22E H 0.5445 -0.1442 0.7066 0.098 Uiso 1 1 calc R . . H22F H 0.5956 -0.2154 0.7157 0.098 Uiso 1 1 calc R . . C225 C 0.6498(13) -0.1515(13) 0.6557(9) 0.075(7) Uani 1 1 d U . . H22G H 0.7064 -0.1736 0.6567 0.090 Uiso 1 1 calc R . . H22H H 0.6178 -0.1703 0.6236 0.090 Uiso 1 1 calc R . . C226 C 0.6565(14) -0.0751(14) 0.6529(9) 0.073(6) Uani 1 1 d U . . H22I H 0.5988 -0.0560 0.6484 0.088 Uiso 1 1 calc R . . H22J H 0.6884 -0.0631 0.6188 0.088 Uiso 1 1 calc R . . C231 C 0.7795(13) 0.0591(11) 0.6279(7) 0.057(5) Uani 1 1 d U . . H231 H 0.7402 0.0520 0.5958 0.068 Uiso 1 1 calc R . . C232 C 0.8491(12) -0.0009(13) 0.6223(8) 0.073(6) Uani 1 1 d U . . H23A H 0.8941 0.0059 0.6505 0.087 Uiso 1 1 calc R . . H23B H 0.8232 -0.0476 0.6280 0.087 Uiso 1 1 calc R . . C233 C 0.8865(12) 0.0046(16) 0.5628(8) 0.078(6) Uani 1 1 d U . . H23C H 0.9312 -0.0313 0.5585 0.093 Uiso 1 1 calc R . . H23D H 0.8415 -0.0060 0.5355 0.093 Uiso 1 1 calc R . . C234 C 0.9236(14) 0.0759(13) 0.5499(8) 0.073(6) Uani 1 1 d U . . H23E H 0.9435 0.0769 0.5109 0.088 Uiso 1 1 calc R . . H23F H 0.9728 0.0848 0.5745 0.088 Uiso 1 1 calc R . . C235 C 0.8562(11) 0.1342(13) 0.5589(7) 0.065(6) Uani 1 1 d U . . H23G H 0.8820 0.1810 0.5530 0.078 Uiso 1 1 calc R . . H23H H 0.8096 0.1283 0.5318 0.078 Uiso 1 1 calc R . . C236 C 0.8225(12) 0.1288(14) 0.6175(7) 0.070(6) Uani 1 1 d U . . H23I H 0.7817 0.1672 0.6240 0.084 Uiso 1 1 calc R . . H23J H 0.8697 0.1346 0.6441 0.084 Uiso 1 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 Ru1 0.0507(7) 0.0584(10) 0.0437(7) 0.0076(10) 0.0094(8) 0.0122(11) Si1 0.053(4) 0.043(5) 0.045(3) 0.000 0.003(3) 0.000 P1 0.042(3) 0.056(4) 0.046(3) 0.000(3) 0.010(2) 0.009(3) P2 0.056(3) 0.069(4) 0.047(3) 0.009(3) 0.006(2) 0.012(3) C111 0.057(12) 0.048(13) 0.058(10) -0.006(9) 0.002(10) 0.020(10) C112 0.098(15) 0.107(19) 0.101(14) -0.031(16) -0.045(14) 0.048(13) C113 0.16(2) 0.090(19) 0.106(15) -0.044(13) -0.041(16) 0.069(16) C114 0.118(16) 0.082(18) 0.055(11) -0.005(12) -0.039(10) 0.035(14) C115 0.073(13) 0.069(15) 0.063(12) 0.007(11) -0.013(10) 0.038(11) C116 0.052(11) 0.061(14) 0.046(10) -0.004(9) 0.007(8) 0.020(9) C121 0.096(13) 0.056(12) 0.037(8) -0.001(10) 0.015(9) -0.022(13) C122 0.091(15) 0.12(2) 0.046(11) -0.012(12) 0.008(11) -0.014(13) C123 0.15(2) 0.12(2) 0.120(19) -0.005(17) -0.001(17) -0.051(19) C124 0.14(2) 0.11(3) 0.16(2) -0.065(19) 0.040(19) -0.018(19) C125 0.16(2) 0.19(3) 0.12(2) -0.09(2) 0.002(17) -0.07(2) C126 0.15(2) 0.16(2) 0.087(16) -0.031(17) 0.022(15) 0.012(18) C131 0.057(14) 0.108(19) 0.057(11) 0.044(12) -0.021(9) -0.009(12) C132 0.13(2) 0.20(3) 0.081(15) 0.038(18) 0.011(14) -0.032(19) C133 0.18(3) 0.19(3) 0.100(16) 0.000(18) 0.108(18) -0.05(2) C134 0.18(3) 0.23(3) 0.15(2) -0.04(2) 0.16(2) -0.08(2) C135 0.19(3) 0.24(3) 0.111(19) 0.07(2) 0.05(2) -0.12(2) C136 0.087(17) 0.13(2) 0.068(13) 0.036(14) -0.010(11) -0.026(15) C211 0.048(11) 0.081(15) 0.040(10) 0.019(10) -0.029(9) -0.006(11) C212 0.080(13) 0.091(17) 0.051(11) -0.006(11) -0.021(10) 0.047(12) C213 0.079(14) 0.102(17) 0.069(12) 0.005(13) -0.023(12) 0.064(15) C214 0.083(12) 0.107(16) 0.062(11) -0.010(12) 0.001(13) 0.022(14) C215 0.079(13) 0.072(15) 0.064(12) 0.004(12) -0.003(11) -0.001(11) C216 0.060(13) 0.074(16) 0.068(13) 0.009(13) 0.019(11) -0.007(13) C221 0.052(11) 0.044(14) 0.062(10) -0.001(9) 0.019(9) -0.004(9) C222 0.067(13) 0.082(16) 0.065(12) 0.023(12) 0.009(10) 0.012(11) C223 0.068(13) 0.091(18) 0.088(13) 0.041(14) 0.012(10) 0.028(13) C224 0.062(15) 0.084(16) 0.100(14) 0.003(12) -0.011(12) -0.008(12) C225 0.046(12) 0.085(17) 0.095(14) -0.007(13) 0.000(10) -0.006(12) C226 0.061(13) 0.079(17) 0.080(13) 0.002(13) 0.007(11) 0.000(13) C231 0.065(13) 0.078(16) 0.029(9) -0.009(9) 0.009(8) 0.009(11) C232 0.052(12) 0.095(17) 0.072(12) 0.003(12) 0.014(10) 0.023(11) C233 0.056(13) 0.115(18) 0.062(13) -0.006(13) 0.010(10) 0.005(14) C234 0.046(12) 0.113(18) 0.060(11) -0.021(11) 0.008(11) -0.011(12) C235 0.053(11) 0.093(18) 0.048(9) -0.012(11) 0.004(8) -0.009(11) C236 0.053(11) 0.096(17) 0.061(11) -0.004(13) 0.026(9) -0.011(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 Si1 2.2037(14) . ? Ru1 P1 2.302(5) . ? Ru1 P2 2.322(5) . ? Si1 Ru1 2.2037(14) 7_657 ? P1 C121 1.81(2) . ? P1 C131 1.88(2) . ? P1 C111 1.907(18) . ? P2 C221 1.85(2) . ? P2 C211 1.891(17) . ? P2 C231 1.906(17) . ? C111 C116 1.44(2) . ? C111 C112 1.58(3) . ? C112 C113 1.54(3) . ? C113 C114 1.57(3) . ? C114 C115 1.51(3) . ? C115 C116 1.54(2) . ? C121 C126 1.50(3) . ? C121 C122 1.54(3) . ? C122 C123 1.52(3) . ? C123 C124 1.47(4) . ? C124 C125 1.55(4) . ? C125 C126 1.62(4) . ? C131 C132 1.43(3) . ? C131 C136 1.46(3) . ? C132 C133 1.64(3) . ? C133 C134 1.57(4) . ? C134 C135 1.27(4) . ? C135 C136 1.54(3) . ? C211 C212 1.54(3) . ? C211 C216 1.57(3) . ? C212 C213 1.54(3) . ? C213 C214 1.55(3) . ? C214 C215 1.55(3) . ? C215 C216 1.52(3) . ? C221 C226 1.54(3) . ? C221 C222 1.56(2) . ? C222 C223 1.52(3) . ? C223 C224 1.44(3) . ? C224 C225 1.54(3) . ? C225 C226 1.46(3) . ? C231 C236 1.51(3) . ? C231 C232 1.60(3) . ? C232 C233 1.55(3) . ? C233 C234 1.51(3) . ? C234 C235 1.56(3) . ? C235 C236 1.51(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 Si1 Ru1 P1 100.59(17) . . ? Si1 Ru1 P2 112.37(19) . . ? P1 Ru1 P2 146.48(17) . . ? Ru1 Si1 Ru1 176.2(5) . 7_657 ? C121 P1 C131 101.8(9) . . ? C121 P1 C111 99.9(10) . . ? C131 P1 C111 104.7(10) . . ? C121 P1 Ru1 113.5(8) . . ? C131 P1 Ru1 113.1(6) . . ? C111 P1 Ru1 121.4(5) . . ? C221 P2 C211 102.6(9) . . ? C221 P2 C231 99.1(9) . . ? C211 P2 C231 108.3(9) . . ? C221 P2 Ru1 115.7(6) . . ? C211 P2 Ru1 117.9(7) . . ? C231 P2 Ru1 111.4(6) . . ? C116 C111 C112 110.9(17) . . ? C116 C111 P1 118.7(12) . . ? C112 C111 P1 109.6(13) . . ? C113 C112 C111 107.1(18) . . ? C112 C113 C114 108.7(19) . . ? C115 C114 C113 110(2) . . ? C114 C115 C116 109.9(17) . . ? C111 C116 C115 113.0(14) . . ? C126 C121 C122 105(2) . . ? C126 C121 P1 120.7(18) . . ? C122 C121 P1 114.8(11) . . ? C123 C122 C121 116.1(18) . . ? C124 C123 C122 108(3) . . ? C123 C124 C125 108(3) . . ? C124 C125 C126 105(3) . . ? C121 C126 C125 102(2) . . ? C132 C131 C136 110(2) . . ? C132 C131 P1 124.4(17) . . ? C136 C131 P1 112.6(15) . . ? C131 C132 C133 108(3) . . ? C134 C133 C132 107(2) . . ? C135 C134 C133 118(3) . . ? C134 C135 C136 126(3) . . ? C131 C136 C135 114(2) . . ? C212 C211 C216 110.1(19) . . ? C212 C211 P2 115.8(15) . . ? C216 C211 P2 111.0(13) . . ? C213 C212 C211 109.4(16) . . ? C212 C213 C214 105.8(18) . . ? C213 C214 C215 110(2) . . ? C216 C215 C214 111.0(18) . . ? C215 C216 C211 107.5(18) . . ? C226 C221 C222 107.7(15) . . ? C226 C221 P2 114.6(14) . . ? C222 C221 P2 112.4(13) . . ? C223 C222 C221 109.5(17) . . ? C224 C223 C222 110.7(18) . . ? C223 C224 C225 116.4(18) . . ? C226 C225 C224 103(2) . . ? C225 C226 C221 118(2) . . ? C236 C231 C232 107.7(17) . . ? C236 C231 P2 113.4(13) . . ? C232 C231 P2 117.9(13) . . ? C233 C232 C231 107.1(17) . . ? C234 C233 C232 113(2) . . ? C233 C234 C235 110.4(18) . . ? C236 C235 C234 108.8(18) . . ? C235 C236 C231 112.0(18) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.685 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.105 #====END data_(3) _database_code_CSD 208493 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H84 O6 P2 Ru2 Si3' _chemical_formula_weight 1033.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Ru Ru -1.2594 0.8363 '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 9.8062(12) _cell_length_b 14.959(2) _cell_length_c 18.710(3) _cell_angle_alpha 93.103(17) _cell_angle_beta 99.303(16) _cell_angle_gamma 99.352(16) _cell_volume 2663.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.0 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.267 _exptl_absorpt_correction_T_max 0.719 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 167 frames (5 min per frame) were obtained with 0 < \f < 250.5\% and with the crystals rotated through 1.5\% in \f. Coverage of the unique set was over 95.6% complete to at least 21.49\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 180(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 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 16046 _diffrn_reflns_av_R_equivalents 0.1070 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 21.49 _reflns_number_total 5827 _reflns_number_gt 4210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1356P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5827 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0882 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1774 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.70789(7) 0.49775(4) 0.74606(4) 0.0285(3) Uani 1 1 d . . . Ru2 Ru 0.59570(7) 0.31687(4) 0.77280(3) 0.0264(3) Uani 1 1 d . . . P1 P 0.7989(2) 0.64974(14) 0.73656(12) 0.0274(6) Uani 1 1 d . . . P2 P 0.5059(2) 0.16899(14) 0.79497(11) 0.0242(5) Uani 1 1 d . . . Si1 Si 0.6816(3) 0.35810(18) 0.66606(15) 0.0459(8) Uani 1 1 d . . . Si2 Si 0.4644(3) 0.43814(17) 0.74565(15) 0.0401(7) Uani 1 1 d . . . Si3 Si 0.7789(3) 0.4229(2) 0.84964(16) 0.0465(8) Uani 1 1 d . . . O11 O 0.5789(9) 0.3482(5) 0.5865(3) 0.056(2) Uani 1 1 d . . . O12 O 0.8135(9) 0.3146(5) 0.6429(4) 0.061(2) Uani 1 1 d . . . O21 O 0.3368(8) 0.4064(5) 0.6750(4) 0.059(2) Uani 1 1 d . . . O22 O 0.3991(7) 0.4992(4) 0.8021(4) 0.0507(19) Uani 1 1 d . . . O31 O 0.9316(9) 0.3898(6) 0.8650(5) 0.078(3) Uani 1 1 d . . . O32 O 0.7753(9) 0.4710(5) 0.9303(4) 0.057(2) Uani 1 1 d . . . C11 C 0.6230(18) 0.3921(10) 0.5268(6) 0.088(5) Uani 1 1 d . . . H11A H 0.6691 0.4547 0.5431 0.132 Uiso 1 1 calc R . . H11B H 0.5413 0.3928 0.4891 0.132 Uiso 1 1 calc R . . H11C H 0.6890 0.3593 0.5070 0.132 Uiso 1 1 calc R . . C12 C 0.9496(13) 0.3218(10) 0.6889(7) 0.076(4) Uani 1 1 d . . . H12A H 0.9724 0.3805 0.7179 0.114 Uiso 1 1 calc R . . H12B H 1.0212 0.3174 0.6585 0.114 Uiso 1 1 calc R . . H12C H 0.9472 0.2725 0.7213 0.114 Uiso 1 1 calc R . . C21 C 0.2901(17) 0.4601(12) 0.6220(9) 0.114(7) Uani 1 1 d . . . H21A H 0.3426 0.5222 0.6329 0.171 Uiso 1 1 calc R . . H21B H 0.1900 0.4606 0.6208 0.171 Uiso 1 1 calc R . . H21C H 0.3046 0.4356 0.5747 0.171 Uiso 1 1 calc R . . C22 C 0.2643(15) 0.4708(9) 0.8174(8) 0.080(4) Uani 1 1 d . . . H22A H 0.1955 0.4640 0.7724 0.120 Uiso 1 1 calc R . . H22B H 0.2426 0.5163 0.8516 0.120 Uiso 1 1 calc R . . H22C H 0.2604 0.4124 0.8390 0.120 Uiso 1 1 calc R . . C31 C 1.0059(17) 0.3756(14) 0.9280(7) 0.108(6) Uani 1 1 d . . . H31A H 1.0425 0.4339 0.9566 0.163 Uiso 1 1 calc R . . H31B H 1.0843 0.3460 0.9190 0.163 Uiso 1 1 calc R . . H31C H 0.9458 0.3365 0.9550 0.163 Uiso 1 1 calc R . . C32 C 0.6571(14) 0.4965(9) 0.9530(6) 0.066(3) Uani 1 1 d . . . H32A H 0.6249 0.5433 0.9231 0.099 Uiso 1 1 calc R . . H32B H 0.6813 0.5207 1.0041 0.099 Uiso 1 1 calc R . . H32C H 0.5821 0.4433 0.9479 0.099 Uiso 1 1 calc R . . C111 C 0.8672(9) 0.6687(6) 0.6504(5) 0.030(2) Uani 1 1 d . . . H111 H 0.7852 0.6433 0.6116 0.036 Uiso 1 1 calc R . . C112 C 0.9080(11) 0.7675(6) 0.6329(5) 0.038(2) Uani 1 1 d . . . H11D H 0.8324 0.8018 0.6404 0.045 Uiso 1 1 calc R . . H11E H 0.9948 0.7966 0.6662 0.045 Uiso 1 1 calc R . . C113 C 0.9314(12) 0.7703(7) 0.5547(5) 0.049(3) Uani 1 1 d . . . H11F H 0.9644 0.8340 0.5454 0.059 Uiso 1 1 calc R . . H11G H 0.8409 0.7486 0.5218 0.059 Uiso 1 1 calc R . . C114 C 1.0388(12) 0.7120(7) 0.5369(6) 0.051(3) Uani 1 1 d . . . H11H H 1.0406 0.7100 0.4841 0.061 Uiso 1 1 calc R . . H11I H 1.1334 0.7404 0.5629 0.061 Uiso 1 1 calc R . . C115 C 1.0048(12) 0.6179(7) 0.5583(5) 0.046(3) Uani 1 1 d . . . H11J H 1.0833 0.5855 0.5524 0.055 Uiso 1 1 calc R . . H11K H 0.9201 0.5855 0.5251 0.055 Uiso 1 1 calc R . . C116 C 0.9788(10) 0.6143(6) 0.6366(5) 0.035(2) Uani 1 1 d . . . H11L H 0.9491 0.5503 0.6463 0.042 Uiso 1 1 calc R . . H11M H 1.0672 0.6387 0.6704 0.042 Uiso 1 1 calc R . . C121 C 0.6686(10) 0.7273(6) 0.7359(5) 0.033(2) Uani 1 1 d . . . H121 H 0.7208 0.7908 0.7372 0.040 Uiso 1 1 calc R . . C122 C 0.5989(11) 0.7217(6) 0.8018(5) 0.042(3) Uani 1 1 d . . . H12D H 0.6717 0.7360 0.8460 0.050 Uiso 1 1 calc R . . H12E H 0.5495 0.6587 0.8029 0.050 Uiso 1 1 calc R . . C123 C 0.4950(12) 0.7863(7) 0.8027(6) 0.053(3) Uani 1 1 d . . . H12F H 0.5451 0.8498 0.8057 0.064 Uiso 1 1 calc R . . H12G H 0.4497 0.7787 0.8461 0.064 Uiso 1 1 calc R . . C124 C 0.3834(12) 0.7677(7) 0.7345(7) 0.056(3) Uani 1 1 d . . . H12H H 0.3279 0.7061 0.7335 0.067 Uiso 1 1 calc R . . H12I H 0.3188 0.8122 0.7348 0.067 Uiso 1 1 calc R . . C125 C 0.4513(11) 0.7750(7) 0.6675(6) 0.043(3) Uani 1 1 d . . . H12J H 0.5001 0.8382 0.6666 0.052 Uiso 1 1 calc R . . H12K H 0.3778 0.7607 0.6236 0.052 Uiso 1 1 calc R . . C126 C 0.5556(10) 0.7109(6) 0.6661(5) 0.038(2) Uani 1 1 d . . . H12L H 0.6017 0.7198 0.6230 0.045 Uiso 1 1 calc R . . H12M H 0.5052 0.6473 0.6617 0.045 Uiso 1 1 calc R . . C131 C 0.9387(13) 0.7012(6) 0.8137(7) 0.065(4) Uani 1 1 d . . . H131 H 0.8963 0.6811 0.8565 0.077 Uiso 1 1 calc R . . C132 C 1.0610(14) 0.6663(8) 0.8238(8) 0.078(4) Uani 1 1 d . . . H13A H 1.1145 0.6855 0.7850 0.094 Uiso 1 1 calc R . . H13B H 1.0370 0.5992 0.8181 0.094 Uiso 1 1 calc R . . C133 C 1.1589(13) 0.6960(8) 0.9000(7) 0.067(4) Uani 1 1 d . . . H13C H 1.1164 0.6644 0.9383 0.080 Uiso 1 1 calc R . . H13D H 1.2513 0.6777 0.8992 0.080 Uiso 1 1 calc R . . C134 C 1.1790(14) 0.7975(8) 0.9175(7) 0.067(4) Uani 1 1 d . . . H13E H 1.2138 0.8109 0.9703 0.081 Uiso 1 1 calc R . . H13F H 1.2530 0.8270 0.8920 0.081 Uiso 1 1 calc R . . C135 C 1.066(2) 0.8353(10) 0.9002(11) 0.154(11) Uani 1 1 d . . . H13G H 1.0987 0.9016 0.9012 0.185 Uiso 1 1 calc R . . H13H H 1.0106 0.8257 0.9398 0.185 Uiso 1 1 calc R . . C136 C 0.9640(12) 0.8062(6) 0.8281(6) 0.054(3) Uani 1 1 d . . . H13I H 1.0039 0.8348 0.7878 0.065 Uiso 1 1 calc R . . H13J H 0.8738 0.8268 0.8306 0.065 Uiso 1 1 calc R . . C211 C 0.3724(9) 0.1121(5) 0.7173(5) 0.028(2) Uani 1 1 d . . . H211 H 0.4209 0.1186 0.6743 0.034 Uiso 1 1 calc R . . C212 C 0.2477(10) 0.1600(7) 0.6993(6) 0.044(3) Uani 1 1 d . . . H21D H 0.2810 0.2259 0.6983 0.053 Uiso 1 1 calc R . . H21E H 0.1882 0.1515 0.7372 0.053 Uiso 1 1 calc R . . C213 C 0.1606(12) 0.1210(7) 0.6245(6) 0.055(3) Uani 1 1 d . . . H21F H 0.0759 0.1495 0.6151 0.066 Uiso 1 1 calc R . . H21G H 0.2169 0.1367 0.5861 0.066 Uiso 1 1 calc R . . C214 C 0.1162(11) 0.0183(7) 0.6204(6) 0.047(3) Uani 1 1 d . . . H21H H 0.0464 0.0031 0.6525 0.057 Uiso 1 1 calc R . . H21I H 0.0709 -0.0042 0.5700 0.057 Uiso 1 1 calc R . . C215 C 0.2398(11) -0.0293(6) 0.6428(5) 0.038(2) Uani 1 1 d . . . H21J H 0.3026 -0.0220 0.6063 0.046 Uiso 1 1 calc R . . H21K H 0.2052 -0.0951 0.6439 0.046 Uiso 1 1 calc R . . C216 C 0.3225(10) 0.0086(6) 0.7172(5) 0.033(2) Uani 1 1 d . . . H21L H 0.4047 -0.0219 0.7291 0.040 Uiso 1 1 calc R . . H21M H 0.2627 -0.0034 0.7546 0.040 Uiso 1 1 calc R . . C221 C 0.6361(9) 0.0926(5) 0.8055(4) 0.024(2) Uani 1 1 d . . . H221 H 0.5878 0.0324 0.8173 0.029 Uiso 1 1 calc R . . C222 C 0.6943(10) 0.0770(6) 0.7346(5) 0.035(2) Uani 1 1 d . . . H22D H 0.6162 0.0486 0.6956 0.042 Uiso 1 1 calc R . . H22E H 0.7358 0.1363 0.7195 0.042 Uiso 1 1 calc R . . C223 C 0.8058(11) 0.0159(7) 0.7441(6) 0.046(3) Uani 1 1 d . . . H22F H 0.7617 -0.0460 0.7529 0.056 Uiso 1 1 calc R . . H22G H 0.8456 0.0114 0.6990 0.056 Uiso 1 1 calc R . . C224 C 0.9235(11) 0.0534(7) 0.8077(6) 0.049(3) Uani 1 1 d . . . H22H H 0.9925 0.0117 0.8136 0.059 Uiso 1 1 calc R . . H22I H 0.9725 0.1132 0.7972 0.059 Uiso 1 1 calc R . . C225 C 0.8665(11) 0.0640(7) 0.8771(6) 0.051(3) Uani 1 1 d . . . H22J H 0.9444 0.0887 0.9173 0.061 Uiso 1 1 calc R . . H22K H 0.8216 0.0037 0.8891 0.061 Uiso 1 1 calc R . . C226 C 0.7578(10) 0.1284(7) 0.8692(5) 0.040(2) Uani 1 1 d . . . H22L H 0.8042 0.1897 0.8604 0.048 Uiso 1 1 calc R . . H22M H 0.7199 0.1335 0.9149 0.048 Uiso 1 1 calc R . . C231 C 0.4302(12) 0.1592(6) 0.8798(5) 0.040(3) Uani 1 1 d . . . H231 H 0.5227 0.1747 0.9132 0.048 Uiso 1 1 calc R . . C232 C 0.3926(11) 0.0669(6) 0.9055(5) 0.037(2) Uani 1 1 d . . . H23A H 0.3154 0.0313 0.8692 0.044 Uiso 1 1 calc R . . H23B H 0.4746 0.0357 0.9072 0.044 Uiso 1 1 calc R . . C233 C 0.3488(18) 0.0656(8) 0.9775(7) 0.078(4) Uani 1 1 d . . . H23C H 0.2838 0.0076 0.9776 0.093 Uiso 1 1 calc R . . H23D H 0.4333 0.0634 1.0139 0.093 Uiso 1 1 calc R . . C234 C 0.285(2) 0.1345(9) 1.0030(8) 0.103(6) Uani 1 1 d . . . H23E H 0.3036 0.1385 1.0567 0.124 Uiso 1 1 calc R . . H23F H 0.1822 0.1168 0.9872 0.124 Uiso 1 1 calc R . . C235 C 0.3285(16) 0.2257(7) 0.9795(6) 0.063(4) Uani 1 1 d . . . H23G H 0.2490 0.2592 0.9780 0.076 Uiso 1 1 calc R . . H23H H 0.4064 0.2588 1.0167 0.076 Uiso 1 1 calc R . . C236 C 0.374(3) 0.2280(10) 0.9085(11) 0.194(15) Uani 1 1 d . . . H23I H 0.2919 0.2356 0.8725 0.233 Uiso 1 1 calc R . . H23J H 0.4443 0.2842 0.9109 0.233 Uiso 1 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 Ru1 0.0256(5) 0.0215(4) 0.0381(5) 0.0042(3) 0.0061(3) 0.0019(3) Ru2 0.0266(5) 0.0209(4) 0.0310(4) 0.0044(3) 0.0046(3) 0.0019(3) P1 0.0238(14) 0.0196(11) 0.0373(13) 0.0035(10) 0.0022(10) 0.0017(9) P2 0.0236(14) 0.0188(11) 0.0311(12) 0.0032(9) 0.0074(10) 0.0033(9) Si1 0.054(2) 0.0378(16) 0.0448(16) 0.0032(12) 0.0133(14) 0.0001(13) Si2 0.0349(18) 0.0333(15) 0.0499(16) 0.0081(12) 0.0021(13) 0.0036(12) Si3 0.0407(19) 0.0474(17) 0.0471(16) 0.0000(13) -0.0005(14) 0.0045(13) O11 0.082(6) 0.050(4) 0.032(4) -0.003(3) 0.015(4) -0.005(4) O12 0.074(6) 0.052(4) 0.065(5) -0.006(4) 0.034(4) 0.015(4) O21 0.037(5) 0.071(5) 0.061(5) 0.004(4) -0.007(4) 0.005(4) O22 0.030(5) 0.039(4) 0.086(5) -0.007(3) 0.018(4) 0.009(3) O31 0.050(6) 0.105(7) 0.073(6) 0.011(5) -0.025(5) 0.031(5) O32 0.071(6) 0.055(5) 0.037(4) -0.006(3) 0.000(4) 0.004(4) C11 0.129(14) 0.087(10) 0.044(7) 0.020(7) 0.023(8) -0.002(9) C12 0.040(9) 0.106(11) 0.083(9) 0.015(8) 0.019(7) 0.004(7) C21 0.081(12) 0.143(15) 0.101(12) 0.077(11) -0.030(9) -0.008(10) C22 0.073(11) 0.065(8) 0.100(10) -0.012(7) 0.021(8) 0.007(7) C31 0.070(12) 0.20(2) 0.062(9) 0.020(10) 0.013(8) 0.049(11) C32 0.067(10) 0.085(9) 0.054(7) 0.014(6) 0.017(6) 0.031(7) C111 0.019(5) 0.026(5) 0.047(5) 0.008(4) 0.007(4) 0.002(4) C112 0.034(6) 0.032(5) 0.047(6) 0.007(4) 0.012(5) -0.003(4) C113 0.056(8) 0.046(6) 0.044(6) 0.021(5) 0.007(5) 0.005(5) C114 0.047(8) 0.059(7) 0.047(6) 0.000(5) 0.017(5) 0.005(5) C115 0.039(7) 0.048(6) 0.051(6) 0.000(5) 0.015(5) 0.006(5) C116 0.030(6) 0.032(5) 0.045(5) 0.010(4) 0.011(4) 0.007(4) C121 0.028(6) 0.031(5) 0.040(5) 0.004(4) 0.005(4) 0.005(4) C122 0.042(7) 0.029(5) 0.058(6) 0.003(4) 0.014(5) 0.007(4) C123 0.050(8) 0.038(6) 0.081(8) 0.009(5) 0.038(6) 0.008(5) C124 0.043(7) 0.036(6) 0.093(9) 0.016(6) 0.007(6) 0.015(5) C125 0.034(7) 0.040(6) 0.057(6) 0.001(5) 0.006(5) 0.011(4) C126 0.024(6) 0.035(5) 0.053(6) 0.007(4) -0.001(5) 0.008(4) C131 0.073(9) 0.025(5) 0.075(8) 0.004(5) -0.049(7) 0.008(5) C132 0.065(9) 0.055(7) 0.099(10) -0.021(7) -0.034(8) 0.018(7) C133 0.048(8) 0.058(7) 0.079(8) 0.008(6) -0.028(7) 0.002(6) C134 0.058(9) 0.067(8) 0.063(7) -0.014(6) -0.026(6) 0.011(6) C135 0.159(18) 0.052(8) 0.20(2) -0.060(10) -0.135(17) 0.042(10) C136 0.060(8) 0.030(5) 0.059(7) -0.003(5) -0.028(6) 0.010(5) C211 0.031(6) 0.019(4) 0.030(5) 0.003(4) 0.001(4) -0.003(4) C212 0.024(6) 0.040(6) 0.060(6) -0.013(5) -0.006(5) 0.003(4) C213 0.040(7) 0.061(7) 0.056(7) -0.002(5) -0.017(5) 0.014(5) C214 0.028(6) 0.055(7) 0.051(6) -0.008(5) -0.009(5) 0.005(5) C215 0.037(6) 0.035(5) 0.041(5) -0.007(4) 0.005(5) 0.003(4) C216 0.035(6) 0.023(5) 0.037(5) 0.000(4) 0.003(4) -0.005(4) C221 0.026(6) 0.019(4) 0.029(4) 0.009(3) 0.004(4) 0.005(4) C222 0.028(6) 0.036(5) 0.040(5) -0.002(4) 0.004(4) 0.009(4) C223 0.046(8) 0.045(6) 0.054(6) 0.004(5) 0.021(5) 0.014(5) C224 0.027(6) 0.048(6) 0.077(8) 0.022(5) 0.006(5) 0.017(5) C225 0.037(7) 0.057(7) 0.060(7) 0.019(5) 0.005(5) 0.016(5) C226 0.030(6) 0.053(6) 0.037(5) 0.006(4) -0.001(4) 0.015(5) C231 0.052(7) 0.022(5) 0.052(6) 0.005(4) 0.022(5) 0.007(4) C232 0.039(6) 0.035(5) 0.040(5) 0.010(4) 0.012(4) 0.008(4) C233 0.133(14) 0.049(7) 0.079(9) 0.025(6) 0.075(9) 0.037(8) C234 0.20(2) 0.060(9) 0.076(9) 0.012(7) 0.086(11) 0.024(10) C235 0.104(11) 0.043(6) 0.054(7) 0.006(5) 0.047(7) 0.015(6) C236 0.44(4) 0.048(9) 0.178(19) 0.051(10) 0.26(3) 0.083(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 P1 2.331(2) . ? Ru1 Si3 2.355(3) . ? Ru1 Si2 2.408(3) . ? Ru1 Si1 2.456(3) . ? Ru1 Ru2 2.8529(10) . ? Ru2 P2 2.329(2) . ? Ru2 Si1 2.364(3) . ? Ru2 Si3 2.408(3) . ? Ru2 Si2 2.419(3) . ? P1 C131 1.858(9) . ? P1 C121 1.859(9) . ? P1 C111 1.861(9) . ? P2 C221 1.842(8) . ? P2 C211 1.855(8) . ? P2 C231 1.861(10) . ? Si1 O11 1.641(8) . ? Si1 O12 1.645(9) . ? Si2 O22 1.632(8) . ? Si2 O21 1.656(7) . ? Si3 O31 1.640(9) . ? Si3 O32 1.644(8) . ? O11 C11 1.417(14) . ? O12 C12 1.451(15) . ? O21 C21 1.376(14) . ? O22 C22 1.402(16) . ? O31 C31 1.329(15) . ? O32 C32 1.399(14) . ? C111 C116 1.512(13) . ? C111 C112 1.535(13) . ? C112 C113 1.521(14) . ? C113 C114 1.536(15) . ? C114 C115 1.484(15) . ? C115 C116 1.531(14) . ? C121 C122 1.503(14) . ? C121 C126 1.550(12) . ? C122 C123 1.516(15) . ? C123 C124 1.522(16) . ? C124 C125 1.512(16) . ? C125 C126 1.514(13) . ? C131 C132 1.373(17) . ? C131 C136 1.552(13) . ? C132 C133 1.582(15) . ? C133 C134 1.511(16) . ? C134 C135 1.326(19) . ? C135 C136 1.539(16) . ? C211 C212 1.516(13) . ? C211 C216 1.545(12) . ? C212 C213 1.547(13) . ? C213 C214 1.521(15) . ? C214 C215 1.516(14) . ? C215 C216 1.522(12) . ? C221 C226 1.547(12) . ? C221 C222 1.548(13) . ? C222 C223 1.530(13) . ? C223 C224 1.528(14) . ? C224 C225 1.504(16) . ? C225 C226 1.544(14) . ? C231 C236 1.366(17) . ? C231 C232 1.496(13) . ? C232 C233 1.480(15) . ? C233 C234 1.391(18) . ? C234 C235 1.474(17) . ? C235 C236 1.469(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 P1 Ru1 Si3 121.55(9) . . ? P1 Ru1 Si2 125.03(9) . . ? Si3 Ru1 Si2 91.71(10) . . ? P1 Ru1 Si1 133.52(9) . . ? Si3 Ru1 Si1 91.72(10) . . ? Si2 Ru1 Si1 80.37(10) . . ? P1 Ru1 Ru2 174.16(7) . . ? Si3 Ru1 Ru2 54.07(7) . . ? Si2 Ru1 Ru2 53.96(7) . . ? Si1 Ru1 Ru2 52.23(7) . . ? P2 Ru2 Si1 124.74(9) . . ? P2 Ru2 Si3 127.31(9) . . ? Si1 Ru2 Si3 92.71(11) . . ? P2 Ru2 Si2 126.86(9) . . ? Si1 Ru2 Si2 82.01(11) . . ? Si3 Ru2 Si2 90.14(10) . . ? P2 Ru2 Ru1 179.55(7) . . ? Si1 Ru2 Ru1 55.22(7) . . ? Si3 Ru2 Ru1 52.35(7) . . ? Si2 Ru2 Ru1 53.58(7) . . ? C131 P1 C121 102.8(5) . . ? C131 P1 C111 108.4(6) . . ? C121 P1 C111 103.4(4) . . ? C131 P1 Ru1 114.0(3) . . ? C121 P1 Ru1 114.3(3) . . ? C111 P1 Ru1 113.0(3) . . ? C221 P2 C211 103.4(4) . . ? C221 P2 C231 103.1(4) . . ? C211 P2 C231 109.0(5) . . ? C221 P2 Ru2 114.4(3) . . ? C211 P2 Ru2 111.3(3) . . ? C231 P2 Ru2 114.8(3) . . ? O11 Si1 O12 99.7(4) . . ? O11 Si1 Ru2 122.1(3) . . ? O12 Si1 Ru2 119.8(3) . . ? O11 Si1 Ru1 119.1(3) . . ? O12 Si1 Ru1 124.3(3) . . ? Ru2 Si1 Ru1 72.55(8) . . ? O22 Si2 O21 105.5(4) . . ? O22 Si2 Ru1 111.3(3) . . ? O21 Si2 Ru1 128.5(3) . . ? O22 Si2 Ru2 127.7(3) . . ? O21 Si2 Ru2 110.9(3) . . ? Ru1 Si2 Ru2 72.45(9) . . ? O31 Si3 O32 100.4(5) . . ? O31 Si3 Ru1 122.0(4) . . ? O32 Si3 Ru1 118.8(3) . . ? O31 Si3 Ru2 114.8(3) . . ? O32 Si3 Ru2 127.9(3) . . ? Ru1 Si3 Ru2 73.57(8) . . ? C11 O11 Si1 121.4(8) . . ? C12 O12 Si1 124.4(8) . . ? C21 O21 Si2 126.7(9) . . ? C22 O22 Si2 121.0(7) . . ? C31 O31 Si3 128.6(10) . . ? C32 O32 Si3 125.4(7) . . ? C116 C111 C112 110.4(8) . . ? C116 C111 P1 115.3(6) . . ? C112 C111 P1 117.2(6) . . ? C113 C112 C111 110.0(8) . . ? C112 C113 C114 112.9(8) . . ? C115 C114 C113 111.8(9) . . ? C114 C115 C116 113.1(8) . . ? C111 C116 C115 111.4(8) . . ? C122 C121 C126 109.7(8) . . ? C122 C121 P1 112.0(6) . . ? C126 C121 P1 112.8(6) . . ? C121 C122 C123 112.5(8) . . ? C122 C123 C124 110.6(9) . . ? C125 C124 C123 110.2(9) . . ? C124 C125 C126 111.6(8) . . ? C125 C126 C121 111.3(8) . . ? C132 C131 C136 112.8(10) . . ? C132 C131 P1 117.8(9) . . ? C136 C131 P1 116.9(6) . . ? C131 C132 C133 114.9(11) . . ? C134 C133 C132 111.1(9) . . ? C135 C134 C133 115.8(11) . . ? C134 C135 C136 121.1(14) . . ? C135 C136 C131 109.6(9) . . ? C212 C211 C216 110.4(7) . . ? C212 C211 P2 114.0(6) . . ? C216 C211 P2 117.6(6) . . ? C211 C212 C213 110.0(8) . . ? C214 C213 C212 112.3(9) . . ? C215 C214 C213 111.9(8) . . ? C214 C215 C216 111.9(8) . . ? C215 C216 C211 109.9(7) . . ? C226 C221 C222 110.2(8) . . ? C226 C221 P2 111.4(6) . . ? C222 C221 P2 111.9(5) . . ? C223 C222 C221 111.9(7) . . ? C224 C223 C222 111.1(8) . . ? C225 C224 C223 111.0(9) . . ? C224 C225 C226 110.6(8) . . ? C225 C226 C221 110.8(8) . . ? C236 C231 C232 117.2(10) . . ? C236 C231 P2 121.8(8) . . ? C232 C231 P2 118.7(7) . . ? C233 C232 C231 115.4(8) . . ? C234 C233 C232 120.9(11) . . ? C233 C234 C235 116.3(13) . . ? C236 C235 C234 115.7(10) . . ? C231 C236 C235 122.6(13) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 21.49 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.555 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.148 #====END