Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in Journal of the Chemical Society, Chemical Communication ; _publ_contact_author 'Prof Daniel Touchard' _publ_contact_author_address ; Prof Daniel Touchard Institut de Chimie de Rennes UMR 6509 CNRS Universite de Rennes Organometalliques et Catalyse Campus de Beaulieu Rennes 35042 FRANCE ; _publ_contact_author_email ' DANIEL.TOUCHARD@UNIV-RENNES1.FR' _publ_requested_journal 'J. Chem. Soc.,Chem. Comm.' #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; New homobimetallic annulated C7 ruthenium complex via a [2+2] coupling reaction ; loop_ _publ_author_name _publ_author_address 'Rigaut, Stephane' ; Institut de Chimie de Rennes UMR-6509 CNRS Universite de Rennes: Organometallique et Catalyse. Campus de Beaulieu 35042 Rennes, France ; 'Le Pichon, Luc' ; Institut de Chimie de Rennes UMR-6509 CNRS Universite de Rennes: Organometallique et Catalyse. Campus de Beaulieu 35042 Rennes, France ; 'Daran, Jean-Claude' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; 'Touchard, Daniel' ; Institut de Chimie de Rennes UMR-6509 CNRS Universite de Rennes: Organometallique et Catalyse. Campus de Beaulieu 35042 Rennes, France ; 'Dixneuf, Pierre' ; Institut de Chimie de Rennes UMR-6509 CNRS Universite de Rennes: Organometallique et Catalyse. Campus de Beaulieu 35042 Rennes, France ; #============================================================================== _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R., SIR97, J. Appl. Cryst. (1999), 32, 115-119. L. J. Farrugia, ORTEP3 for Windows, J. Appl. Crystallogr. 1997, 30, 565. Farrugia L. J., WINGX, J. Appl. Crystallogr. 1999, 32, 837. Sheldrick, G.M. (1997). SHELXL97, program for crystal structure refinement, University of Gottingen. 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_(3) _database_code_CSD 162902 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H48 Cl1 F3 P4 Ru1' _chemical_formula_structural 'C58 H48 CL F3 P4.5 RU1' _chemical_formula_sum 'C58 H48 Cl1 F3 P4 Ru1' _chemical_compound_source 'synthesis as described' _chemical_formula_weight 1077.85 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' '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' '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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7811(10) _cell_length_b 12.1069(14) _cell_length_c 20.503(2) _cell_angle_alpha 95.204(13) _cell_angle_beta 98.910(12) _cell_angle_gamma 101.264(13) _cell_volume 2334.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 24.20 _exptl_crystal_description 'flat box' _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1103 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_factor_muR 0.000 _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_absorpt_correction_T_min 0.2367 _exptl_absorpt_correction_T_max 0.6975 _exptl_absorpt_Rmerge_before 0.0599 _exptl_absorpt_Rmerge_after 0.0577 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS) equipped with an Oxford Cryosystems cooler device. The crystal-to-detector distance was 80 mm. 167 frames (5 min per frame) were obtained with 0 < \f < 250.5\% and with the crystals oscillated through 1.5\% in \f. Coverage of the unique set was over 93% complete to at least 24.2\%. 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_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 19015 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0384 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.20 _reflns_number_total 6976 _reflns_number_gt 5466 _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_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0498P)^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 6976 _refine_ls_number_parameters 592 _refine_ls_number_restraints 336 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.004 _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 0.42482(2) 0.906548(17) 0.725712(10) 0.01587(8) Uani 1 1 d . . . Cl1 Cl 0.40232(7) 0.87606(6) 0.60220(3) 0.02382(16) Uani 1 1 d . . . P1 P 0.0000 0.0000 0.0000 0.0367(3) Uani 1 2 d SU . . P11 P 0.57693(7) 0.77789(6) 0.74710(3) 0.01876(16) Uani 1 1 d . . . P21 P 0.64319(7) 1.04648(6) 0.75341(3) 0.01892(16) Uani 1 1 d . . . P31 P 0.21217(7) 0.76247(6) 0.69727(3) 0.01980(16) Uani 1 1 d . . . P41 P 0.26368(7) 1.03124(6) 0.70773(3) 0.01896(16) Uani 1 1 d . . . F11 F 0.0153(3) -0.02346(19) -0.07548(11) 0.0673(7) Uani 1 1 d U . . F12 F -0.0012(2) -0.13072(17) 0.00807(10) 0.0502(5) Uani 1 1 d U . . F13 F -0.1667(2) -0.0291(2) -0.02048(14) 0.0694(7) Uani 1 1 d U . . C1 C 0.4396(3) 0.9334(2) 0.82118(14) 0.0193(6) Uani 1 1 d U . . C2 C 0.4612(3) 0.9544(2) 0.88191(14) 0.0245(6) Uani 1 1 d U . . C3 C 0.4832(3) 0.9805(2) 0.94978(14) 0.0234(6) Uani 1 1 d U . . C4 C 0.5100(5) 0.9168(3) 1.00565(17) 0.0598(12) Uani 1 1 d U . . C11 C 0.7583(3) 0.8584(2) 0.75181(14) 0.0229(6) Uani 1 1 d U . . H11A H 0.8266 0.8164 0.7733 0.027 Uiso 1 1 calc R . . H11B H 0.7774 0.8682 0.7064 0.027 Uiso 1 1 calc R . . C21 C 0.7767(3) 0.9735(2) 0.79179(14) 0.0227(6) Uani 1 1 d U . . H21A H 0.8728 1.0190 0.7925 0.027 Uiso 1 1 calc R . . H21B H 0.7652 0.9641 0.8382 0.027 Uiso 1 1 calc R . . C31 C 0.0755(3) 0.8306(2) 0.65628(14) 0.0243(6) Uani 1 1 d U . . H31A H 0.0923 0.8447 0.6111 0.029 Uiso 1 1 calc R . . H31B H -0.0194 0.7811 0.6524 0.029 Uiso 1 1 calc R . . C41 C 0.0842(3) 0.9422(2) 0.69875(15) 0.0249(6) Uani 1 1 d U . . H41A H 0.0627 0.9273 0.7432 0.030 Uiso 1 1 calc R . . H41B H 0.0136 0.9825 0.6775 0.030 Uiso 1 1 calc R . . C111 C 0.5789(3) 0.7223(2) 0.82782(14) 0.0215(6) Uani 1 1 d U . . C112 C 0.4517(3) 0.6630(2) 0.84154(15) 0.0277(7) Uani 1 1 d U . . H112 H 0.3674 0.6525 0.8095 0.033 Uiso 1 1 calc R . . C113 C 0.4471(3) 0.6193(3) 0.90158(16) 0.0324(7) Uani 1 1 d U . . H113 H 0.3600 0.5781 0.9102 0.039 Uiso 1 1 calc R . . C114 C 0.5679(4) 0.6352(3) 0.94867(15) 0.0327(7) Uani 1 1 d U . . H114 H 0.5641 0.6061 0.9900 0.039 Uiso 1 1 calc R . . C115 C 0.6945(4) 0.6937(3) 0.93574(15) 0.0323(7) Uani 1 1 d U . . H115 H 0.7785 0.7041 0.9680 0.039 Uiso 1 1 calc R . . C116 C 0.6994(3) 0.7376(2) 0.87528(15) 0.0271(7) Uani 1 1 d U . . H116 H 0.7869 0.7784 0.8668 0.033 Uiso 1 1 calc R . . C121 C 0.5838(3) 0.6529(2) 0.69106(14) 0.0242(6) Uani 1 1 d U . . C122 C 0.5751(3) 0.6612(2) 0.62360(15) 0.0303(7) Uani 1 1 d U . . H122 H 0.5566 0.7283 0.6067 0.036 Uiso 1 1 calc R . . C123 C 0.5931(4) 0.5726(3) 0.58087(16) 0.0372(8) Uani 1 1 d U . . H123 H 0.5883 0.5796 0.5348 0.045 Uiso 1 1 calc R . . C124 C 0.6180(4) 0.4747(3) 0.60426(17) 0.0393(8) Uani 1 1 d U . . H124 H 0.6301 0.4139 0.5745 0.047 Uiso 1 1 calc R . . C125 C 0.6254(4) 0.4645(3) 0.67089(18) 0.0423(9) Uani 1 1 d U . . H125 H 0.6421 0.3963 0.6871 0.051 Uiso 1 1 calc R . . C126 C 0.6087(4) 0.5531(3) 0.71451(16) 0.0342(8) Uani 1 1 d U . . H126 H 0.6144 0.5458 0.7605 0.041 Uiso 1 1 calc R . . C211 C 0.6583(3) 1.1693(2) 0.81603(14) 0.0248(7) Uani 1 1 d U . . C212 C 0.7437(4) 1.1827(3) 0.87746(16) 0.0423(9) Uani 1 1 d U . . H212 H 0.7942 1.1258 0.8893 0.051 Uiso 1 1 calc R . . C213 C 0.7565(5) 1.2793(3) 0.92248(19) 0.0574(11) Uani 1 1 d U . . H213 H 0.8173 1.2889 0.9644 0.069 Uiso 1 1 calc R . . C214 C 0.6814(4) 1.3602(3) 0.90620(18) 0.0456(9) Uani 1 1 d U . . H214 H 0.6893 1.4254 0.9372 0.055 Uiso 1 1 calc R . . C215 C 0.5951(4) 1.3477(3) 0.84545(18) 0.0382(8) Uani 1 1 d U . . H215 H 0.5425 1.4037 0.8344 0.046 Uiso 1 1 calc R . . C216 C 0.5848(3) 1.2526(2) 0.80013(16) 0.0303(7) Uani 1 1 d U . . H216 H 0.5266 1.2448 0.7576 0.036 Uiso 1 1 calc R . . C221 C 0.7350(3) 1.1166(2) 0.69117(14) 0.0221(6) Uani 1 1 d U . . C222 C 0.8366(3) 1.2168(3) 0.71038(17) 0.0330(7) Uani 1 1 d U . . H222 H 0.8614 1.2476 0.7560 0.040 Uiso 1 1 calc R . . C223 C 0.9019(4) 1.2721(3) 0.66328(18) 0.0381(8) Uani 1 1 d U . . H223 H 0.9705 1.3408 0.6768 0.046 Uiso 1 1 calc R . . C224 C 0.8681(4) 1.2284(3) 0.59793(17) 0.0385(8) Uani 1 1 d U . . H224 H 0.9117 1.2678 0.5660 0.046 Uiso 1 1 calc R . . C225 C 0.7712(3) 1.1275(3) 0.57769(16) 0.0387(8) Uani 1 1 d U . . H225 H 0.7487 1.0970 0.5321 0.046 Uiso 1 1 calc R . . C226 C 0.7064(3) 1.0706(3) 0.62478(15) 0.0319(7) Uani 1 1 d U . . H226 H 0.6420 0.9996 0.6112 0.038 Uiso 1 1 calc R . . C311 C 0.2066(3) 0.6391(2) 0.63758(14) 0.0242(6) Uani 1 1 d U . . C312 C 0.1666(3) 0.6404(3) 0.56958(15) 0.0328(7) Uani 1 1 d U . . H312 H 0.1401 0.7060 0.5538 0.039 Uiso 1 1 calc R . . C313 C 0.1650(4) 0.5478(3) 0.52459(17) 0.0405(8) Uani 1 1 d U . . H313 H 0.1379 0.5501 0.4783 0.049 Uiso 1 1 calc R . . C314 C 0.2024(4) 0.4528(3) 0.54675(17) 0.0399(8) Uani 1 1 d U . . H314 H 0.1988 0.3883 0.5159 0.048 Uiso 1 1 calc R . . C315 C 0.2448(4) 0.4506(3) 0.61305(18) 0.0383(8) Uani 1 1 d U . . H315 H 0.2724 0.3850 0.6281 0.046 Uiso 1 1 calc R . . C316 C 0.2481(3) 0.5435(2) 0.65883(16) 0.0304(7) Uani 1 1 d U . . H316 H 0.2788 0.5413 0.7049 0.036 Uiso 1 1 calc R . . C321 C 0.1192(3) 0.6989(2) 0.76089(15) 0.0239(6) Uani 1 1 d U . . C322 C 0.0199(3) 0.5962(2) 0.74540(17) 0.0329(7) Uani 1 1 d U . . H322 H -0.0019 0.5581 0.7013 0.039 Uiso 1 1 calc R . . C323 C -0.0468(4) 0.5500(3) 0.79463(19) 0.0416(9) Uani 1 1 d U . . H323 H -0.1121 0.4789 0.7843 0.050 Uiso 1 1 calc R . . C324 C -0.0199(4) 0.6053(3) 0.85779(18) 0.0413(9) Uani 1 1 d U . . H324 H -0.0651 0.5721 0.8912 0.050 Uiso 1 1 calc R . . C325 C 0.0731(3) 0.7096(3) 0.87322(17) 0.0386(8) Uani 1 1 d U . . H325 H 0.0889 0.7495 0.9167 0.046 Uiso 1 1 calc R . . C326 C 0.1431(3) 0.7555(3) 0.82503(15) 0.0302(7) Uani 1 1 d U . . H326 H 0.2082 0.8265 0.8359 0.036 Uiso 1 1 calc R . . C411 C 0.2584(3) 1.0933(2) 0.62913(14) 0.0224(6) Uani 1 1 d U . . C412 C 0.3857(3) 1.1404(2) 0.61000(15) 0.0289(7) Uani 1 1 d U . . H412 H 0.4725 1.1464 0.6397 0.035 Uiso 1 1 calc R . . C413 C 0.3876(4) 1.1784(3) 0.54852(16) 0.0353(8) Uani 1 1 d U . . H413 H 0.4752 1.2098 0.5360 0.042 Uiso 1 1 calc R . . C414 C 0.2622(4) 1.1706(3) 0.50529(16) 0.0363(8) Uani 1 1 d U . . H414 H 0.2631 1.1943 0.4624 0.044 Uiso 1 1 calc R . . C415 C 0.1362(4) 1.1287(3) 0.52464(17) 0.0388(8) Uani 1 1 d U . . H415 H 0.0495 1.1261 0.4957 0.047 Uiso 1 1 calc R . . C416 C 0.1343(3) 1.0898(3) 0.58616(16) 0.0324(7) Uani 1 1 d U . . H416 H 0.0461 1.0605 0.5988 0.039 Uiso 1 1 calc R . . C421 C 0.2442(3) 1.1458(2) 0.76825(14) 0.0228(6) Uani 1 1 d U . . C422 C 0.2262(3) 1.1228(3) 0.83163(15) 0.0316(7) Uani 1 1 d U . . H422 H 0.2315 1.0499 0.8442 0.038 Uiso 1 1 calc R . . C423 C 0.2008(4) 1.2048(3) 0.87679(17) 0.0399(8) Uani 1 1 d U . . H423 H 0.1884 1.1879 0.9201 0.048 Uiso 1 1 calc R . . C424 C 0.1931(4) 1.3110(3) 0.85941(18) 0.0416(9) Uani 1 1 d U . . H424 H 0.1744 1.3671 0.8904 0.050 Uiso 1 1 calc R . . C425 C 0.2125(4) 1.3349(3) 0.79745(18) 0.0434(9) Uani 1 1 d U . . H425 H 0.2087 1.4085 0.7855 0.052 Uiso 1 1 calc R . . C426 C 0.2376(4) 1.2534(3) 0.75152(16) 0.0357(8) Uani 1 1 d U . . H426 H 0.2504 1.2712 0.7084 0.043 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 0.01878(12) 0.01647(12) 0.01230(12) 0.00180(8) 0.00315(9) 0.00327(8) Cl1 0.0299(4) 0.0259(3) 0.0148(3) 0.0027(3) 0.0045(3) 0.0035(3) P1 0.0356(7) 0.0385(7) 0.0325(7) 0.0074(5) -0.0002(6) 0.0030(5) P11 0.0211(4) 0.0185(3) 0.0174(4) 0.0023(3) 0.0041(3) 0.0053(3) P21 0.0203(4) 0.0181(3) 0.0172(4) 0.0018(3) 0.0025(3) 0.0021(3) P31 0.0214(4) 0.0189(3) 0.0178(4) 0.0016(3) 0.0030(3) 0.0018(3) P41 0.0207(4) 0.0196(4) 0.0175(4) 0.0038(3) 0.0039(3) 0.0055(3) F11 0.105(2) 0.0574(14) 0.0404(13) 0.0087(11) 0.0204(13) 0.0128(14) F12 0.0579(13) 0.0421(11) 0.0496(12) 0.0114(10) 0.0065(11) 0.0076(10) F13 0.0337(11) 0.0652(15) 0.101(2) 0.0197(14) -0.0062(12) 0.0016(11) C1 0.0195(13) 0.0166(13) 0.0222(16) 0.0021(11) 0.0059(12) 0.0030(11) C2 0.0291(15) 0.0245(15) 0.0202(16) 0.0017(12) 0.0045(13) 0.0067(12) C3 0.0293(15) 0.0259(15) 0.0159(14) 0.0015(12) 0.0044(13) 0.0082(12) C4 0.113(4) 0.051(2) 0.0162(17) 0.0001(16) 0.009(2) 0.024(2) C11 0.0207(14) 0.0255(15) 0.0244(15) 0.0036(12) 0.0064(12) 0.0073(12) C21 0.0189(14) 0.0253(15) 0.0238(15) 0.0059(12) 0.0021(12) 0.0047(12) C31 0.0200(14) 0.0270(15) 0.0225(15) 0.0039(12) -0.0007(12) 0.0003(12) C41 0.0226(14) 0.0271(15) 0.0271(16) 0.0085(13) 0.0058(13) 0.0066(12) C111 0.0295(15) 0.0187(14) 0.0189(14) 0.0037(11) 0.0053(13) 0.0097(12) C112 0.0292(16) 0.0299(16) 0.0249(16) 0.0056(13) 0.0052(14) 0.0074(13) C113 0.0379(18) 0.0294(16) 0.0321(18) 0.0078(14) 0.0129(15) 0.0055(14) C114 0.052(2) 0.0283(16) 0.0212(16) 0.0083(13) 0.0077(16) 0.0124(15) C115 0.0403(18) 0.0328(17) 0.0228(16) 0.0048(13) -0.0037(14) 0.0115(15) C116 0.0296(16) 0.0252(15) 0.0262(16) 0.0042(12) 0.0021(14) 0.0068(13) C121 0.0237(14) 0.0238(15) 0.0251(16) -0.0015(12) 0.0053(13) 0.0063(12) C122 0.0393(17) 0.0246(15) 0.0285(17) 0.0024(13) 0.0104(15) 0.0074(13) C123 0.049(2) 0.0355(18) 0.0275(17) -0.0032(14) 0.0140(16) 0.0077(16) C124 0.048(2) 0.0308(18) 0.039(2) -0.0079(15) 0.0150(17) 0.0085(15) C125 0.059(2) 0.0254(17) 0.047(2) 0.0035(15) 0.0109(19) 0.0194(16) C126 0.047(2) 0.0302(17) 0.0296(18) 0.0070(14) 0.0079(16) 0.0173(15) C211 0.0289(15) 0.0217(14) 0.0221(15) 0.0014(12) 0.0070(13) 0.0003(12) C212 0.063(2) 0.0317(18) 0.0279(18) -0.0043(14) -0.0062(17) 0.0142(17) C213 0.090(3) 0.041(2) 0.033(2) -0.0094(17) -0.011(2) 0.015(2) C214 0.069(2) 0.0267(17) 0.038(2) -0.0090(15) 0.014(2) 0.0056(17) C215 0.0424(19) 0.0255(16) 0.049(2) 0.0039(15) 0.0159(18) 0.0075(14) C216 0.0323(17) 0.0254(15) 0.0329(17) 0.0018(13) 0.0075(14) 0.0048(13) C221 0.0194(14) 0.0236(14) 0.0246(15) 0.0069(12) 0.0038(12) 0.0059(12) C222 0.0348(17) 0.0271(16) 0.0351(18) -0.0003(13) 0.0100(15) 0.0009(14) C223 0.0400(19) 0.0277(17) 0.048(2) 0.0085(15) 0.0197(17) 0.0000(14) C224 0.0424(19) 0.0387(19) 0.043(2) 0.0227(16) 0.0229(17) 0.0101(16) C225 0.0361(18) 0.057(2) 0.0248(17) 0.0099(15) 0.0102(15) 0.0073(16) C226 0.0282(16) 0.0377(17) 0.0262(16) 0.0031(13) 0.0055(14) -0.0019(14) C311 0.0244(15) 0.0202(14) 0.0251(16) -0.0009(12) 0.0044(13) -0.0005(12) C312 0.0410(18) 0.0300(17) 0.0259(17) -0.0018(13) 0.0032(15) 0.0080(14) C313 0.047(2) 0.042(2) 0.0277(18) -0.0060(15) 0.0043(16) 0.0051(16) C314 0.049(2) 0.0306(18) 0.040(2) -0.0044(15) 0.0162(17) 0.0041(15) C315 0.045(2) 0.0230(16) 0.051(2) 0.0078(15) 0.0204(18) 0.0060(14) C316 0.0332(17) 0.0269(16) 0.0327(17) 0.0047(13) 0.0118(15) 0.0051(13) C321 0.0199(14) 0.0251(15) 0.0281(16) 0.0064(12) 0.0055(13) 0.0057(12) C322 0.0309(16) 0.0261(16) 0.0413(19) 0.0013(14) 0.0145(15) 0.0004(13) C323 0.0389(19) 0.0305(17) 0.059(2) 0.0102(16) 0.0245(18) 0.0024(15) C324 0.042(2) 0.045(2) 0.047(2) 0.0217(17) 0.0265(18) 0.0119(16) C325 0.0360(18) 0.051(2) 0.0305(18) 0.0079(15) 0.0107(15) 0.0088(16) C326 0.0280(16) 0.0358(17) 0.0268(16) 0.0052(14) 0.0072(14) 0.0042(14) C411 0.0310(16) 0.0184(14) 0.0200(15) 0.0038(11) 0.0049(13) 0.0099(12) C412 0.0283(16) 0.0331(17) 0.0264(16) 0.0095(13) 0.0040(14) 0.0074(13) C413 0.0437(19) 0.0323(17) 0.0344(18) 0.0139(14) 0.0159(17) 0.0072(15) C414 0.060(2) 0.0328(17) 0.0209(16) 0.0118(13) 0.0095(17) 0.0148(16) C415 0.0414(19) 0.044(2) 0.0285(17) 0.0150(15) -0.0063(16) 0.0077(16) C416 0.0291(16) 0.0389(18) 0.0293(17) 0.0112(14) 0.0011(14) 0.0072(14) C421 0.0216(14) 0.0230(15) 0.0250(15) 0.0031(12) 0.0041(13) 0.0074(12) C422 0.0449(19) 0.0270(16) 0.0261(16) 0.0065(13) 0.0105(15) 0.0106(14) C423 0.058(2) 0.0366(18) 0.0289(18) 0.0042(14) 0.0158(17) 0.0131(16) C424 0.052(2) 0.0365(19) 0.039(2) -0.0047(15) 0.0154(17) 0.0136(16) C425 0.065(2) 0.0291(18) 0.042(2) 0.0049(15) 0.0147(19) 0.0196(17) C426 0.050(2) 0.0303(17) 0.0320(18) 0.0083(14) 0.0138(16) 0.0143(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 C1 1.933(3) . ? Ru1 P11 2.3789(8) . ? Ru1 P31 2.3940(8) . ? Ru1 P41 2.3978(8) . ? Ru1 P21 2.4064(8) . ? Ru1 Cl1 2.4948(7) . ? P1 F13 1.580(2) . ? P1 F13 1.580(2) 2 ? P1 F11 1.583(2) . ? P1 F11 1.583(2) 2 ? P1 F12 1.604(2) . ? P1 F12 1.604(2) 2 ? P11 C11 1.834(3) . ? P11 C121 1.834(3) . ? P11 C111 1.841(3) . ? P21 C21 1.834(3) . ? P21 C211 1.842(3) . ? P21 C221 1.846(3) . ? P31 C311 1.830(3) . ? P31 C31 1.839(3) . ? P31 C321 1.843(3) . ? P41 C421 1.834(3) . ? P41 C411 1.837(3) . ? P41 C41 1.844(3) . ? C1 C2 1.225(4) . ? C2 C3 1.372(4) . ? C3 C4 1.457(5) . ? C3 C4 1.459(5) 2_677 ? C3 C3 2.031(5) 2_677 ? C4 C3 1.459(5) 2_677 ? C11 C21 1.515(4) . ? C31 C41 1.520(4) . ? C111 C116 1.378(4) . ? C111 C112 1.392(4) . ? C112 C113 1.387(4) . ? C113 C114 1.375(5) . ? C114 C115 1.378(4) . ? C115 C116 1.396(4) . ? C121 C122 1.387(4) . ? C121 C126 1.390(4) . ? C122 C123 1.378(4) . ? C123 C124 1.369(5) . ? C124 C125 1.375(5) . ? C125 C126 1.385(4) . ? C211 C212 1.377(5) . ? C211 C216 1.382(4) . ? C212 C213 1.395(5) . ? C213 C214 1.370(6) . ? C214 C215 1.370(5) . ? C215 C216 1.389(4) . ? C221 C226 1.388(4) . ? C221 C222 1.391(4) . ? C222 C223 1.389(4) . ? C223 C224 1.360(5) . ? C224 C225 1.377(5) . ? C225 C226 1.396(4) . ? C311 C316 1.384(4) . ? C311 C312 1.391(4) . ? C312 C313 1.382(4) . ? C313 C314 1.368(5) . ? C314 C315 1.362(5) . ? C315 C316 1.389(4) . ? C321 C326 1.390(4) . ? C321 C322 1.397(4) . ? C322 C323 1.386(4) . ? C323 C324 1.365(5) . ? C324 C325 1.382(5) . ? C325 C326 1.383(4) . ? C411 C416 1.376(4) . ? C411 C412 1.394(4) . ? C412 C413 1.382(4) . ? C413 C414 1.379(5) . ? C414 C415 1.371(5) . ? C415 C416 1.387(4) . ? C421 C422 1.383(4) . ? C421 C426 1.387(4) . ? C422 C423 1.381(4) . ? C423 C424 1.378(5) . ? C424 C425 1.361(5) . ? C425 C426 1.386(5) . ? 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 C1 Ru1 P11 86.01(9) . . ? C1 Ru1 P31 100.67(8) . . ? P11 Ru1 P31 95.00(3) . . ? C1 Ru1 P41 92.13(9) . . ? P11 Ru1 P41 177.01(2) . . ? P31 Ru1 P41 83.03(3) . . ? C1 Ru1 P21 79.98(8) . . ? P11 Ru1 P21 83.15(3) . . ? P31 Ru1 P21 178.01(3) . . ? P41 Ru1 P21 98.84(3) . . ? C1 Ru1 Cl1 178.49(9) . . ? P11 Ru1 Cl1 95.49(3) . . ? P31 Ru1 Cl1 79.41(3) . . ? P41 Ru1 Cl1 86.38(3) . . ? P21 Ru1 Cl1 99.99(3) . . ? F13 P1 F13 180.0 . 2 ? F13 P1 F11 90.37(15) . . ? F13 P1 F11 89.63(15) 2 . ? F13 P1 F11 89.63(15) . 2 ? F13 P1 F11 90.37(15) 2 2 ? F11 P1 F11 180.00(19) . 2 ? F13 P1 F12 90.26(12) . . ? F13 P1 F12 89.74(12) 2 . ? F11 P1 F12 89.70(11) . . ? F11 P1 F12 90.30(11) 2 . ? F13 P1 F12 89.74(12) . 2 ? F13 P1 F12 90.26(12) 2 2 ? F11 P1 F12 90.30(11) . 2 ? F11 P1 F12 89.70(11) 2 2 ? F12 P1 F12 180.0(2) . 2 ? C11 P11 C121 99.00(12) . . ? C11 P11 C111 104.21(13) . . ? C121 P11 C111 102.38(13) . . ? C11 P11 Ru1 106.69(10) . . ? C121 P11 Ru1 126.12(10) . . ? C111 P11 Ru1 115.44(9) . . ? C21 P21 C211 102.76(14) . . ? C21 P21 C221 101.18(13) . . ? C211 P21 C221 100.24(12) . . ? C21 P21 Ru1 106.13(9) . . ? C211 P21 Ru1 119.51(9) . . ? C221 P21 Ru1 123.86(10) . . ? C311 P31 C31 103.67(14) . . ? C311 P31 C321 102.71(13) . . ? C31 P31 C321 99.78(13) . . ? C311 P31 Ru1 119.16(9) . . ? C31 P31 Ru1 106.21(9) . . ? C321 P31 Ru1 122.25(10) . . ? C421 P41 C411 104.19(13) . . ? C421 P41 C41 98.10(12) . . ? C411 P41 C41 102.96(13) . . ? C421 P41 Ru1 126.06(10) . . ? C411 P41 Ru1 115.63(9) . . ? C41 P41 Ru1 106.25(10) . . ? C2 C1 Ru1 174.4(2) . . ? C1 C2 C3 178.3(3) . . ? C2 C3 C4 134.2(3) . . ? C2 C3 C4 134.1(3) . 2_677 ? C4 C3 C4 91.7(3) . 2_677 ? C2 C3 C3 179.7(3) . 2_677 ? C4 C3 C3 45.89(18) . 2_677 ? C4 C3 C3 45.80(19) 2_677 2_677 ? C3 C4 C3 88.3(3) . 2_677 ? C21 C11 P11 109.48(18) . . ? C11 C21 P21 108.8(2) . . ? C41 C31 P31 107.4(2) . . ? C31 C41 P41 109.54(18) . . ? C116 C111 C112 118.7(3) . . ? C116 C111 P11 123.2(2) . . ? C112 C111 P11 118.1(2) . . ? C113 C112 C111 120.5(3) . . ? C114 C113 C112 120.3(3) . . ? C113 C114 C115 119.8(3) . . ? C114 C115 C116 120.0(3) . . ? C111 C116 C115 120.7(3) . . ? C122 C121 C126 118.8(3) . . ? C122 C121 P11 118.8(2) . . ? C126 C121 P11 122.2(2) . . ? C123 C122 C121 120.4(3) . . ? C124 C123 C122 120.5(3) . . ? C123 C124 C125 119.9(3) . . ? C124 C125 C126 120.2(3) . . ? C125 C126 C121 120.1(3) . . ? C212 C211 C216 118.9(3) . . ? C212 C211 P21 122.2(2) . . ? C216 C211 P21 119.0(2) . . ? C211 C212 C213 120.3(3) . . ? C214 C213 C212 120.0(4) . . ? C213 C214 C215 120.4(3) . . ? C214 C215 C216 119.6(3) . . ? C211 C216 C215 120.9(3) . . ? C226 C221 C222 118.5(3) . . ? C226 C221 P21 121.3(2) . . ? C222 C221 P21 120.2(2) . . ? C223 C222 C221 120.4(3) . . ? C224 C223 C222 120.4(3) . . ? C223 C224 C225 120.6(3) . . ? C224 C225 C226 119.5(3) . . ? C221 C226 C225 120.6(3) . . ? C316 C311 C312 118.1(3) . . ? C316 C311 P31 120.7(2) . . ? C312 C311 P31 121.2(2) . . ? C313 C312 C311 121.0(3) . . ? C314 C313 C312 120.0(3) . . ? C315 C314 C313 120.0(3) . . ? C314 C315 C316 120.7(3) . . ? C311 C316 C315 120.2(3) . . ? C326 C321 C322 118.7(3) . . ? C326 C321 P31 120.0(2) . . ? C322 C321 P31 121.3(2) . . ? C323 C322 C321 119.8(3) . . ? C324 C323 C322 120.8(3) . . ? C323 C324 C325 120.2(3) . . ? C324 C325 C326 119.7(3) . . ? C325 C326 C321 120.8(3) . . ? C416 C411 C412 118.1(3) . . ? C416 C411 P41 122.9(2) . . ? C412 C411 P41 118.9(2) . . ? C413 C412 C411 121.0(3) . . ? C414 C413 C412 119.9(3) . . ? C415 C414 C413 119.6(3) . . ? C414 C415 C416 120.5(3) . . ? C411 C416 C415 120.8(3) . . ? C422 C421 C426 118.4(3) . . ? C422 C421 P41 119.2(2) . . ? C426 C421 P41 122.2(2) . . ? C423 C422 C421 120.6(3) . . ? C424 C423 C422 120.4(3) . . ? C425 C424 C423 119.4(3) . . ? C424 C425 C426 120.8(3) . . ? C425 C426 C421 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.485 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.075