Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Dr Rainer F. Winter' _publ_contact_author_address ; Institut fur Anorganische Chemie Universit=E4t Stuttgart Pfaffenwaldring 55 Stuttgart D-70569 GERMANY ; _publ_contact_author_phone '049 711 6854193' _publ_contact_author_fax '049 711 6854241' _publ_contact_author_email winter@iac.uni-stuttgart.de _publ_requested_journal 'Dalton Transactions' _publ_requested_coeditor_name ? _publ_section_title ; Aminoallenylidene complexes of ruthenium(II) from the regioselective addition of secondary amines to butatrienylidene intermediates: a combined experimental and theoretical study of the hindered rotation around the CN-bond ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Winter, Rainer' ; Institut fur Anorganische Chemie Universitat Stuttgart Pfaffenwaldring 55 70569 Stuttgart Bundesrepublik Deutschland ; 'Hartmann, Stephan' ; Institut fur Anorganische Chemie Universitat Stuttgart Pfaffenwaldring 55 70569 Stuttgart Bundesrepublik Deutschland ; 'Zalis, Stanislav' ; Heyrovsky Institute of Physical Chemistry Academy of Science of the Czech Republik Dolejskova 3 Prague Czech Republik ; 'Klinkhammer, Karl Wilhelm' ; Institut fur Anorganische Chemie Johannes-Gutenberg-Universitat Mainz Duesbergweg 10-14 55099 Mainz Bundesrepublik Deutschland ; #============================================================================ data_diffoq _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H57 Cl F6 N P4 Ru Sb' _chemical_formula_weight 1312.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8677(9) _cell_length_b 24.811(3) _cell_length_c 21.3714(16) _cell_angle_alpha 90.00 _cell_angle_beta 106.557(4) _cell_angle_gamma 90.00 _cell_volume 6540.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 9 _cell_measurement_theta_max 12 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4 4-circle-diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12324 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 24.00 _reflns_number_total 10209 _reflns_number_gt 6170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XScans' _computing_cell_refinement 'Siemens XScans' _computing_data_reduction 'Siemens XScans' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker Shelxtl 5.1 - XP' _computing_publication_material 'Bruker Shelxtl' _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^)+(0.0860P)^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 10209 _refine_ls_number_parameters 790 _refine_ls_number_restraints 979 _refine_ls_R_factor_all 0.1212 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1785 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.015 _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 0.01421(4) 0.68928(2) 0.25381(2) 0.02231(17) Uani 1 1 d . . . Cl1 Cl 0.02830(15) 0.71349(7) 0.14412(8) 0.0305(4) Uani 1 1 d . . . P11 P -0.02376(16) 0.59699(7) 0.23867(9) 0.0291(4) Uani 1 1 d . . . P12 P 0.17884(15) 0.64178(7) 0.27938(9) 0.0278(4) Uani 1 1 d . . . C10 C 0.1151(6) 0.5755(3) 0.2832(4) 0.0312(17) Uani 1 1 d . . . H10A H 0.1432 0.5470 0.2600 0.037 Uiso 1 1 calc R . . H10B H 0.1215 0.5641 0.3285 0.037 Uiso 1 1 calc R . . C111 C -0.1193(7) 0.5665(3) 0.2770(4) 0.040(2) Uani 1 1 d . . . C112 C -0.0899(7) 0.5527(3) 0.3434(4) 0.044(2) Uani 1 1 d . . . H112 H -0.0164 0.5536 0.3693 0.052 Uiso 1 1 calc R . . C113 C -0.1743(10) 0.5373(4) 0.3705(5) 0.065(3) Uani 1 1 d . . . H113 H -0.1568 0.5277 0.4154 0.078 Uiso 1 1 calc R . . C114 C -0.2786(9) 0.5360(4) 0.3341(6) 0.066(3) Uani 1 1 d . . . H114 H -0.3334 0.5260 0.3537 0.080 Uiso 1 1 calc R . . C115 C -0.3057(7) 0.5486(3) 0.2712(5) 0.056(3) Uani 1 1 d . . . H115 H -0.3797 0.5471 0.2463 0.067 Uiso 1 1 calc R . . C116 C -0.2280(7) 0.5637(3) 0.2412(4) 0.045(2) Uani 1 1 d . . . H116 H -0.2490 0.5723 0.1960 0.054 Uiso 1 1 calc R . . C121 C -0.0549(6) 0.5611(3) 0.1614(4) 0.0360(18) Uani 1 1 d . . . C122 C -0.0965(7) 0.5884(3) 0.1025(4) 0.049(2) Uani 1 1 d . . . H122 H -0.1091 0.6261 0.1020 0.058 Uiso 1 1 calc R . . C123 C -0.1189(9) 0.5594(4) 0.0446(4) 0.074(3) Uani 1 1 d . . . H123 H -0.1466 0.5775 0.0041 0.089 Uiso 1 1 calc R . . C124 C -0.1013(9) 0.5042(4) 0.0454(5) 0.073(3) Uani 1 1 d . . . H124 H -0.1169 0.4848 0.0054 0.087 Uiso 1 1 calc R . . C125 C -0.0618(9) 0.4778(4) 0.1030(5) 0.071(3) Uani 1 1 d . . . H125 H -0.0494 0.4400 0.1033 0.085 Uiso 1 1 calc R . . C126 C -0.0397(7) 0.5057(3) 0.1611(4) 0.048(2) Uani 1 1 d . . . H126 H -0.0138 0.4869 0.2012 0.057 Uiso 1 1 calc R . . C131 C 0.2583(6) 0.6316(3) 0.2207(3) 0.0310(17) Uani 1 1 d . . . C132 C 0.2166(6) 0.6017(3) 0.1641(3) 0.0376(18) Uani 1 1 d . . . H132 H 0.1442 0.5886 0.1537 0.045 Uiso 1 1 calc R . . C133 C 0.2781(7) 0.5910(4) 0.1233(4) 0.054(2) Uani 1 1 d . . . H133 H 0.2482 0.5699 0.0853 0.065 Uiso 1 1 calc R . . C134 C 0.3831(7) 0.6099(4) 0.1358(4) 0.052(2) Uani 1 1 d . . . H134 H 0.4267 0.6008 0.1081 0.062 Uiso 1 1 calc R . . C135 C 0.4232(7) 0.6428(4) 0.1907(4) 0.061(3) Uani 1 1 d . . . H135 H 0.4932 0.6584 0.1992 0.073 Uiso 1 1 calc R . . C136 C 0.3600(7) 0.6526(3) 0.2329(4) 0.047(2) Uani 1 1 d . . . H136 H 0.3883 0.6743 0.2706 0.056 Uiso 1 1 calc R . . C141 C 0.2883(6) 0.6490(3) 0.3540(3) 0.0310(17) Uani 1 1 d . . . C142 C 0.3067(7) 0.6994(3) 0.3842(3) 0.044(2) Uani 1 1 d . . . H142 H 0.2563 0.7279 0.3699 0.053 Uiso 1 1 calc R . . C143 C 0.4021(8) 0.7073(4) 0.4367(4) 0.061(3) Uani 1 1 d . . . H143 H 0.4169 0.7417 0.4566 0.074 Uiso 1 1 calc R . . C144 C 0.4717(8) 0.6663(4) 0.4585(4) 0.057(3) Uani 1 1 d . . . H144 H 0.5357 0.6725 0.4931 0.069 Uiso 1 1 calc R . . C145 C 0.4520(7) 0.6159(5) 0.4317(4) 0.063(3) Uani 1 1 d . . . H145 H 0.4997 0.5869 0.4490 0.075 Uiso 1 1 calc R . . C146 C 0.3600(7) 0.6077(4) 0.3778(4) 0.050(2) Uani 1 1 d . . . H146 H 0.3474 0.5732 0.3578 0.060 Uiso 1 1 calc R . . P21 P -0.15434(15) 0.73308(7) 0.22077(8) 0.0264(4) Uani 1 1 d . . . P22 P 0.04088(15) 0.78206(7) 0.27702(8) 0.0255(4) Uani 1 1 d . . . C20 C -0.0960(6) 0.8013(3) 0.2256(3) 0.0325(17) Uani 1 1 d . . . H20A H -0.1323 0.8272 0.2476 0.039 Uiso 1 1 calc R . . H20B H -0.0953 0.8154 0.1824 0.039 Uiso 1 1 calc R . . C211 C -0.2514(5) 0.7355(3) 0.2684(3) 0.0288(16) Uani 1 1 d . . . C212 C -0.2582(6) 0.6917(3) 0.3091(3) 0.0372(18) Uani 1 1 d . . . H212 H -0.2096 0.6621 0.3137 0.045 Uiso 1 1 calc R . . C213 C -0.3365(6) 0.6921(4) 0.3425(4) 0.048(2) Uani 1 1 d . . . H213 H -0.3448 0.6617 0.3677 0.058 Uiso 1 1 calc R . . C214 C -0.4012(7) 0.7361(4) 0.3389(4) 0.051(2) Uani 1 1 d . . . H214 H -0.4526 0.7361 0.3632 0.061 Uiso 1 1 calc R . . C215 C -0.3953(6) 0.7801(4) 0.3019(4) 0.051(2) Uani 1 1 d . . . H215 H -0.4417 0.8102 0.3000 0.061 Uiso 1 1 calc R . . C216 C -0.3181(6) 0.7795(3) 0.2664(4) 0.043(2) Uani 1 1 d . . . H216 H -0.3119 0.8099 0.2407 0.051 Uiso 1 1 calc R . . C221 C -0.2436(5) 0.7223(3) 0.1389(3) 0.0280(16) Uani 1 1 d . . . C222 C -0.3173(6) 0.6795(3) 0.1286(4) 0.0388(19) Uani 1 1 d . . . H222 H -0.3251 0.6596 0.1649 0.047 Uiso 1 1 calc R . . C223 C -0.3790(7) 0.6658(4) 0.0665(4) 0.048(2) Uani 1 1 d . . . H223 H -0.4283 0.6364 0.0601 0.058 Uiso 1 1 calc R . . C224 C -0.3683(7) 0.6954(4) 0.0134(4) 0.057(2) Uani 1 1 d . . . H224 H -0.4108 0.6862 -0.0294 0.068 Uiso 1 1 calc R . . C225 C -0.2978(7) 0.7374(4) 0.0221(4) 0.059(3) Uani 1 1 d . . . H225 H -0.2904 0.7571 -0.0145 0.071 Uiso 1 1 calc R . . C226 C -0.2366(7) 0.7514(3) 0.0847(3) 0.047(2) Uani 1 1 d . . . H226 H -0.1891 0.7814 0.0906 0.056 Uiso 1 1 calc R . . C231 C 0.1385(6) 0.8248(3) 0.2544(3) 0.0279(16) Uani 1 1 d . . . C232 C 0.1232(6) 0.8800(3) 0.2512(3) 0.0344(18) Uani 1 1 d . . . H232 H 0.0590 0.8952 0.2573 0.041 Uiso 1 1 calc R . . C233 C 0.2026(8) 0.9136(3) 0.2388(4) 0.051(2) Uani 1 1 d . . . H233 H 0.1933 0.9516 0.2379 0.061 Uiso 1 1 calc R . . C234 C 0.2923(7) 0.8920(4) 0.2282(4) 0.056(2) Uani 1 1 d . . . H234 H 0.3458 0.9149 0.2195 0.067 Uiso 1 1 calc R . . C235 C 0.3071(7) 0.8359(4) 0.2298(4) 0.056(2) Uani 1 1 d . . . H235 H 0.3703 0.8209 0.2221 0.068 Uiso 1 1 calc R . . C236 C 0.2310(6) 0.8027(3) 0.2424(3) 0.0382(19) Uani 1 1 d . . . H236 H 0.2407 0.7648 0.2431 0.046 Uiso 1 1 calc R . . C241 C 0.0498(6) 0.8067(3) 0.3588(3) 0.0318(17) Uani 1 1 d . . . C242 C 0.1497(7) 0.8210(3) 0.4002(3) 0.041(2) Uani 1 1 d . . . H242 H 0.2116 0.8203 0.3843 0.050 Uiso 1 1 calc R . . C243 C 0.1620(8) 0.8365(3) 0.4645(4) 0.052(2) Uani 1 1 d . . . H243 H 0.2315 0.8459 0.4921 0.062 Uiso 1 1 calc R . . C244 C 0.0742(10) 0.8379(4) 0.4878(4) 0.061(3) Uani 1 1 d . . . H244 H 0.0827 0.8477 0.5319 0.073 Uiso 1 1 calc R . . C245 C -0.0264(9) 0.8253(3) 0.4479(4) 0.060(3) Uani 1 1 d . . . H245 H -0.0879 0.8275 0.4640 0.072 Uiso 1 1 calc R . . C246 C -0.0391(7) 0.8090(3) 0.3826(4) 0.043(2) Uani 1 1 d . . . H246 H -0.1088 0.7996 0.3552 0.051 Uiso 1 1 calc R . . C1 C 0.0148(5) 0.6771(3) 0.3439(3) 0.0241(15) Uani 1 1 d . . . C2 C 0.0226(6) 0.6703(3) 0.4015(3) 0.0349(18) Uani 1 1 d . . . C3 C 0.0150(7) 0.6664(3) 0.4653(3) 0.0375(19) Uani 1 1 d . . . C31 C -0.0834(8) 0.6921(4) 0.4798(4) 0.067(3) Uani 1 1 d . . . H31A H -0.1333 0.6638 0.4851 0.100 Uiso 1 1 calc R . . H31B H -0.1203 0.7157 0.4435 0.100 Uiso 1 1 calc R . . H31C H -0.0596 0.7133 0.5200 0.100 Uiso 1 1 calc R . . N4 N 0.0840(6) 0.6407(3) 0.5113(3) 0.053(2) Uani 1 1 d . . . C41 C 0.0713(9) 0.6389(5) 0.5794(4) 0.083(4) Uani 1 1 d . . . H41A H 0.0732 0.6757 0.5965 0.124 Uiso 1 1 calc R . . H41B H 0.1307 0.6179 0.6078 0.124 Uiso 1 1 calc R . . H41C H 0.0019 0.6221 0.5782 0.124 Uiso 1 1 calc R . . C5 C 0.1825(8) 0.6185(4) 0.5038(5) 0.064(3) Uani 1 1 d . . . H5A H 0.1829 0.6207 0.4576 0.076 Uiso 1 1 calc R . . H5B H 0.1893 0.5802 0.5173 0.076 Uiso 1 1 calc R . . C51 C 0.2790(8) 0.6519(4) 0.5481(4) 0.060(3) Uani 1 1 d . . . C52 C 0.3774(8) 0.6265(5) 0.5800(5) 0.078(3) Uani 1 1 d . . . H52 H 0.3839 0.5884 0.5780 0.094 Uiso 1 1 calc R . . C53 C 0.4636(8) 0.6570(7) 0.6138(4) 0.084(4) Uani 1 1 d . . . H53 H 0.5293 0.6392 0.6357 0.101 Uiso 1 1 calc R . . C54 C 0.4597(10) 0.7124(6) 0.6176(5) 0.083(4) Uani 1 1 d . . . H54 H 0.5220 0.7327 0.6394 0.100 Uiso 1 1 calc R . . C55 C 0.3648(11) 0.7365(5) 0.5894(6) 0.089(4) Uani 1 1 d . . . H55 H 0.3600 0.7746 0.5928 0.106 Uiso 1 1 calc R . . C56 C 0.2726(10) 0.7079(4) 0.5552(5) 0.086(4) Uani 1 1 d . . . H56 H 0.2060 0.7262 0.5369 0.103 Uiso 1 1 calc R . . Sb1A Sb 0.23723(18) 0.44677(8) 0.43676(12) 0.0762(7) Uani 0.550(3) 1 d PDU A 1 F1 F 0.3607(5) 0.4366(4) 0.4131(4) 0.155(6) Uani 0.550(3) 1 d PDU A 1 F2 F 0.1138(5) 0.4570(4) 0.4605(4) 0.130(5) Uani 0.550(3) 1 d PDU A 1 F3 F 0.2366(9) 0.5175(2) 0.4145(7) 0.104(9) Uani 0.293(10) 1 d PDU A 1 F4 F 0.3176(6) 0.4629(6) 0.5193(3) 0.090(7) Uani 0.293(10) 1 d PDU A 1 F5 F 0.1568(6) 0.4307(6) 0.3542(3) 0.180(13) Uani 0.293(10) 1 d PDU A 1 F6 F 0.2378(9) 0.3761(2) 0.4590(7) 0.195(15) Uani 0.293(10) 1 d PDU A 1 Sb1B Sb 0.2280(3) 0.43807(12) 0.4006(2) 0.1262(15) Uani 0.450(3) 1 d PDU A 2 F7 F 0.2680(10) 0.3741(3) 0.3732(6) 0.217(10) Uani 0.450(3) 1 d PDU A 2 F8 F 0.3104(10) 0.4735(5) 0.3575(6) 0.213(11) Uani 0.450(3) 1 d PDU A 2 F9 F 0.1880(10) 0.5021(3) 0.4280(6) 0.111(6) Uani 0.450(3) 1 d PDU A 2 F10 F 0.1455(10) 0.4026(5) 0.4436(6) 0.300(15) Uani 0.450(3) 1 d PDU A 2 F11 F 0.1127(8) 0.4413(5) 0.3281(4) 0.131(7) Uani 0.450(3) 1 d PDU A 2 F12 F 0.3433(8) 0.4350(5) 0.4731(5) 0.281(14) Uani 0.450(3) 1 d PDU A 2 F3B F 0.2835(9) 0.3979(5) 0.5022(6) 0.090(8) Uani 0.257(10) 1 d PDU B 3 F4B F 0.1715(8) 0.3932(5) 0.3817(6) 0.124(10) Uani 0.257(10) 1 d PDU B 3 F5B F 0.1909(9) 0.4956(5) 0.3714(6) 0.172(14) Uani 0.257(10) 1 d PDU B 3 F6B F 0.3029(8) 0.5004(5) 0.4918(7) 0.190(15) Uani 0.257(10) 1 d PDU B 3 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 0.0236(3) 0.0232(3) 0.0216(3) 0.0005(2) 0.0088(2) 0.0004(3) Cl1 0.0368(10) 0.0333(9) 0.0246(9) 0.0011(7) 0.0140(8) -0.0007(8) P11 0.0313(10) 0.0246(10) 0.0333(10) 0.0002(8) 0.0122(9) -0.0001(9) P12 0.0268(11) 0.0278(10) 0.0310(10) 0.0015(8) 0.0118(9) 0.0019(8) C10 0.038(4) 0.017(4) 0.040(4) 0.012(3) 0.013(4) 0.004(3) C111 0.049(5) 0.017(4) 0.060(5) -0.001(4) 0.027(5) 0.005(4) C112 0.061(6) 0.030(4) 0.048(5) 0.003(4) 0.028(4) -0.014(4) C113 0.100(9) 0.063(6) 0.055(6) 0.002(5) 0.058(6) -0.014(6) C114 0.064(7) 0.042(5) 0.120(10) -0.003(6) 0.070(7) -0.011(5) C115 0.039(5) 0.042(5) 0.099(8) 0.010(5) 0.039(6) -0.001(4) C116 0.038(5) 0.036(5) 0.066(6) 0.008(4) 0.021(4) 0.005(4) C121 0.038(5) 0.032(4) 0.044(4) -0.005(4) 0.020(4) -0.008(4) C122 0.051(5) 0.041(5) 0.051(5) -0.013(4) 0.010(4) -0.015(4) C123 0.108(9) 0.074(7) 0.042(5) -0.017(5) 0.023(6) -0.042(7) C124 0.091(9) 0.069(7) 0.069(7) -0.040(6) 0.041(7) -0.035(7) C125 0.079(8) 0.050(6) 0.090(8) -0.025(6) 0.033(7) -0.022(6) C126 0.065(6) 0.033(5) 0.046(5) -0.013(4) 0.018(5) -0.008(4) C131 0.026(4) 0.032(4) 0.035(4) 0.007(3) 0.009(3) 0.008(3) C132 0.033(4) 0.051(5) 0.031(4) 0.001(4) 0.012(4) -0.002(4) C133 0.054(6) 0.075(7) 0.032(4) -0.012(4) 0.011(4) 0.005(5) C134 0.046(5) 0.077(7) 0.038(5) 0.001(5) 0.023(4) 0.012(5) C135 0.039(5) 0.091(8) 0.061(6) -0.003(5) 0.026(5) -0.008(5) C136 0.035(5) 0.056(6) 0.052(5) -0.014(4) 0.016(4) -0.004(4) C141 0.025(4) 0.047(5) 0.023(4) 0.003(3) 0.010(3) 0.007(4) C142 0.052(5) 0.049(5) 0.028(4) 0.002(4) 0.007(4) -0.004(4) C143 0.053(6) 0.091(8) 0.037(5) -0.010(5) 0.006(5) -0.022(6) C144 0.044(6) 0.093(8) 0.031(5) 0.002(5) 0.003(4) -0.002(6) C145 0.032(5) 0.102(9) 0.045(5) 0.018(5) -0.004(4) 0.017(5) C146 0.037(5) 0.064(6) 0.048(5) 0.004(4) 0.010(4) 0.007(5) P21 0.0253(10) 0.0298(10) 0.0259(9) 0.0027(8) 0.0104(8) 0.0017(8) P22 0.0287(10) 0.0243(10) 0.0256(9) -0.0025(8) 0.0112(8) -0.0015(8) C20 0.032(4) 0.035(4) 0.029(4) 0.004(3) 0.007(3) 0.000(3) C211 0.018(4) 0.041(4) 0.026(4) -0.002(3) 0.005(3) 0.002(3) C212 0.032(4) 0.050(5) 0.032(4) 0.000(4) 0.013(3) -0.008(4) C213 0.039(5) 0.069(6) 0.036(4) 0.005(4) 0.011(4) -0.011(5) C214 0.029(5) 0.088(7) 0.037(5) -0.011(5) 0.013(4) -0.011(5) C215 0.023(4) 0.067(6) 0.061(6) -0.014(5) 0.009(4) 0.015(4) C216 0.026(4) 0.049(5) 0.051(5) 0.003(4) 0.008(4) 0.006(4) C221 0.018(4) 0.037(4) 0.028(4) 0.002(3) 0.005(3) 0.003(3) C222 0.034(4) 0.047(5) 0.039(4) 0.011(4) 0.015(4) -0.003(4) C223 0.048(5) 0.054(5) 0.041(5) -0.004(4) 0.009(4) -0.011(4) C224 0.047(5) 0.084(7) 0.033(4) 0.001(5) 0.002(4) -0.001(6) C225 0.045(6) 0.087(7) 0.039(5) 0.021(5) 0.001(4) -0.019(5) C226 0.044(5) 0.058(5) 0.032(4) 0.008(4) 0.002(4) -0.015(4) C231 0.036(4) 0.020(4) 0.029(4) 0.002(3) 0.011(3) 0.001(3) C232 0.042(5) 0.031(4) 0.034(4) -0.004(3) 0.016(4) -0.008(4) C233 0.071(7) 0.029(4) 0.057(5) -0.007(4) 0.025(5) -0.015(5) C234 0.052(6) 0.057(6) 0.066(6) -0.002(5) 0.030(5) -0.022(5) C235 0.040(5) 0.068(6) 0.067(6) -0.003(5) 0.024(5) -0.001(5) C236 0.041(5) 0.033(4) 0.045(4) 0.000(4) 0.019(4) 0.006(4) C241 0.049(5) 0.020(4) 0.031(4) 0.004(3) 0.019(4) -0.001(4) C242 0.055(5) 0.039(5) 0.031(4) -0.002(3) 0.013(4) 0.007(4) C243 0.068(7) 0.047(5) 0.033(5) -0.006(4) 0.001(5) -0.005(5) C244 0.106(9) 0.048(5) 0.033(5) -0.013(4) 0.026(6) -0.021(6) C245 0.084(8) 0.047(6) 0.068(6) -0.012(5) 0.053(6) -0.013(5) C246 0.054(5) 0.046(5) 0.037(4) -0.013(4) 0.028(4) -0.014(4) C1 0.027(4) 0.024(4) 0.021(4) -0.004(3) 0.008(3) -0.001(3) C2 0.032(4) 0.042(5) 0.026(4) 0.003(3) 0.001(3) -0.004(4) C3 0.045(5) 0.042(4) 0.024(4) 0.006(3) 0.008(4) -0.015(4) C31 0.086(7) 0.089(7) 0.043(5) 0.007(5) 0.047(5) 0.006(6) N4 0.065(5) 0.062(5) 0.028(4) 0.008(3) 0.008(4) -0.019(4) C41 0.112(9) 0.112(9) 0.019(4) 0.009(5) 0.011(5) -0.030(8) C5 0.068(7) 0.059(6) 0.063(6) 0.019(5) 0.017(6) 0.006(5) C51 0.057(6) 0.074(7) 0.048(5) 0.015(5) 0.015(5) -0.008(5) C52 0.051(7) 0.099(9) 0.077(7) 0.026(6) 0.005(6) 0.016(6) C53 0.031(6) 0.171(14) 0.040(6) 0.011(8) -0.005(5) -0.008(8) C54 0.070(9) 0.123(11) 0.052(7) 0.010(7) 0.010(6) -0.030(9) C55 0.096(10) 0.076(8) 0.082(8) 0.001(6) 0.008(8) -0.029(8) C56 0.075(8) 0.060(7) 0.101(9) 0.013(6) -0.009(7) -0.005(6) Sb1A 0.0734(13) 0.0426(9) 0.1112(17) -0.0087(10) 0.0240(14) -0.0054(8) F1 0.098(10) 0.227(15) 0.169(12) 0.020(11) 0.085(10) 0.008(10) F2 0.110(10) 0.150(12) 0.124(10) -0.062(9) 0.025(8) -0.002(9) F3 0.135(17) 0.074(12) 0.080(13) 0.059(10) -0.006(12) -0.025(12) F4 0.082(12) 0.151(16) 0.035(9) 0.029(10) 0.013(9) 0.044(11) F5 0.18(2) 0.181(19) 0.146(17) -0.128(15) -0.014(15) -0.001(16) F6 0.18(2) 0.16(2) 0.26(2) 0.016(16) 0.086(16) -0.006(16) Sb1B 0.122(2) 0.0512(15) 0.147(3) 0.0110(18) -0.057(2) 0.0003(14) F7 0.221(18) 0.097(12) 0.267(18) -0.019(13) -0.037(14) 0.023(13) F8 0.214(18) 0.179(17) 0.270(19) 0.013(15) 0.107(15) -0.027(15) F9 0.115(12) 0.126(12) 0.094(10) -0.008(10) 0.034(9) 0.001(10) F10 0.30(2) 0.27(2) 0.32(2) 0.137(16) 0.067(16) 0.000(17) F11 0.097(11) 0.124(12) 0.134(12) -0.004(10) -0.031(10) 0.019(10) F12 0.243(19) 0.27(2) 0.27(2) 0.041(16) -0.026(15) 0.058(16) F3B 0.080(13) 0.106(15) 0.072(12) 0.001(11) 0.001(11) -0.049(12) F4B 0.139(16) 0.100(15) 0.126(15) -0.096(12) 0.028(13) 0.008(13) F5B 0.17(2) 0.149(19) 0.18(2) 0.075(16) 0.017(16) -0.003(16) F6B 0.18(2) 0.17(2) 0.20(2) -0.025(16) 0.033(16) -0.026(16) _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 1.947(6) . ? Ru1 P11 2.3446(19) . ? Ru1 P21 2.3474(19) . ? Ru1 P12 2.349(2) . ? Ru1 P22 2.3593(19) . ? Ru1 Cl1 2.4763(17) . ? P11 C121 1.819(7) . ? P11 C111 1.823(8) . ? P11 C10 1.848(7) . ? P12 C141 1.812(7) . ? P12 C131 1.847(7) . ? P12 C10 1.849(7) . ? C111 C116 1.392(11) . ? C111 C112 1.404(10) . ? C112 C113 1.422(12) . ? C113 C114 1.346(14) . ? C114 C115 1.326(13) . ? C115 C116 1.385(11) . ? C121 C126 1.388(10) . ? C121 C122 1.395(11) . ? C122 C123 1.389(11) . ? C123 C124 1.388(14) . ? C124 C125 1.360(14) . ? C125 C126 1.378(11) . ? C131 C136 1.364(10) . ? C131 C132 1.391(10) . ? C132 C133 1.360(10) . ? C133 C134 1.383(12) . ? C134 C135 1.401(12) . ? C135 C136 1.397(11) . ? C141 C146 1.375(11) . ? C141 C142 1.396(10) . ? C142 C143 1.420(11) . ? C143 C144 1.347(13) . ? C144 C145 1.368(13) . ? C145 C146 1.412(11) . ? P21 C221 1.819(7) . ? P21 C211 1.823(7) . ? P21 C20 1.842(7) . ? P22 C231 1.812(7) . ? P22 C241 1.824(7) . ? P22 C20 1.852(7) . ? C211 C216 1.383(10) . ? C211 C212 1.411(10) . ? C212 C213 1.391(10) . ? C213 C214 1.363(12) . ? C214 C215 1.363(12) . ? C215 C216 1.409(11) . ? C221 C226 1.389(10) . ? C221 C222 1.397(10) . ? C222 C223 1.381(10) . ? C223 C224 1.390(11) . ? C224 C225 1.359(12) . ? C225 C226 1.389(11) . ? C231 C232 1.383(9) . ? C231 C236 1.398(10) . ? C232 C233 1.399(11) . ? C233 C234 1.349(12) . ? C234 C235 1.406(12) . ? C235 C236 1.363(11) . ? C241 C246 1.379(10) . ? C241 C242 1.383(11) . ? C242 C243 1.393(10) . ? C243 C244 1.357(13) . ? C244 C245 1.368(13) . ? C245 C246 1.417(11) . ? C1 C2 1.217(9) . ? C2 C3 1.398(9) . ? C3 N4 1.290(10) . ? C3 C31 1.526(12) . ? N4 C5 1.432(12) . ? N4 C41 1.512(9) . ? C5 C51 1.567(13) . ? C51 C56 1.402(14) . ? C51 C52 1.405(13) . ? C52 C53 1.368(14) . ? C53 C54 1.379(16) . ? C54 C55 1.339(16) . ? C55 C56 1.398(14) . ? Sb1A F5 1.817(5) . ? Sb1A F6 1.817(5) . ? Sb1A F1 1.817(5) . ? Sb1A F3 1.817(5) . ? Sb1A F4 1.817(5) . ? Sb1A F2 1.817(5) . ? Sb1B F10 1.816(5) . ? Sb1B F7 1.817(5) . ? Sb1B F12 1.817(5) . ? Sb1B F11 1.817(5) . ? Sb1B F9 1.817(5) . ? Sb1B F8 1.817(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 85.78(19) . . ? C1 Ru1 P21 96.5(2) . . ? P11 Ru1 P21 105.80(7) . . ? C1 Ru1 P12 86.7(2) . . ? P11 Ru1 P12 71.38(7) . . ? P21 Ru1 P12 175.64(7) . . ? C1 Ru1 P22 89.12(19) . . ? P11 Ru1 P22 173.78(7) . . ? P21 Ru1 P22 71.22(7) . . ? P12 Ru1 P22 111.91(7) . . ? C1 Ru1 Cl1 173.35(19) . . ? P11 Ru1 Cl1 100.07(6) . . ? P21 Ru1 Cl1 85.04(6) . . ? P12 Ru1 Cl1 92.14(6) . . ? P22 Ru1 Cl1 85.23(6) . . ? C121 P11 C111 101.7(3) . . ? C121 P11 C10 104.9(3) . . ? C111 P11 C10 109.0(3) . . ? C121 P11 Ru1 126.0(3) . . ? C111 P11 Ru1 118.9(2) . . ? C10 P11 Ru1 94.4(2) . . ? C141 P12 C131 99.7(3) . . ? C141 P12 C10 106.9(3) . . ? C131 P12 C10 104.3(3) . . ? C141 P12 Ru1 125.4(2) . . ? C131 P12 Ru1 123.2(2) . . ? C10 P12 Ru1 94.3(2) . . ? P11 C10 P12 95.6(3) . . ? C116 C111 C112 118.8(8) . . ? C116 C111 P11 118.3(6) . . ? C112 C111 P11 122.3(6) . . ? C111 C112 C113 117.5(9) . . ? C114 C113 C112 121.4(9) . . ? C115 C114 C113 120.8(9) . . ? C114 C115 C116 121.1(9) . . ? C115 C116 C111 120.3(8) . . ? C126 C121 C122 119.7(7) . . ? C126 C121 P11 119.6(6) . . ? C122 C121 P11 120.7(6) . . ? C123 C122 C121 118.8(8) . . ? C124 C123 C122 120.6(10) . . ? C125 C124 C123 120.3(9) . . ? C124 C125 C126 120.1(10) . . ? C125 C126 C121 120.6(9) . . ? C136 C131 C132 118.8(7) . . ? C136 C131 P12 120.3(6) . . ? C132 C131 P12 120.9(6) . . ? C133 C132 C131 120.7(8) . . ? C132 C133 C134 121.8(8) . . ? C133 C134 C135 117.7(8) . . ? C136 C135 C134 120.0(8) . . ? C131 C136 C135 120.8(8) . . ? C146 C141 C142 119.3(7) . . ? C146 C141 P12 121.6(6) . . ? C142 C141 P12 118.8(6) . . ? C141 C142 C143 118.9(8) . . ? C144 C143 C142 120.6(9) . . ? C143 C144 C145 121.3(9) . . ? C144 C145 C146 119.1(9) . . ? C141 C146 C145 120.8(9) . . ? C221 P21 C211 101.4(3) . . ? C221 P21 C20 109.0(3) . . ? C211 P21 C20 105.8(3) . . ? C221 P21 Ru1 119.8(2) . . ? C211 P21 Ru1 124.6(2) . . ? C20 P21 Ru1 94.7(2) . . ? C231 P22 C241 101.5(3) . . ? C231 P22 C20 107.8(3) . . ? C241 P22 C20 105.7(3) . . ? C231 P22 Ru1 125.8(2) . . ? C241 P22 Ru1 119.6(2) . . ? C20 P22 Ru1 94.0(2) . . ? P21 C20 P22 95.8(3) . . ? C216 C211 C212 118.7(7) . . ? C216 C211 P21 121.8(6) . . ? C212 C211 P21 119.4(5) . . ? C213 C212 C211 119.5(8) . . ? C214 C213 C212 119.9(8) . . ? C213 C214 C215 122.7(8) . . ? C214 C215 C216 118.0(8) . . ? C211 C216 C215 121.2(8) . . ? C226 C221 C222 117.7(6) . . ? C226 C221 P21 123.5(6) . . ? C222 C221 P21 118.5(5) . . ? C223 C222 C221 121.1(7) . . ? C222 C223 C224 119.3(8) . . ? C225 C224 C223 120.7(8) . . ? C224 C225 C226 119.7(8) . . ? C221 C226 C225 121.3(8) . . ? C232 C231 C236 119.7(7) . . ? C232 C231 P22 119.6(6) . . ? C236 C231 P22 120.7(5) . . ? C231 C232 C233 119.8(8) . . ? C234 C233 C232 120.1(8) . . ? C233 C234 C235 120.3(8) . . ? C236 C235 C234 120.2(8) . . ? C235 C236 C231 119.8(7) . . ? C246 C241 C242 118.1(7) . . ? C246 C241 P22 122.3(6) . . ? C242 C241 P22 119.4(6) . . ? C241 C242 C243 121.6(8) . . ? C244 C243 C242 119.8(8) . . ? C243 C244 C245 120.3(8) . . ? C244 C245 C246 120.1(8) . . ? C241 C246 C245 120.0(8) . . ? C2 C1 Ru1 175.6(6) . . ? C1 C2 C3 170.8(8) . . ? N4 C3 C2 123.6(8) . . ? N4 C3 C31 118.9(7) . . ? C2 C3 C31 117.4(7) . . ? C3 N4 C5 123.0(7) . . ? C3 N4 C41 120.5(8) . . ? C5 N4 C41 116.0(8) . . ? N4 C5 C51 107.7(8) . . ? C56 C51 C52 117.8(10) . . ? C56 C51 C5 121.9(9) . . ? C52 C51 C5 120.2(10) . . ? C53 C52 C51 119.4(11) . . ? C52 C53 C54 123.0(12) . . ? C55 C54 C53 117.6(12) . . ? C54 C55 C56 122.5(12) . . ? C55 C56 C51 119.5(11) . . ? F5 Sb1A F6 90.01(6) . . ? F5 Sb1A F1 90.04(6) . . ? F6 Sb1A F1 90.00(6) . . ? F5 Sb1A F3 89.99(6) . . ? F6 Sb1A F3 179.98(9) . . ? F1 Sb1A F3 90.02(6) . . ? F5 Sb1A F4 179.97(9) . . ? F6 Sb1A F4 90.01(6) . . ? F1 Sb1A F4 89.99(6) . . ? F3 Sb1A F4 89.99(6) . . ? F5 Sb1A F2 90.01(6) . . ? F6 Sb1A F2 90.00(6) . . ? F1 Sb1A F2 179.96(7) . . ? F3 Sb1A F2 89.98(6) . . ? F4 Sb1A F2 89.97(6) . . ? F10 Sb1B F7 90.03(6) . . ? F10 Sb1B F12 90.03(6) . . ? F7 Sb1B F12 90.02(6) . . ? F10 Sb1B F11 90.02(6) . . ? F7 Sb1B F11 90.03(6) . . ? F12 Sb1B F11 179.93(9) . . ? F10 Sb1B F9 90.02(6) . . ? F7 Sb1B F9 179.95(8) . . ? F12 Sb1B F9 90.00(6) . . ? F11 Sb1B F9 89.96(6) . . ? F10 Sb1B F8 179.97(10) . . ? F7 Sb1B F8 89.99(6) . . ? F12 Sb1B F8 89.99(6) . . ? F11 Sb1B F8 89.96(6) . . ? F9 Sb1B F8 89.96(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.995 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.104