Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_nm3 _database_code_depnum_ccdc_archive 'CCDC 293457' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 F12 N6 P2 Ru' _chemical_formula_weight 885.60 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' 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 9.0813(8) _cell_length_b 10.6974(9) _cell_length_c 17.7534(14) _cell_angle_alpha 87.438(2) _cell_angle_beta 85.6830(10) _cell_angle_gamma 83.579(2) _cell_volume 1707.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2806 _cell_measurement_theta_min 3.018 _cell_measurement_theta_max 28.931 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7314 _exptl_absorpt_correction_T_max 0.9935 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10813 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.2594 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 29.05 _reflns_number_total 7717 _reflns_number_gt 3414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0493P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7717 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2104 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.1716 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _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 0.49648(8) 0.26096(7) 0.75681(4) 0.0219(2) Uani 1 1 d . . . N101 N 0.6143(7) 0.4017(6) 0.7087(3) 0.0250(16) Uani 1 1 d . . . C102 C 0.5714(9) 0.5282(8) 0.7107(4) 0.031(2) Uani 1 1 d . . . H10A H 0.4783 0.5563 0.7358 0.037 Uiso 1 1 calc R . . C103 C 0.6579(10) 0.6169(8) 0.6776(4) 0.035(2) Uani 1 1 d . . . H10D H 0.6239 0.7041 0.6790 0.042 Uiso 1 1 calc R . . C104 C 0.7928(10) 0.5768(9) 0.6431(5) 0.038(2) Uani 1 1 d . . . H10B H 0.8553 0.6364 0.6215 0.045 Uiso 1 1 calc R . . C105 C 0.8392(9) 0.4492(9) 0.6395(4) 0.032(2) Uani 1 1 d . . . H10C H 0.9318 0.4207 0.6140 0.039 Uiso 1 1 calc R . . C106 C 0.7483(8) 0.3630(8) 0.6736(4) 0.026(2) Uani 1 1 d . . . C107 C 0.7859(8) 0.2267(8) 0.6731(4) 0.0238(19) Uani 1 1 d . . . C108 C 0.9119(9) 0.1671(9) 0.6343(5) 0.040(2) Uani 1 1 d . . . H10E H 0.9804 0.2155 0.6064 0.049 Uiso 1 1 calc R . . C109 C 0.9364(10) 0.0365(9) 0.6367(5) 0.038(2) Uani 1 1 d . . . H10F H 1.0194 -0.0059 0.6091 0.046 Uiso 1 1 calc R . . C110 C 0.8388(9) -0.0297(9) 0.6798(5) 0.040(2) Uani 1 1 d . . . H11B H 0.8565 -0.1189 0.6838 0.048 Uiso 1 1 calc R . . C111 C 0.7141(9) 0.0312(8) 0.7177(4) 0.029(2) Uani 1 1 d . . . H11A H 0.6463 -0.0163 0.7467 0.034 Uiso 1 1 calc R . . N112 N 0.6887(6) 0.1586(6) 0.7134(3) 0.0216(16) Uani 1 1 d . . . N201 N 0.4102(7) 0.2188(7) 0.6583(3) 0.0267(17) Uani 1 1 d . . . C202 C 0.4228(8) 0.2805(9) 0.5921(5) 0.037(2) Uani 1 1 d . . . H20A H 0.4593 0.3605 0.5904 0.045 Uiso 1 1 calc R . . C203 C 0.3850(10) 0.2336(11) 0.5245(5) 0.054(3) Uani 1 1 d . . . H20C H 0.3923 0.2812 0.4782 0.065 Uiso 1 1 calc R . . C204 C 0.3368(10) 0.1153(11) 0.5282(6) 0.054(3) Uani 1 1 d . . . H20D H 0.3128 0.0793 0.4833 0.065 Uiso 1 1 calc R . . C205 C 0.3232(9) 0.0492(10) 0.5962(5) 0.044(3) Uani 1 1 d . . . H20E H 0.2911 -0.0325 0.5982 0.053 Uiso 1 1 calc R . . C206 C 0.3563(8) 0.1023(9) 0.6614(5) 0.030(2) Uani 1 1 d . . . C207 C 0.3352(8) 0.0465(8) 0.7365(5) 0.029(2) Uani 1 1 d . . . C208 C 0.2632(9) -0.0612(9) 0.7534(6) 0.044(3) Uani 1 1 d . . . H20B H 0.2292 -0.1057 0.7142 0.053 Uiso 1 1 calc R . . C209 C 0.2427(10) -0.1012(10) 0.8264(6) 0.052(3) Uani 1 1 d . . . H20F H 0.1918 -0.1733 0.8382 0.063 Uiso 1 1 calc R . . C210 C 0.2940(9) -0.0397(8) 0.8842(5) 0.039(2) Uani 1 1 d . . . H21B H 0.2811 -0.0686 0.9354 0.046 Uiso 1 1 calc R . . C211 C 0.3648(8) 0.0656(8) 0.8643(4) 0.028(2) Uani 1 1 d . . . H21A H 0.3999 0.1104 0.9031 0.033 Uiso 1 1 calc R . . N212 N 0.3859(6) 0.1069(6) 0.7929(4) 0.0217(16) Uani 1 1 d . . . N301 N 0.3191(7) 0.3805(6) 0.7987(3) 0.0219(16) Uani 1 1 d . . . C302 C 0.1900(8) 0.4149(8) 0.7672(4) 0.0256(19) Uani 1 1 d . . . H30B H 0.1698 0.3755 0.7228 0.031 Uiso 1 1 calc R . . C303 C 0.0862(8) 0.5063(8) 0.7978(4) 0.029(2) Uani 1 1 d . . . H30A H -0.0037 0.5286 0.7740 0.035 Uiso 1 1 calc R . . C304 C 0.1105(9) 0.5655(8) 0.8621(5) 0.033(2) Uani 1 1 d . . . H30C H 0.0402 0.6299 0.8825 0.039 Uiso 1 1 calc R . . C305 C 0.2403(9) 0.5280(7) 0.8956(4) 0.0254(19) Uani 1 1 d . . . H30E H 0.2601 0.5647 0.9410 0.030 Uiso 1 1 calc R . . C306 C 0.3419(8) 0.4366(8) 0.8631(4) 0.0234(19) Uani 1 1 d . . . C307 C 0.4810(8) 0.3892(7) 0.8945(4) 0.0241(19) Uani 1 1 d . . . H30D H 0.5080 0.4196 0.9404 0.029 Uiso 1 1 calc R . . N308 N 0.5677(7) 0.3040(6) 0.8581(3) 0.0209(15) Uani 1 1 d . . . C309 C 0.7091(8) 0.2613(7) 0.8877(4) 0.0211(18) Uani 1 1 d . . . C310 C 0.7985(8) 0.3482(7) 0.9111(4) 0.026(2) Uani 1 1 d . . . H31C H 0.7678 0.4361 0.9076 0.031 Uiso 1 1 calc R . . C311 C 0.9333(8) 0.3029(8) 0.9396(4) 0.030(2) Uani 1 1 d . . . H31E H 0.9944 0.3606 0.9569 0.036 Uiso 1 1 calc R . . C312 C 0.9803(8) 0.1762(8) 0.9432(4) 0.026(2) Uani 1 1 d . . . H31D H 1.0730 0.1472 0.9628 0.031 Uiso 1 1 calc R . . C313 C 0.8926(9) 0.0913(8) 0.9183(4) 0.034(2) Uani 1 1 d . . . H31A H 0.9256 0.0038 0.9202 0.040 Uiso 1 1 calc R . . C314 C 0.7568(8) 0.1334(7) 0.8904(4) 0.0246(19) Uani 1 1 d . . . H31B H 0.6965 0.0750 0.8731 0.030 Uiso 1 1 calc R . . P10 P -0.3201(2) 0.7442(2) 0.89940(13) 0.0292(6) Uani 1 1 d . . . F11 F -0.4653(5) 0.6762(6) 0.9205(3) 0.0648(17) Uani 1 1 d . . . F12 F -0.1736(6) 0.8105(5) 0.8776(3) 0.0646(17) Uani 1 1 d . . . F13 F -0.3807(6) 0.8528(5) 0.9551(3) 0.0654(17) Uani 1 1 d . . . F14 F -0.2564(6) 0.6359(5) 0.8430(3) 0.0509(15) Uani 1 1 d . . . F15 F -0.3982(5) 0.8203(5) 0.8318(3) 0.0494(14) Uani 1 1 d . . . F16 F -0.2419(6) 0.6656(5) 0.9669(3) 0.0545(16) Uani 1 1 d . . . P20 P 0.7924(3) 0.3243(2) 0.42832(13) 0.0354(6) Uani 1 1 d . . . F21 F 0.9309(6) 0.3471(6) 0.4736(3) 0.0702(19) Uani 1 1 d . . . F22 F 0.6566(6) 0.2963(7) 0.3828(3) 0.074(2) Uani 1 1 d . . . F23 F 0.7834(8) 0.1936(6) 0.4736(4) 0.091(2) Uani 1 1 d . . . F24 F 0.8060(8) 0.4514(6) 0.3833(3) 0.086(2) Uani 1 1 d . . . F25 F 0.6830(6) 0.3933(6) 0.4902(3) 0.080(2) Uani 1 1 d . . . F26 F 0.9016(6) 0.2543(6) 0.3655(3) 0.076(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0179(3) 0.0231(4) 0.0249(4) -0.0032(3) -0.0012(3) -0.0024(3) N101 0.026(4) 0.028(4) 0.022(4) 0.004(4) -0.002(3) -0.007(3) C102 0.032(5) 0.024(5) 0.036(5) -0.005(4) -0.005(4) -0.004(4) C103 0.048(6) 0.021(5) 0.038(5) -0.001(4) 0.000(4) -0.011(5) C104 0.036(6) 0.039(6) 0.042(5) 0.006(5) -0.007(4) -0.021(5) C105 0.026(5) 0.044(6) 0.027(5) -0.007(5) 0.004(4) -0.004(5) C106 0.022(4) 0.039(6) 0.017(4) -0.006(4) 0.000(3) -0.009(4) C107 0.024(5) 0.027(5) 0.022(4) -0.001(4) -0.006(4) -0.005(4) C108 0.023(5) 0.041(6) 0.056(6) -0.005(5) 0.002(4) 0.004(5) C109 0.034(5) 0.035(6) 0.042(6) -0.007(5) 0.005(4) 0.010(5) C110 0.023(5) 0.033(6) 0.064(7) -0.018(5) -0.005(5) 0.000(4) C111 0.025(5) 0.023(5) 0.037(5) -0.006(4) 0.000(4) 0.000(4) N112 0.016(4) 0.026(4) 0.025(4) -0.007(3) -0.004(3) -0.006(3) N201 0.025(4) 0.037(5) 0.017(4) 0.003(4) 0.000(3) -0.001(4) C202 0.025(5) 0.052(7) 0.036(5) 0.000(5) -0.003(4) -0.007(5) C203 0.047(6) 0.088(9) 0.029(5) -0.005(6) -0.011(5) -0.007(6) C204 0.045(6) 0.083(9) 0.041(6) -0.018(7) -0.001(5) -0.026(6) C205 0.031(5) 0.048(7) 0.052(6) -0.011(6) 0.005(5) -0.001(5) C206 0.017(4) 0.038(6) 0.036(5) -0.022(5) 0.005(4) -0.002(4) C207 0.019(5) 0.027(5) 0.041(5) -0.016(5) 0.002(4) -0.003(4) C208 0.033(6) 0.038(6) 0.065(7) -0.008(6) -0.016(5) -0.009(5) C209 0.033(6) 0.040(7) 0.082(8) 0.007(7) 0.010(6) -0.010(5) C210 0.030(5) 0.029(6) 0.054(6) 0.010(5) 0.012(4) -0.005(4) C211 0.022(5) 0.025(5) 0.032(5) -0.004(4) 0.006(4) 0.007(4) N212 0.015(4) 0.022(4) 0.028(4) 0.005(3) 0.002(3) -0.005(3) N301 0.021(4) 0.020(4) 0.024(4) 0.007(3) -0.004(3) 0.000(3) C302 0.024(5) 0.024(5) 0.028(5) 0.002(4) 0.001(4) -0.007(4) C303 0.018(4) 0.040(6) 0.027(5) 0.001(4) 0.000(4) 0.005(4) C304 0.020(5) 0.028(5) 0.048(6) 0.002(5) 0.000(4) 0.005(4) C305 0.032(5) 0.016(4) 0.029(5) -0.002(4) -0.001(4) -0.006(4) C306 0.018(4) 0.023(5) 0.028(4) 0.002(4) -0.001(3) 0.000(4) C307 0.023(4) 0.025(5) 0.026(4) -0.009(4) -0.004(4) -0.004(4) N308 0.017(4) 0.020(4) 0.028(4) -0.006(3) -0.004(3) -0.006(3) C309 0.026(5) 0.021(5) 0.018(4) -0.006(4) 0.000(3) -0.006(4) C310 0.031(5) 0.010(4) 0.037(5) -0.001(4) -0.006(4) -0.001(4) C311 0.014(4) 0.034(5) 0.043(5) 0.000(5) -0.009(4) -0.003(4) C312 0.020(4) 0.024(5) 0.032(5) 0.004(4) -0.013(4) 0.010(4) C313 0.041(6) 0.018(5) 0.042(5) -0.005(4) -0.014(4) 0.005(4) C314 0.029(5) 0.020(5) 0.026(4) -0.004(4) -0.006(4) -0.008(4) P10 0.0287(13) 0.0225(13) 0.0373(14) -0.0010(12) -0.0052(11) -0.0051(11) F11 0.040(3) 0.077(4) 0.083(4) 0.018(4) -0.006(3) -0.036(3) F12 0.041(3) 0.055(4) 0.101(5) 0.000(4) -0.002(3) -0.023(3) F13 0.081(4) 0.052(4) 0.061(4) -0.029(3) 0.005(3) 0.007(3) F14 0.064(4) 0.034(3) 0.054(3) -0.011(3) -0.009(3) 0.010(3) F15 0.053(3) 0.048(3) 0.043(3) 0.013(3) -0.005(3) 0.007(3) F16 0.058(4) 0.058(4) 0.048(3) 0.007(3) -0.025(3) 0.000(3) P20 0.0337(14) 0.0368(16) 0.0365(14) -0.0076(13) -0.0007(11) -0.0055(12) F21 0.052(4) 0.106(5) 0.064(4) -0.025(4) -0.013(3) -0.043(4) F22 0.041(3) 0.131(6) 0.053(3) -0.013(4) -0.015(3) -0.007(4) F23 0.126(6) 0.051(4) 0.107(5) 0.038(4) -0.059(5) -0.045(4) F24 0.128(6) 0.046(4) 0.075(4) 0.025(4) 0.020(4) -0.005(4) F25 0.064(4) 0.112(6) 0.064(4) -0.039(4) 0.032(3) -0.024(4) F26 0.048(4) 0.086(5) 0.095(4) -0.059(4) 0.002(3) 0.010(3) _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 N308 2.045(6) . ? Ru1 N301 2.056(6) . ? Ru1 N201 2.057(6) . ? Ru1 N101 2.061(7) . ? Ru1 N112 2.070(6) . ? Ru1 N212 2.077(6) . ? N101 C106 1.356(9) . ? N101 C102 1.367(10) . ? C102 C103 1.381(11) . ? C102 H10A 0.9500 . ? C103 C104 1.361(11) . ? C103 H10D 0.9500 . ? C104 C105 1.386(12) . ? C104 H10B 0.9500 . ? C105 C106 1.394(11) . ? C105 H10C 0.9500 . ? C106 C107 1.459(11) . ? C107 N112 1.350(9) . ? C107 C108 1.396(10) . ? C108 C109 1.390(12) . ? C108 H10E 0.9500 . ? C109 C110 1.364(11) . ? C109 H10F 0.9500 . ? C110 C111 1.385(10) . ? C110 H11B 0.9500 . ? C111 N112 1.356(10) . ? C111 H11A 0.9500 . ? N201 C202 1.326(10) . ? N201 C206 1.387(10) . ? C202 C203 1.400(11) . ? C202 H20A 0.9500 . ? C203 C204 1.382(14) . ? C203 H20C 0.9500 . ? C204 C205 1.376(12) . ? C204 H20D 0.9500 . ? C205 C206 1.380(10) . ? C205 H20E 0.9500 . ? C206 C207 1.444(11) . ? C207 N212 1.351(9) . ? C207 C208 1.397(12) . ? C208 C209 1.352(12) . ? C208 H20B 0.9500 . ? C209 C210 1.380(12) . ? C209 H20F 0.9500 . ? C210 C211 1.377(11) . ? C210 H21B 0.9500 . ? C211 N212 1.331(9) . ? C211 H21A 0.9500 . ? N301 C302 1.344(9) . ? N301 C306 1.355(9) . ? C302 C303 1.379(10) . ? C302 H30B 0.9500 . ? C303 C304 1.373(10) . ? C303 H30A 0.9500 . ? C304 C305 1.373(10) . ? C304 H30C 0.9500 . ? C305 C306 1.382(10) . ? C305 H30E 0.9500 . ? C306 C307 1.450(10) . ? C307 N308 1.297(9) . ? C307 H30D 0.9500 . ? N308 C309 1.443(9) . ? C309 C314 1.388(10) . ? C309 C310 1.397(10) . ? C310 C311 1.389(9) . ? C310 H31C 0.9500 . ? C311 C312 1.374(11) . ? C311 H31E 0.9500 . ? C312 C313 1.381(11) . ? C312 H31D 0.9500 . ? C313 C314 1.385(10) . ? C313 H31A 0.9500 . ? C314 H31B 0.9500 . ? P10 F13 1.584(5) . ? P10 F15 1.587(5) . ? P10 F11 1.589(5) . ? P10 F12 1.591(5) . ? P10 F14 1.596(5) . ? P10 F16 1.597(5) . ? P20 F24 1.558(6) . ? P20 F25 1.576(5) . ? P20 F22 1.586(5) . ? P20 F23 1.589(6) . ? P20 F21 1.589(5) . ? P20 F26 1.591(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 N308 Ru1 N301 78.6(2) . . ? N308 Ru1 N201 176.0(3) . . ? N301 Ru1 N201 98.0(2) . . ? N308 Ru1 N101 87.0(2) . . ? N301 Ru1 N101 95.2(3) . . ? N201 Ru1 N101 95.4(3) . . ? N308 Ru1 N112 98.9(2) . . ? N301 Ru1 N112 173.4(3) . . ? N201 Ru1 N112 84.6(2) . . ? N101 Ru1 N112 78.4(3) . . ? N308 Ru1 N212 98.8(3) . . ? N301 Ru1 N212 90.2(2) . . ? N201 Ru1 N212 79.0(3) . . ? N101 Ru1 N212 172.8(3) . . ? N112 Ru1 N212 96.3(3) . . ? C106 N101 C102 118.0(7) . . ? C106 N101 Ru1 115.7(6) . . ? C102 N101 Ru1 126.3(6) . . ? N101 C102 C103 122.7(8) . . ? N101 C102 H10A 118.6 . . ? C103 C102 H10A 118.6 . . ? C104 C103 C102 118.7(8) . . ? C104 C103 H10D 120.7 . . ? C102 C103 H10D 120.7 . . ? C103 C104 C105 120.1(9) . . ? C103 C104 H10B 119.9 . . ? C105 C104 H10B 119.9 . . ? C104 C105 C106 119.3(8) . . ? C104 C105 H10C 120.4 . . ? C106 C105 H10C 120.4 . . ? N101 C106 C105 121.2(8) . . ? N101 C106 C107 114.9(7) . . ? C105 C106 C107 123.9(7) . . ? N112 C107 C108 120.6(8) . . ? N112 C107 C106 115.4(7) . . ? C108 C107 C106 124.1(8) . . ? C109 C108 C107 119.5(9) . . ? C109 C108 H10E 120.2 . . ? C107 C108 H10E 120.2 . . ? C110 C109 C108 118.6(8) . . ? C110 C109 H10F 120.7 . . ? C108 C109 H10F 120.7 . . ? C109 C110 C111 121.0(9) . . ? C109 C110 H11B 119.5 . . ? C111 C110 H11B 119.5 . . ? N112 C111 C110 120.1(8) . . ? N112 C111 H11A 119.9 . . ? C110 C111 H11A 119.9 . . ? C107 N112 C111 120.2(7) . . ? C107 N112 Ru1 115.2(5) . . ? C111 N112 Ru1 124.3(5) . . ? C202 N201 C206 118.7(7) . . ? C202 N201 Ru1 126.8(6) . . ? C206 N201 Ru1 113.6(5) . . ? N201 C202 C203 123.3(9) . . ? N201 C202 H20A 118.3 . . ? C203 C202 H20A 118.3 . . ? C204 C203 C202 117.2(10) . . ? C204 C203 H20C 121.4 . . ? C202 C203 H20C 121.4 . . ? C205 C204 C203 120.6(9) . . ? C205 C204 H20D 119.7 . . ? C203 C204 H20D 119.7 . . ? C204 C205 C206 119.7(10) . . ? C204 C205 H20E 120.2 . . ? C206 C205 H20E 120.2 . . ? C205 C206 N201 120.4(8) . . ? C205 C206 C207 124.6(9) . . ? N201 C206 C207 115.0(7) . . ? N212 C207 C208 119.6(8) . . ? N212 C207 C206 116.1(8) . . ? C208 C207 C206 124.2(8) . . ? C209 C208 C207 119.1(9) . . ? C209 C208 H20B 120.5 . . ? C207 C208 H20B 120.5 . . ? C208 C209 C210 121.5(10) . . ? C208 C209 H20F 119.3 . . ? C210 C209 H20F 119.3 . . ? C211 C210 C209 117.0(9) . . ? C211 C210 H21B 121.5 . . ? C209 C210 H21B 121.5 . . ? N212 C211 C210 122.6(8) . . ? N212 C211 H21A 118.7 . . ? C210 C211 H21A 118.7 . . ? C211 N212 C207 120.2(7) . . ? C211 N212 Ru1 125.5(6) . . ? C207 N212 Ru1 114.2(5) . . ? C302 N301 C306 117.4(6) . . ? C302 N301 Ru1 127.8(5) . . ? C306 N301 Ru1 114.7(5) . . ? N301 C302 C303 121.6(7) . . ? N301 C302 H30B 119.2 . . ? C303 C302 H30B 119.2 . . ? C304 C303 C302 121.2(8) . . ? C304 C303 H30A 119.4 . . ? C302 C303 H30A 119.4 . . ? C305 C304 C303 117.3(8) . . ? C305 C304 H30C 121.3 . . ? C303 C304 H30C 121.3 . . ? C304 C305 C306 119.7(8) . . ? C304 C305 H30E 120.1 . . ? C306 C305 H30E 120.1 . . ? N301 C306 C305 122.7(7) . . ? N301 C306 C307 113.2(7) . . ? C305 C306 C307 124.1(7) . . ? N308 C307 C306 118.1(7) . . ? N308 C307 H30D 120.9 . . ? C306 C307 H30D 120.9 . . ? C307 N308 C309 118.0(6) . . ? C307 N308 Ru1 114.7(5) . . ? C309 N308 Ru1 126.9(5) . . ? C314 C309 C310 120.6(7) . . ? C314 C309 N308 119.2(7) . . ? C310 C309 N308 120.2(7) . . ? C311 C310 C309 118.2(7) . . ? C311 C310 H31C 120.9 . . ? C309 C310 H31C 120.9 . . ? C312 C311 C310 121.3(8) . . ? C312 C311 H31E 119.3 . . ? C310 C311 H31E 119.3 . . ? C311 C312 C313 119.9(7) . . ? C311 C312 H31D 120.0 . . ? C313 C312 H31D 120.0 . . ? C312 C313 C314 120.1(7) . . ? C312 C313 H31A 119.9 . . ? C314 C313 H31A 119.9 . . ? C313 C314 C309 119.7(8) . . ? C313 C314 H31B 120.1 . . ? C309 C314 H31B 120.1 . . ? F13 P10 F15 90.5(3) . . ? F13 P10 F11 90.1(3) . . ? F15 P10 F11 90.4(3) . . ? F13 P10 F12 90.8(3) . . ? F15 P10 F12 89.8(3) . . ? F11 P10 F12 179.1(4) . . ? F13 P10 F14 179.0(3) . . ? F15 P10 F14 89.6(3) . . ? F11 P10 F14 91.0(3) . . ? F12 P10 F14 88.2(3) . . ? F13 P10 F16 90.2(3) . . ? F15 P10 F16 179.1(3) . . ? F11 P10 F16 89.1(3) . . ? F12 P10 F16 90.7(3) . . ? F14 P10 F16 89.7(3) . . ? F24 P20 F25 90.6(4) . . ? F24 P20 F22 91.8(4) . . ? F25 P20 F22 90.8(3) . . ? F24 P20 F23 178.4(4) . . ? F25 P20 F23 90.6(4) . . ? F22 P20 F23 89.2(3) . . ? F24 P20 F21 89.7(4) . . ? F25 P20 F21 90.6(3) . . ? F22 P20 F21 177.9(4) . . ? F23 P20 F21 89.3(3) . . ? F24 P20 F26 89.4(3) . . ? F25 P20 F26 179.5(3) . . ? F22 P20 F26 88.7(3) . . ? F23 P20 F26 89.3(4) . . ? F21 P20 F26 89.9(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C307 H30D F11 0.95 2.65 3.323(9) 128.4 2_567 C305 H30E F16 0.95 2.91 3.130(9) 94.5 2_567 C211 H21A F13 0.95 2.55 3.377(9) 145.0 2_567 C205 H20E F22 0.95 2.82 3.684(12) 151.9 2_656 C205 H20E F23 0.95 2.38 3.202(12) 145.2 2_656 C104 H10B F21 0.95 2.49 3.282(11) 140.7 2_766 C111 H11A F15 0.95 2.31 3.167(10) 150.0 1_645 C313 H31A F12 0.95 2.51 3.251(10) 134.5 1_645 C310 H31C F14 0.95 2.38 3.255(9) 153.6 1_655 C310 H31C F16 0.95 2.70 3.551(9) 148.8 1_655 C307 H30D F11 0.95 2.79 3.220(10) 108.8 1_655 C305 H30E F11 0.95 2.87 3.324(9) 110.2 1_655 _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.751 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.154 # Attachment 'NM4.CIF' data_nm4 _database_code_depnum_ccdc_archive 'CCDC 293458' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H27 B Cl F4 N5 Ru' _chemical_formula_weight 716.93 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' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 '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 11.0703(12) _cell_length_b 11.8803(13) _cell_length_c 13.2873(15) _cell_angle_alpha 92.061(8) _cell_angle_beta 110.294(10) _cell_angle_gamma 104.768(11) _cell_volume 1569.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7523 _cell_measurement_theta_min 2.909 _cell_measurement_theta_max 28.371 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6988 _exptl_absorpt_correction_T_max 0.9045 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 10104 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0905 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.98 _reflns_number_total 7236 _reflns_number_gt 5155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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^)+(0.0656P)^2^+0.9993P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7236 _refine_ls_number_parameters 432 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1503 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.022 _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 0.16618(4) 0.31461(3) -0.04389(3) 0.03040(13) Uani 1 1 d . . . Cl1 Cl -0.03722(12) 0.29368(10) -0.00927(12) 0.0436(3) Uani 1 1 d . . . N101 N 0.0858(4) 0.1541(3) -0.1413(3) 0.0321(9) Uani 1 1 d . . . C102 C 0.0197(5) 0.1310(5) -0.2504(5) 0.0500(10) Uani 1 1 d . . . H10A H 0.0012 0.1939 -0.2895 0.031(12) Uiso 1 1 d R . . C103 C -0.0231(6) 0.0187(5) -0.3072(5) 0.0579(16) Uani 1 1 d . . . H10B H -0.0612 0.0004 -0.3894 0.067(18) Uiso 1 1 d R . . C104 C 0.0033(6) -0.0727(5) -0.2535(4) 0.0495(14) Uani 1 1 d . . . H10C H -0.0242 -0.1495 -0.2918 0.047(15) Uiso 1 1 d R . . C105 C 0.0714(5) -0.0519(4) -0.1413(4) 0.0372(11) Uani 1 1 d . . . H10D H 0.0904 -0.1147 -0.1023 0.035(13) Uiso 1 1 d R . . C106 C 0.1110(5) 0.0618(4) -0.0874(5) 0.0430(9) Uani 1 1 d . . . C107 C 0.1848(5) 0.0920(4) 0.0306(5) 0.0447(10) Uani 1 1 d . . . N108 N 0.2190(3) 0.2094(3) 0.0627(3) 0.0294(8) Uani 1 1 d . . . C109 C 0.2835(5) 0.2552(4) 0.1681(4) 0.0378(11) Uani 1 1 d . . . C110 C 0.3181(6) 0.1811(5) 0.2450(5) 0.0526(15) Uani 1 1 d . . . H11A H 0.3486 0.2184 0.3152 0.058(17) Uiso 1 1 d R . . C111 C 0.2863(6) 0.0611(5) 0.2127(4) 0.0468(13) Uani 1 1 d . . . H11B H 0.3121 0.0107 0.2649 0.062(18) Uiso 1 1 d R . . C112 C 0.2181(5) 0.0156(4) 0.1048(4) 0.0345(11) Uani 1 1 d . . . H11C H 0.1943 -0.0664 0.0822 0.059(17) Uiso 1 1 d R . . C113 C 0.3069(5) 0.3827(4) 0.1872(4) 0.0383(12) Uani 1 1 d . . . N114 N 0.2640(4) 0.4338(3) 0.0958(4) 0.0382(10) Uani 1 1 d . . . C115 C 0.2783(5) 0.5517(4) 0.1062(5) 0.0445(14) Uani 1 1 d . . . H11D H 0.2486 0.5863 0.0421 0.07(2) Uiso 1 1 d R . . C116 C 0.3368(5) 0.6198(4) 0.2074(5) 0.0430(9) Uani 1 1 d . . . H11E H 0.3437 0.7013 0.2108 0.08(2) Uiso 1 1 d R . . C117 C 0.3825(5) 0.5703(4) 0.2973(5) 0.0447(10) Uani 1 1 d . . . H11F H 0.4249 0.6185 0.3656 0.063(18) Uiso 1 1 d R . . C118 C 0.3674(6) 0.4486(5) 0.2891(5) 0.0532(15) Uani 1 1 d . . . H11G H 0.3980 0.4140 0.3531 0.045(16) Uiso 1 1 d R . . N201 N 0.1215(4) 0.4274(3) -0.1578(4) 0.0400(10) Uani 1 1 d . . . C202 C 0.0216(6) 0.4779(5) -0.1809(5) 0.0500(10) Uani 1 1 d . . . H20A H -0.0377 0.4629 -0.1425 0.08(2) Uiso 1 1 d R . . C203 C -0.0007(7) 0.5498(5) -0.2598(6) 0.0628(12) Uani 1 1 d . . . H20B H -0.0733 0.5833 -0.2752 0.10(3) Uiso 1 1 d R . . C204 C 0.0807(6) 0.5710(5) -0.3209(5) 0.0540(11) Uani 1 1 d . . . H20C H 0.0627 0.6151 -0.3799 0.12(3) Uiso 1 1 d R . . C205 C 0.1864(6) 0.5210(5) -0.2957(5) 0.0582(11) Uani 1 1 d . . . H20D H 0.2456 0.5347 -0.3341 0.049(15) Uiso 1 1 d R . . C206 C 0.2050(5) 0.4517(4) -0.2138(4) 0.0396(12) Uani 1 1 d . . . C207 C 0.3125(5) 0.3957(4) -0.1789(4) 0.0365(11) Uani 1 1 d . . . H20E H 0.3747 0.4014 -0.2142 0.044(14) Uiso 1 1 d R . . N208 N 0.3188(4) 0.3383(3) -0.0984(3) 0.0327(9) Uani 1 1 d . . . C209 C 0.4170(4) 0.2737(4) -0.0655(4) 0.0339(11) Uani 1 1 d . . . C210 C 0.5070(5) 0.2951(5) 0.0400(5) 0.0439(13) Uani 1 1 d . . . H21A H 0.5062 0.3537 0.0901 0.050(16) Uiso 1 1 d R . . C211 C 0.5988(5) 0.2306(5) 0.0732(5) 0.0543(15) Uani 1 1 d . . . H21B H 0.6623 0.2465 0.1454 0.07(2) Uiso 1 1 d R . . C212 C 0.5979(6) 0.1429(5) 0.0006(6) 0.0582(11) Uani 1 1 d . . . H21C H 0.6597 0.0978 0.0238 0.09(2) Uiso 1 1 d R . . C213 C 0.5075(6) 0.1219(5) -0.1048(6) 0.0628(12) Uani 1 1 d . . . H21D H 0.5071 0.0623 -0.1545 0.10(2) Uiso 1 1 d R . . C214 C 0.4166(6) 0.1877(5) -0.1389(5) 0.0540(11) Uani 1 1 d . . . H21E H 0.3549 0.1736 -0.2117 0.07(2) Uiso 1 1 d R . . B10 B 0.2645(8) 0.3089(9) 0.5182(5) 0.075(3) Uani 1 1 d D . . F11 F 0.3249(5) 0.4261(5) 0.5564(5) 0.1227(19) Uani 1 1 d D A . F12A F 0.356(7) 0.266(5) 0.493(9) 0.146(3) Uani 0.20(4) 1 d PD A 1 F13A F 0.162(7) 0.307(5) 0.421(4) 0.138(4) Uani 0.20(4) 1 d PD A 1 F14A F 0.201(5) 0.231(3) 0.566(4) 0.109(4) Uani 0.20(4) 1 d PD A 1 F12 F 0.3509(19) 0.2649(14) 0.488(2) 0.146(3) Uani 0.80(4) 1 d PD A 2 F13 F 0.1508(16) 0.2975(15) 0.4358(11) 0.138(4) Uani 0.80(4) 1 d PD A 2 F14 F 0.2482(18) 0.2597(13) 0.6063(13) 0.109(4) Uani 0.80(4) 1 d PD A 2 C1 C 0.805(2) 0.151(3) 0.4510(18) 0.156(12) Uani 0.552(10) 1 d PG B 1 H1A H 0.8865 0.1794 0.4386 0.187 Uiso 0.552(10) 1 calc PR B 1 C2 C 0.759(3) 0.2286(15) 0.4986(16) 0.20(2) Uani 0.552(10) 1 d PG B 1 H2A H 0.8080 0.3093 0.5187 0.241 Uiso 0.552(10) 1 calc PR B 1 C3 C 0.640(3) 0.188(3) 0.5169(13) 0.21(2) Uani 0.552(10) 1 d PG B 1 H3A H 0.6078 0.2404 0.5494 0.246 Uiso 0.552(10) 1 calc PR B 1 C4 C 0.5674(17) 0.070(3) 0.4876(16) 0.187(17) Uani 0.552(10) 1 d PG B 1 H4A H 0.4861 0.0416 0.5000 0.225 Uiso 0.552(10) 1 calc PR B 1 C5 C 0.614(3) -0.0075(17) 0.4399(14) 0.161(11) Uani 0.552(10) 1 d PG B 1 H5A H 0.5646 -0.0882 0.4199 0.193 Uiso 0.552(10) 1 calc PR B 1 C6 C 0.733(3) 0.033(2) 0.4217(13) 0.127(9) Uani 0.552(10) 1 d PG B 1 H6A H 0.7648 -0.0193 0.3892 0.153 Uiso 0.552(10) 1 calc PR B 1 C7 C 0.8834(8) 0.1748(9) 0.4744(9) 0.059(5) Uani 0.448(10) 1 d PG B 2 H7A H 0.9598 0.1475 0.4844 0.071 Uiso 0.448(10) 1 calc PR B 2 C8 C 0.8976(8) 0.2811(8) 0.5309(7) 0.050(4) Uani 0.448(10) 1 d PG B 2 H8A H 0.9837 0.3265 0.5795 0.060 Uiso 0.448(10) 1 calc PR B 2 C9 C 0.7858(11) 0.3210(9) 0.5162(8) 0.066(5) Uani 0.448(10) 1 d PG B 2 H9A H 0.7955 0.3937 0.5548 0.079 Uiso 0.448(10) 1 calc PR B 2 C10 C 0.6598(9) 0.2545(12) 0.4450(10) 0.087(7) Uani 0.448(10) 1 d PG B 2 H10E H 0.5834 0.2818 0.4350 0.104 Uiso 0.448(10) 1 calc PR B 2 C11 C 0.6456(8) 0.1482(12) 0.3886(11) 0.112(9) Uani 0.448(10) 1 d PG B 2 H11H H 0.5595 0.1028 0.3400 0.134 Uiso 0.448(10) 1 calc PR B 2 C12 C 0.7574(10) 0.1083(9) 0.4033(11) 0.079(7) Uani 0.448(10) 1 d PG B 2 H12B H 0.7477 0.0357 0.3647 0.095 Uiso 0.448(10) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0311(2) 0.02333(19) 0.0454(3) 0.00477(15) 0.02189(17) 0.01137(14) Cl1 0.0404(7) 0.0309(6) 0.0772(10) 0.0155(6) 0.0376(7) 0.0168(5) N101 0.031(2) 0.032(2) 0.037(2) 0.0077(17) 0.0137(18) 0.0132(17) C102 0.050(2) 0.041(2) 0.070(3) 0.021(2) 0.026(2) 0.0221(18) C103 0.068(4) 0.052(4) 0.037(3) -0.004(3) 0.006(3) 0.008(3) C104 0.059(4) 0.037(3) 0.044(3) -0.004(2) 0.013(3) 0.009(3) C105 0.034(3) 0.029(2) 0.048(3) 0.003(2) 0.014(2) 0.010(2) C106 0.0353(19) 0.0310(18) 0.067(3) -0.0057(18) 0.0268(18) 0.0079(15) C107 0.038(2) 0.038(2) 0.059(3) -0.0142(18) 0.0247(18) 0.0047(16) N108 0.0266(19) 0.0270(19) 0.040(2) -0.0009(16) 0.0181(17) 0.0089(16) C109 0.040(3) 0.036(3) 0.042(3) -0.003(2) 0.024(2) 0.007(2) C110 0.068(4) 0.051(3) 0.034(3) -0.001(3) 0.018(3) 0.011(3) C111 0.060(4) 0.045(3) 0.039(3) 0.011(2) 0.018(3) 0.020(3) C112 0.039(3) 0.031(2) 0.038(3) 0.009(2) 0.016(2) 0.015(2) C113 0.040(3) 0.032(3) 0.046(3) -0.009(2) 0.026(2) 0.003(2) N114 0.042(2) 0.028(2) 0.056(3) 0.0004(19) 0.033(2) 0.0090(18) C115 0.043(3) 0.028(2) 0.075(4) 0.000(3) 0.038(3) 0.009(2) C116 0.0353(19) 0.0310(18) 0.067(3) -0.0057(18) 0.0268(18) 0.0079(15) C117 0.038(2) 0.038(2) 0.059(3) -0.0142(18) 0.0247(18) 0.0047(16) C118 0.055(3) 0.052(3) 0.053(4) -0.013(3) 0.029(3) 0.006(3) N201 0.040(2) 0.031(2) 0.061(3) 0.0120(19) 0.028(2) 0.0161(18) C202 0.050(2) 0.041(2) 0.070(3) 0.021(2) 0.026(2) 0.0221(18) C203 0.066(3) 0.052(3) 0.096(4) 0.027(2) 0.047(3) 0.035(2) C204 0.056(3) 0.052(2) 0.071(3) 0.021(2) 0.034(2) 0.028(2) C205 0.058(3) 0.056(3) 0.085(3) 0.028(2) 0.042(2) 0.032(2) C206 0.045(3) 0.029(2) 0.057(3) 0.010(2) 0.029(3) 0.017(2) C207 0.041(3) 0.031(2) 0.046(3) 0.005(2) 0.027(2) 0.011(2) N208 0.035(2) 0.0253(19) 0.042(2) 0.0005(17) 0.0171(18) 0.0113(16) C209 0.030(2) 0.032(2) 0.049(3) 0.006(2) 0.022(2) 0.014(2) C210 0.039(3) 0.044(3) 0.057(4) 0.007(3) 0.025(3) 0.017(2) C211 0.037(3) 0.070(4) 0.060(4) 0.016(3) 0.016(3) 0.024(3) C212 0.058(3) 0.056(3) 0.085(3) 0.028(2) 0.042(2) 0.032(2) C213 0.066(3) 0.052(3) 0.096(4) 0.027(2) 0.047(3) 0.035(2) C214 0.056(3) 0.052(2) 0.071(3) 0.021(2) 0.034(2) 0.028(2) B10 0.083(6) 0.129(8) 0.032(4) -0.002(4) 0.018(4) 0.068(6) F11 0.097(4) 0.131(5) 0.152(5) -0.020(4) 0.060(3) 0.037(3) F12A 0.214(6) 0.199(6) 0.112(5) 0.034(4) 0.098(5) 0.151(5) F13A 0.140(6) 0.130(5) 0.088(5) -0.026(4) -0.045(5) 0.072(4) F14A 0.145(9) 0.145(7) 0.048(7) 0.015(6) 0.036(7) 0.059(6) F12 0.214(6) 0.199(6) 0.112(5) 0.034(4) 0.098(5) 0.151(5) F13 0.140(6) 0.130(5) 0.088(5) -0.026(4) -0.045(5) 0.072(4) F14 0.145(9) 0.145(7) 0.048(7) 0.015(6) 0.036(7) 0.059(6) C1 0.21(4) 0.17(3) 0.12(2) 0.07(2) 0.06(2) 0.08(3) C2 0.40(7) 0.14(2) 0.13(2) 0.06(2) 0.12(3) 0.15(3) C3 0.34(6) 0.24(4) 0.104(19) 0.03(3) 0.07(3) 0.21(4) C4 0.13(2) 0.34(6) 0.12(2) 0.08(3) 0.030(18) 0.13(3) C5 0.17(3) 0.16(2) 0.087(17) 0.019(15) -0.036(16) 0.04(2) C6 0.18(3) 0.11(2) 0.099(15) 0.026(15) 0.042(17) 0.072(19) C7 0.059(10) 0.086(12) 0.047(10) 0.022(8) 0.018(7) 0.047(9) C8 0.059(8) 0.063(9) 0.029(7) 0.015(6) 0.012(6) 0.023(7) C9 0.096(12) 0.072(11) 0.046(9) 0.010(8) 0.031(8) 0.044(10) C10 0.053(10) 0.128(18) 0.079(14) -0.017(12) 0.020(9) 0.035(10) C11 0.054(10) 0.138(19) 0.125(19) -0.045(15) 0.017(11) 0.026(11) C12 0.054(10) 0.071(14) 0.095(18) -0.026(13) 0.018(10) 0.007(10) _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 N108 1.959(4) . ? Ru1 N208 2.020(4) . ? Ru1 N114 2.064(4) . ? Ru1 N101 2.065(4) . ? Ru1 N201 2.073(4) . ? Ru1 Cl1 2.4052(12) . ? N101 C102 1.358(7) . ? N101 C106 1.366(6) . ? C102 C103 1.390(8) . ? C102 H10A 0.9497 . ? C103 C104 1.359(8) . ? C103 H10B 1.0172 . ? C104 C105 1.396(7) . ? C104 H10C 0.9499 . ? C105 C106 1.394(6) . ? C105 H10D 0.9497 . ? C106 C107 1.474(8) . ? C107 N108 1.358(6) . ? C107 C112 1.385(7) . ? N108 C109 1.350(6) . ? C109 C110 1.389(8) . ? C109 C113 1.467(6) . ? C110 C111 1.391(7) . ? C110 H11A 0.9251 . ? C111 C112 1.379(7) . ? C111 H11B 0.9496 . ? C112 H11C 0.9498 . ? C113 N114 1.367(7) . ? C113 C118 1.387(7) . ? N114 C115 1.365(6) . ? C115 C116 1.390(7) . ? C115 H11D 0.9501 . ? C116 C117 1.346(8) . ? C116 H11E 0.9500 . ? C117 C118 1.408(7) . ? C117 H11F 0.9500 . ? C118 H11G 0.9500 . ? N201 C202 1.339(6) . ? N201 C206 1.360(6) . ? C202 C203 1.372(8) . ? C202 H20A 0.9500 . ? C203 C204 1.392(8) . ? C203 H20B 0.9499 . ? C204 C205 1.390(7) . ? C204 H20C 0.9501 . ? C205 C206 1.379(8) . ? C205 H20D 0.9488 . ? C206 C207 1.454(6) . ? C207 N208 1.280(6) . ? C207 H20E 0.9497 . ? N208 C209 1.442(5) . ? C209 C210 1.378(7) . ? C209 C214 1.385(7) . ? C210 C211 1.388(7) . ? C210 H21A 0.9499 . ? C211 C212 1.390(8) . ? C211 H21B 0.9495 . ? C212 C213 1.378(9) . ? C212 H21C 0.9501 . ? C213 C214 1.393(8) . ? C213 H21D 0.9498 . ? C214 H21E 0.9493 . ? B10 F13 1.322(11) . ? B10 F14A 1.332(17) . ? B10 F12 1.363(9) . ? B10 F11 1.372(9) . ? B10 F12A 1.373(18) . ? B10 F14 1.373(11) . ? B10 F13A 1.383(19) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 H1A 0.9500 . ? C2 C3 1.3900 . ? C2 H2A 0.9500 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 H7A 0.9500 . ? C8 C9 1.3900 . ? C8 H8A 0.9500 . ? C9 C10 1.3900 . ? C9 H9A 0.9500 . ? C10 C11 1.3900 . ? C10 H10E 0.9500 . ? C11 C12 1.3900 . ? C11 H11H 0.9500 . ? C12 H12B 0.9500 . ? 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 N108 Ru1 N208 99.07(15) . . ? N108 Ru1 N114 79.61(16) . . ? N208 Ru1 N114 98.32(15) . . ? N108 Ru1 N101 79.01(15) . . ? N208 Ru1 N101 86.13(15) . . ? N114 Ru1 N101 158.59(16) . . ? N108 Ru1 N201 176.50(15) . . ? N208 Ru1 N201 77.46(15) . . ? N114 Ru1 N201 100.31(17) . . ? N101 Ru1 N201 101.10(16) . . ? N108 Ru1 Cl1 89.86(11) . . ? N208 Ru1 Cl1 170.07(12) . . ? N114 Ru1 Cl1 87.50(11) . . ? N101 Ru1 Cl1 91.36(11) . . ? N201 Ru1 Cl1 93.63(11) . . ? C102 N101 C106 117.5(4) . . ? C102 N101 Ru1 128.4(3) . . ? C106 N101 Ru1 114.0(3) . . ? N101 C102 C103 122.6(5) . . ? N101 C102 H10A 118.9 . . ? C103 C102 H10A 118.6 . . ? C104 C103 C102 119.8(5) . . ? C104 C103 H10B 115.2 . . ? C102 C103 H10B 124.3 . . ? C103 C104 C105 119.0(5) . . ? C103 C104 H10C 120.4 . . ? C105 C104 H10C 120.6 . . ? C106 C105 C104 119.3(5) . . ? C106 C105 H10D 120.4 . . ? C104 C105 H10D 120.3 . . ? N101 C106 C105 121.8(5) . . ? N101 C106 C107 115.2(4) . . ? C105 C106 C107 122.9(5) . . ? N108 C107 C112 121.0(5) . . ? N108 C107 C106 111.7(5) . . ? C112 C107 C106 127.3(5) . . ? C109 N108 C107 121.3(4) . . ? C109 N108 Ru1 118.7(3) . . ? C107 N108 Ru1 120.0(4) . . ? N108 C109 C110 119.3(4) . . ? N108 C109 C113 113.3(4) . . ? C110 C109 C113 127.4(5) . . ? C109 C110 C111 119.8(5) . . ? C109 C110 H11A 112.6 . . ? C111 C110 H11A 126.8 . . ? C112 C111 C110 120.0(5) . . ? C112 C111 H11B 120.0 . . ? C110 C111 H11B 120.0 . . ? C111 C112 C107 118.5(5) . . ? C111 C112 H11C 120.7 . . ? C107 C112 H11C 120.8 . . ? N114 C113 C118 121.3(5) . . ? N114 C113 C109 114.9(4) . . ? C118 C113 C109 123.8(5) . . ? C115 N114 C113 118.9(4) . . ? C115 N114 Ru1 127.4(4) . . ? C113 N114 Ru1 113.4(3) . . ? N114 C115 C116 121.1(6) . . ? N114 C115 H11D 118.1 . . ? C116 C115 H11D 120.8 . . ? C117 C116 C115 120.2(5) . . ? C117 C116 H11E 121.6 . . ? C115 C116 H11E 118.2 . . ? C116 C117 C118 119.9(5) . . ? C116 C117 H11F 119.1 . . ? C118 C117 H11F 121.0 . . ? C113 C118 C117 118.6(6) . . ? C113 C118 H11G 122.0 . . ? C117 C118 H11G 119.5 . . ? C202 N201 C206 117.8(5) . . ? C202 N201 Ru1 127.3(4) . . ? C206 N201 Ru1 114.8(3) . . ? N201 C202 C203 122.5(6) . . ? N201 C202 H20A 119.4 . . ? C203 C202 H20A 118.0 . . ? C202 C203 C204 120.1(5) . . ? C202 C203 H20B 120.6 . . ? C204 C203 H20B 119.3 . . ? C205 C204 C203 117.6(6) . . ? C205 C204 H20C 120.7 . . ? C203 C204 H20C 121.6 . . ? C206 C205 C204 119.3(5) . . ? C206 C205 H20D 120.2 . . ? C204 C205 H20D 120.4 . . ? N201 C206 C205 122.5(5) . . ? N201 C206 C207 112.9(4) . . ? C205 C206 C207 124.6(5) . . ? N208 C207 C206 116.7(4) . . ? N208 C207 H20E 121.7 . . ? C206 C207 H20E 121.6 . . ? C207 N208 C209 119.0(4) . . ? C207 N208 Ru1 117.6(3) . . ? C209 N208 Ru1 122.1(3) . . ? C210 C209 C214 120.6(5) . . ? C210 C209 N208 119.5(4) . . ? C214 C209 N208 119.8(5) . . ? C209 C210 C211 119.9(5) . . ? C209 C210 H21A 120.2 . . ? C211 C210 H21A 119.9 . . ? C210 C211 C212 120.0(6) . . ? C210 C211 H21B 120.0 . . ? C212 C211 H21B 120.1 . . ? C213 C212 C211 119.8(6) . . ? C213 C212 H21C 120.3 . . ? C211 C212 H21C 119.9 . . ? C212 C213 C214 120.4(6) . . ? C212 C213 H21D 119.9 . . ? C214 C213 H21D 119.7 . . ? C209 C214 C213 119.3(6) . . ? C209 C214 H21E 120.4 . . ? C213 C214 H21E 120.3 . . ? F13 B10 F14A 91(3) . . ? F13 B10 F12 111.5(10) . . ? F14A B10 F12 110(3) . . ? F13 B10 F11 108.7(10) . . ? F14A B10 F11 126(2) . . ? F12 B10 F11 108.4(11) . . ? F13 B10 F12A 114(5) . . ? F14A B10 F12A 109(3) . . ? F12 B10 F12A 3(6) . . ? F11 B10 F12A 107(3) . . ? F13 B10 F14 114.2(12) . . ? F14A B10 F14 26.2(17) . . ? F12 B10 F14 109.4(12) . . ? F11 B10 F14 104.3(9) . . ? F12A B10 F14 108(4) . . ? F13 B10 F13A 12(5) . . ? F14A B10 F13A 102(3) . . ? F12 B10 F13A 104(6) . . ? F11 B10 F13A 104(3) . . ? F12A B10 F13A 107(3) . . ? F14 B10 F13A 126(3) . . ? C2 C1 C6 120.0 . . ? C2 C1 H1A 120.0 . . ? C6 C1 H1A 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 H7A 120.0 . . ? C12 C7 H7A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10E 120.0 . . ? C9 C10 H10E 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11H 120.0 . . ? C12 C11 H11H 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12B 120.0 . . ? C7 C12 H12B 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C10 H10E F12 0.95 2.86 3.687(13) 146.6 . C118 H11G F12 0.95 2.65 3.51(3) 150.7 . C110 H11A F12 0.93 2.33 3.21(2) 158.8 . C214 H21E F14 0.95 2.67 3.509(15) 148.3 1_554 C205 H20D F11 0.95 2.42 3.208(8) 139.8 1_554 C7 H7A F14 0.95 2.95 3.64(2) 131.4 1_655 C105 H10D Cl1 0.95 2.69 3.575(5) 154.6 2 C112 H11C Cl1 0.95 2.74 3.643(5) 159.3 2 C104 H10C F13 0.95 2.31 3.203(17) 155.4 2 C203 H20B F13 0.95 2.62 3.267(14) 125.7 2_565 C204 H20C F13 0.95 2.70 3.293(18) 120.8 2_565 C117 H11F F12 0.95 2.56 3.39(3) 145.8 2_666 _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.143 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.103