# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d1397 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H49 N7 Ru, C2 Cl6 H2, P2 F12' _chemical_formula_sum 'C42 H51 Cl6 F12 N7 P2 Ru' _chemical_formula_weight 1257.61 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' N N 0.0061 0.0033 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall 'P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.913(3) _cell_length_b 15.631(2) _cell_length_c 20.393(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.168(3) _cell_angle_gamma 90.00 _cell_volume 5369.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 48828 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.57 _exptl_crystal_description needle _exptl_crystal_colour gold _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6597 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS (sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'Bruker Triumph' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_reflns_number 47744 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.57 _reflns_number_total 12360 _reflns_number_gt 9062 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement APEX2 _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce, 1996)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0847P)^2^+11.5455P] 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 12360 _refine_ls_number_parameters 643 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 0.0798(2) 0.3251(2) 0.13176(18) 0.0241(8) Uani 1 1 d . . . C1S C 0.6492(3) -0.0052(3) 0.0785(2) 0.0396(10) Uani 1 1 d . . . H1S H 0.6162 0.0384 0.0973 0.048 Uiso 1 1 calc R . . C2 C -0.0128(3) 0.2931(3) 0.04965(19) 0.0315(9) Uani 1 1 d . . . H2 H -0.0598 0.2743 0.0271 0.038 Uiso 1 1 calc R . . C2S C 0.8652(3) 0.6715(4) 0.1965(3) 0.0510(13) Uani 1 1 d . . . H2S H 0.8965 0.6955 0.2349 0.061 Uiso 1 1 calc R . . C3 C 0.0513(3) 0.3201(3) 0.02274(19) 0.0321(9) Uani 1 1 d . . . H3 H 0.0570 0.3243 -0.0221 0.039 Uiso 1 1 calc R . . C4 C -0.0474(2) 0.2592(3) 0.16395(19) 0.0282(8) Uani 1 1 d . . . C5 C -0.1363(2) 0.2829(3) 0.1522(2) 0.0344(9) Uani 1 1 d . . . C6 C -0.1729(3) 0.2977(4) 0.2177(2) 0.0439(11) Uani 1 1 d . . . H6A H -0.2268 0.3165 0.2090 0.066 Uiso 1 1 calc R . . H6B H -0.1429 0.3406 0.2428 0.066 Uiso 1 1 calc R . . H6C H -0.1717 0.2452 0.2423 0.066 Uiso 1 1 calc R . . C7 C -0.1834(3) 0.2107(3) 0.1153(2) 0.0434(11) Uani 1 1 d . . . H7A H -0.1835 0.1610 0.1429 0.065 Uiso 1 1 calc R . . H7B H -0.1591 0.1969 0.0759 0.065 Uiso 1 1 calc R . . H7C H -0.2370 0.2292 0.1039 0.065 Uiso 1 1 calc R . . C8 C -0.1497(3) 0.3678(3) 0.1134(2) 0.0433(11) Uani 1 1 d . . . H8A H -0.1406 0.3586 0.0682 0.065 Uiso 1 1 calc R . . H8B H -0.1136 0.4104 0.1321 0.065 Uiso 1 1 calc R . . H8C H -0.2033 0.3869 0.1159 0.065 Uiso 1 1 calc R . . C9 C -0.0536(3) 0.1502(3) 0.2471(2) 0.0317(9) Uani 1 1 d . . . C10 C -0.0630(3) 0.1672(3) 0.3132(2) 0.0347(9) Uani 1 1 d . . . C11 C -0.0904(3) 0.1007(3) 0.3510(2) 0.0455(12) Uani 1 1 d . . . H11 H -0.0969 0.1106 0.3952 0.055 Uiso 1 1 calc R . . C12 C -0.1081(3) 0.0211(4) 0.3247(3) 0.0525(13) Uani 1 1 d . . . H12 H -0.1247 -0.0225 0.3513 0.063 Uiso 1 1 calc R . . C13 C -0.1011(3) 0.0066(3) 0.2591(3) 0.0485(12) Uani 1 1 d . . . H13 H -0.1153 -0.0465 0.2411 0.058 Uiso 1 1 calc R . . C14 C -0.0731(3) 0.0700(3) 0.2185(2) 0.0368(10) Uani 1 1 d . . . C15 C -0.0608(3) 0.0464(3) 0.1486(2) 0.0431(11) Uani 1 1 d . . . H15A H -0.0151 0.0101 0.1482 0.065 Uiso 1 1 calc R . . H15B H -0.0528 0.0974 0.1238 0.065 Uiso 1 1 calc R . . H15C H -0.1068 0.0167 0.1292 0.065 Uiso 1 1 calc R . . C16 C -0.0501(3) 0.2535(3) 0.3449(2) 0.0364(10) Uani 1 1 d . . . H16A H -0.1004 0.2806 0.3484 0.055 Uiso 1 1 calc R . . H16B H -0.0185 0.2882 0.3185 0.055 Uiso 1 1 calc R . . H16C H -0.0230 0.2467 0.3880 0.055 Uiso 1 1 calc R . . C17 C 0.1805(2) 0.3881(3) 0.06412(18) 0.0275(8) Uani 1 1 d . . . C18 C 0.1785(3) 0.4773(3) 0.0699(2) 0.0327(9) Uani 1 1 d . . . C19 C 0.2471(3) 0.5225(3) 0.0604(2) 0.0401(11) Uani 1 1 d . . . H19 H 0.2469 0.5818 0.0645 0.048 Uiso 1 1 calc R . . C20 C 0.3160(3) 0.4818(3) 0.0450(2) 0.0396(10) Uani 1 1 d . . . C21 C 0.3157(3) 0.3943(3) 0.0390(2) 0.0377(10) Uani 1 1 d . . . H21 H 0.3616 0.3668 0.0283 0.045 Uiso 1 1 calc R . . C22 C 0.2487(3) 0.3453(3) 0.0483(2) 0.0343(9) Uani 1 1 d . . . C23 C 0.1029(3) 0.5228(3) 0.0856(3) 0.0456(12) Uani 1 1 d . . . H23A H 0.1123 0.5833 0.0881 0.068 Uiso 1 1 calc R . . H23B H 0.0874 0.5026 0.1270 0.068 Uiso 1 1 calc R . . H23C H 0.0614 0.5111 0.0515 0.068 Uiso 1 1 calc R . . C24 C 0.3909(3) 0.5322(4) 0.0364(3) 0.0596(15) Uani 1 1 d . . . H24A H 0.4327 0.4936 0.0273 0.089 Uiso 1 1 calc R . . H24B H 0.4063 0.5635 0.0760 0.089 Uiso 1 1 calc R . . H24C H 0.3811 0.5715 0.0003 0.089 Uiso 1 1 calc R . . C25 C 0.2518(3) 0.2492(3) 0.0422(3) 0.0466(12) Uani 1 1 d . . . H25A H 0.3016 0.2327 0.0267 0.070 Uiso 1 1 calc R . . H25B H 0.2091 0.2301 0.0115 0.070 Uiso 1 1 calc R . . H25C H 0.2468 0.2237 0.0844 0.070 Uiso 1 1 calc R . . C26 C 0.1255(2) 0.3266(2) 0.19471(18) 0.0234(8) Uani 1 1 d . . . C27 C 0.1024(2) 0.3892(2) 0.24547(19) 0.0257(8) Uani 1 1 d . . . C28 C 0.0275(2) 0.4243(3) 0.2473(2) 0.0290(8) Uani 1 1 d . . . H28 H -0.0116 0.4109 0.2139 0.035 Uiso 1 1 calc R . . C29 C 0.0086(3) 0.4790(3) 0.2977(2) 0.0366(10) Uani 1 1 d . . . H29 H -0.0425 0.5007 0.2979 0.044 Uiso 1 1 calc R . . C30 C 0.0664(3) 0.5008(3) 0.3472(2) 0.0421(11) Uani 1 1 d . . . H30 H 0.0543 0.5364 0.3815 0.050 Uiso 1 1 calc R . . C31 C 0.1417(3) 0.4691(3) 0.3451(2) 0.0449(12) Uani 1 1 d . . . H31 H 0.1810 0.4842 0.3780 0.054 Uiso 1 1 calc R . . C32 C 0.1606(3) 0.4147(3) 0.2948(2) 0.0353(10) Uani 1 1 d . . . H32 H 0.2124 0.3951 0.2939 0.042 Uiso 1 1 calc R . . C33 C 0.2997(3) 0.1704(3) 0.2411(2) 0.0314(9) Uani 1 1 d . . . C34 C 0.3844(3) 0.1584(3) 0.2559(3) 0.0437(11) Uani 1 1 d . . . H34A H 0.4014 0.1865 0.2966 0.066 Uiso 1 1 calc R . . H34B H 0.4121 0.1823 0.2211 0.066 Uiso 1 1 calc R . . H34C H 0.3959 0.0984 0.2598 0.066 Uiso 1 1 calc R . . C35 C 0.1078(3) -0.0046(3) 0.2674(2) 0.0386(10) Uani 1 1 d . . . C36 C 0.1066(4) -0.0926(3) 0.2900(3) 0.0589(16) Uani 1 1 d . . . H36A H 0.0601 -0.1019 0.3128 0.088 Uiso 1 1 calc R . . H36B H 0.1532 -0.1037 0.3192 0.088 Uiso 1 1 calc R . . H36C H 0.1056 -0.1305 0.2529 0.088 Uiso 1 1 calc R . . C37 C 0.1368(3) 0.2402(3) 0.3697(2) 0.0329(9) Uani 1 1 d . . . C38 C 0.1481(3) 0.2659(4) 0.4383(2) 0.0489(13) Uani 1 1 d . . . H38A H 0.1142 0.3136 0.4454 0.073 Uiso 1 1 calc R . . H38B H 0.2025 0.2820 0.4490 0.073 Uiso 1 1 calc R . . H38C H 0.1351 0.2190 0.4657 0.073 Uiso 1 1 calc R . . C39 C 0.1080(3) 0.1167(3) 0.0755(2) 0.0312(9) Uani 1 1 d . . . C40 C 0.1054(3) 0.0773(3) 0.0102(2) 0.0440(11) Uani 1 1 d . . . H40A H 0.0826 0.1169 -0.0222 0.066 Uiso 1 1 calc R . . H40B H 0.0735 0.0265 0.0095 0.066 Uiso 1 1 calc R . . H40C H 0.1582 0.0628 0.0005 0.066 Uiso 1 1 calc R . . Cl1S Cl 0.71185(8) 0.04509(8) 0.02660(6) 0.0507(3) Uani 1 1 d . . . Cl2S Cl 0.58708(8) -0.07940(9) 0.03508(7) 0.0535(3) Uani 1 1 d . . . Cl3S Cl 0.70690(9) -0.05601(11) 0.14292(7) 0.0672(4) Uani 1 1 d . . . Cl4S Cl 0.93064(8) 0.61087(10) 0.15239(7) 0.0567(3) Uani 1 1 d . . . Cl5S Cl 0.79494(14) 0.60322(17) 0.22608(16) 0.1254(10) Uani 1 1 d . . . Cl6S Cl 0.8255(2) 0.75595(17) 0.15126(12) 0.1359(12) Uani 1 1 d . . . F1 F 0.5129(2) 0.3443(3) 0.0830(3) 0.1118(19) Uani 1 1 d . . . F2 F 0.5199(3) 0.2124(6) 0.0408(3) 0.185(4) Uani 1 1 d . . . F3 F 0.6250(2) 0.2729(3) 0.0916(2) 0.0859(12) Uani 1 1 d . . . F4 F 0.5625(3) 0.1639(3) 0.1410(3) 0.127(2) Uani 1 1 d . . . F5 F 0.5566(3) 0.2930(3) 0.17917(19) 0.0934(14) Uani 1 1 d . . . F6 F 0.4470(2) 0.2365(3) 0.1216(2) 0.0884(13) Uani 1 1 d . . . F7 F 0.1965(2) 0.8907(3) 0.07665(19) 0.0832(12) Uani 1 1 d . . . F8 F 0.1560(3) 0.7566(3) 0.0567(2) 0.0932(14) Uani 1 1 d . . . F9 F 0.1682(2) 0.8061(2) 0.15827(15) 0.0635(9) Uani 1 1 d . . . F10 F 0.0490(3) 0.7778(4) 0.1031(2) 0.118(2) Uani 1 1 d . . . F11 F 0.0908(3) 0.9185(3) 0.1248(2) 0.1062(17) Uani 1 1 d . . . F12 F 0.0769(2) 0.8671(2) 0.02346(17) 0.0684(10) Uani 1 1 d . . . N1 N 0.10856(19) 0.3412(2) 0.07365(15) 0.0261(7) Uani 1 1 d . . . N2 N 0.00335(19) 0.2982(2) 0.11812(16) 0.0270(7) Uani 1 1 d . . . N3 N -0.0114(2) 0.2095(2) 0.20662(15) 0.0258(7) Uani 1 1 d . . . N4 N 0.1106(2) 0.1481(2) 0.12557(17) 0.0284(7) Uani 1 1 d . . . N5 N 0.1074(2) 0.0636(2) 0.24896(17) 0.0306(7) Uani 1 1 d . . . N6 N 0.2336(2) 0.1787(2) 0.23016(16) 0.0284(7) Uani 1 1 d . . . N7 N 0.1241(2) 0.2230(2) 0.31536(17) 0.0289(7) Uani 1 1 d . . . P1 P 0.12044(8) 0.83725(8) 0.09274(6) 0.0388(3) Uani 1 1 d . . . P2 P 0.53773(9) 0.25371(9) 0.10816(7) 0.0484(3) Uani 1 1 d . . . Ru1 Ru 0.113827(19) 0.19157(2) 0.219588(15) 0.02482(10) Uani 1 1 d . . . H26 H 0.183(3) 0.333(3) 0.184(2) 0.040(13) Uiso 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 C1 0.0257(19) 0.0226(19) 0.0243(18) -0.0004(14) 0.0028(15) 0.0016(15) C1S 0.045(3) 0.039(2) 0.035(2) 0.0046(19) 0.009(2) 0.008(2) C2 0.034(2) 0.038(2) 0.0222(18) -0.0043(17) 0.0007(16) -0.0036(18) C2S 0.054(3) 0.052(3) 0.048(3) 0.003(2) 0.008(2) 0.007(2) C3 0.035(2) 0.041(2) 0.0209(18) -0.0010(17) 0.0008(16) -0.0014(18) C4 0.029(2) 0.031(2) 0.0245(19) -0.0097(16) 0.0036(16) -0.0079(16) C5 0.025(2) 0.045(3) 0.033(2) -0.0038(19) 0.0032(17) -0.0023(18) C6 0.032(2) 0.059(3) 0.041(3) -0.005(2) 0.0094(19) 0.004(2) C7 0.030(2) 0.057(3) 0.043(3) -0.011(2) -0.0026(19) -0.008(2) C8 0.032(2) 0.051(3) 0.046(3) -0.002(2) 0.002(2) 0.004(2) C9 0.033(2) 0.029(2) 0.035(2) 0.0009(17) 0.0093(17) -0.0018(17) C10 0.035(2) 0.038(2) 0.032(2) -0.0003(18) 0.0073(18) 0.0009(18) C11 0.053(3) 0.053(3) 0.033(2) 0.008(2) 0.013(2) -0.004(2) C12 0.054(3) 0.046(3) 0.060(3) 0.015(3) 0.017(3) -0.010(2) C13 0.049(3) 0.034(3) 0.064(3) -0.004(2) 0.010(2) -0.013(2) C14 0.032(2) 0.032(2) 0.047(3) -0.0051(19) 0.0083(19) -0.0099(18) C15 0.044(3) 0.039(3) 0.047(3) -0.016(2) 0.008(2) -0.012(2) C16 0.039(2) 0.042(3) 0.029(2) -0.0056(19) 0.0074(18) 0.001(2) C17 0.032(2) 0.029(2) 0.0222(18) 0.0023(15) 0.0051(15) -0.0031(16) C18 0.038(2) 0.032(2) 0.029(2) 0.0076(17) 0.0063(17) 0.0045(18) C19 0.044(3) 0.028(2) 0.050(3) 0.008(2) 0.014(2) -0.0008(19) C20 0.038(2) 0.038(2) 0.044(3) 0.006(2) 0.012(2) -0.007(2) C21 0.036(2) 0.037(2) 0.043(2) 0.003(2) 0.016(2) 0.0017(19) C22 0.036(2) 0.036(2) 0.032(2) 0.0007(18) 0.0094(18) -0.0005(19) C23 0.046(3) 0.032(2) 0.061(3) 0.006(2) 0.015(2) 0.007(2) C24 0.049(3) 0.046(3) 0.088(4) 0.008(3) 0.028(3) -0.009(2) C25 0.044(3) 0.034(2) 0.065(3) -0.009(2) 0.024(2) -0.002(2) C26 0.0249(19) 0.0231(19) 0.0222(17) 0.0010(14) 0.0019(14) -0.0007(14) C27 0.035(2) 0.0191(18) 0.0231(18) 0.0032(15) 0.0019(15) -0.0031(15) C28 0.035(2) 0.0252(19) 0.0272(19) -0.0017(16) 0.0040(16) -0.0049(17) C29 0.046(3) 0.032(2) 0.033(2) -0.0016(18) 0.0100(19) -0.0013(19) C30 0.073(3) 0.027(2) 0.027(2) -0.0023(17) 0.009(2) 0.002(2) C31 0.075(4) 0.029(2) 0.028(2) -0.0016(18) -0.017(2) -0.001(2) C32 0.042(2) 0.028(2) 0.034(2) 0.0000(18) -0.0069(19) 0.0017(18) C33 0.038(2) 0.027(2) 0.030(2) -0.0047(16) 0.0045(17) 0.0019(17) C34 0.034(2) 0.048(3) 0.049(3) -0.008(2) 0.000(2) 0.010(2) C35 0.051(3) 0.033(2) 0.032(2) -0.0035(19) 0.009(2) -0.003(2) C36 0.107(5) 0.031(3) 0.042(3) 0.008(2) 0.018(3) -0.005(3) C37 0.037(2) 0.030(2) 0.032(2) 0.0018(17) 0.0041(18) -0.0055(18) C38 0.061(3) 0.058(3) 0.028(2) -0.005(2) 0.004(2) -0.013(3) C39 0.037(2) 0.025(2) 0.032(2) -0.0057(17) 0.0087(17) -0.0059(17) C40 0.058(3) 0.041(3) 0.034(2) -0.012(2) 0.007(2) -0.001(2) Cl1S 0.0631(8) 0.0450(7) 0.0449(7) 0.0124(5) 0.0099(6) -0.0064(6) Cl2S 0.0566(8) 0.0532(8) 0.0500(7) 0.0066(6) 0.0008(6) -0.0063(6) Cl3S 0.0653(9) 0.0820(11) 0.0512(8) 0.0307(8) -0.0112(7) -0.0086(8) Cl4S 0.0520(8) 0.0612(8) 0.0588(8) 0.0139(7) 0.0146(6) 0.0130(6) Cl5S 0.0829(14) 0.1057(17) 0.200(3) 0.0030(18) 0.0804(17) -0.0039(12) Cl6S 0.208(3) 0.1152(19) 0.0888(15) 0.0402(14) 0.0393(17) 0.104(2) F1 0.067(3) 0.108(4) 0.157(4) 0.083(3) -0.012(3) -0.013(2) F2 0.115(4) 0.348(10) 0.098(4) -0.137(5) 0.052(3) -0.105(5) F3 0.050(2) 0.133(4) 0.076(3) -0.008(3) 0.0115(18) -0.003(2) F4 0.143(5) 0.046(2) 0.191(6) 0.006(3) 0.017(4) 0.024(3) F5 0.140(4) 0.084(3) 0.057(2) -0.015(2) 0.012(2) 0.022(3) F6 0.073(3) 0.084(3) 0.115(3) 0.021(2) 0.046(2) -0.011(2) F7 0.072(2) 0.105(3) 0.070(2) 0.037(2) -0.0088(19) -0.034(2) F8 0.101(3) 0.085(3) 0.086(3) -0.032(2) -0.033(2) 0.034(2) F9 0.071(2) 0.071(2) 0.0434(16) 0.0213(15) -0.0186(15) -0.0241(17) F10 0.082(3) 0.162(5) 0.103(3) 0.076(3) -0.032(2) -0.074(3) F11 0.157(4) 0.095(3) 0.065(2) -0.032(2) 0.005(3) 0.051(3) F12 0.091(3) 0.0428(17) 0.063(2) 0.0072(15) -0.0355(19) -0.0036(17) N1 0.0264(17) 0.0298(17) 0.0221(15) 0.0000(13) 0.0023(13) 0.0002(14) N2 0.0261(16) 0.0319(18) 0.0233(15) -0.0038(13) 0.0041(13) -0.0016(14) N3 0.0294(17) 0.0265(17) 0.0217(15) -0.0043(13) 0.0037(13) -0.0045(13) N4 0.0316(18) 0.0223(16) 0.0320(18) -0.0016(14) 0.0067(14) -0.0019(14) N5 0.038(2) 0.0276(18) 0.0272(17) -0.0017(14) 0.0070(14) -0.0011(15) N6 0.0342(19) 0.0231(17) 0.0281(17) 0.0002(13) 0.0036(14) 0.0015(14) N7 0.0353(19) 0.0235(16) 0.0279(18) 0.0005(14) 0.0034(14) -0.0023(14) P1 0.0463(7) 0.0335(6) 0.0348(6) 0.0003(5) -0.0068(5) -0.0047(5) P2 0.0576(8) 0.0416(7) 0.0490(7) -0.0049(6) 0.0219(6) -0.0017(6) Ru1 0.02925(17) 0.02185(16) 0.02357(16) -0.00212(12) 0.00361(11) -0.00138(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.345(5) . ? C1 N2 1.364(5) . ? C1 C26 1.438(5) . ? C1S Cl1S 1.750(5) . ? C1S Cl2S 1.752(5) . ? C1S Cl3S 1.754(5) . ? C1S H1S 0.9800 . ? C2 C3 1.328(6) . ? C2 N2 1.401(5) . ? C2 H2 0.9300 . ? C2S Cl6S 1.712(6) . ? C2S Cl5S 1.745(6) . ? C2S Cl4S 1.764(6) . ? C2S H2S 0.9800 . ? C3 N1 1.394(5) . ? C3 H3 0.9300 . ? C4 N3 1.279(5) . ? C4 N2 1.457(5) . ? C4 C5 1.547(6) . ? C5 C7 1.538(6) . ? C5 C6 1.539(6) . ? C5 C8 1.551(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.398(6) . ? C9 C14 1.408(6) . ? C9 N3 1.468(5) . ? C10 C11 1.396(6) . ? C10 C16 1.503(6) . ? C11 C12 1.377(8) . ? C11 H11 0.9300 . ? C12 C13 1.374(8) . ? C12 H12 0.9300 . ? C13 C14 1.400(7) . ? C13 H13 0.9300 . ? C14 C15 1.505(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C22 1.397(6) . ? C17 C18 1.399(6) . ? C17 N1 1.449(5) . ? C18 C19 1.386(6) . ? C18 C23 1.522(6) . ? C19 C20 1.388(7) . ? C19 H19 0.9300 . ? C20 C21 1.374(7) . ? C20 C24 1.515(7) . ? C21 C22 1.394(6) . ? C21 H21 0.9300 . ? C22 C25 1.508(6) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.502(5) . ? C26 Ru1 2.184(4) . ? C26 H26 1.02(5) . ? C27 C28 1.384(6) . ? C27 C32 1.401(6) . ? C28 C29 1.395(6) . ? C28 H28 0.9300 . ? C29 C30 1.383(7) . ? C29 H29 0.9300 . ? C30 C31 1.371(7) . ? C30 H30 0.9300 . ? C31 C32 1.391(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 N6 1.127(5) . ? C33 C34 1.449(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 N5 1.130(6) . ? C35 C36 1.452(7) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N7 1.141(5) . ? C37 C38 1.452(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 N4 1.131(5) . ? C39 C40 1.464(6) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? F1 P2 1.551(5) . ? F2 P2 1.523(5) . ? F3 P2 1.572(4) . ? F4 P2 1.596(5) . ? F5 P2 1.579(4) . ? F6 P2 1.605(4) . ? F7 P1 1.592(4) . ? F8 P1 1.604(4) . ? F9 P1 1.576(3) . ? F10 P1 1.553(4) . ? F11 P1 1.534(4) . ? F12 P1 1.602(3) . ? N3 Ru1 2.130(3) . ? N4 Ru1 2.030(3) . ? N5 Ru1 2.094(4) . ? N6 Ru1 2.028(4) . ? N7 Ru1 2.006(3) . ? 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 N1 C1 N2 106.9(3) . . ? N1 C1 C26 125.1(4) . . ? N2 C1 C26 127.7(3) . . ? Cl1S C1S Cl2S 111.1(3) . . ? Cl1S C1S Cl3S 109.3(3) . . ? Cl2S C1S Cl3S 110.3(3) . . ? Cl1S C1S H1S 108.7 . . ? Cl2S C1S H1S 108.7 . . ? Cl3S C1S H1S 108.7 . . ? C3 C2 N2 107.5(4) . . ? C3 C2 H2 126.2 . . ? N2 C2 H2 126.2 . . ? Cl6S C2S Cl5S 114.3(4) . . ? Cl6S C2S Cl4S 111.9(3) . . ? Cl5S C2S Cl4S 109.0(3) . . ? Cl6S C2S H2S 107.1 . . ? Cl5S C2S H2S 107.1 . . ? Cl4S C2S H2S 107.1 . . ? C2 C3 N1 107.8(4) . . ? C2 C3 H3 126.1 . . ? N1 C3 H3 126.1 . . ? N3 C4 N2 114.8(3) . . ? N3 C4 C5 130.2(4) . . ? N2 C4 C5 115.0(3) . . ? C7 C5 C6 107.8(4) . . ? C7 C5 C4 110.7(4) . . ? C6 C5 C4 111.3(4) . . ? C7 C5 C8 109.4(4) . . ? C6 C5 C8 105.2(4) . . ? C4 C5 C8 112.2(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 121.7(4) . . ? C10 C9 N3 121.7(4) . . ? C14 C9 N3 115.9(4) . . ? C11 C10 C9 117.6(4) . . ? C11 C10 C16 118.2(4) . . ? C9 C10 C16 124.1(4) . . ? C12 C11 C10 122.0(5) . . ? C12 C11 H11 119.0 . . ? C10 C11 H11 119.0 . . ? C13 C12 C11 119.5(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 121.5(5) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C9 117.7(4) . . ? C13 C14 C15 117.9(4) . . ? C9 C14 C15 124.2(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 121.6(4) . . ? C22 C17 N1 120.6(4) . . ? C18 C17 N1 117.8(4) . . ? C19 C18 C17 118.0(4) . . ? C19 C18 C23 121.4(4) . . ? C17 C18 C23 120.6(4) . . ? C18 C19 C20 121.8(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C19 118.7(4) . . ? C21 C20 C24 120.2(4) . . ? C19 C20 C24 121.0(4) . . ? C20 C21 C22 122.1(4) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C21 C22 C17 117.7(4) . . ? C21 C22 C25 120.1(4) . . ? C17 C22 C25 122.2(4) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C1 C26 C27 118.3(3) . . ? C1 C26 Ru1 98.0(2) . . ? C27 C26 Ru1 115.8(3) . . ? C1 C26 H26 105(3) . . ? C27 C26 H26 113(3) . . ? Ru1 C26 H26 105(3) . . ? C28 C27 C32 117.0(4) . . ? C28 C27 C26 125.0(4) . . ? C32 C27 C26 118.1(4) . . ? C27 C28 C29 122.2(4) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C30 C29 C28 119.7(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 119.0(4) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 121.3(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C31 C32 C27 120.7(4) . . ? C31 C32 H32 119.7 . . ? C27 C32 H32 119.7 . . ? N6 C33 C34 179.0(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N5 C35 C36 178.6(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N7 C37 C38 175.9(5) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C39 C40 179.0(5) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 N1 C3 109.2(3) . . ? C1 N1 C17 126.0(3) . . ? C3 N1 C17 123.7(3) . . ? C1 N2 C2 108.5(3) . . ? C1 N2 C4 126.8(3) . . ? C2 N2 C4 122.9(3) . . ? C4 N3 C9 122.8(3) . . ? C4 N3 Ru1 124.8(3) . . ? C9 N3 Ru1 112.1(3) . . ? C39 N4 Ru1 173.7(3) . . ? C35 N5 Ru1 175.9(4) . . ? C33 N6 Ru1 174.7(3) . . ? C37 N7 Ru1 174.1(4) . . ? F11 P1 F10 98.6(3) . . ? F11 P1 F9 93.3(2) . . ? F10 P1 F9 92.6(2) . . ? F11 P1 F7 87.4(3) . . ? F10 P1 F7 173.8(3) . . ? F9 P1 F7 88.55(18) . . ? F11 P1 F12 89.6(2) . . ? F10 P1 F12 89.6(2) . . ? F9 P1 F12 176.1(2) . . ? F7 P1 F12 88.9(2) . . ? F11 P1 F8 175.8(3) . . ? F10 P1 F8 85.4(3) . . ? F9 P1 F8 87.8(2) . . ? F7 P1 F8 88.6(3) . . ? F12 P1 F8 89.2(2) . . ? F2 P2 F1 93.5(4) . . ? F2 P2 F3 90.0(3) . . ? F1 P2 F3 89.2(3) . . ? F2 P2 F5 177.8(4) . . ? F1 P2 F5 88.6(3) . . ? F3 P2 F5 90.4(3) . . ? F2 P2 F4 91.7(4) . . ? F1 P2 F4 174.5(3) . . ? F3 P2 F4 92.4(3) . . ? F5 P2 F4 86.1(3) . . ? F2 P2 F6 88.2(3) . . ? F1 P2 F6 88.5(2) . . ? F3 P2 F6 177.1(3) . . ? F5 P2 F6 91.5(3) . . ? F4 P2 F6 90.0(3) . . ? N7 Ru1 N6 85.56(14) . . ? N7 Ru1 N4 173.68(14) . . ? N6 Ru1 N4 90.50(14) . . ? N7 Ru1 N5 87.57(13) . . ? N6 Ru1 N5 87.25(14) . . ? N4 Ru1 N5 87.31(13) . . ? N7 Ru1 N3 94.98(13) . . ? N6 Ru1 N3 177.84(13) . . ? N4 Ru1 N3 89.15(13) . . ? N5 Ru1 N3 94.86(13) . . ? N7 Ru1 C26 89.30(14) . . ? N6 Ru1 C26 90.57(14) . . ? N4 Ru1 C26 95.68(14) . . ? N5 Ru1 C26 176.31(14) . . ? N3 Ru1 C26 87.35(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.856 _refine_diff_density_min -1.539 _refine_diff_density_rms 0.104 _database_code_depnum_ccdc_archive 'CCDC 942610'